Advances in X-ray Analysis: Proceedings of the Denver X-ray Conference

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Proceedings of the Denver X-ray Conference

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Hosted annually, the Denver X-ray Conference (DXC) is the world’s leading forum for scientists working in the field of X-ray materials analysis. Presenters are encouraged to submit manuscripts of the work presented at the conference for publication in the latest volume of Advances in X-ray Analysis (AXA). Each year, approximately 30-40 papers are published. Learn More about DXC.

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ISSN 1097-0002 CODEN AXRAAA

Editors-in-Chief Thomas Blanton, International Centre for Diffraction Data, 12 Campus Boulevard, Newtown Square, PA 19073, U.S.A.
Lora Brehm, Dow, Retired, Midland, MI, U.S.A.
Martina Schmeling, Loyola University Chicago, Chicago, IL 60660, U.S.A.

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Advances in X-ray Analysis archives Vol. 1-39 (1957 – 1995) are available from Cambridge Core.

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Advances in X-ray Analysis archives Vol. 1-39 (1957 – 1995) are available here. Separate volumes for Vol. 40-67 are available here.

2023 – VOL672022 – VOL662021 – VOL652020 – VOL642019 – VOL632018 – VOL622017 – VOL612016 – VOL602015 – VOL592014 – VOL582013 – VOL572012 – VOL562011 – VOL552010 – VOL542009 – VOL532008 – VOL522007 – VOL512006 – VOL502005 – VOL492004 – VOL482003 – VOL472002 – VOL462005 – VOL452000 – VOL441999 – VOL431998 – VOL421997 – VOL411996 – VOL40

2023 – VOL67

APPLICATION OF MICRO-XRF IN THE PHARMACEUTICAL INDUSTRYS. Mamedov…A hyperspectral image contains information about the point’s position and the full XRF spectrum. The distribution of elements or compounds may be presented as a map from a hyperspectral image. Such images are essential evidence of counterfeit ph…
APPLICATION OF SPRAY SYNTHESIS AND SOL-GEL COMBUSTION FOR THE PREPARATION OF PRECURSORS FOR SLAG REFERENCE MATERIALSA. Schnickmann, S. Hampel, T. Schirmer, U.E.A. Fittschen…Clausthal-Zellerfeld, Germany *Correspondence: alena.schnickmann@tu-clausthal.de ABSTRACT As new technologies conquer the markets, the demand for raw materials (e.g., lithium) increases. During pyrometallurgical recycling of lithium-ion batterie…
BULK ELASTIC CONSTANTS AND THEIR ROLE IN DIFFRACTIVE STRESS ANALYSIST. Gnaupel-Herold…Calculations of DEC require primarily single crystal elastic constants as input; however, large disparities between elastic properties of multiphase composites generally lead to commensurate differences between the elastic response of individual…
CHARACTERIZATION OF MOS2 FILMS VIA SIMULTANEOUS GRAZING INCIDENCE X-RAY DIFFRACTION AND GRAZING INCIDENCE X-RAY FLUORESCENCE (GIXRD/GIXRF)M.A. Rodriguez, T.F. Babuska, J. Curry, J.J.M. Griego, M.T. Dugger, S.R. Larson,…The tribological properties of MoS2 are highly dependent on morphological attributes such as film thickness, orientation, crystallinity, film density, and stoichiometry. These structural characteristics are controlled by tuning the PVD process p…
CONTROL FILES AS A MEANS FOR IMPROVING QPA RESULTS ON THE HIGHLY COMPLEX MATERIAL EAF SLAGS & SUPPLEMENTARY MATERIALJ.E. Lyza, T.G. Fawcett, S.N. Page…The material typically has a large number of phases (>15) and a significant amorphous contribution, as well as multiple polymorphs and sets of solid solutions, which leads to heavy peak overlap and few, if any, regions of real background. These …
DIFFERENTIATION OF DEPOSITIONAL ENVIRONMENTS USING X-RAY DIFFRACTION RELATIVE PEAK HEIGHT INTENSITIES IN SILICICLASTIC SUCCESSIONMohamed Soua…In addition, this method is presented to test whether ratios of the relative X-ray diffraction peak heights from the 100 and 101 crystallographic planes of quartz are also diagnostic to distinguish between the sandstone depositional environments…
ENERGY DISPERSIVE DIFFRACTION TOMOGRAPHY OF SHARK VERTEBRAL CENTRAJ.-S. Park, R.M. Horn, H. Chen, K.C. James, M.S. Passerotti, L.J. Natanson, S.R. Stock…Cell and Developmental Biology, Feinberg School of Medicine, and Simpson-Querrey Inst., Northwestern Univ., Chicago, IL * Contact author e-mail: s-stock@northwestern.edu ABSTRACT Shark vertebrae and their centra (vertebral bodies) are high perfo…
ICH-Q3D ELEMENTAL IMPURITY ANALYSIS OF ORAL DRUGS AND T. Nakao, T. Sakamoto, T. Shoda,…While the recommended analytical methods are ICP-AES and ICP-MS, alternative methods that meet the validation requirements are also permitted. Energy-dispersive X-ray fluorescence spectrometry (EDXRF) as a nondestructive analysis technique requi…
MICRO-X-RAY FLUORESCENCE COMBINED WITH OPTICAL MICROSCOPY AS A POTENTIAL ALTERNATIVE TO SCANNING ELECTRON MICROSCOPY FOR SELECT MATERIALS APPLICATIONSC.G. Worley, O. Duarte II…However, for applications where ultrahigh spatial resolution is not needed, micro-X- ray fluorescence (MXRF) supplemented with optical microscopy (OM) is a useful alternative to SEM. Further, MXRF has significantly lower detection limits than SE…
POWDER DIFFRACTION PATTERN DENOISING USING HAAR WAVELETS AND A THRESHOLDING RULE FOR POISSON NOISER.B. McClurg…The algorithm uses Haar wavelet transforms and a hard thresholding rule designed specifically for the Poisson noise distribution. Cycle spinning of the transform significantly improves the results. The algorithm contains two parameters: a cut-of…
QUANTITATIVE RIETVELD ANALYSIS OF CRYSTALLINE DEPOSITS TO SUPPORT FAILURE INVESTIGATIONS H. Sitepu, N.M. AlYami, I.M. Al-Zahrani…Adv. X-Ray Anal, 62, 45-56; and references therein]. In this study, the inorganic crystalline materials part (insoluble or non-hydrocarbon) was separated from the hydrocarbon (soluble part) of the unknown sludge deposits from refinery and gas pl…
SMALL ANGLE X-RAY SCATTERING ANALYSES OF DIAGENESIS OF S.R. Stock, J.D. Almer, S. Mays, J.-S. Park…Destructive sampling is rarely an option for bones from archeological collections, and studying only the outermost layer of bone is problematic because this is the material most affected by diagenesis (i.e., post-mortem environmental changes). I…
USE OF RIETVELD REFINEMENT METHOD FOR DESCRIBING STRUCTURAL, TEXTURE AND PHASE ANALYSIS OF X-RAY DIFFRACTION DATA OF A SILICICLASTIC SUCCESSIONMohamed Soua, Husin Sitepu…This paper reports crystal structure, texture and phase analysis of X-ray powder diffraction data of the Middle Permian sandstones obtained from Rietveld refinement with March model for crystallographic preferred orientation correction. The resu…

2022 – VOL66

A CRITICAL EXAMINATION AND RE-DETERMINATION OF THE LITERATURE IBUPROFEN FORM-II STRUCTUREP.S. Whitfield, C.J. Smalley…The lack of literature on Form-II characterization highlights the difficulty in producing a phase-pure sample even in a powder form. Without a higher quality alternative, this defective structure remains as the only entry in the various crystall…
A CRITICAL REVIEW OF NEURAL NETWORKS FOR THE IDENTIFICATION OF POWDER X-RAY DIFFRACTION PATTERNSJ. Schuetzke, N. J. Szymanski, M. Reischl…Previous work has shown that CNNs can be trained to successfully identify crystalline phases from XRD patterns and classify their symmetry, even in multi-phase mixtures. When compared with classical machine learning methods, such as Support Vect…
CHALLENGES OF QUANTITATIVE PHASE ANALYSIS OF SLAGS: A LOOK AT SAMPLE COMPLEXITYJ.E. Lyza, T.G. Fawcett, S.N. Page, K.L. Cook…The number of phases frequently exceeds 10, with certain slag types (EAF, BOF, blends, stainless) having extreme peak overlap, making identification difficult. Another convolution arises from the variable crystallite sizes of phases found in sla…
EVALUATING THE TEMPERATURE DEPENDENCE OF PZT STRUCTURES USING A VIRTUAL REALITY ENVIRONMENTM.A. Rodriguez*, J. Krukar, N.R. Valdez, J.Z. Harris, K.A. Perkins, C. DiAntonio, P. Yang…Crystal structure analysis via Rietveld refinement facilitates materials analysis via the extraction of the structural parameters. These parameters, often obtained as a function of an additional dimension (e.g. pressure), can help to diagnose ma…
IMPROVEMENTS IN PRECISION OF REAL-TIME PULSE HEIGHT ANALYSIS IN MICROCALORIMETER X-RAY DETECTORSS. Thurgate, T. Jach…Issues of concern are nonstationary noise when the pulse takes the TES element into a higher resistance region, and variability of pulse shape with energy. Furthermore, system noise affects the precision analysis of pulse heights in two differen…
LOW TEMPERATURE CRYSTAL STRUCTURES OF THE SOLVENT DIMETHYL CARBONATEP.S. Whitfield…Pure DMC has a melting point of 277 K, so encountering solidification under outdoor climatic conditions is very likely in many locations around the globe. Even eutectic, ethylene carbonate:dimethyl carbonate commercial LiPF6 salt electrolyte for…
MEASUREMENT OF COATING THICKNESS WITH X-RAY DIFFRACTIONM. Witte…Thus, the thickness of different oxide layers of the same element can be determined, e. g. FeO, Fe3O4 and Fe2O3 on Fe-substrate. An approach for such measurement is discussed. Furthermore, with a suitable sample stage a spatially resolved coatin…
MICROSTRUCTURE, RESIDUAL STRESSES, AND PREFERRED ORIENTATION OF LASER ADDITIVE MANUFACTURED H13 TOOL STEELK. Trojan, J. Čapek, J. Čech, N. Ganev, V. Ocelík, K. Kolařík…The presence of tensile residual stresses is detrimental in physical processes as, for instance, fatigue or, in combination with defects, promoting brittle fractures. Further, as the physical and chemical properties in an anisotropic material ma…
SURFACE STRAIN AND RESIDUAL STRESS OF TEXTURED CVD Α-AL2O3 COATING LAYER ON METAL CUTTING TOOLST. Shibata…The easiness and difficulty of surface strain and residual stress modification seemed to depend on the individual crystallite orientation, textures, and post-coat mechanical process parameters. Line profiles of available (hkl) peaks taken by x-r…
X-RAY CHARACTERIZATION OF A METAL-ORGANIC FRAMEWORK DURING DEHYDRATION AND CO2 ADSORPTIONE.P. Jahrman, H.G.T. Nguyen,…Often, these methods have implementations favorable for studying chemical systems under their functioning conditions. This is particularly attractive for adsorbent materials, where descriptions of adsorbate-adsorbent interactions and tools to mo…

2021 – VOL65

A NEW X-RAY DIFFRACTION BASED TECHNIQUE TO STUDY THE EFFECTS OF CYCLIC STRESSES ON THE MICROSTRUCTURE OF FERRITED. Vinci, O. Castelnau, V. Jacquemain, C. Cheuleu, V. Michel, V. Favier, C. Mocuta, N. Ranc…VHCF – domain, and can break under stress amplitudes lower than their ultimate tensile stress (fatigue). The fatigue of materials has been largely characterized with fatigue tests based on hydraulic machines; however, the investigation of the VH…
BEST REFERENCES FOR THE QPA OF PORTLAND CEMENTTim Fawcett, Justin Blanton, Suri Kabekkodu, Tom Blanton, Jessica Lyza, Don Broton…A set of control references were established for phase identification and quantitative analysis using laboratory diffractometers. Both RIR and Rietveld whole pattern fitting methods were used in the analyses. A block refined, parameter restricte…
DETERMINATION OF VOID FRACTION BY X-RAY RADIOGRAPHY Krassimir Stoev, Justin Spencer…X-Ray radiography-based densitometry was identified as a reliable method for detection and characterization of the liquid-phase saturation. In this paper we report on the radiography method developed to measure liquid-phase saturation, and some …
INVERSE POLE FIGURE OF CVD COATING OF METAL CUTTING TOOLS USING XRD BRAGG BRENTANO GEOMETRYTomohiro Shibata…It has been established that the texture of the coating materials especially that of the α-Al2O3 greatly affect the cut performance for some applications. The characterization of the coating texture is thus very important. In this paper inverse …
RECONSTRUCTION AND SUPERRESOLUTION FOR CODED APERTURE FULL-FIELD X-RAY FLUORESCENCE IMAGINGAnicó Kulow, Ana Guilherme Buzanich, Uwe Reinholz, Franziska Emmerling, Sven Hampel, Ursula E.A. Fittschen, Christina Streli, Martin Radtke…Berlin, Germany 2 Vienna University of Technology, Atominstitut, Stadionallee 2, 1020 Vienna, Austria 3 Univ. Grenoble Alpes, CNRS, Grenoble INP, Institut Néel, 38000 Grenoble, France 4 Clausthal University of Technology, Institute of Inorganic …
STANDARDIZATION OF X-RAY STRESS MEASUREMENT BY THE COSΑ METHOD USING TWO-DIMENSIONAL DETECTORYoshihisa Sakaida, Kenji Suzuki, Keisuke Tanaka…In the method, the 211 diffraction of α-Fe by Cr-Kα radiation is recommended for stress measurements. The incident angle ψ0 = 35° and the X-ray elastic constant EX / (1 + νX) = 175 GPa were adopted based on the results of a round robin test. The…
STOICHIOMETRIC CALCULATION OF LITHIUM-CONTAINING PHASES BASED ON SPATIALLY RESOLVED X-RAY ANALYSIS AND VIRTUAL COMPOUNDSThomas Schirmer…Because of the extremely low fluorescence yield and long wavelength of Li Kα an adequate accurate determination of this element is virtually impossible with electron probe microanalysis. However, an approach to assess the lithium containing comp…
TEXTURE AND STRAIN ANALYSIS OF TUNGSTEN FILMS VIA TILT-A-WHIRL METHODOLOGYM. A. Rodriguez*, J. Pillars, N. Valdez, J. J. M. Griego, M. V. Gallegos, J. A. Krukar, A. Polonsky, S. Wolfley…Deposition conditions can significantly impact the resulting W films in terms of the phases present (-BCC, or -A12), microstructural grain orientation (texture), and residual strain. TILT-A-WHIRL methodology has been employed for the evaluatio…
THE REFERENCE INTENSITY RATIO (RIR) METHOD – IMPROVEDTim Fawcett, Justin Blanton, Suri Kabekkodu, Tom Blanton…The great attraction of the method is that it can be performed on a multiphase sample using a single data scan. This was made possible by the publication of thousands of experimental RIR values in the 1970’s, followed two decades later by the ca…

2020 – VOL64

COMPARISON OF DIFFERENT SAMPLE PREPARATION TECHNIQUES IN THE DETERMINATION OF PB IN A CERTIFIED RYE GRASS MATERIAL BY MEANS OF TOTAL REFLECTION X-RAY FLUORESCENCE SPECTROMETRY (TXRF)Jessica Hiller, Ursula E. A. Fittschen…Clausthal-Zellerfeld, Germany *Corresponding author. Email address: jessica.hiller@tu-clausthal.de ABSTRACT A certified rye grass reference material was analyzed to enforce digestion free suspension assisted elemental determination with Total Re…
CULTURAL HERITAGE SCIENCE AND THE MATERIAL OF MEMORYLynn B. Brostoff…Tangible records include physical objects, monuments, works of art, letters and manuscripts, for example; intangible heritage includes that without materiality, such as traditions, events, music, performances. An additional area of cultural heri…
DENSITY AND PHASE DETERMINATION OF PORTLAND CEMENT-BASED PRODUCTS WITH COMPUTED TOMOGRAPHY AND X-RAY DIFFRACTIONKatharina Walbrueck, Steffen Thomas Witzleben…Combined measurements of µ-X- ray computed tomography (µ-XCT) and µ-X-ray diffraction (µ-XRD) offer important scientific and forensic information about hydrated cement systems to develop new products, but also to clarify material failure and cau…
EQUATORIAL ABERRATION FOR POWDER DIFRRACTION DATA COLLECTED BY CONTINUOUS SCAN OF A SILICON STRIP X-RAY DETECTORTakashi Ida…There are four critical angles related to the effects of spill-over of the incident X-ray beam from the specimen face in the CSI-SSXD data. Exact values of cumulants of the equatorial aberration function are efficiently evaluated by 4 × 4 point …
EVALUATION OF X-RAY DIFFRACTION STRESS INSTRUMENTS USING COS-ALPHA AND SIN2ΨTECHNIQUES IN RELATION TO EXISTING STANDARDSM. Belassel, J. Pineault, M. Brauss…The stress results obtained for each technique are presented and their significance explained. It is shown that the residual and applied stresses obtained from simulation and experiments using SET-Cosα and the SET-Sin2ψ produce similar erroneous…
FORENSIC APPLICATIONSOF MICRO-XRF: FROM BULK TO IMAGE ANALYSISS. Mamedov…A hyperspectral image is a set of data containing the entire spectrum collected from each image pixel with coordinates X-Y-Z. This paper aims to demonstrate the application of Multivariate analysis to XRF hyperspectral data sets. Principal Compo…
INVESTIGATION ON VANADIUM SPECIES DISTRIBUTION IN NAFION™ 117 AFTER CYCLIZATION IN A VANADIUM REDOX FLOW BATTERYChristian Lutz, Sven Hampel, Sabine Beuermann, Thomas Turek, Ulrich Kunz, Ana Guilherme Buzanich, Martin Radtke, Ursula E. A. Fittschen…Clausthal-Zellerfeld, Germany 2 Clausthal University of Technology, Institute of Technical Chemistry, Arnold-Sommerfeld- Str. 4, 38678 Clausthal-Zellerfeld, Germany 3 Clausthal University of Technology, Institute of Chemical and Electrochemical …
MICRO-X-RAY FLUORESCENCE CHARACTERIZATION OF PLUTONIUM-BERYLLIUM NEUTRON SOURCESChristopher G. Worley, Kevin J. Kuhn, Lav Tandon…The PuBe samples were doubly contained for analysis to prevent radioactive contamination. Thus, low atomic number elemental analysis was not possible, but transition metal elemental distribution maps were acquired. A lathe was used to open stain…
MODELING OF X-RAY REFLECTIVITY FROM CONTINUOUSLY VARYING PERIODIC STRUCTURESKrassimir Stoev…This is due to the fact that for an X-ray specular reflectivity setup, the scattering vector is always perpendicular to the surface. X-ray optics usually takes advantage of multi-layer structures, which demonstrate relatively high reflectivity f…
PRELIMINARY EXAMINATION FOR REVEALING THE PROVENANCE DEPENDENCY OF THE LATTICE SPACING OF BIOTITE FOR THE PROVENANCE ESTIMATION OF ATAMADAI-TYPE POTTERY (2500–1500 BC) BY XRDShintaro Ichikawa, Kana Miyamoto, and Tsutomu Kurisaki…Fifty-nine of the shards were Atamadai-type pottery in which fragments containing biotite were mixed during the manufacturing process. For the provenance estimation of the biotite temper in the Atamadai-type pottery pieces, the reliance of the b…
PROJECTION-TYPE X-RAY DIFFRACTION IMAGING FOR POLYCRYSTALLINE MATERIALS: APPLICATION TOVICKERS HARDNESS TEST BLOCKSMari Mizusawa, Kenji Sakurai…The way of lattice plane changes due to strain also differs depending on the location. Therefore, it is necessary to analyze the selected region in one sample. While various diffraction topography techniques have been developed for single crysta…
SOLAR OPACITY MOTIVATED TARGET FABRICATION, METROLOGY AND X-RAY OPACITY DATABASE REVISIONH. Huang, K. Sequoia, M. Yamaguchi, K.J. Boehm K. Engelhorn, J. Walker, F. Elsner, J. Tomlin, M. Farrell…This allows benchmarking of the hot opacity values at the solar convection zone base, now accessible at the premium HED facilities run by Department of Energy (DOE)’s National Laboratories, to the room temperature values to better unravel the op…
SPECTRAL CORRECTION FOR TRANSMISSIONX-RAYTUBES FOR USE IN THE QUANTIFICATION SOFTWARE ATI-QUANTElisabeth Holub, Peter Wobrauschek, Peter Kregsamer, Christina Streli…Evaluation relies on simulated x-ray tube spectra, detector efficiency, absorption and inter-element-effect corrections as well as fundamental parameters. Originally, ATI-QUANT was used to evaluate a side-window x-ray tube with thick-anode targe…
THE DIRECT DERIVATION METHOD: QUANTITATIVE PHASE ANALYSIS WITH OBSERVED INTENSITIES AND CHEMICAL COMPOSITION DATAHideo Toraya…Crystal structure parameters are required when we calculate intensities of reflections or diffraction patterns. Intensity can, however, be calculated only with the chemical composition data if it is not of individual reflections but of a total s…
TOTAL REFLECTION X-RAY FLUORESCENCE ANALYSIS OF TRACE ELEMENTS IN HIGH-CONCENTRATION MATRIX SOLUTIONS USING A CARBON-COATED GLASS SUBSTRATETsugufumi Matsuyama, Takumi Furusato, Hikari Takahara, Kouichi Tsuji…In TXRF analysis, a drop (10 µL) of the sample solution is placed and dried on a substrate, such as silicon wafer and quartz slide. The dried residue is then analyzed using a TXRF spectrometer. However, when the sample solution has a high-concen…
TOWARD AUTOMATIC THREAT RECOGNITION FOR AIRPORT X-RAY BAGGAGE SCREENING WITH DEEP CONVOLUTIONAL OBJECT DETECTIONKevin J Liang, John B. Sigman, Gregory P. Spell, Dan Strellis, William Chang, Felix Liu, Tejas Mehta, and Lawrence Carin…At these checkpoints, the TSA employs a fleet of X-ray scanners, such as the Rapiscan 620DV, so Transportation Security Officers (TSOs) can inspect the contents of carry-on possessions. However, identifying and locating all potential threats can…
X-RAY IMAGING OF SILICON DIE WITHIN FULLY PACKAGED SEMICONDUCTOR DEVICESBrian K. Tanner, Patrick J. McNally, Andreas N. Danilewsky…D-79104, Freiburg, Germany ABSTRACT X-ray Diffraction Imaging (Topography) measurements of silicon die warpage within fully packaged commercial Quad Flat No-Lead devices are described. Using synchrotron radiation, we show that the tilt of the la…

2019 – VOL63

A METHOD FOR MAPPING SUBMICRON-SCALE CRYSTALLOGRAPHIC ORDER/DISORDER APPLIED TO HUMAN TOOTH ENAMELR. Free, K. DeRocher, R. Xu, D. Joester, S.R. Stock…The details of this structure are important in multiple human health contexts, from understanding the progression of dental caries (tooth decay) to understanding the process of amelogenesis and related developmental defects. Enamel is composed p…
BI-CROSS VALIDATION OF SPECTRAL CLUSTERING HYPERPARAMETERSSioan Zohar, Chun Hong Yoon…Here we demonstrate that previous work using bi-cross validation (BCV) to determine the number of singular vectors directly maps to the spectral clustering problem of estimating both the number of clusters and hyperparameter values. Applying thi…
C/H RATIO AND O CORRECTIONS FOR XRF ANALYSIS OF SULFUR IN PETROLEUM PRODUCTSK. Kawakyu, T. Moriyama, Y. Kataoka…A fundamental assumption of these test methods is that calibrations are set up with type standards, i.e. test and calibration samples must be matrix matched. Differences in carbon to hydrogen (C/H) ratio or presence of oxygenates affects the abs…
CAREFUL APPROACHES TO QUANTIFY LIGHT ELEMENTS IN COMPLEX MATRICES USING BENCH-TOP ENERGY DISPERSIVE X-RAY FLUORESCENCEPoulami Dutta, Casey McAlpin…As such, most of the quality control analyses are conducted in-house. Many analyses include quantifying elemental concentrations in sample matrices ranging from raw materials to final products. Recent advances in bench-top energy dispersive X-ra…
CRYSTAL STRUCTURE CHARACTERIZATION OF URANIUM-SILICIDES ACCIDENT TOLERANT FUEL BY HIGH TEMPERATURE NEUTRON DIFFRACTIONTashiema L. Wilson, Sven C. Vogel, Joshua T. White, Elizabeth Sooby-Wood, Theodore M. Besmann…Despite the body of work characterizing both fresh and irradiated U3Si2 fuel, there are gaps in crystallographic knowledge. In this study the crystal structure of U3Si2 was investigated and the interstitial site for excess Si was accessed. The e…
DEVELOPMENT OF FLY-SCAN MODE CONFOCAL MICRO-X-RAY FLUORESCENCE ANALYSISTsugufumi Matsuyama, Shohei Mita, Momotaro Nakanishi, Kouichi Tsuji…In CM-XRF, a micro X-ray beam is generated through optical focusing of X-rays. Thus far, CM-XRF has only been performed in step-by-step mode, with the drawback of prolonged measurement times required for elemental mapping, depending on the area …
DIFFRACTED BEAM COLLIMATORS – EXTENDING THE RANGE OF APPLICATIONS FOR 2D DETECTORSDetlef Beckers, Milen Gateshki, Scott Speakman, Vladimir Kogan…D detectors on multi-purpose diffractometers. Traditionally 2D detectors are used in application areas that require small illuminated spots on the sample and do not utilize any diffracted beam collimation systems. In this work we are focusing on…
ELEMENTAL MAPPING OF PASTA SAMPLE USING CONFOCAL MICRO X-RAY FLUORESCENCE SPECTROMETRYHitomi Nakano, Yumiko Nakanishi, Shohei Mita, Momotaro Nakanishi, Shintaro Komatani, Kouichi Tsuji …In this paper, we visualized chlorine (Cl) distribution in boiled pasta by using confocal micro X-ray fluorescence (C-M-XRF). C-M-XRF can obtain 3D mapping images. A problem is that XRF from the inner area of sample is suscetible to absorption. …
HOW TO USE AND HOW NOT TO USE CERTIFIED REFERENCE MATERIALS IN INDUSTRIAL CHEMICAL METROLOGY LABORATORIESJohn R. Sieber…The demand is exacerbated by wide spread misuse of CRMs. When should one use CRMs? When should one not use CRMs? Must labs always use NIST SRMs? How can labs demonstrate analytical capabilities for their accreditation scopes? Why so many questio…
INVESTIGATION OF THE REAL STRUCTURE USING X-RAY DIFFRACTION AS A TOOL FOR LASER WELDING OPTIMIZATIONJiří Čapek, Nikolaj Ganev, Karel Trojan, Stanislav Němeček, Kamil Kolařík…Therefore, high demands are placed on mechanical properties and service life of welded functional components. Because of the heterogeneity of energy and localized fusion during the welding process, high residual stresses are generated in areas n…
MONOCHROMATIC CONFOCAL MICRO X-RAY FLUORESCENCE SPECTROMETRYNaoki Kawahara, Shota Sonoda, Shohei Mita, Tsugufumi Matsuyama, Kouichi Tsuji…In laboratory CM-XRF instruments, polychromatic x-ray focusing sources formed by using an x-ray tube and a polycapillary full-lens optic have been utilized. In this case, high background is one of the problems for trace elemental analysis. In th…
RIETVELD PHASE ANALYSIS OF DEPOSITS FORMED AT DIFFERENT LOCATIONS WITHIN ELECTRIC SUBMERSIBLE PUMPSHusin Sitepu…The electrical submersible pumps are frequently used in oil production to provide a relatively efficient form of artificial lift, to enhance oil production. The main objective of this study is to extend the new sample preparation method [Sitepu …
SPHERICAL OPTICS BY DISLOCATION OF CRYSTAL STRUCTURE Joanna M. Maj, Felix Krasnicki, Boguslaw Slusarczyk…This invention comprises a method of fabricating spherical optics by dislocation. This method eliminates residual stress and aberration caused by the remaining stressful forces. The fabrication by dislocation of the crystal structure is a new me…
SYNTHETIC CALIBRATION REFERENCE MATERIALS FOR X-RAY FLUORESCENCE QUANTITATION OF 22 COMPONENTS IN ANCIENT JAPANESE POTTERYShintaro Ichikawa, Tsutomu Kurisaki…The reference materials were glass beads prepared by mixing chemical reagents (oxides, carbonates, and diphosphate) and fusing with alkali-flux. The calibration curves showed good linearity with correlation coefficients greater than 0.996. Relia…
TOTAL PATTERN ANALYSES FOR NON-CRYSTALLINE MATERIALST.G. Fawcett, S. Gates-Rector, A.M. Gindhart, M. Rost, S.N. Kabekkodu, J.R. Blanton, T.N. Blanton…While the suite of programs is intended for the analysis of any diffraction pattern, particular attention was focused on the analysis of common amorphous, non-crystalline or partially crystalline materials found in minerals, polymers and pharmac…
USE OF A BE-DOME HOLDER FOR TEXTURE AND STRAIN CHARACTERIZATION OF LI METAL THIN FILMS VIA SIN2 METHODOLOGYMark A. Rodriguez, Katharine L. Harrison, Subrahmanyam Goriparti, James J. M. Griego, Brad Boyce, Brian Perdue…X-ray diffraction (XRD) analysis of Li films required preparation and examination within an inert environment, hence a Be-dome sample holder was employed during XRD characterization. Results show that the Li film grown under 1000 kPa displayed a…
VARIOUS APPROACHES TO SURFACE RESIDUAL STRESS AND GRINDING EFFECT OF CERAMIC SURFACESTomohiro Shibata…For commercially available β-Si3N4 insert, using χ tilting (both Cu and Cr Kα radiation), grazing incidence with whole pattern analysis, and Ω tilting techniques were used for residual stress determination with information depth profiles for com…
X-RAY DIFFRACTION STUDY OF MECHANICALLY ALLOYED LI-SN-ZNCheng K. Saw, B. William Choi…Hence, Lithium has to be incorporated into the breeding blanket that surrounds the fusion source. Because of the chemical reactivity of Li with water and air, alternative alloys based on Li were proposed for this replacement. Recent work by LLNL…
X-RAY DIFFRACTON AS A MAJOR TOOL FOR THE ANALYSIS OF PM2.5 AND PM10 AEROSOLSNasser Hamdan, Hussain Alawadhi…The sampling campaign ran over a one-year period with sampling frequency of twice a week for both PM2.5 and PM10. X-ray diffraction (XRD) methods, which are not commonly used in PM analysis, have been utilized successfully to identify crystallin…
X-RAY FLUORESCENCE DATA ANALYSIS USING A BLANK CORRECTION APPROACHAndrew M. Crawford…To do this, many programs initially remove a per-pixel baseline prior to fitting to account for a background XRF continuum. Previously, we demonstrated an alternative background correction where in the average blank spectrum is calculated from n…

2018 – VOL62

3D IMMERSIVE VISUALIZATION OF MICRO-COMPUTED TOMOGRAPHY AND XRD TEXTURE DATASETSMark A. Rodriguez, Tod T. Amon, James J. M. Griego, Harlan Brown-Shaklee, Nicolas Green…Likewise, intuitive evaluation of these 3D datasets can be enhanced by recent advances in Virtual Reality (VR) hardware and software. Additionally, the generation, viewing, and manipulation of 3D X-ray diffraction datasets, such as pole figures …
BEAM MONOCHROMATIZATION CONCEPTS FOR POWDER DIFFRACTIONDetlef Beckers, Milen Gateshki, Detlev J. Götz…Traditional incident monochromators include, for example, Johansson monochromators, 4-crystal-monochromators or the so-called hybrid monochromators – i.e. combinations of a parabolic graded multilayer with a channel cut crystal. Their advantages…
DOES SIZE MATTER? CAN PORTABLE XRF BE USED FOR PROCESS CONTROL?Maggi Loubser…The data will show that the capabilities between the three variations of the technique are comparable, the key factor to this being possible is the introduction of the Silicon Drift Detector (SDD) for handheld XRF. The biggest restrictive factor…
IMPLEMENTATION OF THE SELF-CONSISTENT KRÖNER-ESHELBY MODEL FOR THE CALCULATION OF X-RAY ELASTIC CONSTANTS FOR ANY CRYSTAL SYMMETRYArnold C. Vermeulen, Christopher M. Kube, Nicholas Norberg…With applying appropriate symmetry relations, the point groups of higher crystal symmetries are covered as well. This simplifies the implementation effort to cover the calculations for any crystal symmetry. In the literature several models can b…
INDEXCUB: A READY-TO-USE SET OF ROUTINES FOR X-RAY DIFFRACTION LINE PROFILE ANALYSISAdriana Pérez-Casanova, Héctor Medel-Cobaxin, Flavio F. Contreras-Torres…In this concern, the study of polycrystalline materials underlays the use of appropriate software: free, licensed, proprietary or commercial to assist research on structure determination, structure refinement, and microstructure characterization…
MINERAL ANALYSIS OF RIVER SAND AROUND MT. TSUKUBA FOR PROVENANCE ESTIMATION OF ATAMADAI TYPE POTTERY (2500–1500 BC) FROM HINOKI SITE (TOCHIGI, JAPAN)S. Ichikawa, Y. Sakito, T. Kurisaki…Fifty-five of those were Atamadai type pottery, which might contain some temper fragments from the manufacturing process. The pottery shards were analyzed by X-ray diffractometry (XRD). The mineral analyses were compared with the river sands aro…
MONITORING OF FES2 REACTIONS USING HIGH-TEMPERATURE XRD COUPLED WITH GAS CHROMATOGRAPHYKerry-Ann M. Stirrup, Mark A. Rodriguez, Eric N. Coker, James J. M. Griego, Travis M. Anderson…When FeS2 cathode materials were analyzed in an air environment, reaction of the KCl and LiCl salt phases led to the formation of Li2(SO4) and KFe2S3 phases beginning at ~230 oC. These phases subsequently reacted to generate various forms of pot…
POLYCHROMATIC SIMULTANEOUS WDXRF FOR VALENCE EVALUATION OF CATHODE ACTIVE MATERIALS IN LITHIUM-ION BATTERIESTetsuya Yoneda, Takuro Izumi, Satoshi Tokuda, Susumu Adachi, Kenji Sato, Misako Kobayashi, Takashi Mukai, Hideaki Tanaka, Masahiro Yanagida…The measured energy-identification precision is approximately 20 meV. The precision is sufficient for the valence state evaluation of lithium ion battery (LIB) cathodes through the peak shifts of X-ray fluorescence lines. Ex-situ cathode materia…
QUANTITATIVE PHASE ANALYSIS OF XRD DATA OF SLUDGE DEPOSITS FROM REFINERIES AND GAS PLANTS BY USE OF THE RIETVELD METHODHusin Sitepu, Rasha A. Al-Ghamdi…Powder Diff., 24, 315-326]. Subsequently, the sample preparation methods— developed by the authors — to separate the inorganic materials from the hydrocarbon of the sludge deposits and the other materials, were extended to perform quantitative p…
QUANTITATIVE XRD & XRF ANALYSES — UNIFIED & SIMPLIFIEDFrank H. Chung…New insights led to the three laws of quantitative XRD & XRF analyses: 1. the law of zero matrix effects, 2. the law of constant slope of calibration lines, and 3. the law of binary mixtures. The first two laws change the current concept of quan…
RESIDUAL STRESS ANALYSIS OF CERAMIC CUTTING TOOLS INDUSTRIAL APPLICATIONTomohiro Shibata…From the standard side inclination stress measurement, a large deviation from a linear sin2 ?? dependence of lattice strain was observed near χ ~ 90° indicating a stress gradient along the depth direction near the surface. The information dept…
TRACE ELEMENT ANALYSIS OF WASTE WATER REFERENCE MATERIAL AND ELUATES FROM FLY ASH BY BENCHTOP TOTAL REFLECTION X-RAY FLUORESCENCE SPECTROMETRYAtsushi Ohbuchi, Wataru Matsuda, Hikari Takahara, Satoshi Ikeda, Yoshiyuki Kataoka, Kengo Fujii, Yuya Koike…Quantitative results were obtained using the internal standard method. The results obtained for a number of harmful elements present in a wide range of concentrations were in good agreement with standard values in waste water reference samples. …
X-RAY FLUORESCENCE AND RAMAN SPECTROSCOPY DATA FUSION FOR ANALYSIS OF DUCT TAPES: INTRA ROLL AND INTER PRODUCT CORRELATIONSS. Mamedov…XRF provides information about elemental composition of the material, whereas Raman spectroscopy offers molecular information. The purpose of this paper is to demonstrate the application of Principal Component Analysis (PCA) to classification of…
XRD ANALYSIS OF ILLITE-SMECTITE INTERSTRATIFICATION IN CLAYS FROM OIL SANDS ORESB. Patarachao, D.D. Tyo, A. Zborowski, K. Davis, J. Kung, S. Ng, P.H.J. Mercier…Identification and quantification of clay minerals are therefore important to the oil sands industry. Two estuarine (E3 and E7) and two marine (M13 and M18) oil sands were used in this study. Separation of <2 µm clay solids was accomplished usin…

2017 – VOL61

A POLYCAPILLARY BASED METHOD OF MONOCHROMATIC TIME-RESOLVED X-RAY REFLECTIVITYH. Joress, A.R. Woll, J.D. Brock…Our method, implemented at the Cornell High Energy Synchrotron Source (CHESS), utilizes a polycapillary X-ray optic to create a nominally-planar converging fan of radiation incident on a sample surface, providing a range of incident angles. An a…
AN EMPIRICAL DERIVATION OF THE X-RAY OPTIC TRANSMISSION PROFILE USED IN CALIBRATING THE PLANETARY INSTRUMENT FOR X-RAY LITHOCHEMISTRY (PIXL) FOR MARS 2020C.M. Heirwegh, W.T. Elam, D.T. Flannery, A.C. Allwood…Through a straightforward method of dividing a measured ‘blank’ spectrum over one calculated assuming no optic influence, a rudimentary profile was formed. A simple boxcar-smoothing algorithm was implemented to approximate the complete profile w…
BRAGG DIFFRACTION TRANSMISSION MICROSCOPY USING HIGHLY MONOCHROMATIC X-RAYSS. Stoupin, T. Kolodziej, A. Said, A. Campello, Y. Shvyd’ko…Quantitative information on the strain distribution was extracted from transmission images generated by scanning the energy of the incident X-rays through the reflectivity curve of a high-indexed diamond Bragg reflection. The use of transmission…
CHALLENGES ENCOUNTERED USING MXRF TO COLLECT ELEMENTAL INFORMATION FROM SMALL ISOLATED SAMPLE FEATURESC.G. Worley, N. Xu…In the first example, MXRF elemental mapping was used to examine a uranium (U) pellet, and tiny sporadic spots were located containing relatively high concentrations of tungsten (W) or lead (Pb). Because these spots were so small and isolated, t…
DEVELOPMENT OF THE MICROGAP SEALED PROPORTIONAL COUNTER FOR SOFT X-RAYA. Stratilatov, R. Creighton, J. Barron, M. Zappe, K. Kozaczek…The MicroGap detector is simple in design, has significantly higher counting rate than a conventional single wire proportional counter, very good energy resolution, and works at lower bias voltage. This detector is designed as a substitute for s…
ENERGY DISPERSIVE X-RAY DIFFRACTION TO ANSWER THE QUESTION: “WHAT’S IN THE BOX?”S. Dorkings, K. Moss, J. Kirk, M. Lebessis, H. Keith, K. Brown, J. Khong, R. Speller, R. Moss…ABSTRACT A novel design has been produced for a portable X-ray diffraction (XRD) instrument for enabling bomb disposal experts to identify materials within suspicious items they are called to make safe. This design includes an innovative collima…
EVALUATION OF PORTABLE X-RAY FLUORESCENCE SPECTROMETERS FOR IN VIVO QUANTIFICATION OF BONE STRONTIUM AND LEAD ON THE BASIS OF THE MINIMUM DETECTABLE LIMIT: A PHANTOM STUDYE. Da Silva, G. Mankovskii, B. Kirkham, J. Groves, M. Gherase, D.E.B. Fleming, A. Pejović-Milić…XRF systems offer flexible, portable and relatively low cost solutions for the potential monitoring of humans for such elements. To date, there has been some application of both tungsten-target and silver-target pXRF systems for bone lead determ…
FINGER PRINT MINERALS FOR PROVENANCE ESTIMATION OF ATAMADAI-TYPE POTTERY (2500–1500 BC) FROM HINOKI SITE (TOCHIGI, JAPAN) USING POWDER XRDS. Ichikawa, M. Morikawa, T. Kurisaki, T. Yamaguchi…Fifty-nine of these were Atamadai-type pottery. The pottery shards were assayed by X-ray diffractometry to estimate finger print minerals for provenance study of the Atamadai-type pottery. The Atamadai-type pottery contained plagioclase, hornble…
GEOMETRY AND ALGORITHMS TO EXPAND 2ϴ COVERAGE OF 2D DETECTORB.B. He…For many applications, especially phase analysis and structure refinement, it is crucial for the 2D pattern to have a large 2θ range sufficient to cover as many diffraction rings as necessary. The 2θ range covered by a 2D detector is determined …
IN SITU XRD STUDIES OF MICROSTRUCTURAL CHANGES IN STEELM. Witte, I. Janssen…In order to carry out such measurements a XRD with area detector was equipped with a commercial heating stage. The aim is to determine the range of possible in situ XRD applications and to optimize the measurement and evaluation procedures for s…
INDUSTRIAL AND FORENSIC APPLICATION OF MICRO-XRF: GLASS ANALYSISS. Mamedov…XRF analysis has the potential to solve a wide variety of problems, associated with forensic science. The purpose of this paper is to demonstrate the application of Principal Component Analysis (PCA) to classification of window glasses from diff…
INVESTIGATING PHOTOCHEMICAL EFFECTS OF MICRO-XRF ANALYISIS ON COMMON GEOCHEMICAL COMPOUNDSS. Menachekanian, D.T. Flannery, C.M. Heirwegh, M.L. Tuite, C.S. Jamieson, R. Hodyss, K. Williford…We performed a preliminary study of the effects of intense and prolonged exposure to X-ray radiation from a micro- focus XRF instrument on the chemical composition of two organic compounds representative of molecules commonly reported from the t…
MINERAL IDENTIFICATION BY ELEMENTAL COMPOSITION: A NEW TOOL WITH PDF-4 DATABASEST.G. Fawcett, J.R. Blanton, S.N. Kabekkodu, T.N. Blanton…Many minerals have characteristic elemental profiles that can often distinguish the mineral from others by their composition differences. In Release 2016 ICDD® PDF-4 databases 20,670 unique compositions have been identified out of 45,497 mineral…
PRACTICAL APPLICATION OF PORTABLE XRF IN MINERAL EXPLORATIOND. Arne…The use of pXRF to generate data for public reporting purposes requires careful sampling methodologies to obtain representative analyses, estimation of realistic lower limits of detection for key elements, and calibration of the instrument. Repr…
RELATION BETWEEN INTENSITY OF XANES PRE-EDGE AND XES KΒ5 OF VANADIUM AND MANGANESE COMPOUNDST. Yamamoto…X-ray emission spectra were reproduced from references previously reported, and X-ray absorption spectra were recorded with a laboratory-type spectrometer. Samples with four-fold tetrahedral coordination gave more intense pre-edge peaks and Kβ5 …
RESIDUAL STRESS CHARACTERIZATION OF PVD COATED CARBIDE – INDUSTRIAL APPLICATIONT. Shibata, B. Sargent…Ti1-xAlxN alloys have better oxidation resistance and superior mechanical properties at elevated temperature than TiN. With more Al atoms in the TiN lattice to form solid solutions, the bonding nature changes from metallic Ti-N to covalent Al-N,…
RESIDUAL STRESS MEASUREMENT OF HIGH-DENSITY POLYETHYLENE PIPE WITH TWO-DIMENSIONAL X-RAY DIFFRACTIONM. Ren, C. Zheng, Y. Shi, Y. Tang, B. He…This method utilizes a two-dimensional detector to collect data of a selected diffraction ring and rotates the sample with only one ψ-tilt angle 22.5° and φ scan that covers 0° ~ 360° with 45° intervals. The diffraction ring of ca. 36° 2θ angle (C…
SPATIALLY RESOLVED TEXTURE AND MICROSTRUCTURE EVOLUTION OF ADDITIVELY MANUFACTURED AND GAS GUN DEFORMED 304L STAINLESS STEEL INVESTIGATED BY NEUTRON DIFFRACTION AND ELECTRON BACKSCATTER DIFFRACTIONS. Takajo, D.W. Brown, B. Clausen, G.T. Gray III, C.M. Knapp, D.T. Martinez, C.P. Trujillo, S.C. Vogel…Vogel1 1Los Alamos National Laboratory, Los Alamos, NM 87545, USA. 2JFE Steel Corporation, Kurashiki 712, Japan. ABSTRACT In this study, we report the characterization of a 304L stainless steel cylindrical projectile produced by additive manufac…
SURFACE FINISH THICKNESS DETERMINATION ON PRINTED CIRCUIT BOARDS SUB-STRUCTURES USING XRF AND SEMF. Bogani…For example, gold plated surfaces are widely used in finishing of electronic components because they offer low contact resistance and great protection against corrosion. Thickness measurement of surface finish is critical to validate that the pr…
USE OF MULTIVARIATE ANALYSIS FOR DETECTING ORIENTATION CHANGES IN STEEL VIA LAUE DIFFRACTION ARTIFACTS WITHIN XRF SPECTRAM.A. Rodriguez, M.H. Van Benthem, J.J.M. Griego, S. DeJong, D.F. Susan, P. Yang, C.D. Mowry, D. Enos, K.A. Stirrup…We report on measurements of several Stainless Steel witness samples originating from the same alloy lot. One set was collected as-received and the second set was measured after mechanical rolling. Texture changes resulting from the rolling proc…
WAVELENGTH-DISPERSIVE XRF IMAGING USING SOLLER SLITS AND 2D DETECTORS Aida, M. Yamanashi, T. Sakumura, K. Matsushita, T. Shoji, N. Kawahara, K. Tsuji…X-ray Instrument Division, Rigaku Corporation, 3-9-12, Matsubara-cho, Akishima-shi, Tokyo, 196-8666, Japan 3X-ray Research Laboratory, Rigaku Corporation, 14-8 Akaoji-cho, Takatsuki-shi, Osaka 569-1146, Japan ABSTRACT A new wavelength-dispersive…
WORKSHOP ON CHALLENGES IN XRF ANALYSIS FOR RELIABLE X-RAY SPECTRAJ. Kawai, K. Yoshida, R. Tanaka…Kawai, Kyoto University, for spectral interpretation, S. Ichikawa, Fukuoka University, for sample preparation, and Y. Uehara, Mitsubishi Electric Co., for soft X-ray detection. The present part is limited to the spectral interpretation, with emp…
X-RAY POLE FIGURE ANALYSIS ON BIAXIALLY ORIENTED POLYETHYLENE FILMS WITH SEQUENTIAL BIAXIAL DRAWINGY. Tang, M. Ren, H. Shi, D. Gao, B. He…The results track the evolution of pole figures of the (110), (200) and (020) lattice planes of linear low density polyethylene (LLDPE) film during the first deformation step, machine direction orientation (MDO), and the second deformation proce…
XRF ANALYSIS BY FP CALIBRATION USING STANDARDS WITH UNKNOWN COMPONENTSK. Kawakyu, T. Moriyama, Y. Kataoka…The quantification procedure of unknown samples with FP method was proposed by Criss and Birks (1968). The theoretical intensity equations in these approaches are dependent not on absolute mass fractions but mass fraction ratios of elements, imp…

2016 – VOL60

A 2D PIXEL DETECTOR FOR VERY HIGH-RATE X- AND GAMMA-RAY SPECTROSCOPY AND IMAGINGE. Nygård , N. Malakhov, P. Weilhammer, O. Dorholt , O. M. Røhne, T. Nagano , K. Yamamoto…The underlying reasoning behind it, as well as early results from the evaluation of the first prototype, is presented. INTRODUCTION A 2D pixel detector concept with full spectroscopy feature in each pixel has been developed. The concept is versa…
A NEW IN SITU REACTION CHAMBER IN DEBYE-SCHERRER GEOMETRYT. Hartmann, S. Correll, S. Welzmiller…INTRODUCTION Up to the recent past, commercially available reaction chambers have strictly been built in reflection geometry to be mounted on Bragg/Brentano or Theta/Theta goniometers. In spite of all their construction-related disadvantages, su…
APPLICATION OF METAL IMPURITY TRACE ANALYSIS IN PHARMACEUTICAL MATERIALS USING UNIQUE FP METHOD FOR ASSESSMENT ELEMENTS BASED ON ICH Q3DH. Furukawa, N. Ichimaru, S. Watanabe, K. Suzuki, E. Terashita, M. Nishino, H. Ochi, D. Davis, C. Yomota…Kobe Pharmaceutical University, Kobe, Japan ABSTRACT The International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) Q3D guideline presenting a policy for limiting metals for 24 elements such as cadm…
ARCHAEOLOGICAL CHARACTERIZATION OF ANCIENT POTTERY FROM OSHIMA AND HACHIJOJIMA ISLANDS (TOKYO, JAPAN) ACCORDING TO CHEMICAL COMPOSITION OBTAINED BY XRF ANALYSISS. Ichikawa, T. Matsumoto, T. Nakamura…For provenance estimation, the pottery shards were assayed by X-ray fluorescence using a glass bead sample preparation method. The calibration curves for this method were obtained using 10 synthetic standards containing the following analytes: N…
CALCULATION AND MEASUREMENTS OF XRD SPECTRA OF N-H EXTENDED SOLIDS UNDER HIGH PRESSUREI.G. Batyrev, S.P. Coleman, J.A. Ciezak-Jenkins, J.P. Larentzos…The structure of N-H at high pressure was determined from computational modelling using the evolutionary program USPEX, which was based on VASP plane wave density functional theory (DFT) calculations. A set of LAMMPS tools and shell scripts took…
COMBINING SAMPLE PRECONCENTRATION AND ION EXCHANGE CHROMATOGRAPHY TO QUANTIFY GALLIUM AND TRACE URANIUM IN PLUTONIUM USING POLARIZED-BEAM EDXRFAdministrator…The sample is dissolved, and the plutonium matrix is removed with ion exchange (IE) chromatography. Gallium and uranium are eluted from the IE column, and gallium is analyzed in solution. To concentrate the uranium, the specimens analyzed for ga…
DISCRIMINATING WINDOW AND BOTTLE GLASS FRAGMENTS BASED ON TRACE ELEMENTSAdministrator…In previous work, glass fragments of soda bottles were analyzed by micro X-ray fluorescence spectrometry per the ASTM method with the modification of collecting two spectra from the same measurement position, one without filtering and one with f…
FIRST INDIRECT X-RAY IMAGING TESTS WITH AN 88-MM DIAMETER SINGLE CRYSTALA.H. Lumpkin, A.T. Macrander…The crystal was bonded to a fiber optic plate (FOP) for mechanical support and to allow the option for FO coupling to a large format camera. This configuration resolution was compared to that of self-supported 25-mm diameter crystals, with and w…
HIGH TEMPERATURE PHASE TRANSFORMATION OF IRON SULFIDES. Mlowe, N. Revaprasadu, S.S. Garje…ABSTRACT Studies on the phase transformation of iron sulfide nanoparticles synthesized employing a high temperature route by pyrolysis of heterocyclic iron(III) dithiocarbamate complexes revealed that the properties solely dependent on the tempe…
INVESTIGATION OF HEAVY METALS IN ZEBRAFISH TISSUE BY TOTAL REFLECTION X-RAY FLUORESCENCE SPECTROMETRYM. Schmeling, E. Jamka, J. Arroyo, K. Niaz, T. Trinh…Some heavy metals like zinc and copper are essential for enzymatic and metabolic function while others like lead and mercury are toxic and interfere with biological pathways. Zebrafish are a very popular model organism for monitoring toxicity of…
LABORATORY-TYPE POLYCHROMATIC SIMULTANEOUS WDXRF USING A SILICON STRIP DETECTOR FOR CHEMICAL STATE ANALYSISK. Sato, A. Nishimura, M. Kaino, S. Adachi…The X-rays dispersed by a flat analyzing crystal are detected simultaneously by different SSD channels, and a high energy resolution is achieved by limiting the measurement range. For Cr, we used a spectrometer with a range from 5.3 to 6.3 keV, …
MATERIALS ASSURANCE THROUGH ORTHOGONALMATERIALS MEASUREMENTS: X-RAY FLUORESCENCE ASPECTSM.A. Rodriguez, M.H. Van Benthem, D.F. Susan, J.J. M. Griego, P. Yang, C.D. Mowry, D.G. Enos…We document the use of Principal Component Analysis (PCA) of XRF data on compositionally similar and dissimilar stainless steels for the purpose of testing the feasibility of employing XRF spectra to parse and bin these alloys as the same or sig…
MONITORING PERFORMANCE OF DIFFRACTING CRYSTALS WITHOUT DETECTION OF THE REFLECTED X-RAYSAdministrator…Outside of the Bragg reflection region a 5-fold enhancement in the electric current was observed while the X-ray beam was incident on the working inclined surface of the crystal. Within the Bragg reflection region the electric current as a funct…
NEW NEUTRON TIME-OF-FLIGHT (TOF) CAPABILITY IN PDF-4+ RELATIONAL DATABASES: DIGITIZED DIFFRACTION PATTERNS AND I/IC FOR QUANTITATIVE PHASES ANALYSISJ. Faber, S. Kabekkodu, J. Blanton, T. Blanton, T. Fawcett…These diffraction patterns can all be calculated on-the-fly. Three TOF results can be realized: the live calculation of on-the fly diffraction patterns, the population of static PDF® cards, and data for search/match tables for phase identificati…
PORE NETWORK ANALYSIS OF CARBONATE ROCKS BY TOMOGRAPHIC IMAGES TAKEN AT MULTIPLE SPATIAL RESOLUTIONSR. Nagata, C.R. Appoloni, P. José dos Reis…Since carbonate rocks have a large range of pores sizes, their pore network is highly complex and have been the main object of many studies. X-ray computed tomography is a powerful technique that have been used to study petrophysical properties …
POWDER XRD AND TEM STUDY ON CRYSTAL STRUCTURE AND INTERSTRATIFICATION OF ZN-CHLORITE (BAILEYCHLORE)Administrator…Rule and Frank Radke in 1988 for the honor of Professor Sturges W. Bailey of the University of Wisconsin – Madison, USA. Baileychlore occurs as dark green chlorite on calcite veins from garnet-vesuvianite skarn clasts at Red Dome ore deposit, Ch…
SIDE-COATED TAGWOODS AND THE FORMATION OF DENSE AGGREGATES OF INTERTWINED TAGWOOD STRINGSF. Peyronel, D. Pink, B. Quinn, A. Marangoni…We employed a Bonse-Hart instrument at the Advanced Photon Source, ANL. Unified fit and Guinier-Porod models were used to fit the data to obtain three parameters: scatterer shape, average scatterer linear dimensions, and fractal dimensions of ag…
SINGLE CRYSTAL STRUCTURE ANALYSIS OF DESIGNER DRUGS CIRCULATING IN THE JAPANESE DRUG MARKET BY THE SYNCHROTRON RADIATION X-RAY DIFFRACTIONT. Hashimoto, R. Hanajiri, N. Yasuda, Y. Nakamura, N. Mizuno, S. Honda, S. Hayakawa, Y. Nishiwaki, S. Kimura…In order to determine the absolute structures of four new designer drugs derived from medicines (methylphenidate and phenmetrazine) x-ray single crystal structure analyses were performed using the BL26B1 beamline of synchrotron radiation facilit…
STRUCTURAL DESIGN AND CHARACTERIZATION OF VANADIUM-BASED PHOSPHATES AS CATHODE MATERIALS FOR LI-ION BATTERIESQ. Kuang, X. Liu, Y. Zhao…State Key Laboratory of Luminescent Materials and Devices, South China University of Technology, Guangzhou 510641, China * Corresponding author. Tel.: +86-20-87111963, E-mail address: sckq@scut.edu.cn ABSTRACT The present Li-ion batteries (LIBs)…
TEMPERATURE DEPENDENCY OF MORPHOLOGY OF CONVENTIONAL THERMOPLASTIC AND LIGNIN-BASED POLYURETHANES USING WAXS AND SAXSK. Walbrueck, S. Klein, J. Rumpf, M. Schulze, S. Witzleben…Polyether and polyether/ester based TPU (thermoplastic polyurethanes) were investigated with wide-angle XRD (X-ray diffraction) and SAXS (small angle X-ray scattering). Furthermore, SAXS measurements were performed in the temperature range of 30…
THROUGH THICKNESS TEXTURE GRADIENT PREDICTION OF 5XXX SERIES ALUMINUM AFTER SHEET ROLLING OPERATIONSJ. Ho, S. Dennis, A. Tabei , H. Garmestani…Theoretical models tend to account only for the idealized plane-strain compression resultant at the center of the material, thereby allowing for the assumption of a homogeneous texture with orthorhombic stress. This potentially leaves a largely …
X-RAY ANALYSIS OF FE3O4 MAGNETIC NANOPARTICLESAdministrator…The effect of the crystallite size on the lattice strain and the magnetic property of the MNPs are discussed. INTRODUCTION Iron oxide exhibit a number of potential applications aiming for improved quality of life. For example, because of its bi…
X-RAY FLUORESCENCE, RAMAN AND MULTIVARIATE STATISTICS ANALYSIS OF ARCHAEOLOGICAL POTTERY FROM SÃO LUIZ, MA, BRAZILR.A. Ikeoka, C.R. Appoloni, O.H. Marcori, A.M. Bandeira…Prof. Almeida Prado, 1466 CEP 05508-900, Cidade Universitária, São Paulo, SP – Brasil ABSTRACT This work concerns the archaeometric analysis of ceramic fragments from archaeological excavations carried out in “Sambaqui do Bacanga”, ‘Sambaqui do …

2015 – VOL59

A NEW BENCHTOP TXRF SPECTROMETERFlannery, David T (3225-Caltech)…The optical alignment of the multilayer was made and confirmed by two strategies: a) following the X-ray beam with a CCD camera; b) collecting the spectra of the X-ray beam before and after the multilayer, using a second detector in front of the…
C/H AND O CORRECTION BY A SCATTERED X-RAY INTERNAL STANDARD FOR XRF ANALYSIS OF OILSK. Kawakyu, A. Morikawa, K. Watanabe, Y. Yamada, Y. Kataoka…Absorption and enhancement by coexisting inorganic elements such as additives in lubricating oils affect intensities as well. Analysis errors caused by these effects can be avoided using standards matrix matched to test samples. However, such st…
CHALLENGE OF TRACE ANALYSIS FOR PHARMACEUTICAL PRODUCTS AND FOOD USING THEORETICAL SCATTERED X-RAYSH. Furukawa*, N. Ichimaru, S. Watanabe, K. Suzuki, M. Nishino, H. Ochi, D. Davis…ABSTRACT The United States Pharmacopeia (USP) has recently established guidelines for general analysis using X-ray Fluorescence (XRF) methodology. XRF is an attractive methodology because it does not require chemical pretreatment and allows for …
CHARACTERISATION OF X-RAY REFLECTIVITY OF FLAT AND CURVED PYROLYTIC GRAPHITE MOSAIC CRYSTALSY. Van Haarlem, J. Tickner…We have measured the X-ray reflection properties of a variety of flat and doubly-curved HOPG and HAPG materials. Measurements of mosaicity and peak and integrated reflectivity were made as a function of crystal thickness, the method of material …
COMBINED ELEMENTAL XRF AND PHASE XRD ANALYSES OF A METEORITEF. Tañeza-Casco, T. Witzke, N. Norberg…Knowing more about the composition and mineral phases of meteorites bring us a step closer to understanding how the solar system was formed. X -ray diffraction (XRD) is a good technique used to investigate phase composition of meteorites, but it…
CRYSTAL STRUCTURE REFINEMENTS OF PYROPE-MAJORITE SOLID SOLUTIONS BETWEEN PRP100MJ0 AND PRP17MJ83S. M. Antao, N. S. Suarez Nieto, L.A. Cruickshank, G. D. Gwanmesia…The Prp-Mj solid solutions, [8] X3 [6] Y2 [4] Z3 [4] O12, from Prp100, Mg3[Al]2Si3O12, to Mj100, Mg3[MgSi]2Si3O12, are expressed as Mg3(MgxSixAl2-2x)Si3O12, 0  x  1, and are formed by cation exchange in the Y site because 2Al 3+ (0.535 Å) = M…
DISCRIMINATING GLASS FRAGMENTS USING MICRO-XRF SPECTROMETRY WITH POLY-CAPILLARY OPTICSFlannery, David T (3225-Caltech)…The typical issue is to compare glass fragmets from a kow source to fragmets from a ukow source ad show that the ukow fragmets are either cosistet or icosistet with the kow fragmets. There are various testig methods available to the aalyst iclud…
EDGE-ABSORPTION NON-DISPERSIVE X-RAY FLUORESCENCE SPECTROSCOPYJ. Van Wagoner*, S. Cornaby, S. Kamtekar, K. Kozaczek…A non-dispersive XRF (NDXRF) system will instead use a set of filters in front of a simple x-ray flux counter, such as a proportional counter, photodiode or scintillation counter. The filters on an NDXRF system are selected to allow or block out…
ENHANCING PDF DATA QUALITY ON A LABORATORY POWDER DIFFRACTOMETERT. Hartmann, L. Fink, N. Schrodt…INTRODUCTION In the recent past, the calculation of the pair distribution function (PDF) became more and more common as a new method to obtain structural information from complex materials beyond the Bragg equation and crystallographic PXRD anal…
INVESTIGATION OF NANOSTRUCTURE MATERIALS FOR DEVELOPING NEW X-RAY REFERENCE MATERIALSB.Kodess, P.Kodess…The diffraction pattern of the nitrides steel of this batch of steel samples includes various broadenings of Bragg reflections occurring because of distortion of the crystal lattice. In the round-robin experiment eight organizations participated…
LOW POWER TXRF KITJ. Kawai, H. Shino, H. Nagai, Y. Nakajima…Those who want to use these kind of portable TXRF spectrometers know very well about the technical details of the X-ray experiment, and thus a kit is sometimes enough. With a screwdriver, the TXRF spectrometer can be assembled, and the users can…
MICROXRF ANALYSIS OF ASTROBIOLOGICALLY-SIGNIFICANT GEOLOGICAL SAMPLESD. T. Flannery, A. C. Allwood, W. T. Elam, R. Hodyss, D. R. Thompson and L. Wade…Here, we set out to demonstrate µm-cm scale micro-XRF elemental mapping of ancient (~3.5 Ga) microbial sedimentary features using a prototype of the Planetary Instrument for X-ray Lithochemistry (PIXL). The micro-XRF system provided rapid, textu…
MONITORING OF COS2 REACTIONS USING HIGH TEMPERATURE XRD COUPLED WITH GAS CHROMATOGRAPHY (GC)M.A. Rodriguez, J.J.M. Griego, C.D. Mowry, A.S. Pimentel, T.M. Anderson, E.N. Coker…When CoS2 cathode materials were analyzed in an air environment, oxidation of the K(Br,Cl) salt phase in the cathode led to the formation of K2SO4 that subsequently reacted with the pyrite-type CoS2 phase leading to cathode decomposition between…
NEW CAPABILITIES FOR ANALYSIS OF ORGANIC MATERIALS USING THE ICDD PDF-4/ORGANICS DATABASES. Kabekkodu, S. Gates, A. Gindhart, M. Rost, T. Blanton, T. Fawcett…There are several formats intended to serve different groups of users. The PDF-4/Organics™ database is designed to help analyze materials, with an emphasis on organics, by powder diffraction techniques. It works seamlessly with commercial analys…
ONE SHOT ANALYSIS USING WIDE-RANGE HIGH-SPEED DETECTORR. Ogawa*, Y. Okamoto, H. Sekiguchi, H. Furukawa, K. Koyanagi, D. Davis…It is necessary to scan a wide range of angles in order to collect a pattern of peaks for identification in qualitative analysis, whereas only a few specific peaks need to be acquired for quantitative analysis. “OneSight”, a wide-range high-spee…
RESULTS FROM A NEW LOW-Z HIGH-Z TXRF SPECTROMETERK. Sanyal, B. Kanrar, S. Dhara, N.L. Misra, P. Wobrauschek*, C. Streli…The spectrometer does not require LN2 cooling for detector and water cooling for anodes of X-ray tubes. These features make it very compact and well suited for a Radiochemistry laboratory. The capability of the instrument was tested in terms of …
SAMPLE PREPARATION FOR TXRF ANALYSIS OF METAL PARTICLES IN USED MACHINE OILS AND PRELIMINARY RESEARCH FOR APPLICATION OF PRINCIPAL COMPONENT ANALYSIST. Matsuno, Y. Tabuchi, R. Hosomi, T. Hasegawa, N. Kometani, K. Tsuji…When used vacuum pump oil was measured by TXRF, quantitative TXRF analysis was difficult with internal standard technique because homogeneous solution was not obtained. Thus, a surfactant was added to the sample to mix the oil and the solution h…
SECONDARY EXITATION OBSERVED IN LATERAL SCAN USING CONFOCAL MICRO-XRFN. Kawahara, T. Matsuno, K. Tsuji, Y. Takimoto…A lateral scan near the border was performed at different depths. Characteristic secondary excitation of iron was observed in the Fe Kα intensity profile at 40 µm in depth, while it was not observed by lateral scan near the surface. In addition,…
SINGLE-CRYSTAL STRUCTURE ANALYSIS OF DRUG POWDER SAMPLE BY SYNCHROTRON RADIATION MICROBEAM X-RAYT. Hashimoto, S. Honda, N. Yasuda, S. Kimura, S. Hayakawa, Y. Nishiwaki, M. Takata…To demonstrate the usefulness of synchrotron radiation (SR) microbeam X-ray structure analysis, we applied the method to determine the structure of diphenidine hydrochloride and 4-methoxy-PCP hydrochloride whose crystal structures are unknown. T…
SYNCHROTRON X-RAY DIFFRACTION OF A FRICTION STIR PROCESSED AL0.1COCRFENI HIGH ENTROPY ALLOYN.A Ley, M. Komarasamy, R. Mishra, M.L. Young, M. Carl…HEAs have advantages over traditional alloys due to their lack of precipitate formation and growth at higher temperatures and their reduced cost because of cheaper alloying components. In this study, we examine an Al0.1CoCrFeNi HEA after frictio…
THE BENEFITS OF SMALL SPOT MAPPING ANALYSIS IN PRODUCTION PROCESS TROUBLESHOOTING USING AN EDXRF SPECTROMETERF. Tañeza-Casco…Often, the inhomogeneity can be traced back to an error in the production process of a product. By knowing the sample homogeneity, manufacturers can trace back and optimize their process in order to create better quality products. Small spot ana…
THIN FILM XRF SPECIMEN PREPARATION: IMPROVEMENTS OVER THE DRIED SPOT APPROACHFlannery, David T (3225-Caltech)…Dissolved plutonium metal samples were cast as small drops on Kapton film, and a surfactant was added to disperse the solution uniformly across the Kapton. After drying the specimens, they were sealed in a cell for analysis. The method provided …
WD-XRF IMAGING WITH POLYCAPILLARY OPTICS UNDER GLANCING INCIDENCE GEOMETRYY. Takimoto, M. Yamanashi, S. Kato, T. Shoji, N. Kometani, K. Tsuji…In this spectrometer, a straight type polycapillary optic was applied instead of a Soller slit which is used in conventional WD-XRF spectrometers. The straight type polycapillary optic worked as a 2D collimator for fluorescent X-rays to keep the…
WORLDWIDE DISTRIBUTION OF TOTAL-REFLECTION X-RAY FLUORESCENCE, ITS CAPACITY, ACCEPTANCE AND TRENDS. A SURVEY.R. Klockenkämper, A. von Bohlen…Users come from scientific institutes, from working places at synchrotron beam-lines and from labs in semiconductor fabs. The capacity of TXRF will be demonstrated by nine different examples of analysis. TXRF has some special characteristic adva…
X-RAY AND NEUTRON TOTAL SCATTERING ANALYSIS OF HY∙(BI0.2CA0.55SR0.25)(AG0.25NA0.75)NB3O10∙XH2O PEROVSKITE NANOSHEET BOOKLETS WITH STACKING DISORDERP. Metz*, B. Cladek, S.T. Misture, J. Neuefeind, K. Page, R. Koch…The perovskite layer contents were defined initially using combined synchrotron x-ray and neutron Rietveld refinement of the parent Aurivillius structure. The structure of the subsequently ion exchanged material, which is disordered in its stack…
X-RAY FLUORESCENCE DETERMINATION WITH MICRO-GLASS BEADS USING ONE-MILLIGRAM OF ARCHAEOLOGICAL SAMPLES. Ichikawa, T. Nakamura…Calibration curves for this method were obtained using synthetic standards, prepared by compounding chemical reagents (oxides, carbonates, and diphosphates) containing the analytes, The calibrations had good linearity and lower limits of detecti…
X‐RAY INVESTIGATIONS OF SOLID SOLUTIONS AND PHASE TRANSITIONS OF MONOCALCIUMALUMINATE AND MONOBARIUMALUMINATE USE IN CEMENT, PHOSPHORESCENCE AND RADIATION PROTECTION APPLICATIONSH. Pöllman, R. Kaden…Based on Calcium Aluminate Cements, the replacement of calcium by strontium and barium leads to cements which can be used at elevated temperatures in refractory applications. Alkaline earth aluminates also can be used in the field of phosphoresc…

2014 – VOL58

A NEW METHODICAL APPROACH BASED ON COMPTON SCATTERING AND XRF: QUANTITATIVE ANALYSIS OF CO2 AND LOSS ON IGNITION IN QUICKLIMEM. Inoue, Y. Yamada, M. Kitamura, N. Gotoh, N. Kawahara, M. Mantler…Total LOI is determined by the Compton scattered Rh K tube radiation which is used di- rectly in the calibration equation. The resulting calibration curve for LOI including matrix cor- rection shows an accuracy of 0.15 mass%. The carbon content …
A NEW MULTISTRIP DIFFRACTION DETECTOR WITH ENERGY RESOLUTIONP. Storer, N. Absalom, R. Clapp…The detector is a fast readout 1D solid state silicon strip detector which can be retrofitted to a diffractometer goniometer arm or any other X-ray system to count X-rays. The detector uses a 96 strip silicon sensor with associated counting and …
ADVANCED X-RAY WINDOW DESIGN AND TESTINGM. Harker, J. Abbott, J. Wong…The manufacturing process is currently limited to 40°C with differential pressure. Many detector manufacturers would like to go to higher temperatures for quicker and more effective outgassing of the detector assembly. At Moxtek, Inc. a manufact…
AGING OF EXPLOSIVE CRYSTALS (RDX) INVESTIGATED BY X-RAY DIFFRACTIONM. Herrmann, M.A. Bohn…The investigations revealed different behavior of the RDX types. Whereas microstrain released in I-RDX, further crystal damage occurred in S-RDX during the aging treatment. INTRODUCTION AND AGING Reduced sensitivity (RS) variants of high explosi…
CHARACTERIZATION AND QUANTIFICATION OF THE BEAM PROFILE OF POLYCAPILLARY LENSES .. AN APPLICATION STUDYM. Bremekamp, J. Leske, B. Nensel, V. Rößiger, M. Haller, J. Bogert, S. Bjoumikova…V). A quantification of this effect is a prerequisite for any microstructural quantitative analysis. In this contribution we characterize and quantify the intensity beam profile of different polycapillaries and predict the impact on the quantifi…
CHARACTERIZATION OF A PORTABLE X-RAY DEVICE FOR RESIDUAL STRESS MEASUREMENTSJ. Ling, S.-Y. Lee…In order to quantify the instrument precision and accuracy of the stress values, a series of measurements with stress-free ferrite powder and a solid platinum specimen were conducted using both the traditional sin2 and the less- methods. The pre…
CHARACTERIZATION OF NAFION PROTON EXCHANGE MEMBRANE FILMS USING WIDE-ANGLE X-RAY DIFFRACTIONT.N. Blanton, R. Koestner…Pores in a Nafion membrane allow for the movement of cations, however the membrane does not conduct anions or electrons. Depending on the manufacturing process, the cation conductivity of a Nafion membrane can be modified to meet a specified app…
COMPARISON OF DIFFERENT EXCITATION MODES FOR THE ANALYSIS OF LIGHT ELEMENTS WITH A TXRF VACUUM CHAMBERJ. Prost, P. Wobrauschek, C. Streli…In the first set of experiments two water- cooled high-power X-ray tubes with Cr (Z = 25) and Cu (Z = 29) anodes respectively were compared with an air-cooled low power tube with Mo anode (Z = 42) and a thin Be window for the transmission of Mo-…
CONTROL OF SPHERICAL OPTICS STRESS BY X-RAY TOPOGRAPHYR.Vitt, J. Maj, S. Krasnicki, L. Maj , G. Navrotski, P. Chow, S. Mikula…The crystal bending is characterized by x-ray topography. Examples of recorded topographic images and the corresponding rocking curves are presented. Use of the new technology can lead to production of nearly uniformly concave single-crystal sui…
CRYSTAL ORIENTATION MEASUREMENTS USING SEM-EBSD UNDER UNCONVENTIONAL CONDITIONSK. Kunze…The vast majority of EBSD measurements is applied to planar and polished surfaces of polycrystalline bulk specimen. In this contribution we present examples of using EBSD and EDX to analyze specimens that are not flat, not planar, or not bulk – …
EDXRF STUDIES ON ANCIENT CHINESE CERAMICSY. Gong, J. Gu, Y. Xiong…Since the 1990s, Shanghai Museum has carried out a number of projects involving the analysis of ancient Chinese ceramics. A few application examples using either benchtop XRF or micro-XRF system are described in this paper in order to give reade…
EFFECT OF WELDING PARAMETERS ON RESIDUAL STRESSES OF FRICTION STIR WELDED ALUMINUM ALLOYZ. Dou, C. Ma, P. Zhang, Y. Li, M. Wang, P. Dong, L. Chen, L. Zheng, J. Zhang…Institute of Materials, China Academy of Engineering Physics, Mianyang, 621700, China; 3. Sichuan Yijing Technology Group Co., LTD., Mianyang, 621700, China; 4. Southwest Technology and Engineering Research Institute, Chongqing 400039, China; 5….
EXPLOITING MYTHEN DETECTOR FOR HIGH-ACCURACY STRUCTURE ANALYSISD. Šišak Jung, Ch. Hörmann…Based on the MYTHEN detector, this work addresses two topics: (i) what is single-photon counting and (ii) how does this technology enhance accuracy in structure analysis using XRPD data. (i) The first topic covers basics of single-photon-countin…
FLUX COMPARISONS OF MINIATURE X-RAY SOURCES: XRF WATTAGE-MAPS BY APPLICATIONS. Cornaby, K. Kozaczek…ULTRA-LITE® have a voltage range of 4 to 50 kV and a power range of 0.1 to 4 watts, and are designed for handheld devices which can easily be powered by a battery. X-ray sources such as the Moxtek,. MAGPRO®, have voltage range of 4 to 60 kV and …
HUMIDITY EXPERIMENTS ON A LABORATORY DIFFRACTOMETER WITH A FULLY AUTOMATIC COUPLED TEMPERATURE-HUMIDITY CONTROLO. Narygina, H. van Weeren, C. Resch, S. Zellnitz…Due to the strong dependence of RH from T the experimental path through T-RH space should be chosen very carefully in order to avoid strong fluctuations in RH and possible condensation inside a non-ambient chamber. We have developed and tested t…
IN-SITU ENERGY-DISPERSIVE X-RAY DIFFRACTION STUDY OF A COMMERCIAL LITHIUM IRON PHOSPHATE/GRAPHITE 18650 CELLW. Paxton, Z. Zhong, T. Tsakalakos…Time-resolved energy-dispersive X-ray diffraction (EDXRD) spectra were collected using a germanium energy detector at a fixed angle of 3 degrees. The data show the full evolution of lithium-ions moving from the graphite negative electrode to the…
LOCATING TRACE PLUTONIUM IN CONTAMINATED SOIL USING MICRO-XRF IMAGINGC.G. Worley, K.J. Spencer, H. Boukhalfa, R.C. Roback…Because the specimen had previously been prepared for analysis by scanning electron microscopy, it was coated with gold to eliminate electron beam charging. However, this significantly hindered efforts to detect plutonium by MXRF. The gold L pea…
MECHANICAL STRESS X-RAY EMISSION FROM PIEZOELECTRIC MATERIALS. Imashuku, S. Hifumi, K. Yokoi, S. Matsuoka, J. Kawai…In the report, we speculated that piezoelectricity of sugar candy was related to the X-ray emission. Here, we investigated optical and X-ray spectra of piezoelectric materials in order to clarify the relationship between piezoelectricity and mec…
MINERALOGICAL EFFECTS OF SULFUR IN HANDHELD XRFM. Cameron, A. Seyfarth…The spectra were calculated with three different calibration methods to quantify the S effect on Fe and to determine what calibration method would best compensate for the effect in a handheld XRF instrument. Empirically-determined matrix coeffic…
NEW NEUTRON DIFFRACTION DATA CAPABILITY IN THE PDF-4+ 2014 RELATIONAL DATABASEJ. Faber, C. Crowder, J. Blanton, S. Kabekkodu, O. Gourdon, T. Blanton, T. Fawcett…Elements in the periodic table often have quite different scattering amplitudes. Unlike standard laboratory x-ray sources, neutrons are available both at nuclear reactors and pulsed sources. These facilities are available world-wide. In this pap…
QUANTITATIVE TEXTURE ANALYSIS VIA TILT-A-WHIRL ANDMAUDM.A. Rodriguez, J.D. Carroll, J.J.M. Griego, L.A. Deibler…We have extended our analysis to incorporate the use of the software MAUD to obtain quantitative texture characterization. With this new functionality, we have characterized single-crystal Tantalum dogbone tension bars before and after loading. …
RECONSTRUCTION OF ORIGINAL INTENSITY FROM COVERED SAMPLESR.I. Barabash, T.R. Watkins, R.A. Meisner, T.D. Burchell, T.M. Rosseel…While candidate covering films appear visually transparent, they are not necessarily x-ray transparent. Each film material has unique beam attenuation. Further amorphous peaks can be superimposed onto those from the sample. To reconstruct the sc…
RESPONSE FUNCTION OF SILICON DRIFT DETECTORS FOR LOW ENERGY X-RAYSR.H. Redus, A.C. Huber…An incomplete charge collection (ICC) layer of 100 to 200 nm is often found near the surface of the active volume of these SDDs. X-rays interacting in the ICC layer cause significant differences from the ideal Gaussian photopeak response due to …
SECONDARY EXCITATION PROCESS FOR QUANTITATIVE CONFOCAL 3D-XRF ANALYSISK. Tsuji, A. Tabe, P. Wobrauscheck, C. Streli…E-mail: tsuji@a-chem.eng.osaka-cu.ac.jp ABSTRACT X-ray fluorescence (XRF) is a well established method for quantitative elemental analysis. For accurate quantification, secondary excitation has to be taken into account. In this paper, the second…
SIMULATION TOOLS AND REFERENCES FOR THE ANALYSIS OF NANOMATERIALST.G. Fawcett, S.N. Kabekkodu, J.R. Blanton, C.E. Crowder, T.N. Blanton…These tools are embedded software in the PDF-4 relational database family. The tools include algorithms to help in phase identification, crystallite size and distribution measurements, and measuring molecular orientation. In addition to these to…
STRESS DETERMINATION THROUGH DIFFRACTION: ESTABLISHING THE LINK BETWEEN KRÖNER AND VOIGT/REUSS LIMITSC.E. Murray, J.L. Jordan-Sweet, S.W. Bedell, E.T. Ryan…X-ray elastic constants (XEC) relate the strain as measured using x-rays to the state of stress in a quasi-isotropic ensemble of grains. However, the corresponding interaction models (e.g: Voigt and Reuss limits) often possess unlikely assumptio…
STRUCTURAL CHARACTERIZATION OF NEW TERNARY YTTRIUM.. RARE EARTH SESQUIOXIDES FORMED BY THE SOL..GEL TECHNIQUEG. Rafailov, I. Dahan, Z. Porat, D. Moglyanski, R. Zach, J. Zabicky, G. Kimmel…These were divided into two groups, each composed of the same elements but at different stoichiometric ratios; the first group included Y2EuDyO6, YEu2DyO6 and YEuDy2O6, and the second group included Y2EuGdO6, YEu2GdO6 and YEuGd2O6. The compounds…
STRUCTURAL VARIATIONS IN PYROPE-ALMANDINE SOLID SOLUTIONSS.M. Antao, M. Zaman, N.S. Suarez Nieto, V.L. Gontijo, R.A. Marr…Electron- microprobe analyses (EMPA) indicate homogeneous compositions for all the samples and HRPXRD data show that they are all single phases. Light microscopy shows that they are all optically isotropic. Several linear structural trend lines …
THE MEASUREMENT OF MASS ATTENUATION COEFFICIENT AT CU K.. WAVELENGTH OF POWDER XRD SAMPLES USING PARALLEL BEAM GEOMETRY.N.A. Raftery, B.W. Halstead, J.L. Watts…ABSTRACT In some circumstances, such as the use of the external standard method for Quantitative Phase Analysis (QPA) by X-ray powder diffraction (XRPD), it is necessary to have an accurate estimate of the sample mass attenuation coefficient at …
USE OF THE RIETVELD METHOD FOR DESCRIBING STRUCTURE AND TEXTURE IN XRD DATA OF SCALE DEPOSITS FORMED IN OIL AND GAS PIPELINES: AN IMPORTANT INDUSTRIAL CHALLENGEH. Sitepu, Rasha A. Al-Ghamdi, S.R. Zaidi, S. Shen…Preferred orientation can cause serious systematic errors in both quantitative phase analysis and crystal structure determination. It has been indicated that the generalized spherical harmonic (GSH) description provided a better Rietveld fit tha…
XRD PHASE IDENTIFICATION AND RESIDUAL STRESS ANALYSIS OF THE TURBINE BLADE SAMPLES BEFORE AND AFTER HEAT TREATMENTS. Shen, A.H. Mustafa, S.R. Zaidi, H. Sitepu; A.Y. Kawaie…Their physical properties and microstructure may degrade after long operating hours. Heat treatment is an industry recognized technique to restore the material to its original properties or best possible condition. In this study, a first stage t…

2013 – VOL57

A NEW “CHAIN” OF EVENTS: POLYMERS IN THE POWDER DIFFRACTION FILETM (PDF®)S.D. Gates, T.N. Blanton, T.G. Fawcett…Initially, the PDF was geared towards the identification of unknown crystalline materials by comparison of d-spacings and peak intensities. Today, the International Centre for Diffraction Data (ICDD) maintains and continuously enhances the quali…
AEROSOL FILTER ANALYSIS USING POLARIZED OPTICS EDXRF WITH THIN FILM FP METHODT. Moriyama, A. Morikawa, M. Doi, S. Fess…XRF is an important at- mospheric aerosol monitoring tool for inorganic component analysis, because XRF is rapid and easy analysis method. In particular EDXRF has drawn attention for aerosol analysis. However EDXRF has difficulties that (1) many…
CHARACTERIZING FUNDAMENTAL PARAMETERS BASED ANALYSIS FOR SOIL-CERAMIC MATRICES IN POLARIZED ENERGY DISPERSIVE X-RAY FLUORESCENCE SPECTROMETRY (PEDXRF)W.A. Abuhani, N. Dasgupta-Schubert, L.M. Villaseñor Cendejas…Mexico. * Correspondence: abuhani.waleed@gmail.com ABSTRACT Analytical PEDXRF spectrometry (PEDXRFS) represents a substantial advancement over conventional XRF. The higher Signal to Noise (S/N) commensurate with background lowering and better en…
COMPARISON OF CALCULATION METHODS FOR ANALYSIS OF SOIL SAMPLESMichelle Cameron…A full FP, full empirical, and hybrid calibration were tested. The empirical calibration gave better results for standards within the calibration range and for most standards outside the calibration range. Effects of increasing LOI were mixed, a…
DIFFERENTIATION OF SURFACE CONTAMINANTS AND IMPLANTED MATERIAL ON GENESIS SOLAR WIND SAMPLES USING TOTAL REFLECTION X-RAY FLUORESCENCE SPECTROMETRY AND GRAZING INCIDENCE X-RAY FLUORESCENCEM. Schmeling, P.J. Eng, J.E. Stubbs, Y. Choi, I.V. Veryovkin…Unfortunately the space craft crash landed upon return to Earth shattering the collectors into small fragments and exposing them to desert soil and spacecraft debris. Thus only small fragments are available for analysis with each having differen…
EVALUATION OF FUNDAMENTAL PARAMETERS FOR QUANTITATIVE X-RAY FLUORESCENCE OF POLYOLEFINSD.W. Burns, M. Wright, S. Yusuf…XRF is a matrix dependent analysis and accurate results require standards of similar matrices. The preparation of blended, matrix-matched polymer standards requires extensive effort and resources. Another quantitative approach is fundamental par…
EXAMINING ELEMENTAL DISTRIBUTIONS IN THREE DIMENSIONS USING TWO-DIMENSIONAL MICRO-XRF IMAGINGC.G. Worley, P.T. Martinez, K.J. Kuhn, L. Tandon…In addition to collecting two-dimensional elemental distribution maps of the coupon surface, three-dimensional elemental information was inferred based upon attenuation differences between the high energy U L and low energy U M X-rays. Only alum…
EXPERIMENTAL STUDY ON THE ENERGY DEPENDENCE OF PHOTOIONIZATION CROSS-SECTIONS IN SUBSHELLS USING AN EDX SPECTROMETERM. Doi, N. Kawahara, S. Hara, M. Mantler…Conventionally its values are derived by the assumption that the jump ratios between sub-shells have no energy dependency. However, cal- culations based on recent theoretical cross sections and elaborate experiments with synchrotron radiation so…
HEAVY METAL ANALYSIS IN LENS AND AQUEOUS HUMOR OF CATARACT PATIENTS BY TOTAL REFLECTION X-RAY FLUORESCENCE SPECTROMETRYM. Schmeling, B.I. Gaynes, S. Tidow-Kebritchi…To shed light into this subject, aqueous humor and lens samples were collected from 14 cataract patients to study the presence and concentration of selected metals in the eye. Subjects undergoing routine cataract surgery were consecutively enrol…
IN-SITU MONITORING OF VANADIUM DIOXIDE FORMATION USING HIGH TEMPERATURE XRDM.A. Rodriguez, N.S. Bell, J.J. M. Griego, C.V. Edney, P.G. Clem…Synthesis of VO2 can be challenging due to the variability of vanadium oxide phases that may be formed. We have employed High Temperature X-Ray Diffraction (HTXRD) to monitor the reaction process of Vanadium Oxide Precursor (VOP) powders to form…
INVESTIGATION OF X-RAY EMISSION FROM PYROELECTRIC CRYSTALK. Ohira, S. Imashuku, J. Kawai…At the same time, we examined an electron irradiation area using a fluorescent plate. When the cooling rate of a LiTaO3 crystal was over 0.3 K/s, X-ray emission continued for less than 15 seconds. X-ray emission stopped by a discharge between th…
ISO 9516-1 SIMPLIFIED BORATE FUSION / WDXRF ANALYTICAL METHOD FOR IRON ORE INCLUDING TOTAL IRON ANALYSIS: PART 2M. Bouchard, A. Milliard, S. Rivard, S. Ness…This updated method allows for the simplification of both laboratory and spectrometry processes and so, in comparison with the original ISO method, becomes less restrictive in practice. This method was used to prepare a large variety of iron ore…
LOW COST ROLLED X-RAY PRISM LENSES TO INCREASE PHOTON FLUX DENSITY IN DIFFRACTOMETRY EXPERIMENTSH. Vogt, A. Last, J. Mohr, F. Marschall, K.U. Mettendorf, R. Eisenhower, M. Simon…Due to its comparably easy fabrication method and the large aperture the so called Rolled X-ray Prism Lenses (RXPL) have the potential to be used with X-ray tubes in industrial environment as a low cost alternative to existing optics. The lens i…
MATERIALS CHARACTERIZATION FROM DIFFRACTION INTENSITY DISTRIBUTION IN . DIRECTIONBob He…The 2θ-profile can be evaluated for phase identification, crystal structure refinement and many applications with many existing algorithms and software. In order to evaluate the materials structure associated with the intensity distribution alon…
MICRO X-RAY FLUORESCENCE IN FOOD FORENSICS & FOOD SAFETYV.L. St. Jeor, C.A. Lendon…It is also compared to electron-based Energy Dispersive Spectroscopy (EDS). Both systems are generally considered non-destructive methods for determining elemental composition; however µXRF demonstrates specific advantages for elements heavier t…
MICROANALYSIS OF RARE-EARTH ELEMENTS USING AN ELECTRON BEAM FROM A PYROELECTRIC CRYSTALS. Imashuku, A. Imanishi, K. Hanasaki, K. Ohira, I. Ohtani, J. Kawai…We utilized characteristic X-rays and visible lights emitted from rare-earth elements for the analysis. Only characteristic X-rays of rare-earth elements contained in a sample was detected by focusing the electron beam on an area with a diameter…
OUT OF PLANE ORIENTATION AND CRYSTALLINITY OF BIAXIALLY STRETCHED POLYETHYLENE TEREPHTHALATES. Bandla, M. Allahkarami, J.C. Hanan…Polyethylene terephthalate (PET), a semi-crystalline polymer, exhibits a microstructure reliant on process and thermal history. PET undergoes strain-induced crystallization, making it sensitive to mechanical stretching. As the level of crystalli…
PERFORMANCE COMPARISON OF PORTABLE XRF INSTRUMENTS: A MINERAL EXPLORATION INDUSTRY PROSPECTIVEN.W. Brand, C.J. Brand…The advancement over the past decade in handheld or portable XRF instruments allows for real time ‘fit for purpose’ data to be collected allowing for real time assessments and decisions to be made assuming the instruments are used correctly and …
RESIDUAL STRESS AND QUANTITATIVE PHASE MAPPING ON COMPLEX GEOMETRIESM. Allahkarami, J.C. Hanan…Implementing complex curved surfaces in engineering components in combination with finite element geometry optimization has become a prevalent means of designing a part. Measuring residual stresses using X-ray diffraction on complex curved surfa…
REVISIT OF FORENSIC ANALYSIS OF ARSENIC POISONING CASE 1998Windows ユーザー…The spectra were measured at SPring-8 synchrotron facility by Nakai in December 1998 and Mo, Sn, Sb, and Bi were used as index elements at that time to demonstrate that the suspected saleswoman’s pesticide and that found near the curry pot were …
STABILITY AND STRUCTURE CHANGES OF NA-TITANATE NANOTUBES AT HIGH TEMPERATURE AND HIGH PRESSURElcx…Our results show that the nanotubes can be stable at ~ 400 °C. Higher temperature annealing of nanotubes result in opening and flattening of the nanotubes, and subsequent structural transformation to Na2Ti6O13-based structure via an intermediate…
STUDY OF IMPURITIES IN SRM 640C AND SRM 660A USING DIFFRACTION DATA FROM 11BM AT THE APSJohn Faber…These samples are used to calibrate the instrument and are contained in thin-wall Kapton ® containers. GSAS and GSAS-II were used to fit the experimental data. The structures for these SRMs are well established and the fitted models here are in …
THE ELECTRONIC AGE – EDX AND OTHER MODERN TECHNIQUES TO THE PRESENT AND BEYONDM. Mantler…Naturally this has its origin in the early transis- tors and the first semiconductor junction detectors of the late 1940’s. It was followed by refinement of semiconductor detector technology in general and particularly by the in- vention of Li-d…
THE GENERALIZED SIN2 . METHOD AN ADVANCED SOLUTION FOR X-RAY STRESS ANALYSIS IN TEXTURED MATERIALSA. Haase, M. Klatt, A. Schafmeister, R. Stabenow, B. Ortner…According to EN 15305 there is currently no existing solution for this problem. A method is presented that solves this problem. It is based on two tools: i) The use of a 1D detector having a large capture angle that yields the full diffraction p…
UNDERFILM CORROSION OF STEEL SHEETS OBSERVED BY CONFOCAL 3D-XRF TECHNIQUEK. Akioka, T. Nakazawa, T. Doi, M. Arai, K. Tsuji…A painted steel sheet was prepared by applying electrodeposition coating onto an electro galvanized steel sheet with a zinc phosphate conversion coating. The spatial resolution of the confocal micro-XRF was about 10.9 μm at an energy of 17.4 keV…
USAGE OF THE X-RAY TOPOGRAPHY UNIT FOR PRODUCING HIGH-QUALITY CONCAVE OPTICSJ. Maj, C. Harmata, L. Maj, G. Navrotski, P. Chow, L. Assoufid…However, the systematic approach for the use of the topography unit for the construction of high-quality concave optics has never been published. Residual stress in permanent concave bending optics has been a long-standing issue that had remaine…
X-RAY DIFFRACTION CHARACTERIZATION OF A DISTORTED DEBYE-SCHERRER FILM STRIP – THE EFFECT OF DEACETYLATION ON CELLULOSE TRIACETATE AND AN IMPROVED STRUCTURAL MODEL FOR CELLULOSE IIT.N. Blanton, J.A. Kaduk. Q. Johnson…An investigation using X-ray diffraction, XRD, was carried out to determine the cause of the physical change in the film strip. As expected, silver phases were detected, due to the photographic capture layer coated on the surface of all traditio…
X-RAY INVESTIGATIONS OF SOLID SOLUTIONS OF MONOCALCIUM ALUMINATE AND MONOSTRONTIUM ALUMINATE IMPORTANT PHASES IN CEMENT AND PHOSPHORESCENCE MATERIALSH. Pöllmann, R. Kaden…The amount of incorporation of foreign ions influences the hydration behaviour. Strontium aluminate is an important phase in producing phosphorescent materials when doped with REE as like Eu, Dy, La. These monoaluminates occur in different modif…
X-RAY SCATTERING ON CASEIN MICELLES AND HIGH DENSITY LIPOPROTEIN (HDL) GRANULES DURING PROCESSING OF FOODSDr. Ronald Gebhardt…Interactions with surfaces and interfaces during processing lead to changes in their structure and functional properties. We use surface-sensitive X-ray scattering to explore structural changes occuring in CM during cross-flow filtration and in …

2012 – VOL56

ANALYTICAL METHOD FOR OBSERVED POWDER DIFFRACTION INTENSITY DATA BASED ON MAXIMUM LIKELIHOOD ESTIMATIONT. Ida, F. Izumi…The method can optimize not only the parameters adjusted in the Rietveld refinement, but also parameters to specify errors in a model for the statistical properties of the observed intensity. The results of the structure refinements about fluora…
APPLICATION OF MICRO-XRF FOR NUCLEAR MATERIALS CHARACTERIZATION AND PROBLEM SOLVINGC.G. Worley, L. Tandon, P.T. Martinez, D.L. Decker…Scanning Electron Microscopy). Up until the past 10 to 15 years, Micro-X-ray fluorescence (MXRF) instrumentation had been relatively uncommon, and even currently, it is underutilized for spatially resolved nuclear materials analysis and imaging….
CHARACTERIZATION OF X-RAY IRRADIATED GRAPHENE OXIDE COATINGS USING X-RAY DIFFRACTION, X-RAY PHOTOELECTRON SPECTROSCOPY, AND ATOMIC FORCE MICROSCOPYT.N. Blanton, D. Majumdar…X-ray Diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), and Atomic Force Microscopy (AFM) have been used to characterize GO before and after irradiation. Results indicate that GO exposed to high-energy radiation is converted to an amorp…
COMPARING EXISTING MAC TABLES – HINTS TO POSSIBLE DEVELOPMENTSPierre Caussin…The idea of comparing table i not new (De Boer), but current oftware tool make it poible to quickly develop interactive oftware to analyze the dicrepancie in finer detail and get hint to the reaon for the difference. Such a tool ha been created …
DESIGN OF AN IN-SITU XRF INSTRUMENT FOR ELEMENTAL DIFFUSION MEASUREMENTSW.T. Elam, T. Grundl, O.X. Leupin, M. Descostes…Quantifying concentration gradients of the diffusing tracers requires the lowest possible detection limits, so we have performed calculations to aid in the experiment and apparatus design. Calculating the minimum detection limit (MDL) requires k…
DETERMINATION OF THE EFFICIENCY OF A SILICON DRIFT DETECTOR (SDD) BY MONTE CARLO SIMULATIONA. Rakotondrajoa, G. Buzanich, M. Radtke, U. Reinholz, H. Riesemeier, L. Vincze, R. Raboanary…This work presents a new approach in determining this efficiency, having the advantages to be fast and easy to implement, making it a good alternative to the more time-consuming standard method. Primarily, a multielement reference material was m…
ELEMENTAL DEPTH PROFILING OF FORENSIC SAMPLES BY CONFOCAL 3D-XRF METHODS. Emoto, K. Otsuki, K. Nakano, K. Tsuji…E-mail: tsuji@a-chem.eng.osaka-cu.ac.jp ABSTRACT We report the feasibility of discrimination of leather samples related to forensic science by applying confocal 3D-XRF method. The laboratory made confocal 3D-XRF has a spatial resolution of about…
FIELD APPLICATIONS OF PXRF FOR CULTURAL HERITAGE DIAGNOSTICS: RAPID IN-FIELD ARCHAEOLOGICAL ANALYSES IN THE FAYNAN ANCIENT COPPER PRODUCTION ZONE, JORDANK. Bennallack, L. Hahn, T.E. Levy…Levy, Ph.D., Department of Anthropology, California Institute of Telecommunication and Information Technology, University of California, San Diego ABSTRACT The development of portable scientific instruments for characterizing archaeological mate…
HIGH RESOLUTION TRACE ELEMENT DISTRIBUTION AND STRUCTURE OF THE MUSSEL SHELL PERNA VIRIDIS FROM MANILA BAY, PHILIPPINESV.A. Innis-Samson, M. Mizusawa, K. Sakurai…XRD shows an amorphous structure for the green pigment on the surface followed immediately by an aragonite structure with a slight deviation from the reference data. Micro-XRF with 20 keV excitation energy shows the major elements Ca, Br and Sr …
IMPROVEMENT OF X-RAY REFLECTIVITY CALCULATIONS ON A MULTILAYERED SURFACEY. Fujii…However, the calculated result showed a strange phenomenon in that the amplitude of the oscillation due to interference effects increases in the case of a specific roughness of the surface. We proposed that the strange result has its origin in a…
METHODS FOR MOUNTING RADIOACTIVE POWDERS FOR XRD ANALYSISL.N. Squires, R.D. Mariani, T. Hartmann, J.R. Kennedy…Since these materials are easily dispersed, it is not possible to prepare them for analysis in a standard laboratory fume hood or on a laboratory bench top. The materials must be contained to ensure that no radioactive contamination is released …
MICRO X-RAY BEAM PRODUCED WITH A SINGLE GLASS CAPILLARY FOR XRF ANALYSISS. Komatani, S. Hirano, T. Aoyama, Y. Yokota, H. Ueda, K. Tsuji…Kisshoin-Miyanohigashi-cho, Minami-ku, Kyoto, Kyoto 601-8510, Japan ABSTRACT XRF analysis is available for the quantification of elements and provides a great advantage in material science. Although XRF analysis has the advantage of nondestructi…
MOXTEK.S NEW ULTRA-LITE X-RAY SOURCES: PERFORMACE CHARACTERIZATIONSS. Cornaby, S. Morris, J. Smith, D. Reynolds, K. Kozaczek…The characterization test fall into three categories: environmental stress, X-ray flux and spot stability and repeatability, and a multi-settings evaluation. Examples are given of data collected from these characterization tests from evaluation …
MULTI LENGTH SCALE CHARACTERISATION OF AUSTENITE IN TRIP STEELS USING HIGH-ENERGY X-RAY DIFFRACTIONR. Blondé, E. Jimenez-Melero, L. Zhao, J.P. Wright, E. Brück, S. van der Zwaag, N.H. van Dijk…The stability of austenite has been studied at different length scales during tensile tests and at variable temperatures down to 153 K. A powder diffraction analysis has been performed to correlate the macroscopic behavior of the material to the…
NANOCRYSTALLINE ZINC OXIDE POWDER FOR X-RAY DIFFRACTION METROLOGYJ.P. Cline, J.J. Ritter, D. Black, J.E. Bonevich, A. Henins…The size of the crystallites is determined by the specifics of the thermal processing which were chosen to yield crystallites in two size ranges, one with a distribution centered at approximately 15 nm and another centered at 70 nm. The resultin…
PHASE TRANSITION BEHAVIOR OF A PROCESSED THERMAL BATTERYJ.J.M. Griego, M.A Rodriguez, D.E. Wesolowski…The transition of interest in this paper is the formation of Li7Si3 from Li13Si4 (initial anode material). The unit cell conditions during Li13Si4 transition to Li7Si3 show a contraction of 0.04 and 0.02 Å (a and b-axis respectively), an expansi…
PROBING LARGE WAVEVECTOR PHONONS AT THE NANOSCALE VIA X-RAY THERMAL DIFFUSE SCATTERINGG. Gopalakrishnan, M.V. Holt, K.M. McElhinny, D.A. Czaplewski, P.G. Evans…Experimental probes for phonons with large wavevectors have been largely based on inelastic x-ray and neutron scattering. The signals of inelastic scattering techniques become impractically weak in small ensembles of nanoscale objects, which pos…
QUICK X-RAY REFLECTIVITY OF SPHERICAL SAMPLESK. Stoev, K. Sakurai…This new setup for quick X-ray reflectivity allows measurements to be done within seconds, thus permitting studies of the time evolution of chemical, thermal, and mechanical changes at the surfaces and interfaces of different materials. Since th…
SELECTED APPLICATIONS OF RIETVELD-XRD ANALYSIS FOR RAW MATERIALS OF THE ALUMINUM INDUSTRYF.R. Feret…XRD quantitative phase analysis in the aluminum industry witnessed a steady deployment of the Rietveld method, which at present progressively replaces existing methodologies in research and plant laboratories. Rietveld analysis not only helped t…
SYNTHESIS AND CRYSTALLOGRAPHIC STUDY OF CATION SUBSTITUTED NZP MATERIALS: NA1+XZR2-XMXP3O12 (M=SB, AL, CR AND X=0.1)R. Chourasia, O.P. Shrivastava…It was found that large number of hazardous cations could be loaded in NZP based matrix without significant change of three-dimensional framework structure. Starting from the raw powder diffraction data of polycrystalline solid phases, crystal s…
THE STRUCTURAL CHARACTERIZATION OF A NEW FORM OF CLENBUTEROL, A WELL KNOWN DECONGESTANT AND BRONCHODILATOR ALSO USED AS A PERFORMANCE-ENHANCING DRUGR. Toro, J. Bruno-Colmenárez, G. Díaz de Delgado, J.M. Delgado…Unidad de Caracterización Estructural de Materiales, Instituto Zuliano de Investigaciones Tecnológicas (INZIT), La Cañada, Zulia, Venezuela. ABSTRACT Clenbuterol hydrochloride is an active pharmaceutical ingredient usually prescribed for the tre…
TILT-A-WHIRL: A TEXTURE ANALYSIS PACKAGE FOR 3D RENDERING OF POLE FIGURES USING MATLABM.A. Rodriugez, M.R. Pearl, M.H. Van Benthem, J.J.M. Griego, J. Pillars…The software routines facilitate phase identification, texture analysis via pole figure visualization, and macrostrain determination. The use of principal component analysis with multivariate curve resolution (PCA/MCR) revealed the extraction of…
USE OF THE RIETVELD METHOD FOR DESCRIBING STRUCTURE AND TEXTURE IN XRD DATA OF DOLOMITE [CAMG(CO3)2] AND HYDROMAGNESITE [MG5(CO3)4(OH)2(H2O)4] POWDERSH. Sitepu, Rasha A. Al-Ghamdi…The results showed that the structural parameters along with the bond lengths agree reasonably well with the single-crystal XRD results. Also, the Rietveld refinement provided reasonable fits for the uniaxially-pressed dolomite and hydromagnesit…
X-RAY DIFFRACTION IMAGING FOR PREDICTIVE METROLOGY OF CRACK PROPAGATION IN 450MM DIAMETER SILICON WAFERSB.K. Tanner, J. Wittge, P. Vagovič, T. Baumbach, D. Allen, P.J. McNally, R. Bytheway, D. Jacques, M.C. Fossati, D.K. Bowen, J. Garagorri, M.R. Elizalde, A.N. Danilewsky…University of Freiburg, Kristallographie, Geowissenschaftliches Institut, Freiburg, Germany 3Karlsruhe Institute of Technology, Institut für Synchrotronstrahlung, Karlsruhe, Germany 4Dublin City University, School of Electronic Engineering, Dubl…
XRAY FLUORESCENCE ASSISTED, MULTISPECTRAL IMAGING OF HISTORIC DRAWINGSS. Stout, F. Kuester, M. Seracini…This information, provides a critical step towards establishing the genesis of an artifact as well as its current state of conservation. A major challenge that remains is the accurate calibration and subsequent fusion of the different data asset…
XRF ANALYSIS OF HIGH GAIN-ON-IGNITION SAMPLES BY FUSION METHOD USING FUNDAMENTAL PARAMETER METHODM. Watanabe, H. Inoue, Y. Yamada, M. Feeney, L. Oelofse, Y. Kataoka…This report describes a FP method for the analysis of non-oxide samples such as metals made into fusion beads. During the fusion process, all non-oxide elements in the sample are oxidized and gain on ignition (GOI) occurs. Volatile elements such…
XRF SENSITIVITY IMPROVEMENT WITH A NOVEL CAPACITIVE CONCENTRATION CELLC. Bupp, D. Dietrich…This method relies upon the fundamental principles of capacitive deionization, where an electrical double-layer capacitor is used to temporarily capture dissolved ions in a semi-selective manner. The efficiency and capacity of an electrical doub…

2011 – VOL55

A SOFTWARE FOR DIFFRACTION STRESS FACTOR CALCULATIONS FOR TEXTURED MATERIALSThomas Gnäupel-Herold…All grain-interaction models that can use the crystallite orientation distribution function (ODF) are incorporated, including Kröner, Hill, inverse Kröner, and Reuss. The functions of the software include: reading the ODF in common textual forma…
AN INVESTIGATION OF THE ACCURACY OF DIFFRACTION STRESS EVALUATION OF TEXTURED MATERIALST. Gnäupel-Herold, A. Creuziger, M.A. Iadicola…Most x-ray diffractometers can be used to perform a measurement of lattice strain vs. tilt angle, which is then converted into stress. The apparent simplicity of the conversion (the sin2ø law comes to mind) betrays the fact that elastic and plas…
ANALYSIS OF TCLP EXTRACTS BY X-RAY FLUORESCENCED.S. Kendall, B.A. Burns, J.A. Suggs, J.J. Mackey…Environmental Protection Agency (EPA) to determine if a waste material is hazardous; the TCLP test is widely used by the environmental testing community. The elements of concern for toxicity are arsenic, barium, cadmium, chromium, lead, mercury,…
CALIBRATION OF X-RAY IMAGING DEVICES FOR ACCURATE INTENSITY MEASUREMENTM.J. Haugh, M. Charest, P. Ross, J. Lee, M. Schneider, N. Palmer, A. Teruya…The X-ray sources that are used for calibration are both diode type and diode/fluorescer combinations. Calibrating the X-ray detectors is key to accurate calibration of the X-ray sources. Both energy dispersive detectors and photodiodes measurin…
COMPUTER-AIDED ENGINEERING DESIGN OF HTXRD RESISTIVE HEATING STRIPS TO MINIMIZE SAMPLE TEMPERATURE GRADIENTSR. Chandrasekaran, A.R. Drews…Typically, HTXRD stages use a resistive heating strip, where the ends that form the electrical current contacts are maintained near ambient temperature. Because of thermal conduction to the current contacts, the temperature distribution along th…
DESIGN AND MEASUREMENT WITH A NEW PORTABLE X-RAY CAMERA FOR FULL-FIELD FLUORESCENCE IMAGINGI. Ordavo, A. Bjeoumikhov, S. Bjeoumikhova, G. Buzanich, R. Gubzhokov, R. Hartmann, S. Ihle, N. Langhoff, A. Liebel, M. Radtke, U. Reinholz, H. Riesemeier, O. Scharf, H. Soltau…München, Germany 2PNDetector GmbH, Emil-Nolde-Str. 10, 81735, München, Germany 3IFG – Institute for Scientific Instruments GmbH, Rudower Chaussee 29/31, 12489 Berlin, Germany 4BAM Federal Institute for Materials Research and Testing, 12200 Berli…
DEVELOPMENT AND EVALUATION OF A NEW SAXS SYSTEM FOR BIOLOGICAL SAMPLESN. Suzuki, K. Sasaki, A. Criswell, J.D. Ferrara, L. Jiang, M. Degen…More recently SAXS has been recognized as a complementary tool for extracting structural information from biological systems where X-ray crystallographic methods have failed. SAXS is also considered a useful tool to study behavior of a macromole…
DEVELOPMENT OF 2D DISPERSIVE DEVICE FOR XRF IMAGING SPECTROMETERT. Ohmori, M. Hatayama, H. Takenaka, K. Tsuji…Usually, scanning-type elemental mapping is performed. That means, a sample stage is scanned to a fixed X-ray micro beam. XRF analysis is performed at the scanned points, leading to 2D elemental mapping. One of the drawbacks of this technique is…
DEVELOPMENT OF A PALM-SIZE ELECTRON PROBE X-RAY ANALYZERS. Imashuku, A. Imanishi, J. Kawai…Energy of obtained continuous X-rays and lower limits of detection of transition metals (titanium, iron, and nickel) were evaluated. End point energy (Duane-Hunt limit) of obtained continuous X-rays was about 40 keV, but the palm-size EPMA can a…
ELECTROLYTIC PHASE EXTRACTION: AN OLD TECHNIQUE TO EVALUATE PRECIPITATES IN NITINOLR.G. Baggerly…The shape memory effect results from a reversible martensitic phase transformation. An increasing solubility range with temperature on the Ni rich side can produce a precipitation reaction resulting in a slight matrix composition adjustment with…
EXPERIMENT VERIFICATION FOR THE DEPENDENCE OF THE X-RAY DIFFRACTION LINE PROFILEWITH THE ABSORPTION OF SAMPLEK. Liu, H. Chen…It was supposed that the line profile is broadened by the size of the crystalline, and also broadened by instrument. We proposed recently, (Kejia Liu et al, Adv. in X-ray analysis, 54, 17(2010) that there is still another effect which broadenin…
FAST ELEMENTAL MAPPING WITH MICRO-XRFM. Haschke, U. Rossek, R. Tagle, U. Waldschläger…New components like X-ray tubes with high brilliance, optics with better transmission efficiency and detectors with high count rate capability offer possibilities for improvement in the analytical performance of these instruments. This paper dis…
FEASIBILITY OF SUB-MICRON XRF COMBINED TO SCANNING PROBE MICROSCOPYM. Dehlinger, C. Fauquet, F. Jandard, A. Bjeoumikhov, A. Erko, I. Zizak, S. Ferrero, D. Pailharey, B. Dahmani, D. Tonneau…Corresponding author: Prof D. Tonneau tonneau@cinam.univ-mrs.fr ABSTRACT In-lab high lateral resolution XRF tools are needed, mainly in the field of microelectronics and solar cell industries, as non destructive in-depth chemical analysis equipm…
GUNSHOT RESIDUE INVESTIGATIONS USING TXRFAlexander Wastl, Bettina Bogner, Peter Kregsamer, Peter Wobrauschek, Christina Streli…It is very important for a police investigation at a crime scene to gain as much information from such residues as possible. Due to the minute amounts of residue available, total reflection x-ray fluorescence analysis (TXRF) seems well suited fo…
IMPROVEMENT OF DETECTION LIMITS OF A PORTABLE TXRF BY REDUCING ELECTRICAL NOISES. Imashuku, D.P. Tee, Y. Nakae, J. Kawai, Osami Wada…Spectral background of the TXRF spectrometer decreased by keeping the detector away from analog-to-digital convertor, electromagnetic shielding of X-ray tube with ethylene propylene electric conductive rubber tape, and grounding all instrument c…
IN SEARCH FOR A REFINABLE MODEL OF NANOCRYSTALSB. Palosz…The appropriate technique for structural analysis of nanocrystals is powder diffraction. Parameters that are derived from routine diffraction studies (crystal phase, lattice parameters, size, strain, etc.) do not necessarily contain any informat…
MICROSTRUCTURE OF THE PLASTIC BONDED EXPLOSIVE KS32M. Herrmann, P.B. Kempa, U. Förter-Barth, W. Arnold…Different non-destructive diffraction techniques such as rocking curve imaging were applied in order to characterize the microstructure and ingredients of PBX KS32, including its behavior in shock-loading tests. The investigations revealed a sig…
MULTIVARIATE STATISTICAL ANALYSIS OF MICRO-XRF SPECTRAL IMAGESM.A. Rodriguez, P.G. Kotula, J.J.M. Griego, J.E. Heath, S.J. Bauer, D.E. Wesolowski…The separation of components into individual histograms enables separation of overlapping peaks, which is useful in qualitatively determining the presence of chemical species that have overlapping emission lines, and holds potential for quantita…
ON THE USE OF MONTE CARLO BASED METHODS TO EDXRF QUANTITATIVE ANALYSISkozul…An elemental stratified sampling variance reduction technique has been implemented in the CEARXRF code (version 5). In this case it refers to using the same number of histories for each element X-ray spectrum so that the same statistics are appr…
QUANTITATIVE XRD BULK AND CLAY MINERALOGICAL DETERMINATION OF PALEOSOL SECTION OF UNAYZAH AND BASAL KHUFF CLASTICS IN SAUDI ARABIAS. Shen, S.R. Zaidi, B.A. Mutairi, A.A. Shehry, S.A. Hamoud, F.S. Khaldi, F.A. Edhaim, H. Sitepu…Quantitative XRD bulk mineralogical determination was achieved using Rietveld refinement method whereas Quantitative XRD clay mineralogical determination of clay-size fraction was obtained using RIR method. The XRD results indicate that the samp…
RIETVELD QUANTITATIVE ANALYSIS OF SUPER DUPLEX STAINLESS STEELJ.L. Garin, R.L. Mannheim…The thermal processing of the samples proceeded at temperatures in the range from 1073 K to 1223 K for periods of time from 1 to 96 h. This procedure permitted an accurate quantification of the microstructural components such as austenite, ferri…
STEPS TOWARD ACCURATE LARGE AREA ANALYZES OF GENESIS SOLAR WIND SAMPLES: EVALUATION OF SURFACE CLEANING METHODS USING TOTAL REFLECTION X-RAY FLUORESCENCE SPECTROMETRYMartina Schmeling*1, Donald S. Burnett 2, Amy J.G. Jurewicz3, Igor V. Veryovkin4…The Genesis mission collected solar wind during a period of 854 days by embedding the charged particles into collectors made of various ultra clean materials such as silicon, sapphire and silicon-on-sapphire. The sample return capsule unexpected…
STRATEGY OF FUSION BEAD CORRECTION IN XRF ANALYSIS OF POWDERSH. Homma, H. Inoue, M. Feeney, L. Oelofse, Y. Kataoka…These calibrations include matrix effects, weighing inaccuracies, loss on ignition (LOI), gain on ignition (GOI), decomposition of oxidizing agent and evaporation of flux. The corrections for these common sources of error in the fusion method ar…
STRESSES IN YTTERBIUM SILICATE MULTILAYER ENVIRONMENTAL BARRIER COATINGSF. Stolzenburg, J. Almer, K.N. Lee, B.J. Harder, K.T. Faber…Harder Durability and Protective Coatings Branch, NASA Glenn Research Center, Cleveland, OH 44315 K.T. Faber Northwestern University, Department of Materials Science and Engineering, Evanston, IL 60208 The internal stresses of plasma-sprayed mul…
STRUCTURE DETERMINATION OF THE SILVER CARBOXYLATE DIMER [AG(O2C20H39)]2, SILVER ARACHIDATE, USING POWDER X-RAY DIFFRACTION METHODSP.W. Stephens, J.A. Kaduk, T.N. Blanton, D.R. Whitcomb, S.T. Misture, M. Rajeswaran…Dearborn, Chicago, IL 60616, USA c Eastman Kodak Company, Research Laboratories, Rochester, NY 14650-2106, USA d Carestream Health, 1 Imation Way, Oakdale, MN 55128, USA e Alfred University, New York State College of Ceramics, Alfred, NY 14802, …
SURFACE RELAXATION IN NANO-DIAMONDS EXAMINEDWITH APPLICATION OF THE REAL AND RECIPROCAL SPACE METHODSS. Stelmakh, E. Grzanka, S. Gierlotka, B. Palosz…Both real (PDF) and reciprocal (Bragg) space analyses were employed to examine a tentative core-shell model of nanodiamond grains. Elaboration of diffraction data was based on the concept of the “apparent lattice parameters” (alp) calculated for…
SYNCHROTRON X-RAYMICROBEAM CHARACTERIZATION OF SMECTIC A LIQUID CRYSTALS UNDER ELECTRIC FIELDA. Iida, Y. Takanishi…The layer shrinkage due to the tilted smectic arrangement is mitigated by local layer deformation. This paper presents detailed measurements of the local layer spacing under the electroclinic effect of the chiral SmA phase in a surface-stabilize…
THE POSSIBILITY OF USING HANDHELD XRF IN CEMENT APPLICATIONSkozul…Results are discussed for measurements of powders, pressed pellets, and unprepared rock samples. Variations in calibration assumptions are also discussed, which allow better tailoring of a calibration to measurement of different matrices. INTROD…
UNDERSTANDING STRESS GRADIENTS IN MICROELECTRONIC METALLIZATIONC.E. Murray, E.T. Ryan, P.R. Besser, C. Witt, J.L. Jordan-Sweet, M.F. Toney…Watson Research Center, Yorktown Heights, NY. 5Stanford Synchrotron Radiation Lightsource, Menlo Park, CA ABSTRACT The manufacture of ultra-large scale integration technology requires many thermal cycles that can impose significant strain within…
USE OF MONTE CARLO SIMULATION METHODS TO IMPROVE X-RAY DETECTOR RESPONSE FUNCTIONkozul…A semi-empirical detector response function using Gaussian peak models and exponential tails was used to characterize the detector response functions. And the use of Monte Carlo method to simulate the detector response has been developed to pred…
USE OF THE RIETVELD METHOD FOR DESCRIBING STRUCTURE AND TEXTURE IN XRD DATA OF DOLOMITE [CAMG(CO3)2] AND HYDROMAGNESITE [MG5(CO3)4(OH)2(H2O)4] POWDERSH. Sitepu…The results showed that the structural parameters along with the bond lengths agree reasonably well with the single-crystal XRD results. Also, the Rietveld refinement provided reasonable fits for the uniaxially-pressed dolomite and hydromagnesit…
USING IN-SITU TECHNIQUES TO PROBE HIGH TEMPERATURE REACTIONS: THERMOCHEMICAL CYCLES FOR THE PRODUCTION OF SYNTHETIC FUELS FROM CO2 ANDWATERE.N. Coker, M.A. Rodriguez, A. Ambrosini, J.E. Miller, E.B. Stechel…Such cycles utilize solar-thermal energy to reduce the metal oxide, which is then re-oxidized by H2O or CO2, producing H2 or CO, respectively. Mixing ferrites with zirconia or yttria-stabilized zirconia (YSZ) greatly improves their cyclability. …
X-RAY DIFFRACTION CHARACTERIZATION OF NEW TERNARY YTTRIUM.RARE EARTH OXIDES FORMED BY THE SOL.GEL TECHNIQUEG. Rafailov, Z. Porat, I. Dahan, R. Zach, G. Kimmel, D. Mogilyansky, K. Rechav, J. Zabicky…These were divided into two groups, each composed of the same elements but at different stoichiometric ratios; the first one included Y2EuErO6, YEu2ErO6, and YEuEr2O6, and the second included Y2EuHoO6, YEu2HoO6 and YEuHo2O6. The compounds were s…
X-RAY DIFFRACTION CHARACTERIZATION OF POLYMER INTERCALATED GRAPHITE OXIDET.N. Blanton, D. Majumdar…The oxidation of graphite results in the formation of epoxide groups as well as C-OH and COOH groups. It is the presence of some of these moieties that allows GO to be dispersed in water, allowing for its use in waterborne formulations. Although…
X-RAY MEASUREMENTS OF NANOMETER THICK TAXO1-X AND HFXO1-X FILMS ON SILICON SUBSTRATES FOR THICKNESS AND COMPOSITION DETERMINATIONF.J. Cadieu, I. Vander, Y. Rong, R.W. Zuneska…Sponsored by the International Centre for Diffraction Data (ICDD). This document is provided by ICDD in cooperation with the authors and presenters of the DXC for the express purpose of educating the scientific community. All copyrights for the …

2010 – VOL54

A MULTIDIMENSIONAL INVESTIGATION USING X-RAY DIFFRACTION AND COMPUTED TOMOGRAPHYH. Pöllmann, R. Meier, G. Blaj, U. Riedl…INTRODUCTION Classical X-ray investigations of mortar and concrete bars in laboratory can show phases, phase distributions and even quantification of occurring phases. The new technique now provides the possibility of evaluation of microstructur…
A NOVEL SAMPLE PRESSING TECHNIQUE TO REDUCE PREFERRED ORIENTATION USING THE BACK-PRESSED PRESENTATION METHODCopyright ©JCPDS-International Centre for Diffraction Data 2011 ISSN 1097-0002…In Bragg-Brentano geometry the avoidance of preferred orientation, sample displacement and surface roughness would be goals of any sample presentation technique. A mixture of 90 wt% gypsum and 10 wt% corundum was prepared by miconising in a McCr…
ADVANTAGES AND DISADVANTAGES OF BAYESIAN METHODS FOR OBTAINING XRF NET INTENSITIESW.T. Elam, B. Scruggs, F. Eggert, J. Nicolosi…The method has several advantages, among them that the total counts are preserved and that the a priori information is incorporated in a natural manner. These make it, for example, less sensitive to errors in the peak position, widths, and alpha…
ALTERNATIVE STRATEGIES FOR XAFS DATA ANALYSIS USING FEFF AND MATHEMATICA 7Copyright ©JCPDS-International Centre for Diffraction Data 2011 ISSN 1097-0002…Its primary use has been in supporting a path by path analysis of experimental data using auxiliary programs such as IFEFFIT, Artemis, SixPack, etc. In this paper several alternative strategies for XAFS analysis that combine FEFF and Mathematica…
ASSESSING THE ENVIRONMENT WITH X-RAY FLUORESCENCE SPECTROMETRYJ. Boman, J.B.C. Pettersson, M. Gatari, A. Wagner, P. Molnar…Box 30197-00100, Nairobi, Kenya 3Department of Applied Physics, Chalmers University of Technology, SE-412 96 Gothenburg, Sweden Department of Occupational and Environmental Medicine, Sahlgrenska University Hospital & University of Gothenburg, Bo…
BINDING OF MN-DEOXYRIBONUCLEOSIDE TRIPHOSPHATES TO THE ACTIVE SITE OF THE DNA POLYMERASE OF BACTERIOPHAGE T7B. Akabayov, C.C. Richardson…Mg2+, as an example, mediates binding of deoxyribonucleoside 5′-triphosphates followed by their hydrolysis in the active site of DNA polymerase. It is difficult to study the binding of Mg2+ to an active site because: 1) Mg2+ is spectroscopically…
CALCULATED POWDER X-RAY DIFFRACTION LINE PROFILES VIA ABSORPTIONK. Liu, H. Chen…The results showed that the line profile function depends on the absorption coefficient of the sample. The observed aluminum PXRD patterns are in excellent agreement with the calculated line profile functions derived from absorption. This work a…
COMPOSITION AND LAYER THICKNESS OF COPPER-INDIUMGALLIUM- SELENIUM AND MOLYBDENUM LAYERS ON GLASS BY XRAY FLUORESCENCE SPECTROSCOPYL.L. Brehm, T.T. Hasan, D.A. Libby, T.R. Bryden…One such application is the evaluation of copper-indium-gallium-selenium (CIGS) on molybdenum (Mo) coated glass substrates to support solar cell research and development efforts. Several analytical technologies are available for elemental analys…
DEVELOPMENT OF AN IN SITU X-RAY DIFFRACTION SYSTEM FOR HYDROTHERMAL REACTIONS AND ITS APPLICATION TO AUTOCLAVED AERATED CONCRETE FORMATIONJ. Kikuma, M. Tsunashima, T. Ishikawa, S. Matsuno, A. Ogawa, K. Matsui…The system includes a novel autoclave cell for transmission XRD with thin beryllium windows, a two-dimensional photon-counting pixel array detector, and uses high energy X-rays from a synchrotron radiation source. The temperature and pressure in…
ENHANCEMENT OF XRF INTENSITY BY USING AU COATED GLASS-CAPILLARYT. Nakazawa, K. Nakano, M. Yoshida, K. Tsuji…Au was electroplated on an inner wall of the glass-capillary with a thickness of 100 nm. The Au coated glass-capillary was attached to a micro focus x-ray tube. The XRF intensity from the pure metal samples was measured by a silicon drift x-ray …
EVOLUTION OF TEXTURE AND DISLOCATION DISTRIBUTIONS IN HIGH-DUCTILE AUSTENITIC STEEL DURING DEFORMATIONS. Sato, T. Yoshimura, N. Yamada, K. Wagatsuma, S. Suzuki…K. ABSTRACT Fe-Mn-C austenitic steels exhibit outstanding high-ductile deformation in their plastic regions along with significant microstructural evolution. In this study, to characterize the microstructural evolution during deformation of thes…
GLANCING INCIDENCE XRF FOR THE ANALYSIS OF EARLY CHINESE BRONZE MIRRORSR.W. Zuneska, Y. Rong, I. Vander, F.J. Cadieu…The mirrors were archived to be from either 200 BCE-200 CE and from approximately the 800 CE period. Glancing incidence X-Ray excitation proofed highly useful for obtaining the elemental composition from the fluorescence measure. Measure of the …
GLANCING XRD AND XRF FOR THE STUDY OF TEXTURE DEVELOPMENT IN SMCO BASED FILMS SPUTTERED ONTO SILICON SUBSTRATESF.J. Cadieu, I. Vander, Y. Rong, R.W. Zuneska…The films formed a disordered TbCu7-type structure for a range of Sm concentrations with an accompanying variation in the crystallite lattice parameters. Since in a film the θ positions of the X-ray diffraction lines stayed constant, it is reas…
GLOBAL CEMENT AND RAW MATERIALS FUSION/XRF ANALYTICAL SOLUTION: PART 2M. Bouchard, J. Anzelmo, S. Rivard, A. Seyfarth, L. Arias, K. Behrens, S. Durali-Müller…The results of two well known cement chemical analysis Standard Methods were also presented. These results proved that this robust analytical method is able to qualify by the ASTM C 114 [2] and ISO/DIS 29581-2 [3] norms. This robust analytical m…
IMPROVED MATERIAL IDENTIFICATION METHODS THROUGH TARGETED DATA MININGT.G. Fawcett, C.E. Crowder, S.N. Kabekkodu, J.A. Kaduk…The data mining attempts to intelligently mimic the thought process of experts in materials and analytical methods to combine several “data clues” for a successful identification process. The clues can come from the diffraction experiment, but a…
IN SITU HIGH-TEMPERATURE X-RAY DIFFRACTION CHARACTERIZATION OF SILVER SULFIDE, AG2ST. Blanton, S. Misture, N. Dontula, S. Zdzieszynski…The mineral acanthite is a monoclinic crystalline form of Ag2S that is stable to 176 ºC. Upon heating above 176 ºC, there is a phase conversion to a body- centered cubic (BCC) form referred to as argentite. Further heating above 586 ºC results i…
IN SITU MEASUREMENTS REVEAL PHASE AND TEXTURE EVOLUTION IN SOLUTION DEPOSITED PZT THIN FILMSK. Nittala, G.L. Brennecka, D.S. Robinson, J.L. Jones…The transient/intermediate phases present in the thin film during perovskite phase nucleation have been suggested to cause this variation in texture with heating rate. To understand the interrelationship between the transient/intermediate phases…
IN SITU TIME-RESOLVED X-RAY DIFFRACTION OF TOBERMORITE FORMATION PROCESS UNDER HYDROTHERMAL CONDITION: INFLUENCE OF REACTIVE AL COMPOUNDK. Matsui, A. Ogawa, J. Kikuma, M. Tsunashima, T. Ishikawa, S. Matsuno…High-energy X-rays from a synchrotron radiation source in combination with a newly developed autoclave cell and a photon-counting pixel array detector were used. XRD measurements were conducted in a temperature range of 100190 °C throughout 12 …
IN-SITU OBSERVATION OF ERD2 FORMATION DURING D2 LOADING VIA NEUTRON DIFFRACTIONM.A. Rodriguez, C.S. Snow, R.R. Wixom, A. Llobet, J.F. Browning…This experiment tracked the conversion of Er metal to the α erbium deuteride (solid-solution) phase and then on to the β (fluorite) phase. Complete conversion to ErD2.0 was accomplished at 10 Torr D2 pressure with deuterium fully occupying the t…
INVESTIGATION OF MICROSTRUCTURAL CHANGES IN IMPACTED POLYUREA COATINGS USING SMALL ANGLE X-RAY SCATTERING (SAXS)E. Balizer, J. Fedderly, G. Lee, W. Mock, Jr., S. Bartyczak…The polyurea layer of the post mortem bilayers was characterized on a molecular level by Small Angle Synchrotron X-ray Scattering (SAXS) at the Avdanced Photon Source at Argonne National Lab. Analysis revealed that hard domains of the polyureas …
MACROSCOPIC X-RAY FLUORESCENCE CAPABILITY FOR LARGESCALE ELEMENTAL MAPPINGH.M. Volz, G.J. Havrilla, R.M. Aikin, Jr., V.M. Montoya…These elemental differences across a part have a huge impact on materials properties so that identifying variations will help industry immensely with process optimization and quality control. Therefore, a nondestructive method of obtaining spati…
MULTIALIQUOT CELL APPROACH FOR STRUCTURE DETERMINATION FROM POWDER DIFFRACTION OF HIGH SYMMETRY COMPOUNDSCopyright ©JCPDS-International Centre for Diffraction Data 2011 ISSN 1097-0002…Application of aliquot cells as building units for the larger cell of high symmetry is expected to facilitate the structure solution with direct space methods, in order to decrease time for the model search in a large-scale unit cell. Indexing a…
NEAR-SURFACE IN-VITRO STUDIES OF PLASMA SPRAYED HYDROXYAPATITE COATINGST.P. Ntsoane, M. Topic, R. Bucher…Subsequent to spraying, the samples were incubated in simulated body fluid for periods varying from 1 and 56 days. Quantitative phase analysis, employing TOPAS software, showed an opposite trend in the two main phases in the coating viz. HAp and…
STANDARD REFERENCE MATERIAL 660B FOR X-RAY METROLOGYD.R. Black, D. Windover, A. Henins, J. Filliben, J.P. Cline…This report describes SRM 660b, the third generation of this powder diffraction SRM used primarily for determination of the Instrument Profile Function (IPF). It is certified with respect to lattice parameter. It consists of approximately 6 g La…
STRAIN-INDUCED TEXTURE DEVELOPMENT IN THE MAGNESIUM ALLOY AZ31S. Huang, D. Li, Y. Peng, J. Allison…Understanding the formability of lightweight alloys is one key to their successful introduction in vehicles. We present results of X-Ray diffraction and electron back-scatter diffraction texture measurements in as-cast and uniaxially compressed …
STRUCTURAL REFINEMENT OF BAXSR1-XSO4 USING X-RAY POWDER DIFFRACTION DATAH. Sitepu, S.R. Zaidi…X-ray powder diffraction (XRD) data of the fused barium-strontium sulfate powders were measured using a powder diffractometer with a copper X-ray tube. The XRD data were refined using Rietveld analysis with generalized spherical harmonic descrip…
THE STRUCTURE OF MARIALITE (ME6) AND MEIONITE (ME93) IN SPACE GROUPS P42/N AND I4/M, AND THE ABSENCE OF PHASE TRANSITIONS IN THE SCAPOLITE SERIESS.M. Antao, I. Hassan…Vesuvius, Italy was obtained using synchrotron high-resolution powder X-ray diffraction (HRPXRD) data and Rietveld structure refinements. Their structure was refined in space groups I4/m and P42/n, and similar results were obtained. The Me6 samp…
TRACE ELEMENT ANALYSIS USING EDXRF WITH POLARIZED OPTICST. Moriyama, S. Ikeda, M. Doi, S. Fess…Accurate analysis down to ppm level can be achieved even in complex sample composition with the quantification software. The scattering FP method corrects for non-measuring components in samples such as coal fly ash, soils and biological samples…
ULTRATHIN LAYER DEPOSITIONS . A NEW TYPE OF REFERENCE SAMPLES FOR HIGH PERFORMANCE XRF ANALYSISM. Kraemer, R. Dietsch, Th. Holz, D. Weißbach, G. Falkenberg, R. Simon, U. Fittschen, T. Krugmann, M. Kolbe, M. Müller, B. Beckhoff…D-22603 Hamburg, Germany; 3) Institute for Synchrotron Radiation, FZ Karlsruhe, Hermann-von-Helmholtz-Platz 1, D-76344 Eggenstein, Germany; 4) Institute for Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg, G…
WASTE REDUCTION AND PROCESS IMPROVEMENTS IN THE ANALYSIS OF PLUTONIUM BY X-RAY FLUORESCENCE: RESULTS FROM MULTIPLE DATA SETSC.G. Worley, C.B. Soderberg, L.E. Townsend…These changes included reducing sample sizes, reducing ion exchange process volumes, using cheaper reagent grade acids, eliminating the use of HF acid, and using more robust containment film for sample analysis. Relative precision and accuracy a…
XAFS STUDIES OF NI, TA AND NB CHLORIDES IN THE IONIC LIQUID 1-ETHYL-3- METHYL IMIDAZOLIUM CHLORIDE / ALUMINUM CHLORIDEW.E. O’Grady, D.F. Roeper, K.I. Pandya, G.T. Cheek…In order to understand the interactions of these metal ions with ionic liquids, we have investigated their structures in situ with X-ray Absorption Spectroscopy (XAS). The ionic liquid used in this study is 1-methyl-3-ethylimidazolium chloride (…
XRD ANISOTROPIC BROADENING OF NANO-CRYSTALLITESY. Wang, S.L.I. Chan, R. Amal, Y.R. Shen, K. Kiatkittipong…In such a case, the crystallite size must be described by multi-dimensional lengths, possible with a polar orientation. Experiments on β-Ni(OH)2, β-TiO2 and anatase were carried. Results show that the model can explain the characteristics of nan…

2009 – VOL53

ABSOLUTE THICKNESS DETERMINATION OF SMCO FILMS ON SILICON SUBSTRATES UTILIZING X-RAY DIFFRACTION AND THEIR COMPOSITION MEASUREMENTS BY EXRFI. Vander, R.W. Zuneska, F.J. Cadieu…X-Ray diffraction of Cu Kα radiation has been used to measure the intensity of the (400) reflection from bare silicon substrates and as attenuated by sputter coated Co and SmCo based films on Si substrates. A 4-axis research diffractometer allow…
APPLICATION OF A PORTABLE TXRF SPECTROMETER TO DETERMINE TRACE AMOUNTS OF TOXIC ELEMENTSS. Kunimura, J. Kawai…Although non-monochromatic X-rays from a 5 W X-ray tube (Tube voltage: 25 kV) are used, the trace amounts of these elements are detected. This portable spectrometer is applied to analysis of river water, a leaching solution of a toy, and a lipst…
APPLICATION OF X-RAY DIFFRACTION FOR RESIDUAL STRESS ANALYSIS ON CANADIAN NAVAL PLATFORMSS.P. Farrell, L.W. MacGregor…This is a significant concern for the Canadian Navy, where the superposition of applied stresses on residual stresses may adversely affect the performance, safe operational envelope and service life of naval structures. The ability to elucidate …
BIFOCAL MINIATURE TOROIDAL SHAPED X-RAY MIRRORSS. Cornaby, D.-M. Smilgies, D.H. Bilderback…At CHESS we traditionally use glass single-bounce monocapillary optics for a wide range of x-ray experiments to get a fine x-ray beam of 5 to 20 μm. This miniture toroidal mirror was prepared by designing and fabricating an x-ray focusing capil…
BRIDGING THE PRICE/PERFORMANCE GAP BETWEEN SILICON DRIFT AND SILICON PIN DIODE DETECTORSD. Hullinger, K. Decker, J. Smith, C. Carter…Increasing the thickness of PIN diodes (and, correspondingly, the thickness of the depletion region within the diode) significantly reduces the diode capacitance and results in improved performance. For example, the new Moxtek XPIN-6 detector (w…
CALCULATION METHODS OF X-RAY SPECTRA: A COMPARATIVE STUDYB. Chyba, M. Mantler, H. Ebel, R. Svagera…This paper discusses two calculation methods for tube spectra: an analytical program based on algorithms by H. Ebel and the MCNP software package based on Monte-Carlo code. The calculated data were also compared to measured spectra generated on …
CHARACTERIZATION OF AGING BEHAVIOR OF PRECIPITATES AND DISLOCATIONS IN COPPER-BASED ALLOYSS. Sato, Y. Takahashi, K. Wagatsuma, S. Suzuki…A small angle X-ray scattering (SAXS) method was used for characterizing the growth behavior of the precipitates with aging. The results showed that the precipitates grew gradually to a few nanometers in radius in the alloy aged under the condit…
COMBINED MULTIPLE-EXCITATION FP METHOD FOR MICRO-XRF ANALYSIS OF DIFFICULT SAMPLESW.T. Elam, B. Scruggs, J. Nicolosi…A primary beam filter is commonly used to eliminate diffractive artifacts as well as tube characteristic lines, but this dramatically reduces the sensitivity to lighter elements. One way around this is to collect a spectrum with unfiltered excit…
DUAL DETECTION X-RAY FLUORESCENCE CRYOTOMOGRAPHY AND -MAPPING ON THE MODEL ORGANISM DAPHNIA MAGNAB. De Samber, S.Vanblaere, R. Evens, K. De Schamphelaere, G. Wellenreuther, F. Ridouitt, G. Silversmit, T. Schoonjans, B. Vekemans, B. Masschaele, L. Van Hoorebeke, K. Rickers, G. Falkenberg, I. Szaloki, C. Janssen, L. Vincze…Szaloki, 2C. Janssen and 1L. Vincze 1X-ray Microspectroscopy andmaging (XMI), Ghent University, Krijgslaan 281, B-9000 Ghent, Belgium 2Laboratory of Environmental Toxicology and Aquatic Ecology, Ghent University, Jozef Plateaustraat 22, B-9000 G…
ENERGY-DISPERSIVE X-RAY FLUORESCENCE ANALYSIS OF MONOAND POLYCRYSTALS OF SELENIDE SPINELS BY FUNDAMENTAL PARAMETER METHODR. Sitko, B. Zawisza, E. Malicka…Zn+2, V+3, Ga+3) by energy-dispersive X-ray fluorescence spectrometry (EDXRF) is presented. The monocrystals of spinels (sizes from ca. 1 to 5 mm) were analyzed without any treatment. The polycrystals were powdered and pressed into pellets of 10…
EXPERIMENTAL PARAMETERS FOR XRFANALYSIS OF SOILSY. Imanishi, A. Bando, S. Komatani, S.-I. Wada, K. Tsuji…We investigated the influence of the thickness of soil layer, the grain size of soils, and the water content in soils on XRF intensity. Since high-energy XRF such as Cd Kα was detected in deep inside of soils, a thickness of 10 mm was recommende…
FUSION MONITORS FOR X-RAY FLUORESCENCE X ANALYSISD. Levesque, M. Bouchard, L. Bérubé…However, drift and bias contributions from the fusion technique, burner position, fluxer to fluxer, mould effects and other contributors were difficult to assess and quantify. The Fusion MonitorsTM from Claisse are introduced as a novel quality …
GLOBAL CEMENT AND RAW MATERIALS FUSION/XRF ANALYTICAL SOLUTIONM. Bouchard, J. Anzelmo, S. Rivard, A. Seyfarth, L. Arias, K. Behrens, S. Durali-Müller…This method was used to prepare all cements, all process materials, and a very large range of raw materials. The choice of all fusion parameters and all XRF analysis conditions, including calibration corrections, are shown. Two sets of reference…
HUMAN EXPOSURE TO LEAD AND NEW EVIDENCE OF ADVERSE HEALTH EFFECTS: IMPLICATIONS FOR ANALYTICAL MEASUREMENTSP.J. Parsons, K.G. McIntosh…The history of lead poisoning prevention has been defined to some extent by the quality of the analytical methods available for lead measurements, whether in environmental samples or biological tissues and fluids. The quality of blood lead metho…
IN-SITU ANALYSIS OF LIFEPO4 BATTERIES: SIGNAL EXTRACTION BY MULTIVARIATE ANALYSISM.A. Rodriguez, M.H. Van Benthem, D. Ingersoll, S.C. Vogel, H.M. Reiche…Multivariate analysis was successfully applied to the neutron diffraction dataset facilitating in the determination of Li bearing phases participating in the electrochemical reaction in both the anode and cathode as a function of state-of-charge…
INTERNAL STRESSES AND TEXTURE OF NANO-STRUCTURED ALUMINA SCALES GROWING ON FE3AL POLYCRYSTALSP. Brito, H. Pinto, M. Klaus, C. Genzel, A. Pyzalla…Berlin, Germany ABSTRACT The evolution of internal stresses in oxide scales growing on an Fe3Al polycrystal in atmospheric air at 700°C was determined using in-situ energy-dispersive synchrotron x-ray diffraction. Texture analyses were performe
LABORATORY-BASED CHARACTERIZATION OF HETEROEPITAXIAL STRUCTURES: ADVANCED EXPERIMENTS NOT NEEDING SYNCHROTRON RADIATIONP. Zaumseil, A. Giussani, T. Schroeder…This is demonstrated with epi-Germanium on Pr2O3 as buffer material. Pole figure measurements prove that epi-Ge layers grow nearly completely single crystalline with exactly the same in-plane orientation (type A) as the Si(111) substrate, while …
LATEST DEVELOPMENTS IN MICRO AND NANO TOMOGRAPHY AT PETRA IIIA. Haibel, F. Beckmann, T. Dose, J. Herzen, M. Oggureck, M. Müller, A. Schreyer…Novel applications of tomographic techniques allow for high speed in- situ measurements as well as the highest spatial and density resolutions. Additionally, the highly coherent beam enables the application of phase contrast methods in an except…
MINIATURE X-RAY SOURCES AND THE EFFECTS OF SPOT SIZE ON SYSTEM PERFORMANCED. Caruso, M. Dinsmore, S. Cornaby…The result is an x-ray spot that is not well described by a traditional Full Width Half Maximum (FWHM) type of measurement due to the irregular nature of the spots. This paper presents an alternate method called an intensity integral curve that …
MOLYBDENUM CONCENTRATES – COMBINING DEVELOPMENT OF AN XRF BORATE FUSION METHOD WITH CERTIFICATION OF STANDARD REFERENCE MATERIALSJ.R. Sieber, D.I. Lincoln…A new borate fusion approach for molybdenum concentrates has been developed by NIST for use in value assignments of two new Standard Reference Materials (SRMs®). The new borate fusion method is …
MONTE-CARLO SIMULATIONS FOR THE EVALUATION OF VARIOUS INFLUENCE FACTORS ON PROJECTIONS IN COMPUTED TOMOGRAPHYB. Chyba, M. Mantler, M. Reiter…The simulations were carried out by using custom software running on up to 50 nodes of a computer cluster. Comparative calculations were also made by using the software package MCNP (Booth et al., 2003). Tube spectra were calculated with algorit…
NANOSCALE STRAIN CHARACTERIZATION IN MICROELECTRONIC MATERIALS USING X-RAY DIFFRACTIONC.E. Murray, A.J. Ying, S.M. Polvino, I.C. Noyan, Z. Cai…An understanding of the mechanical response of the Si channel regions and their environment is key to the prediction and design of device operation. Because of the complexity of the composite geometries associated with microelectronic circuitry,…
OBSERVATIONS OF SHOCKED METAL SURFACES WITH SINGLE-PULSE X-RAY DIFFRACTIOND.V. Morgan, M. Grover, D. Macy, M. Madlener, G. Stevens, W.D. Turley…Box 5800, M/S 1193, Albuquerque, NM 87185 ABSTRACT A single-pulse X-ray diffraction (XRD) diagnostic has been developed for the investigation of shocked material properties on a very short time scale. The diagnostic, which consists of a 37-stage…
OPTIMIZING XRF CALIBRATION PROTOCOLS FOR ELEMENTAL QUANTIFICATION OF MINERAL SOLIDS FROM ATHABASCA OIL SANDSB. Patarachao, P.H.J. Mercier, J. Kung, J.R. Woods, L.S. Kotlyar, B.D. Sparks, T. McCracken…Bede Technical Associates, 614 Laverendrye Drive, Ottawa, ON, K1J 7C4 ABSTRACT As world reserves of conventional oil keep decreasing, there is greater incentive to further develop the Athabasca oil sands of Alberta (Canada). Oil sands being comp…
PREDICTION AND XRD MEASURING OF RESIDUAL STRESS IN MACHINED WELDED PARTSG. Rafailov, J. Sariel, I. Dahan, R. Reuven, M. Szanto…The measurements were done using both X-Ray diffraction and Hole-Drilling (HD) methods. A numerical simulation of the distribution of residual stress was applied in order to predict the behavior of the stress. The distributions obtained by X-Ray…
PRINCIPLES OF MICROSTRESS EQUILIBRIUM IN TEXTURED METAL MATERIALSY. Perlovich, M. Isaenkova, V. Fesenko…The data treatment involves recalculation of the Bragg angle 2φψ into the relative deviation of the interplanar spacing from the weighted average level Δd/dav. Depending on the texture character, different modes of microstress equilibrium take …
STANDARD REFERENCE MATERIAL 640D FOR X-RAY METROLOGYD.R. Black, D. Windover, A. Henins, D. Gil, J. Filliben, J.P. Cline…This report describes SRM 640d, the fifth generation of this powder diffraction SRM which is certified with respect to lattice parameter. It consists of approximately 7.5 g silicon powder specifically prepared to produce strain-free particles in…
TESTS OF MICROSTRUCTURE RECONSTRUCTION BY FORWARD MODELING OF HEDM DATAC.M. Hefferan, S.F. Li, J. Lind, R.M. Suter…Comparison between the simulated and reconstructed microstructures is examined with consideration to both crystallographic orientation and spatial geometric accuracy. To couple the simulations with the evolving experimental setup at the Advanced…
THE EFFECT OF THE SIGNAL PROCESSOR ON THE LINE SHAPET. Papp, J.A. Maxwell…Minimizing and accounting for these effects are important in reducing the errors in the deconvolution of spectra into component element contributions. This along with the associated rejected event spectrum provides the basis for a more accurate …
THIN FILM XRD TOTAL PATTERN FITTING APPLIED TO STUDY OF EVOLUTION OF MICROSTRUCTURE OF TIO2 FILMSR. Kužel, Z. Matĕj, L. Nichtová…It is an extension of the FOX program for structure determination from powder diffraction and it includes in particular the effects and corrections necessary for thin film analysis when parallel beam geometry and asymmetric detector scan at smal…
TOWARDS SUB-100 NM X-RAY MICROSCOPY FOR TOMOGRAPHIC APPLICATIONSP. Bruyndonckx, A. Sasov, B. Pauwels…Further simulation studies have shown that optimization of the detector response curve and switching from a reflective X- ray target to a transmission target should allow us to reach sub-100 nm resolutions. INTRODUCTION A common way to achieve a…
WASTE REDUCTION AND PROCESS IMPROVEMENTS IN THE ANALYSIS OF PLUTONIUM BY X-RAY FLUORESCENCEC.G. Worley, C.B. Soderberg, L.E. Townsend…These changes were made to minimize waste and improve process safety and efficiency. Sample sizes were reduced, cheaper sample preparation acids were used, and safety improvements were implemented. Using this modified process, results from analy…
X-RAY AND RAMAN SPECTRA STUDIES ON THERMAL ENERGY STORAGE MATERIALS – TRIS(HYDROXYMETHYL)AMINOMETHANEW.-M. Chien, V. Krishna Kamisetty, J.C. Fallas, D. Chandra, E.D. Emmons, A.M. Covington, R.S. Chellappa, R.J. Hemley, S.A. Gramsch, S. Clark…Army Edgewood Chemical Biological Center, AMSRD-ECB-RT-DL/BLDG E5560, 5183 Blackhawk Road, Aberdeen Proving Ground, MD 21010-5424 3 Department of Physics /MS220, University of Nevada, Reno, Reno, NV 89557 4 Carnegie/DOE Alliance Center, Geophysi…
X-RAY DIFFRACTION IMAGING OF DISLOCATION GENERATION RELATED TO MICROCRACKS IN SI-WAFERSJ. Wittge, A. Danilewsky, D. Allen, P. McNally, Z.J. Li, T. Baumbach, E. Gorostegui–Colinas, J. Garagorri, M.R. Elizalde, D. Jacques, M.C.Fossati, D.K. Bowen, B.K.Tanner…The nucleation of dislocations at indents in silicon following rapid thermal annealing (RTA) has been examined by X-ray diffraction imaging (topography). For indentation loads below 200mN, no slip bands were generated from the indent sites follo…

2008 – VOL52

A NEW PROCEDURE FOR THE EVALUATION OF RESIDUAL STRESSES BY THE HOLE DRILLING METHOD BASED ON NEWTON-RAPHSON TECHNIQUEG. Petrucci, M. Scafidi…In the presence of non-uniform residual stresses, the stress field can be determined from the measured relaxed strains using several methods, but the most used is the so called integral method. This method is characterized by some simplification…
A PORTABLE NON-INVASIVE XRD-XRF INSTRUMENT FOR THE STUDY OF ART OBJECTSP. Sarrazin, G. Chiari, M. Gailhanou…Tech. de St Jerome 13397 Marseille, France ABSTRACT A non-invasive XRD/XRF instrument for study of works of art has been developed jointly by the Getty Conservation Institute and inXitu Inc. (California). Many aspects of the instrument are based…
A STUDY OF RESIDUAL STRESSES IN VACUUM PLASMA SPRAYED TUNGSTEN COATINGST.-S. Jun, S.Y. Zhang, G. Appleby-Thomas, P.S. Grant, A.M. Korsunsky…Thick tungsten (W) coatings are potential plasma facing materials in fusion reactors, but the coefficient of thermal expansion (CTE) mismatch between W and Cu or steel substrates leads to large thermally induced stresses and premature failure. W…
AN INNOVATIVE EDXRD VERIFICATION PROBEC.M. Dozier, N. Anibou…Materials may be in solid or powder form, and the technique is non-destructive. Unlike Angular X-ray Diffraction (AXRD), a “white” x-ray beam between 20 and 80 keV is used. This energetic beam can penetrate through relatively thick materials, di…
ANALYSIS OF STRAIN-INDUCED PEAK BROADENING IN TITANIUM ALLOYSF. Hofmann, S. Y. Zhang, T. S. Jun, A. M. Korsunsky…Diffraction peak position is related to average elastic strain within the scattering grains, whilst diffraction peak shape is related to crystallite size and so-called root mean square (RMS) – strain, which refers to the spread of lattice parame…
APPLICATION OF 2-DIMENSIONAL XRD FOR THE CHARACTERIZATION OF THE MICROSTRUCTURE OF SELF-LEVELING COMPOUNDS (SLC)S. Seifert, J. Neubauer, F. Goetz-Neunhoeffer, H. Motzet…A calcium aluminate cement based SLC was prepared on two different substrates (water absorbent and non-water absorbent) to determine the vertical distribu- tion of the crystalline phases. The application of the GADDS enables the detection of the…
APPLICATION OF ENERGY-DISPERSIVE DIFFRACTION TO THE ANALYSIS OF HIGHLY INHOMOGENEOUS RESIDUAL STRESS FIELDS IN THIN FILM STRUCTURESM. Klaus, W. Reimers, Ch. Genzel…By the example of an Al2O3/TiCN on WC coating system we have studied the feasibility for using the coating reflections being stored in the ED diffraction patterns together with the substrate diffraction lines to analyze the residual stress state…
ASSESSING THE QUALITY OF X-RAY OPTIC SURFACES OF SI CRYSTALS CUT BY DIAMOND-WIRE AND ROTATING-BLADE SAWING TECHNIQUESM. Wieczorek, X. Huang, J. Maj, R. Conley, J. Qian, A. Macrander, C. Christensen, J. Hodsden, R. Khachatryan…As a first step toward initializing a systematic study on this topic, we evaluate in this paper the surface quality of two Si (111) wafers cut by a diamond-wire saw and a rotating-blade saw, respectively. We concentrate on revealing lattice stra…
BENEFITS OF IMPROVED RESOLUTION FOR EDXRFR. Redus, T. Pantazis, J. Pantazis, A. Huber, B. Cross…However, there are trade-offs between the highest energy resolution and the highest count rates, and there are practical difficulties in achieving the very best energy resolution. Energy resolution differentiates systems but the benefits of impr…
CHARACTERISTICS OF RESIDUAL STRESS PROFILES IN HARD TURNED VS. GROUND SURFACES WITH AND WITHOUTA WHITE LAYERA.W. Warren, Y.B. Guo…This study aims to clarify the pressing issues for five surface types: hard turned fresh, hard turned with a white layer, ground fresh, ground with a white layer, and as-heat-treated. The key findings are: (i) hard turned fresh surfaces produce …
CHARACTERIZATION OF A NEW BONE RECONSTRUCTED AT THE INTERFACES WITH IMPLANTA. Benmarouane, T. Buslaps, T. Hansen, V. Honkimaki, A. Lodini…Grenoble Cedex 9, France ABSTRACT The use of the implants has become current since 1930. With the improvement of technology, metals have been used in the medical field. As a long-term establishment is a meter of the therapeutic success, it is ne…
COMPLEMENTARITY OF EXPERIMENTAL AND NUMERICAL METHODS FOR DETERMINING RESIDUAL STRESS STATESG. Roy…There are destructive and non-destructive methods to measure strain tensor components and convert them into stress tensor components by a variety of techniques derived from constitutive (material) equations. In this study, four methods for deter…
DETERMINATION OF ACTIVATION ENERGY OF INTERMIXING IN TEXTURED METAL-METAL MULTILAYER FILMS VIA TWO-DIMENSIONAL X-RAY DIFFRACTIONM.A. Rodriguez, D.P. Adams, R.G. Tissot…Kinetic data were collected utilizing an area detector so as to reduce intensity bias from changes in out-of-plane texture during the intermixing reaction. Activation energies for Al/Pt, Ni/Ti, and Co/Al metal-metal multilayer thin films have be…
DETERMINATION OF RESIDUALS STRESSES AROUND BLISTERS IN ZR-2.5%NB PRESSURE TUBESJ.R. Santisteban, A. Steuwer, G. Domizzi, M. Peel…Libertador 8250 Buenos Aires (1429) – ARGENTINA 4 European Synchrotron Radiation Facility 38042 Grenoble – FRANCE ABSTRACT We have used synchrotron X-ray diffraction experiments to measure the strain field introduced by a hydride blister grown o…
DEVELOPMENT OF INDUCTION SURFACE HARDENING PROCESS FOR SMALL DIAMETER CARBON STEEL SPECIMENSD. Suzuki, K. Yatsushiro, S. Shimizu Y. Sugita M. Saito K. Kubota…Marushin Heat Treatment. ABSTRACT In case of induction hardening, the highly frequency generator make a shallow hardened zone. Additionally, hardening for smaller diameter specimen is enabled. In this study, the induction surface hardening proce…
DUAL-AXIS HOLE-DRILLING ESPI RESIDUAL STRESS MEASUREMENTSG.S. Schajer, M. Steinzig…Experimental tests were done on a stressed specimen, and the results supported theoretical expectations. INTRODUCTION Residual stresses play an important role in the strength and dimensional stability of engineering components. The stresses can …
EFFECT OF RESIDUAL STRESSES ON FATIGUE STRENGTH OF SEVERELY SURFACE DEFORMED STEELS BY SHOT PEENINGY. Akiniwa, H. Kimura, T. Sasaki…Medium carbon steel plates were heat treated in two different conditions. The Vickers hardness of material-A and B after heat treatment is 408 and 617 HV, respectively. The specimens were shot-peened with fine cast iron particles of the size of …
EFFECT OF THE HOLE-BOTTOM FILLET RADIUS ON THE RESIDUAL STRESS ANALYSIS BY THE HOLE DRILLING METHODM. Scafidi, E. Valentini, B. Zuccarello…Calenzano, Fi – ITALIA; www.sintechnology.com ABSTRACT The hole drilling method is based on the measuring of the surface relaxed strains when a small hole is drilled on the examined component. From the relaxed strains, measured generally by usin…
EVALUATION OF SUBSTRURUCTURE PARAMETERS BY PEAK PROFILE ANALYSIS OF HIGH-RESOLUTION NEUTRON DIFFRACTION SPECTRAP. Lukas, P. Strunz, V. Davydov, R. Kuzel…However, neutron diffraction facilities of new generation frequently offer the instrumental resolution high enough to study efficiently the effects of broadening of neutron diffraction profiles. The present paper describes the procedure for a de…
EVIDENCE AND ANALYSIS OF THERMAL STATIC STRAIN AGING IN THE DEFORMED SURFACE ZONE OF FINISH-MACHINED HARDENED STEELJ. Gegner, L. Schlier, W. Nierlich…D-57068 Siegen, Germany ABSTRACT After heat treating, finish machining of the hardened steel represents the last manufacturing step of machine elements. The practically most important operation of grinding is applied to achieve edge zone compres…
FINITE ELEMENT ANALYSIS AND NEUTRON DIFFRACTION EVALUATION OF RESIDUAL STRESSES IN STELLITE COATING PRODUCED BY PTA PROCESSA. Nady, H. Bonnefoy, V. KloseK, M.H. Mathon, A. Lodini, A. Baczmanski…Mickiewicza 30, 30-059 Kraków, Poland ABSTRACT A grade 6 cobalt-based superalloy was coated on steel substrate by the Plasma Transferred Arc (PTA) method. The macrostructure and microstructure of the interface and of the Co- based superalloy lay…
FINITE ELEMENT MODELING OF RESIDUAL STRESS PROFILE PATTERNS IN HARD TURNINGY.B. Guo…However, the formation mechanism of the unique RS profile is not yet known. In this study, a novel hybrid finite element modeling approach based on thermal-mechanical coupling and internal state variable plasticity model has been developed to pr…
FLEXIBILITY AND HIGH THROUGHPUT: SUPPORTING SAXS USERS AT A JOINT INDUSTRIAL ACADEMIC BEAMLINES. Weigand, B. Stillwell, W.E. Guise, J.P.G. Quintana, D.T. Keane…This has resulted in a sector with support for a broad range of techniques and sample environments. Among the techniques supported at DND-CAT are small and wide angle scattering, reflectivity, spectroscopy, tomography, and powder diffraction. Th…
GRAIN GROWTH IN NANOCRYSTALLINE COPPER THIN FILMS, INVESTIGATED BY NON-AMBIENT X-RAY DIFFRACTION MEASUREMENTSY. Kuru, M. Wohlschlögel, U. Welzel, E.J. Mittemeijer…Before annealing, the thermoelastic behaviour was investigated excluding the occurrence of thermally activated relaxation processes occurring above ambient temperature by in-situ stress measurements below ambient temperature. On this basis, abov…
IMPROVING TRACE ELEMENT DETECTION IN EDXRF BY REDUCING PILEUP ARTIFACTSW.T. Elam, B. Scruggs, M. Solazzi, J. Nicolosi…These artifacts often appear as extra peaks in the spectrum and can mask (or be mistaken for) weak peaks of trace elements. In X-ray fluorescence (XRF) the background is very small compared to charged-particle excitation techniques. This makes i…
IN-SITU INVESTIGATION OF GRAIN ROTATIONS DURING TENSILE STRAINING OF STEEL WIRESM. Moscicki, H. Pinto, C. Paulman, A. Borbély, A.R. Pyzalla…Helmholtz Centre Berlin for Materials and Energy GmbH, Glienicker Strasse 100, 14109 Berlin, Germany. ABSTRACT A new indexing procedure based on the direct measurement of the possible grain orientation is presented to characterize single grains …
IN-SITU STRESS ANALYSIS OF MULTILAYER ENVIRONMENTAL BARRIER COATINGSB.J. Harder, J. Almer, K.N. Lee, K.T. Faber…Coating stresses during cooling from 1000ºC were measured for as-sprayed and thermally cycled samples. In the as-sprayed state, tensile stresses as high as 75 MPa were measured in the doped-aluminosilicate topcoat at 375ºC, after which a drop in…
IN-SITU STUDY OF THE CYCLIC DEFORMATION BEHAVIOUR OF THE MAGNESIUM BASE WROUGHT ALLOY AZ31 BY MEANS OF HIGH ENERGY SYNCHROTRON DIFFRACTIONJ. Gibmeier, M. Götting, B. Scholtes…Mat. Eng., 34125 Kassel (Germany) ABSTRACT With regard to the processing of structural lightweight components there exists an increasing demand for the application of magnesium base wrought alloys, which are highly textured due to the forming pr…
INFLUENCE OF COLD COMPRESSION ON THE RESIDUAL STRESSES IN 7449 FORGINGSJ.S. Robinson, S. Hossain, C.E. Truman, E.C. Oliver, D.J. Hughes, M.E. Fox…Institut Laue Langevin, 6 rue Jules Horowitz, Grenoble France. 5 Materials Science Centre, University of Manchester, Manchester, UK. ABSTRACT The through-thickness residual stress distributions within three large rectilinear aluminium alloy 7449…
INFLUENCE OF THE SAMPLE MORPHOLOGY ON TOTAL REFLECTION X-RAY FLUORESCENCE ANALYSISC. Horntrich, F. Meirer, C. Streli, P. Kregsamer, G. Pepponi, N. Zoeger, P. Wobrauschek…In general TXRF is known to allow for linear calibration typically using an internal standard for quantification. For small sample amounts (low ng region) the thin film approximation is valid neglecting absorption effects of the exciting and the…
INTERFACE RESIDUAL STRESSES IN DENTAL ZIRCONIA USING LAUE MICRO-DIFFRACTIONH.A. Bale, N. Tamura, P.G. Coelho, J.C. Hanan…Among the ceramic materials, zirconia provides high toughness and crack resistant characteristics. Residual stresses develop in processing due to factors including grain anisotropy and thermal coefficient mismatch. In the present study, polychro…
LAYER GROWING/REMOVING METHOD FOR DETERMINATION OF RESIDUAL STRESSES IN ORTHOTROPIC NON-HOMOGENEOUS CYLINDERSJ. Kõo. J. Valgur…The stresses are calculated from strain measurements on the free stationary surface or from strain measurements on the cyl- inder’s moving surface. The suggested algorithm is programmed for PC. As an illustrative exam- ple, residual growth stres…
LOAD PARTITIONING IN A DUPLEX STAINLESS STEEL WITH SURFACE STRENGTH GRADIENT AND RESIDUAL STRESSESR. Lin Peng, J. Gibmeier, G.C. Chai, S. Johansson…Two loading cycles with a peak tensile strain of 0.5% and 0.87%, respectively, were successively applied and the evolution of stresses in the respective constituent phases (austenite and ferrite) were measured in a 0.026 mm thick surface layer a…
MEASURING RESIDUAL STRESSES IN STAINLESS STEEL – RECENT EXPERIENCES WITHIN A VAMAS EXERCISEA.T. Fry, J.D. Lord…The X-ray diffraction (XRD) technique is one of the most popular methods for measuring residual stress [1], used routinely in quality control and materials characterisation for validating models and design. The VAMAS TWA20 Project 3 activity on …
MG2SI-BASED MULTILAYER XRF ANALYZERS WITH TWO- AND THREE-LAYER STRUCTURE DESIGNY. Platonov, K. Shimizu, H. Kobayashi, G. Fournier, J. Rodriguez…These structures contain two, three or more different layer materials in a single period. The additional third, fourth, etc, layer was introduced for improving performance as well as for application dependent performance flexibility. Three-layer…
MICRO-SCALE RESIDUAL STRESS MEASUREMENT IN STEEL USING FOCUSED ION BEAM SLOTTING AND DIGITAL IMAGE CORRELATIONN. Daynes, G. Horne, P.J. Heard, D.Z.L. Hodgson, A. Shterenlikht…A 20×5×3 mm steel sample was used. The sample was compressed uniaxially to 400 MPa. The sample sur- face was polished down to a grit size of 1 µm and then placed inside the FIB chamber. The sample surface was subjected to uniform FIB exposure (e…
MICROSCOPIC LOAD SHARING IN A DUPLEX STAINLESS STEEL AND THE INFLUENCE OF PHASE PROPERTIESR. Lin Peng, G.C. Chai, A. Ellerman, S. Johansson, T. Manns…X-ray diffraction experiments under in-situ tensile loading with a peak stress close to the 0.2% proof stress were carried out to study the microscopic load sharing and the influence of the relative phase properties. It was observed that under e…
MICROSTRAIN ACCUMULATION IN MULTIPHASE SUPERALLOYSJ. Repper, M. Hofmann, C. Krempaszky, R.C. Wimpory, W. Petry, E. Werner…The elastic diffraction constants for all directions measured are compared to theoretical values calculated by the Kröner model. The differences between the microscopic and the macroscopic material response are given. The accumulation of microst…
MICROSTRUCTURE AND RESIDUAL STRESS FORMATION IN AN AA6040 TO AZ31B FRICTION STIR WELDR.S. Coelho, A. Kostka, H. Pinto, A. Rothkirch, J. dos Santos, A. Pyzalla…The complex material flow promoted by the friction stir welding process results in a fine grained structure in the stir zone of both materials due to dynamic/recovery recrystallization. The interface between the materials is characterized by the…
NATURAL NANOPARTICLE STRUCTURE, PROPERTIES AND REACTIVITY FROM X-RAY STUDIESG.A. Waychunas, B. Gilbert, J.F. Banfield, H. Zhang, Y.-S. Jun, C.S. Kim…Louis, Department of Energy, Environmental and Chemical Engineering 4Chapman University, Department of Chemistry ABSTRACT Synthetic analogs of naturally occurring nanoparticles have been studied by a range of x-ray techniques to determine their …
NEAR SURFACE STRESS GRADIENTS ANALYSIS BY GIXRD ON LASER SHOCKED 6056 ALUMINIUM ALLOY SAMPLESH.B. Song, P. Peyre, V. Ji, C.H. Jiang…Sci. & Engin., Shanghai Jiaotong University, Shanghai, P.R. China ABSTRACT Laser shock peening (LSP) can introduce a compressive stress profile for improving the materials’ surface mechanic properties. 6065 Aluminium alloy is introduced recently…
NEUTRON DIFFRACTION MEASUREMENTS ON A LARGE SIZE ROLLER BEARINGR.H. Vegter, T. Pirling, M. Peel…Since the introduced stress profiles depend on the treatment method and the necessary balancing tensile stresses may have unexpected consequences, it is necessary to quantify the stresses throughout the bearing. Today, most characterization of r…
NEUTRON DIFFRACTION STRESS ANALYSIS OF NEAR SURFACE STRESS GRADIENTS OF SURFACE TREATED STEEL SAMPLESJ. Gibmeier, J. Kornmeier, M. Hofmann…D-85747 Garching, Germany ABSTRACT For a quenched and tempered and subsequently shot peened steel plate of SAE 4140 the residual stress depth distribution was determined non-destructively by means of neutron diffraction at the STRESS-SPEC instru…
NEUTRON DIFFRACTION STUDIES ON STRAIN EVALUATION OF REBAR IN REINFORCED CONCRETEH. Suzuki, M. Kanematsu, K. Kusonoki…At first, absorption coefficients of several kinds of concretes with different compounding ratio of water, cement and aggregate were measured, and it was confirmed that the absorption coefficient of concrete was affected by the amounts of water …
NEUTRON LARMOR DIFFRACTION FOR THE DETERMINATION OF ABSOLUTE LATTICE SPACINGJ. Repper, T. Keller, M. Hofmann, C. Krempaszky, W. Petry, E. Werner…The absolute value of lattice spacing can be measured to an accuracy of 7· 10-5 A. However, absolute determination of the lattice parameter is limited by the quality of the reference specimen used. Absolute lattice spacing determined by Larmor d…
NEW DEVELOPMENTS AT MATERIALS SCIENCE DIFFRACTOMETER STRESS-SPEC AT FRM IIJ. Kornmeier, M. Hofmann, U. Garbe, A. Ostermann, C. Randau, J. Repper, W. Tekouo, G.A. Seidl, R.C. Wimpory, R. Schneider, H.G. Brokmeier…Werkzeugmaschinen und Betriebswissenschaften (iwb), TU München, D-85748 Garching, Germany Abstract The Materials Science Diffractometer STRESS-SPEC at the German neutron source FRM II is designed to meet the demands of non-destructive residual s…
NUMERICAL AND EXPERIMENTAL INVESTIGATION ON SHOT-PEENING INDUCED DEFORMATION. APPLICATION TO SHEET METAL FORMING.F. Cochennec, E. Rouhaud, L. Roucoules, B. Flan…Marie Curie BP2060 10010 TROYES Cedex FRANCE. 2Sisson Lehmann – Wheelabrator group. 24, rue Camille Didier BP39 08000 Charleville- Mezieres Cedex FRANCE. ABSTRACT The peen forming process is commonly used in the aeronautical industry to form lar…
ON THE IMPROVEMENT OF THE FATIGUE BEHAVIOUR OF AUSTENITIC STAINLESS STEELS DUE TO SURFACE RESIDUAL STRESSES PRODUCED BY LOW TEMPERATURE CARBURIZINGG. Minak…Surface hardness over 1000 Vickers and compressive residual stresses whose modulus exceeds 1500 MPa are usually achieved in the carburized layer, thanks to the formation of the so-called “S-phase”, a carbon- supersaturated austenite phase. A sig…
OPERATIONAL RESIDUAL STRESS FORMATION IN VIBRATION-LOADED ROLLING CONTACTJ. Gegner, W. Nierlich…This hitherto unnoticed loading is illustrated by case examples. Smoothing of the machining structure reveals mixed friction. Material aging is shifted towards the surface despite almost indentation-free race- ways. Two distinct types of residua…
OPTIMIZING THE BALANCE OF QUALITY AND TURNAROUND TIME FOR A PROCESS CONTROL XRF LABORATORYS.W. Bowe…Because of the increasing value of the products and increasing production costs, and uses of data outside of process control, the quality of the Smelter Lab assays has become more important. A program was initiated to improve the quality of resu…
PHASE TRANSFORMATIONS INVOLVING RESIDUAL STRESSES DURING GASEOUS NITRIDING OF STEELS. Jegou, R. Kubler, L. Barrallier, F. Roch…This treatment is known in the art but some advances still need to be done in terms of residual stress understanding. Although they originate from volume micro-loading accompanying the precipitation of nitrides, questions about their in-depth di…
PRECONCENTRATION OF ENVIRONMENTAL WATERS BY AGAR FOR XRF ANALYSISK. Nakano, K. Okubo, K. Tsuji…The thin agar film was prepared by drying a homogeneous agar gel after mixing the aqueous sample solution with the agar powder. XRF analysis of the preconcentrated thin agar films containing trace metals showed a good repeatability, because agar…
PRELIMINARY STUDY OF A GEORGIA O’KEEFFE PASTEL DRAWING USING XRF AND ΜXRDL.B. Brostoff, C.I. Maynor, R.J. Speakman…Georgia O’Keeffe. XRF analyses showed that, among other pigments present in the drawing, the red, orange and yellow pigments may possibly be identified with lead- and chromium-based pigments: lead chromates, red and yellow lead oxides, and/or le…
PROCEDURE FOR NONDESTRUCTIVE RS-MEASUREMENTS OF INNER SURFACES OF BALL BEARING COMPONENTSJ. Epp, T. Hirsch…Thus, ideally a complete characterization of the componen residual stress state is required. Magnetic and micromagnetic analysis of residual stresses can represent an important gain of time if compared to X-ray diffraction. Another important adv…
QUANTITATIVE IN-SITU X-RAY DIFFRACTION ANALYSIS OF EARLY HYDRATION OF PORTLAND CEMENT AT DEFINED TEMPERATURESC. Hesse, F. Goetz-Neunhoeffer, J. Neubauer, M. Braeu, P. Gaeberlein…Technical white cement was used for the XRD analysis on a D5000 diffractometer (Siemens). All diffraction patterns of the in-situ measurement which were recorded up to 22 hours of hydration at defined temperatures were analyzed by Rietveld refin…
RADIOACTIVE SAMPLE EFFECTS ON EDXRF SPECTRAC.G. Worley…Radioactive alpha emitters, however, emit X-rays during the alpha decay process that complicates spectral interpretation. This is particularly noticeable when using a portable instrument where the detector is located in close proximity to the in…
RADIOISOTOPE RH-101 AS X-RAY SOURCE FOR INSTRUMENTS ON SPACE MISSIONSCh. Stenzel, Ch. Schroer, B. Lengeler, M. Rasulbaev, R. Vianden…We discuss geological questions which we believe should be answered before any search for biological structures or pre-forms of life. We also suggest a method to produce Rh-101. Key words: Isotopes Rh-101, Am-241, XRD, XRF, Mars, Saturn’s moons …
RELAXATION OF RESIDUAL STRESSES IN THIN FILMS INVESTIGATED USING SYNCHROTRON RADIATUIONT. Matsue, T. Hanabusa, K. Kusaka, O. Sakata…In a previous study, the crystal structure of TiN films deposited by AIP was found to be strongly influenced by the bias voltage during deposition. However, for film thickness of approximately 200 nm, TiN films deposited under bias voltages of –…
RESIDUAL STRESS ANALYSIS WITH MULTIPLE HKL RINGS COLLECTED BY AREA DETECTORSB.B. He, A. Ulyanenkov…The sharp stress gradient, anisotropic grain shape and inhomogeneous phase and microstructure distribution also add difficulties in stress analysis with the conventional X-ray diffraction method. The nonlinear εψφ – sin2ψ behavior, commonly asso…
RESIDUAL STRESS DETERMINATION IN SURFACE TREATED ALUMINA SAMPLES APPLYING BEAM LIMITING MASKST. Manns, A. Rothkirch, B. Scholtes…For this purpose, beam limiting masks were designed, manufactured and investigated in first experiments. Image series taken with a position sensitive CCD-camera demonstrate the ability to detect interferences from gauge volumes beneath the sampl…
RESIDUAL STRESS DISTRIBUTION UNDER HARDENING LAYER OF CARBURIZED TRANSMISSION GEAR BY NEUTRON DIFFRACTIONY. Sakaida, M. Kawauchi, M. Manzanka…The material was chromium-molybdenum steel, SCM420. The carburized case depth was first determined by microscope, and then was measured by micro Vickers hardness tester. The neutron diffractions from Fe-110 and 211 planes were used for stress me…
RESIDUAL STRESS ESTIMATION OF TI CASTING ALLOY BY X-RAY SINGLE CRYSTAL MEASUREMENT METHODA. Shiro, M. Nishida, T. Hanabusa, J. Tian…Since the casting metals involve various kinds of residual stresses due to heat shrinkage, inclusion particles and so on, the accurate estimation of residual stresses is desired in the engineering field. The aim of the present study is to evalua…
RESIDUAL STRESS EVALUATION OF RAILWAY RAILSS. Takahashi, T. Sasaki, Y. Kondoh, Y. Hirose…Fracture mechanics clarification concerning the growth behavior of cracks is needed, in order to decide the inspection period and the cycle [1], [2]. Though the crack progression and influence of residual stress on fatigue strength has been rese…
RESIDUAL STRESS EVOLUTION ANALYSIS IN AZ31 FRICTION STIR WELDS USING X-RAY AND NEUTRON DIFFRACTIONL. Commin, L. Barrallier, J.E. Masse…Assessing the efficiency of new joining techniques, as Friction Stir Welding is then required. During Friction Stir Welding, the welding tool motion induces frictional heating and severe plastic deformation. Then, in addition to the microstructu…
RESIDUAL STRESS MEASUREMENT IN STEEL BEAMS USING THE INCREMENTAL SLITTING TECHNIQUED.Z.L. Hodgson, D.J. Smith, A. Shterenlikht…Initially a study into a number of factors affecting the series expansion ap- proach was conducted. Due to the over-determined nature of the series expansion approach appropriate selection of polynomial series order was necessary to develop the …
RESIDUAL STRESS MEASUREMENTS BY SYNCHROTRON RADIATION FOR RAIL SURFACES DAMAGED BY ROLLING CONTACT FATIGUET. Sasaki, Y. Miyazawa…To accommodate future field measurements, the authors used an area detector type X-ray stress measurement. A method for determining the depth profile of stresses was also conducted. Furthermore, the measurements were made with synchrotron radiat…
RESIDUAL STRESS RELAXATION IN WELDED JOINTS UNDER STATIC AND CYCLIC LOADINGM. Farjian-Sohi, Th. Nitschke-Pagel, K. Dilger…Increased material utilization has necessitated increased consideration of the fatigue problem. In order to achieve a fatigue resistant welded structure, it is necessary to manage and control welding process related factors which reduce the fati…
RESIDUAL STRESSES ANALYSIS IN BRUSH-PLATED GALVANIC COATINGS DEPOSITED FROM NICKEL SULFATE ELECTROLYTEH. Lille, J. Kõo, A. Ryabchikov…To determine residual stresses, a conventional deformation method was used, where a coating is manually deposited on a brass strip substrate in the conditions of restraint bending. The change in the axial strain of the free surface is measured b…
RESIDUAL STRESSES AND DISTORTION SIMULATION OF NITRIDED DISCL. Barrallier, V. Goret, P. Vardon, D. Deloison…The combination of hardening effect and residual stress generation allows explaining the performance treatment. Precipitation phenomena can be linked to the stress and hardening generation. In order to optimize the design of part, modeling of ni…
RESIDUAL STRESSES AND IN-SITU MEASUREMENT OF PHASE TRANSFORMATION IN LOW TRANSFORMATION TEMPERATURE (LTT) WELDING MATERIALST. Kannengiesser, A. Kromm, M. Rethmeier, J. Gibmeier, Ch. Genzel…For this kind of filler materials for the first time high energy synchrotron radiation was applied in order to characterise the effect of lowered martensite start temperatures on the welding residual stresses in-situ by means of en- ergy dispers…
RESIDUAL STRESSES IN BRUSH-PLATED GOLD COATINGH. Lille, J. Kõo, A. Ryabchikov, R. Laaneots…The calculation formula is extended Stoney’s formula which takes into consideration the real shape of the substrate, and the difference between the elasticity moduli and the coefficient of the thermal expansion of the coating and the substrate m…
RESIDUAL STRESSES IN COLD-DRAWN RODS: EFFECT OF A NOVEL POST-DRAWING TREATMENTJ. Ruiz-Hervias, M. Hofmann, J. Rebelo-Kornmeier, V. Luzin, M. Elices…Samples were first subjected to one drawing pass with 20% section reduction and then to a second pass with only 1% section reduction (“skin-pass” treatment). After the first pass, the calculated residual stresses are tensile at the rod surface a…
RESIDUAL STRESSES IN FRICTION STIR WELDING: NUMERICAL SIMULATION AND EXPERIMENTAL VERIFICATIONG. Buffa, L. Fratini, S. Pasta…Both numerical and experimental analyses were carried out to highlight the metallurgical phenomena and induced residual stresses in FS welded blanks. The welding process was simulated using a continuous rigid-viscoplastic finite element model (F…
RESIDUAL STRESSES IN MACHINED AND SHRINK-FITTED ASSEMBLIESB. Su, F. Hossainzadeh, C. Truman, D. Smith…Residual stresses were measured using a combination of deep-hole drilling (DHD) and incremental centre hole drilling (ICHD) techniques. The ICHD method provided near surface residual stress measurements to depths up to about 1mm. The DHD method …
RESIDUAL STRESSES IN NOVEL METAL/CERAMIC COMPOSITES EXHIBITING A LAMELLAR MICROSTRUCTURES. Roy, J. Gibmeier, A. Wanner…These composites are produced by melt infiltration of porous ceramic preforms produced by freeze-casting and subsequent sintering. This production route has a high application potential since it offers a cost-effective way to obtain composites w…
RESIDUAL STRESSES OF EB-PVD THERMAL BARRIER COATINGS EXPOSED TO HIGH TEMPERATUREK. Suzuki, T. Shobu, K. Tanaka…As the top coating, zirconia with 4 mol% yttria was electron beam-physical vapor deposited (EB-PVD) on the rotating substrate. The rotation speeds in the EB-PVD process were 5, 10 and 20rpm. The specimens were exposed to 1273K in air atmosphere …
SMALL CREEP DEFORMATIONS AND RESIDUAL STRESS RELAXATION IN WELDED AND SHOT PEENED AL MG SI CU-ALUMINUM ALLOYST. Hirsch, S. Daichendt…For a laser beam welded AlMgSiCu-alloy, results of applied stress and residual stress relaxation at elevated temperatures 100<T<150°C are presented. These experiments prove the existence of back stresses. The level of these stresses can be estim…
SPATIALLY RESOLVED STRAIN MEASUREMENTS ON MICRO MOULDSA. Kienzler, B. Okolo, V. Schulze, A. Wanner…Surface treatment involved a sequential application of grinding, micro milling and abrasive micro peening processes. The micro-features created at the milled surfaces were studied using a high lateral resolution CCD based Material X-ray Imaging …
STUDY ON COMPUTERIZED TOMOGRAPHY AND STRAIN MAPPING NEAR THE INTERNAL CRACK TIP OF STEEL BAR USING SYNCHROTRON WHITE X-RAYJ. Shibano, K. Kajiwara, K. Kiriyama, T. Shobu, K. Suzuki, T. Arai, S. Miura, M. Kobayashi…JASRI, Kouto Sayo-cho, Sayo-gun, Hyogo, 679-5148 Japan. 3 SPring-8 Service Co., Ltd., Kouto Sayo-cho, Sayo-gun, Hyogo, 679-5148 Japan. 4 Dept. of Tech. and Living Sci., Niigata Univ., 8050, Igarashi-2-no-cho, Niigata, 950-2181 Japan. ABSTRACT A …
SURFACE RESIDUAL STRESSES IN DRY TURNING OF 0.45% C STEELT. Leppert, R. Lin Peng…Depending on their kind and the type of applied loading, the influence of residual stresses can be negative or positive. Tensile residual stresses usually exert highly detrimental impact on several functional aspects such as strength, fatigue li…
SURFACE WORKHARDENING AND RESIDUAL STRESSES INDUCED BY MICRO CUTTING PROCESSESH. Autenrieth, B. Okolo, V. Schulze, A. Wanner…The influence of the ploughing effect on residual stresses, surface deformation and work hardening, and the tool quality were investigated. Tensile residual stresses, caused by the heat generated in the material during the cutting process, were …
SYNCHROTRON XRF ANALYSES OF ELEMENT DISTRIBUTION IN FOSSILIZED SAUROPOD DINOSAUR BONESM. Dumont, N. Zoeger, C. Streli, P. Wobrauschek, G. Falkenberg, P.M. Sander, A.R. Pyzalla…This sheer size of the sauropod leads to scale effects in their biology and physiology that still are inadequately understood. The only remnants of the sauropods are their fossilized bones. These fossilized bones have sustained burial for some h…
THE BASIC RELATIONSHIP BETWEEN RESIDUAL STRESS PROFILE PATTERNS AND FATIGUE LIFE OF PRECISION MACHINED SURFACES IN ROLLING CONTACTY.B. Guo, A.W. Warren…The key findings of this study are: (a) The basic RS profiles by a sharp tool can be fundamentally changed by a turned WL but not a ground WL; (b) The hook shaped RS profile of a turned surface may have about 40% more fatigue life than a ground …
THE EFFECTS OF CASTING PARAMETERS ON RESIDUAL STRESSES AND MICROSTRUCTURE VARIATIONS OF AN AL- SI CAST ALLOYS. Mohsen Sadrossadat, S. Johansson…The microstructure of Al-Si cast alloys is influenced by the morphology of silicon particles (shape, size and distribution), aluminum grain size and dendrite parameters. Dimensional changes resulting from casting caused by residual stresses can …
THE EXTENT OF RELAXATION OF WELD RESIDUAL STRESSES ON CUTTING OUT CROSS-WELD TEST-PIECESJ. Altenkirch, A. Steuwer, M.J. Peel, P.J. Withers…Similarly weld mechanical performance tests are frequently undertaken on cross-weld test-pieces without a proper understanding of the level or influence of retained RS. We present a systematic study of the relaxation of longitudinal RS in thin-p…
USING XRD ELASTIC AND PLASTIC STRAIN DATA TO EVALUATE THE EFFECTIVENESS OF DIFFERENT COLD-WORKING TECHNIQUES IN AEROSPACE MATERIALSB.S. Matlock, D.J. Snoha, S.M. Grendahl…Shot peening and cold expansion of holes are two techniques for imparting beneficial compressive stresses. X-ray diffraction is a direct method for measuring elastic strains. Diffraction peak widths are an indication of plastic strain. Elastic a…
WHY SHOULD WE GIVE UP THE SIN2 METHODB. Ortner…Quantitative comparisons have been made for different fictitious measurements. It is shown that the – unnecessary – loss in accuracy by using the sin2 ψ method is quite significant and by no means negligible. The same course of action has been a…
X-RAY ANALYSIS OF PRECIPITATES FORMED IN COPPER-BASE ALLOYSS.Sato, Y.Takahashi, T.Sanada, K.Shinoda, K.Wagatsuma, S.Suzuki…Ni2Si precipitates with wide nanometer size distribution were formed in the Cu-Ni-Si alloys after a long aging time of 104 s. However, the addition of a small amount of Fe appears to reduce the wide-size distribution of the precipitates in the a…
X-RAY DIFFRACTION CHARACTERIZATION OF MOVPE ZNSE FILMS DEPOSITED ON (100) GAAS USING CONVENTIONAL AND HIGH-RESOLUTION DIFFRACTOMETERST.N. Blanton, C.L. Barnes, M. Holland, K.B. Kahen, S.K. Gupta, F. Bai…ZnSe has a large band gap, 2.76 eV, as well as a near lattice match to GaAs, 5.6688 Å vs. 5.6538 Å, respectively. In this study a metallorganic vapor phase epitaxy (MOVPE) deposition technique is used to produce doped and undoped thin films of Z…
X-RAY DIFFRACTION STUDY OF ANISOTROPIC STATE OF RESIDUAL STRESS AFTER DOWN-CUT AND UP-CUT FACE GRINDINGZ. Pala, N. Ganev, J. Drahokoupil…Nevertheless, there is a pronounced distinction in the fashion of material removal which could lead to unequal states of surface residual stress. By means of X-ray diffraction analysis, ground plates made from three types of steel were investiga…
X-RAY GRAZING INCIDENCE TECHNIQUE . CORRECTIONS IN RESIDUAL STRESS MEASUREMENT . A REVIEWS. Wronski, K. Wierzbanowski, A. Baczmanski, A. Lodini, Ch. Braham, W. Seiler…The most important is the refraction of X-ray wave: it changes the wave length and direction of the beam. The both effects modify a pick position. A corresponding correction was calculated and tested on ferrite powder and on 316L austenite stainl…
X-RAY IN-SITU RESIDUAL STRESS MEASUREMENT OF FIBER REINFORCED PLASTIC COMPOSITEY. Watanabe, M. Nishida, T. Hanabusa…ABSTRACT Recently, the use of fiber-reinforced plastics (FRPs) in industrial applications has been increasing dratically. A reliable method for estiting the stress in FRPs is required. In this study, the residual stresses in FRP samples were mea…
X-RAY MULTIAXIAL STRESS ANALYSIS USING TWO DEBYE RINGST. Sasaki, Y. Kobayashi…In the method of this study, two Debye rings are used for determining stresst hrough the relative change of diffraction data as much as possible like the sin2ø method. It is not necessary to prepare the precise d0 value when the stress component…
X-RAY STRESS MEASUREMENT OF NICKEL-BASE SINGLE CRYSTAL SUPERALLOY USING TWO-DIMENSIONAL DETECTORK. Tanaka, S. Machiya, Y. Akiniwa…The specimen whose surface normal was parallel to [001] direction was oscillated around φ-axis during recording of the X-ray diffraction pattern with a two-dimensional position sensitive proportional counter (PSPC). The stress was determined fro…
XRF OF CULTURAL HERITAGE MATERIALS: ROUND-ROBIN IV – PAINT ON CANVASC. Namowicz, K. Trentelman, C. McGlinchey…In 2008 the round-robin explored the application of XRF to the study of paintings on canvas. Thirteen samples, consisting of both modern and traditional pigments on canvas, were distributed to 25 participating institutions for analysis. The samp…

2007 – VOL51

A BERYLLIUM DOME SPECIMEN HOLDER FOR XRD ANALYSIS OF AIR SENSITIVE MATERIALSMark A. Rodriguez, Timothy J. Boyle, Pin Yang, and Damon L. Harris…The specimen holder has a robust o-ring type seal (>10-9 torr) and no observed intensity artifacts in the 1° to 150° 2θ range. The design also minimizes specimen displacement errors and allows for analysis of both powders and bulk specimens (i.e…
A NEW APPROACH TO FITTING THE SPECTRA FROM THE MARS ROVER ALPHA-PARTICLE X-RAY SPECTROMETERSJohn L. Campbell, May Lee, Brian N. Jones, and John A. Maxwell…Full matrix corrections for both excitation modes are included, and element concentrations are deduced. The code is intended for eventual use in processing spectra from the alpha-particle X-ray spectrometers aboard the Mars Exploration Rovers (M…
A NOVEL 2D ANALYSIS METHOD TO CHARACTERIZE INDIVIDUAL GRAINS USING HIGH-ENERGY X-RAY MICROBEAM DIFFRACTIONE. Jimenez-Melero, N. H. van Dijk, L. Zhao, J. Sietsma, and S. van der Zwaag…Its application to study in situ the martensitic transformation of small individual austenite (fcc) grains embedded in a complex ferritic/bainitic/martensitic (bcc) multiphase microstructure is also reported. INTRODUCTION The design and developm…
ANALYSIS OF PIGMENTS USED IN A JAPANESE PAINTINGYasuhiro Hayakawa, Seiji Shirono, Sadatoshi Miura, and Tomohide Matsushima…A pair of six-panel folding screens entitled The Irises Screens by Ogata Korin, a National Treasure of Japan, was examined. A scientific approach had never been incorporated into its investigation, and its materials and techniques had remained u…
ANALYTICAL METHODS FOR DISCRIMINATING STARDUST IN AEROGEL CAPTURE MEDIASean Brennan, Hope A. Ishii, John P. Bradley, Katharina Luening, Konstantin Ignatyev, and Piero Pianetta…These analytical methods are necessitated by the levels of trace contaminants present in the aerogel. The cometary material disaggregates during deceleration in the aerogel, so fluorescence mapping of the entire track (which can be several milli…
BORON IN GLASS DETERMINATION USING WDXRFAlexander Seyfarth…Advances in XRF instrumentation have enabled improvement in the analysis of boron. Reduced window thickness and high-current capabilities of X-ray tubes, as well as new analyzer crystals, produce a higher intensity boron signal. With correct det…
COMPARISON OF SIMULATED AND EXPERIMENTAL XRPD PATTERNS OF SILVER WITH TWIN FAULTS USING MAUD AND DIFFAXPaul J. Schields, Nicholas Dunwoody, Marc Mamak, Claire Gendron, and Simon Bates…MAUD was used to refine the DIFFaX-simulated patterns to determine systematic differences between these simulation programs. The results indicated the Warren model of twin faults is applicable for fault probabilities <10% and DIFFaX and MAUD fau…
CRYSTALLITE MORPHOLOGY IN GOLD CATALYSTS OBTAINED BY RIETVELD REFINEMENTXim Bokhimi, Antonio Morales, and Rodolfo Zanella…Three-dimensional images of the crystallites were generated in real space, as well as 3-D images of the microstrain distribution in reciprocal space. These images were used to analyze the effect of the different parameters of the refinement mode…
DEVELOPMENT OF A PREDICTIVE LIFE TOOL FOR TAPERED ROLLER BEARINGS USING MEASURED RESIDUAL STRESS AND RETAINED AUSTENITE DATABrent M. Wilson and Matthew G. Dick…Case-carburized tapered roller bearings used in the railroad industry are manufactured with a dual-phase microstructure that consists primarily of tempered martensite and retained austenite. The retained austenite phase is metastable, and will t…
DISLOCATION MODEL OF STRAIN ANISOTROPYTamás Ungár…Based on this theorem strain anisotropy is modeled and accounted for by assuming that strain broadening is caused by dislocations or di. The effect of strain anisotropy is summarized in hkl dependent dislocation contrast factors, which can be ei…
EFFECTS OF HYDROGEN ON THE INTERACTIONS OF FUEL CELL SEALING GLASSES WITH INTERCONNECT ALLOYSS. T. Misture…Experiments under 4% hydrogen and air at temperatures up to 1000 °C showed that both sealants react rapidly with alumina and chromia, but not with NiO. The crystallization of the high-CTE phase BaCrO4 was noted for G18 in contact with chromia or…
ELABORATION ON THE HEXAGONAL GRID AND SPIRAL TRACE SCHEMES FOR POLE FIGURE DATA COLLECTIONAnthony C. Rizzie, Thomas R. Watkins, and E. Andrew Payzant…Applying the concepts of stereographic and equal area projections with geometry, spreadsheets were created to calculate the angular settings of the goniometer. Using the generated settings, the hexagonal grid and spiral trace schemes were progra…
ELASTIC PROPERTIES OF METALLIC THIN FILMS: 2D SYNCHROTRON XRD ANALYSIS DURING IN SITU TENSILE TESTINGG. Geandier, P.-O. Renault, S. Teat, P. Goudeau, and E. Le Bourhis…Model nanometric multilayer W/Au systems exhibiting different microstructures were analyzed. These films are supported by a (thin) polyimide substrate. X-ray diffraction in transmission geometry was used to study the deformations of both phases …
EMPLOYING X-RAY SCATTERING TO CHARACTERIZE MATERIALS WITH GRAIN SIZES IN THE NANO-REGIMEE. A. Laitila and D. E. Mikkola…Observations of X-ray scattering as RMM processing time increases show severe broadening of matrix diffraction peaks, accompanied by the appearance of diffraction peaks resulting from the formation of very small crystallites of TiC and TiH1.92 p…
FILTER DEBRIS ANALYSIS BY ENERGY DISPERSIVE X-RAY FLUORESCENCE APPLIED TO J52P408 ENGINESGary R. Humphrey…This technique, developed by the U.S. Department of Defense’s Joint Oil Analysis Technical Support Center (JOAP-TSC), is termed filter debris analysis (FDA). Six beta prototype instruments capable of performing FDA-EDXRF in an automated mode wer…
FLEXIBLE FILAMENTOUS VIRUS STRUCTURES FROM FIBER DIFFRACTIONGerald Stubbs, Amy Kendall, Michele McDonald, Wen Bian, Timothy Bowles, Sarah Baumgarten, Ian McCullough, Jian Shi, Phoebe Stewart, Esther Bullitt, David Gore, and Said Ghabrial…Analysis of the data in conjunction with cryo-electron microscopy data allowed us to determine the symmetry of the viruses and to make reconstructions of SMV at 19 Å resolution and of another potexvirus, papaya mosaic virus, at 18 Å resolution. …
FULL PATTERN COMPARISON OF EXPERIMENTAL AND CALCULATED POWDER PATTERNS USING THE INTEGRAL INDEX METHOD IN PDF-4+John Faber and Justin Blanton…The software integrated into the PDF-4 (DDView+) provides the ability to calculate fully digitized diffraction patterns for all 272,232 entries (PDF-4+ 2007). To provide a means of quantitative comparison between entries in the Power Diffraction…
GONIOMETER INDUCED BIAS IN PEAK POSITION MAP DATAK. W. Kirchner and K. A. Jones…The confirmed bias adds a complex curvature to the PPMs that runs orthogonal to the XZ plane of the goniometer and whose major folds bend around axes parallel to the Y-axis. INTRODUCTION Through the plotting of X, Y, and θ for each scan of an or…
HANDY WAVEGUIDE TXRF SPECTROMETER FOR NANOGRAM SENSITIVITYShinsuke Kunimura and Jun Kawai…The signal to background ratios of spectra decreased with an increase in incident X-ray beam size. The portable spectrometer was also applied to rainwater and a specimen containing antimony and rare earth elements. Nanograms of elements in these…
HIGH-THROUGHPUT SYSTEM FOR SYNCHROTRON X-RAY POWDER DIFFRACTOMETRYKenichi Kato, Masaki Takata, and Tetsuya Ishikawa…An automatic sample exchanger, image recognition system for automatic sample position alignment, and online detector have been developed and linked to each other by our original control program. As a result, time taken except for X-ray exposure …
IMPLEMENTATION OF THE MONTE CARLO-LIBRARY LEAST-SQUARES APPROACH TO ENERGY DISPERSIVE X-RAY FLUORESCENCE ANALYSISFusheng Li, Weijun Guo, and Robin P. Gardner…This software is a visualization system developed on the Borland C++ Builder platform and has a user-friendly interface to accomplish all qualitative and quantitative tasks easily. The software enables users to run the forward Monte Carlo simula…
IMPROVING THE DETECTION LIMIT IN EDXRF WITH PROPORTIONAL COUNTERI. A. Brytov, A. D. Goganov, and R. I. Plotnikov…This can be achieved by the design of instruments and evacuation or He-inletting in a measurement camera. The objective of this work was to design a simple and inexpensive sulfur analyzer based on a gas proportional counter equipped with an air …
IN SITU STRESS MEASUREMENT OF BIAXIALLY STRAINED ALUMINUM ALLOY 5754-OMark A. Iadicola and Thomas H. Gnaeupel-Herold…The method uses a portable X-ray diffraction (XRD) system to measure in situ stresses during tensile deformations. Calibration of X-ray elastic constants and the effects of texture and intergranular stresses are discussed. Uniaxial data measured…
IN SITU STRUCTURAL ANALYSIS OF BPDA-PPD POLYIMIDE THIN FILM USING TWO-DIMENSIONAL GRAZING INCIDENCE X-RAY DIFFRACTIONJ. Kikuma, T. Nayuki, T. Ishikawa, G. Asano, and S. Matsuno…Optimizing the sample shape, two-dimensional images were measured successfully without sacrificing angle resolution. It has been clearly shown that the crystallization first begins in the in-plane direction, at the curing temperature of 180 °C, …
MICROFOCUSING X-RAY EQUIPMENT FOR THE LAB DIFFRACTOMETERJörg Wiesmann, Jürgen Graf, Christian Hoffmann, Carsten Michaelsen, Alexandra Oehr, Uwe Preckwinkel, Ning Yang, Holger Cordes, and Kurt Erlacher…Measurements with the new low-maintenance, high-brilliance microfocus source IµS equipped with different two-dimensional beam shaping multilayer optics are shown. The comparison of IµS with typical sealed tube fine focus systems shows data of ou…
MICROSCANNING XRF, XANES, AND XRD STUDIES OF THE DECORATED SURFACE OF ROMAN TERRA SIGILLATA CERAMICSC. Mirguet, P. Sciau, P. Goudeau, A. Mehta, P. Pianetta, Z. Liu, and N. Tamura…A mixture Gallic slip sample cross-section showing red and yellow colors was studied. The small (micron) size of the X-ray beam available at Stanford Synchrotron Radiation Laboratory (SSRL) and Advanced Light Source (ALS) synchrotron sources, co…
MINIMAL USE OF STANDARDS FOR QUANTIFYING TRACE ELEMENTS IN PLASTICSW. T. Elam, Bruce Scruggs, Robert B. Shen, Laszlo Herczeg, Andrew Lee, and Joseph A. Nicolosi…The fundamental parameters method, backed up by one or more standards, is used to translate XRF intensities into quantitative information about trace element concentrations. The method includes accounting for variations in sample thickness using…
MONTE CARLO SIMULATIONS OF PROJECTIONS IN COMPUTED TOMOGRAPHYB. Chyba, M. Mantler, and M. Reiter…A meaningful comparison with measurements was therefore possible. Coherent and incoherent scattering as well as excitation of fluorescent radiation are accounted for; multiple sequences of these interactions are followed up to a selectable order…
NEXT GENERATION X-RAY DETECTORS FOR IN-HOUSE XRDTakeyoshi Taguchi, Christian Brönnimann, and Eric F. Eikenberry…PILATUS detectors are two-dimensional hybrid pixel array detectors, which operate in single-photon counting mode. PILATUS detectors feature a very wide dynamic range (1:1,000,000), very short read out time (< 3.0 msec), no readout noise, and ver…
PERFORMANCE OF A BOREHOLE XRF SPECTROMETER FOR PLANETARY EXPLORATIONWarren C. Kelliher, Ingrid A. Carlberg, W. T. Elam, and Ella Willard-Schmoe…It will be used to determine the composition of the Mars regolith at various depths by insertion into a pre-drilled borehole. The primary performance metrics for the instrument are the lower limits of detection over a wide range of the periodic …
PERFORMANCE OF A ROOM TEMPERATURE GAS PROPORTIONAL SCINTILLATION COUNTER IN X-RAY ANALYSIS OF METALLIC ALLOYS EXCITED WITH ALPHA PARTICLESF.I.G.M Borges, S.J.C. do Carmo, T.H.V.T. Dias, F.P. Santos, F.P.S.C. Gil, A.M.F. Trindade, R.M. Curado, C.A.N. Conde…The curved grid technique was used for solid angle compensation and the photosensor is a photomultiplier tube with a 50 mm diameter quartz window. For an energy range between 2.5 and 25 keV it can work at counting rates up to 20,000 events/s, pr…
REAL-SPACE STRAIN MAPPING OF SOI FEATURES USING MICROBEAM X-RAY DIFFRACTIONConal E. Murray, S. M. Polvino, I. C. Noyan, B. Lai, and Z. Cai…Strain engineering in microelectronic technology represents an important aspect of the enhancement in complementary metal-oxide semiconductor (CMOS) device performance. Because of the complexity of the composite geometry associated with microele…
RHOMBOHEDRAL-CUBIC PHASE TRANSITION CHARACTERIZATION OF (PB,GE)TE USING HIGH-TEMPERATURE XRDJ. Sariel, Y. Gelbstein, and I. Dahan…Samples of Bi2Te3 doped Pb1-xGexTe were prepared by powder metallurgy approach. These powder samples were examined by high-temperature XRD and SEM/EDS. A bulk (pressed powder) cylindrical specimen was used for dilatometery characterizations. Acc…
STRESS AND COMPOSITION EVALUATION FOR GRADIENT NITRIDE COATINGST. A. Alexeeva, V. V. Uglov, V. M. Anishchik, S. V. Zlotski, J. Brechbühl, H. Guerault, A. Lazar, A. Ulyanenkov, and T. Baumbach…The deposition was carried out by combining the titanium and chromium plasma flows of various densities. The deposited coatings were found to be two-phase (solid solution and titanium nitride) systems. The residual stress and density depth profi…
THE DEVELOPMENT OF A MULTILAYER MIRROR SYSTEM USING CUKΑ AND CRKΑ RADIATION FOR USE IN MICRO BEAM X-RAY DIFFRACTOMETRYKatsunari Sasaki, Yukio Hirose, Masataka Maeyama, Joseph D. Ferrara, and Toshihiko Sasaki…Multilayer optics technology is a well-known tool to produce a monochromatic micro X-ray beam for XRD. This new optic was combined with a microfocus rotating anode X-ray generator and a cylindrical imaging plate detector to provide a complete du…
THE EVALUATION OF PREFERENTIAL ALIGNMENT OF BIOLOGICAL APATITE (BAP) CRYSTALLITES IN BONE USING A TRANSMISSION X-RAY DIFFRACTION METHODKatsunari Sasaki, Takayoshi Nakano, Yukichi Umakoshi, Joseph D. Ferrara, and Toshihiko Sasaki…The same measurement was done with CuKα radiation. Copper Kα is the most commonly used radiation for powder diffraction because it provides good resolution of the resultant lines but is more cumbersome because it requires slicing the bone into t…
THE STRUCTURE OF CELLULOSESMasahisa Wada, Yoshiharu Nishiyama, Henri Chanzy, Trevor Forsyth, and Paul Langan…The detailed crystal structures determined for cellulose Iβ, an intermediate ammonia-cellulose I complex, and cellulose IIII, reveal a structural transition pathway: hydrogen bonded sheets of chains in cellulose Iβ slip with respect to each othe…
UNDERSTANDING THE COMET WILD 2 MINERALOGY IN SAMPLES FROM THE STARDUST MISSIONFrans J. M. Rietmeijer…This mission became the first successful sample- return mission since the Apollo project. This time the challenges were much less related to the availability of state-of-the-art analytical capabilities. Still, dedicated tools had to be developed…
X-RAY DIFFRACTION STUDIES OF LI-BASED COMPLEX HYDRIDES AFTER PRESSURE CYCLINGWen-Ming Chien, Dhanesh Chandra, and Joshua H. Lamb…The effects of pressure cycling are important for long- term reliability of Li-based hydrides. Commercial grade hydrogen containing low-level impurities (O2, H2O, CO/CO2) was used for this study to show the effect of cycling on hydrogen storage …

2006 – VOL50

AN ENVIRONMENTAL STAGE FOR IN-SITU STUDIES OF BIOPOLYMERS IN HIGH PRESSURE CO2A.V. Nawaby, P.S. Whitfield, X. Liao…This stage is designed to fit onto a normal laboratory powder diffractometer. Together with the use of MoKα radiation and a Bruker Våntec PSD detector, this stage will allow extensive studies on the kinetics of polymer crystallization under sub-…
AN EXAFS STUDY OF PHOTOGRAPHIC DEVELOPMENT IN PHOTOTHERMOGRAHIC FILMST.N. Blanton, D.R. Whitcomb, S.T. Misture…The results of the EXAFS analysis indicate that the intensity for the real-space peak for the Ag-O distance (~2.3 Å) decreases while the real-space peak for the Ag- Ag distance (~2.9 Å) grows with increasing thermal processing of the film. The c…
ANALYSIS OF LOW MASS ABSORPTION MATERIALS USING GLANCING INCIDENCE X-RAY DIFFRACTIONN.A. Raftery, L.K. Bekessy, J. Bowpitt…After conversion for the James relationship there is very little difference between the symmetric and asymmetric parallel beam data for 2θ > 2ω, however care must be taken to properly weight the data in the asymmetric case if it were to be used …
ANOMALOUS SCATTERING FROM SINGLE CRYSTAL SUBSTRATEL.K. Bekessy, N.A. Raftery, S. Russell…There is a broad weak feature at about the expected diffraction angle of 2θh`k`l` and a narrow feature whose position depends solely on the incidence angle. The broad feature is the Bragg diffraction of the X-ray tube spectral components while t…
DEPTH RESOLVED X RAY FLUORESCENCE ANALYSIS OF COPPER CHARGED MUSCOVITE MICAR. Simon, U. Kerdpin, F. Friedrich, W. Faubel, P. Weidler, R. Nüesch…For studies of delamination, the ITC-WGT institute has developed a method to intercalate polyvalent metal ions, like Cu2+, Mg2+, Zn2+ or Al3+ into muscovite. This paper refers to X-ray fluorescence analysis (XRF) of these samples at ANKA synchro…
DESIGN OF SINGLE BOUNCE MONO-CAPILLARY X-RAY OPTICSS. Cornaby, T. Szebenyi, R. Huang, D.H. Bilderback…We have been able to manufacture optics that have produced x-ray spot sizes from 5 to 50 μm, gains in intensity of 10 to 500, divergences from 2 to 9 milliradians, and working distances between the tip of the capillary to the focus ranging from …
DEVELOPMENT AND APPLICATION OF A THULIUM BASED INTERNAL STANDARD METHOD FOR HIGH ACCURACY NICKEL ANALYSISS. Reeves, D. Brown, J. Metz…XRF Scientific Ltd, 24/200 Canterbury Rd, Bayswater, Victoria 3153, Australia ABSTRACT We present a new, relatively inexpensive technique using a thulium (Tm) internally doped flux (type 12:22 SRT) developed by X-Ray Flux Pty.Ltd., and tested an…
DEVELOPMENT OF A QUANTITATIVE EDXRF METHOD FOR DETERMINING THE CONCENTRATION OF PALLADIUM APPLIED TO TOBACCOJ. Lipscomb, M. Chang, T. Danielson, C. Connell, S. Zimmermann…Control and standards were created in-house with different levels of Pd concentration. After application of the Pd in a salt solution, the tobacco had an average oven volatiles (OV) value of 27.6%. Three aliquots were analyzed at each concentrat…
FUNDAMENTAL PARAMETERS ANALYSIS OF ROHS ELEMENTS IN PLASTICSW.T. Elam, R.B. Shen, B. Scruggs, J.A. Nicolosi…XRF is a convenient method for detecting the presence and measuring the amounts of these elements. Reliably quantifying all of these elements in plastics typically requires a large number of standards that are not yet readily available. Because …
HIGH PRESSURE DEFORMATION STUDY OF ZIRCONIUMS.C. Vogel, H. Reiche, D.W. Brown…Studies of active deformation mechanisms, the interplay of deformation with texture and ultimately the development of predictive capabilities for deformation modeling are an active field of research. Parameters studied by diffraction are typical…
MECHANICS OF MICROELECTRONICS STRUCTURES AS REVEALED BY X-RAY DIFFRACTIONC.E. Murray, H. Yan, I.C. Noyan…Math., New York, NY 10027 ABSTRACT The presence of strain distributions within semiconductor features influences many aspects of their behavior. For example, microelectronic technology that incorporates strained silicon improves device performan…
MEDICAL APPLICATIONS OF X-RAY FLUORESCENCE FOR TRACE ELEMENT RESEARCHJ. Börjesson, S. Matsson…Toxic, nonessential, trace elements may cause tempo- rary or permanent damage to various organs and tissues in humans. There is thus a need to con- trol the concentrations. Knowledge of the relations between toxic effects and element concentra- …
NON-DESTRUCTIVE ANALYSIS OF A PAINTING, NATIONAL TREASURE IN JAPANY. Hayakawa , S. Shirono, S. Miura, T. Matsushima, T. Uchida…Several assumptions were made about the materials used in the red and white plum trees drawn on the right and left screen respectively, and the river drawn at the center. By the present investigation, the materials used for the paintings were re…
OPTIMIZATION OF A DRIED RESIDUE SPECIMEN PREPARATION METHOD FOR QUANTIFYING ANALYTES IN PLUTONIUM METAL USING WDXRFC.G. Worley, L.P. Colletti…This technique was developed to eliminate the potential for radioactive liquid to leak into the spectrometer, decrease specimen preparation time, and minimize waste. Samples were cast in µL quantities onto Kapton, and a surfactant was added to d…
PROPERTIES AND GENERAL USE OF THE X-RAY ELASTIC FACTORSB. Ortner…It is shown that the matrix Fij(φ, ψ, hkl) which is usually called X-ray elastic factors, behaves as a second rank tensor. Since this behaviour is the only criterion for the question of whether or not it is a tensor, the F-matrix must be regarde…
QUANTITATIVE ANALYSIS WITH THE TRANSITION EDGE SENSOR MICROCALORIMETER X-RAY DETECTORT. Jach, N. Ritchie,, J. Ullom, J.A. Beall…Two bulk samples of multielement glasses that have been previously characterized by chemical methods for use as standard reference materials were analyzed. The spectra were analyzed against standards using three different correction schemes. In …
RESIDUAL STRESS STATE OF HYDROXYAPATITE GRADED COATING ON CERAMIC SUBSTRATEL. Che, M. Gotoh, L. Yang, Y. Hirose…The present study aims to identify the residual stress distribution behavior in the coating by X-ray diffraction technique and to correlate it to the graded interlayer structure. Residual stress measurement results show the graded compound inter…
SIMULTANEOUS ANALYSIS OF NICKEL, COBALT AND IRON BASE ALLOYS USING THE FUNDAMENTAL PARAMETER METHODY. Kataoka, E. Furusawa, H. Kohno, T. Arai, A. Martin, H. Inoue, M. Mantler…The results obtained were satisfactory and demonstrated that the method can be applied to the analyses of both, major and trace elements using a multi-channel spectrometer. For example, 0.14wt% of accuracy was obtained for nickel within a concen…
SIMULTANEOUS REFINEMENTS WITH COMPLEX COMPOSITIONAL CONSTRAINTS – EXAMPLE OF SINGULAR VALUE DECOMPOSITION TO DIAGNOSE POOR MATRIX CONDITIONINGP.S. Whitfield, I.J. Davidson, P.H.J. Mercier, Y. Le Page, L.D. Mitchell, P.W. Stephens, L.M.D Cranswick, I.P. Swainson…SVDdiagnostic examines both the unprocessed and pre-conditioned matrices and outputs a ‘condition’ number as well as combinations of variables causing pseudo-singularity. Shrewd use of this diagnostic tool allowed structural details to be extrac…
STRESS MITIGATION OF X-RAY BEAMLINE MONOCHROMATORS USING A TOPOGRAPHY TEST UNITJ. Maj, G. Waldschmidt, A. Macrander, I. Koshelev, R. Huang, L.Maj, A. Maj…The device used to mount the crystal has been shown to be a major contributing source of stress. In this case, an adjustable mounting device is an effective method of reducing stresses and improve the rocking curve to levels much closer to ideal…
STRUCTURE DETERMINATION FROM POWDER DIFFRACTION DATA OF SOME MOISTURE-SENSITIVE NETWORK COORDINATION COMPOUNDSP.S. Whitfield, A. Abouimrane, I.J. Davidson…The phases LiX(succinonitrile)2 (X = PF6-, AsF6-, ClO4-) were identified as undesirable phases that formed at low salt concentrations in succinonitrile. The silver analogues of these systems also exist as crystalline phases, but the lithium salt…
STUDIES OF LOCAL AND INTERMEDIATE RANGE STRUCTURE IN CRYSTALLINE AND AMORPHOUS MATERIALS AT HIGH PRESSURE USING HIGH-ENERGY X-RAYSL. Ehm, S.M. Antao, J. Chen, D.R. Locke, F.M. Michel, C.D. Martin, T. Yu, P.L. Lee, P.J. Chupas, S.D. Shastri, Q. Guo, J.B. Parise…Parise1 1Department of Geosciences, Stony Brook University, Stony Brook, NY 11794-2100, USA 2Advanced Photon Source, Argonne National Laboratory, Argonne, IL 60439, USA 3X17B3, National Synchrotron Light Source, Brookhaven National Laboratory, U…
THE ANALYSIS OF STRESS DISTRIBUTION BASED ON MEASUREMENTS USING TWO METHODS OF X-RAY APPLICATIONB. Kucharska…The state of stress was examined in a standard steel tensile test specimen that had been previously ground and then statically loaded with an effective strain of 0.45% and 1%, respectively. Stress measurements were carried out by the sin2ψ metho…
THE CLAISSE-CALCULATOR OF SAMPLES ACIDITY APPLICATIONSF. Claisse…Its operation is briefly described. In addition, the Calculator has been used by the author to explain a) what causes the sample to have a preference for a given flux composition, and b) what causes molten glass sticking to crucibles and moulds….
UNIT CELL EXPANSION IN ERT2 FILMSM.A. Rodriguez, J.F. Browning, C.S. Frazer, C.S. Snow, R.G. Tissot, E.P. Boespflug…Texture analysis of an aged ErT2 film reveals a bimodal (111)/(200) out-of-plane preferred orientation. Sin2ψ analysis reveals significant in-plane macro- strain due to 3He formation/growth. The mechanistic origins regarding these observations a…
VALIDATION OF AN ALKALI REACTION, BORATE FUSION, X-RAY FLUORESCENCE METHOD FOR SILICON METALJ.R. Sieber, E.A. Mackey, A.F. Marlow, R. Paul, R. Martin…Suggested for this purpose by Blanchette (Adv. X-Ray Anal., 45, 415, 2002), the alkali reaction uses LiOH·H2O to convert Si to Li2SiO3. Lithium silicate is fused with lithium borate flux without damage to platinum ware. Once specimens are fused …
X-RAY FLUORESCENCE SPECTROMETRY: DEVELOPMENT OF EFFECTIVE FUSION PROCEDURES FOR LIME PRODUCTSJ.-P. Gagnon…XRF combined with borate fusion is commonly used in production laboratories because it provides fast and accurate analysis. Sample preparation problems arise with samples containing large amounts of carbonates. They are reported to foam and run …
X-RAY STRESS ANALYSIS EMPLOYING THE LATTICE PARAMETER ELLIPSOIDR.E. Ogilvie, U. Kaminaga, H. Sugiyama, J. Nicolich…The semi-axes of the ellipsoid will have the values of (r + εx), (r + εy), and (r + εz), which are replaced by dx, dy, and dz, or for the cubic case, ax, ay, and az. In this technique, at a particular Phi angle (see Figure 1), the two-theta posi…

2005 – VOL49

3D INTERACTIVE DATA LANGUAGE POLE FIGURE VISUALIZATIONC.S. Frazer, M.A. Rodriguez, R.G. Tissot…The data can also be used to calculate quantitative properties such as strain level and to minimize the peak-height texture effects in individual !-2! scans. The collection of the large data sets necessary for the analyses is facilitated by use …
A NEW AREA DETECTOR FOR HIGH-SPEED AND HIGH-SENSITIVITY X-RAY DIFFRACTION ANALYSIST. Taguchi…An XRD system equipped with a conventional 2-kW X-ray source and a D/teX-25 detector has been used to collect ultra-fast XRD patterns at a maximum speed of 160º2θ per minute, more than 30 times faster than a conventional speed of 5º2θ per minute…
ABNORMAL X-RAY EMISSION FROM INSULATORS BOMBARDED WITH LOW ENERGY IONSM. Song, K. Mitsuishi, M. Takeguchi, K. Furuya, R.C. Birtcher…Irradiation with He+, Ga+, Ar+, and Xe+ ions in energy from 5 to 100 keV induces strong characteristic X-ray emission from insulator targets but not from conductive ones. The phenomenon is different from the high energy ion induced X-rays, such …
APPLICATIONS OF X-RAY MICRODIFFRACTION IN THE IMAGING INDUSTRYT.N. Blanton…Case studies are described that demonstrate the use of microXRD for identification of phases, texture, and microstructure morphology of components used in imaging applications. INTRODUCTION Digital imaging is comprised of capture, storage and di…
AVERAGE AND GRAIN SPECIFIC STRAIN OF A COMPOSITE UNDER STRESS USING POLYCHROMATIC MICROBEAM X-RAYSH.A. Bale, J.C. Hanan, N. Tamura, E. Üstündag…In a composite material, however, as the microstructure approaches the fiber diameter, approximations based on a few grains may be misleading. Polychromatic microbeam X-ray diffraction on beamline 7.3.3 at the Advanced Light Source was used to o…
CHARACTER OF THE HIGH-TEMPERATURE STRUCTURAL CHANGES IN CSD2PO4 AND RBD2PO4W. Bronowska…At the transition temperature Ts = 501 K the crystal symmetry rises from monoclinic P21/m to cubic Pm-3m. On the cooling cycle, the high temperature cubic phase of CsD2PO4 persists to the temperature of approx. Ts- 40 deg. The high-temperature p…
CHARACTERIZING PROCESS SEMICONDUCTOR THIN FILMS WITH A CONFOCAL MICRO X-RAY FLUORESCENCE MICROSCOPEC.M. Sparks, E.P. Hastings, G.J. Havrilla, M. Beckstead…Unlike conventional MXRF, confocal MXRF can depth profile sample layers and reduce spectral background. Non-destructive quantification of the silicon dioxide (SiO2) concentration in hafnium silicate (HfSiO) thin films is an example of one applic…
COMPARISON OF TEXTURE IN COPPER AND ALUMINUM THIN FILMS DETERMINED BY XRD AND EBSDJ. Mueller, D. Balzar, R.H. Geiss, D.T. Read, R.R. Keller…However, due to principle differences in data acquisition these techniques can yield disagreeing results. In this paper, we aim to highlight possible error sources with given examples for aluminum and copper thin films. INTRODUCTION Texture in m…
CONSIDERATIONS FOR COLLECTING RELIABLE XRD RESIDUAL STRESS DATA ACROSS THE FULL 2THETA RANGEA.C. Vermeulen…For reliable results it is crucial that systematic errors are absent. The systematic errors considered in this paper are alignment errors like specimen displacement and incident beam misalignment. Verification measurements on a stress-free sampl…
CRYSTALLOGRAPHIC CHANGES IN ELECTRICALLY FATIGUED ACTUATORSJ. Mueller, D. Balzar, S. Hooker…Observed grain sizes were 2.5 m – 4_ m; coherently diffracting domain sizes were 20 nm – 80 nm. A reorientation of c- and a- domains as a result of electrical poling and fatigue was observed, together with changes in the amount of secondary phas…
DATA MINING WITH DIFFERENT TYPES OF X-RAY DATAC.K. Lowe-Ma, A.E. Chen, D. Scholl, C.J. Gilmore, R.J. Thatcher, W. Sverdlik…As optimal performance may not be uniformly distributed throughout parameter space, efficient tools for analyzing data and evaluating large areas of compositional or parameter space are needed. Data mining tools enable moving from the statistics…
DETECTION OF VISIBLE AND LATENT FINGERPRINTS BY MICRO-X-RAY FLUORESCENCEC.G. Worley, S.S. Wiltshire, T.C. Miller, G.J. Havrilla, V. Majidi…In the present work, the spatial elemental imaging capabilities of micro-X-ray fluorescence (MXRF) were used to visualize fingerprint patterns based on inorganic elements present in the prints. A major advantage of using MXRF is that the prints …
DETERMINATION OF THE ELEMENT DISTRIBUTION IN SAUROPOD LONG BONES BY MICRO-XRFR. Ferreyro, N. Zoeger, N. Cernohlawek, C. Jokubonis, C. Streli, P. Wobrauschek, M. Sander, A. Pyzalla…Element distribution maps enable correlations between bone architecture and spatial distribution of the chemical elements. The investigations reveal no significant macroscopic gradients in the element distribution across the fossil bone cross-se…
DEVELOPMENT OF PLASTIC CERTIFIED REFERENCE MATERIALS FOR XRF ANALYSIS (JSAC 0611-0615) CONTAINING PB, CD, CR; PART 1. SAMPLE PREPARATION AND HOMOGENEITY TESTK. Nakano, K. Tsuji, M. Kozaki, K. Kakita, A. Ono, T.Nakamura…Ltd., 2-4 Nakahara shin-machi, Tobata-ku, Kitakyusyu 804-0701 ; Japan 5) The Japan Society for Analytical Chemistry, 2-36-2, Nishigotanda, Shinagawa-ku, Tokyo 141-0031; Japan Abstract New plastic certified reference materials (CRMs) with Pb, Cd …
DEVELOPMENT OF THE MICROSTRUCTURE OF SEVERELY- PLASTICALLY DEFORMED MG ALLOY, ZK60G.M. Stoica, A.E.Payzant, L. Wu, H.H. Liao, J.E. Spruiell, P.K. Liaw…A larger microstrain was observed in the samples deformed by compression at room temperature, as compared to the samples ECAP-ed at 2600C. Crystallographic texture changes due to uniaxial compression suggested a twinning deformation contribution…
DEVELOPMENTS IN FORMULATION ANALYSES BY POWDER DIFFRACTION ANALYSIST.G. Fawcett, J. Faber, F. Needham, S.N. Kabekkodu, C.R. Hubbard, J.A. Kaduk…In this paper, we will focus on a complimentary development, the growth and application of a comprehensive database based on the Powder Diffraction File (PDF®). The PDF® is an edited and standardized combination of several crystallographic data…
ELECTRIC FIELD INFLUENCE ON EMISSION OF CHARACTERISTIC X-RAY FROM AL2O3 TARGETS BOMBARDED BY SLOW XE+ IONSJ.C. Rao, M. Song, K. Mitsuishi, M. Takeguchi, K. Furuya…The electric field influence on emission of the X-rays of constitute elements in the specimens was investigated. The energy dispersive X-ray spectroscopy (EDS) spectra show that the characteristic X-ray of Al-Kα seems to be depressed by the appl…
EXPERIMENTAL STUDY OF X-RAY ENERGY SPECTRUM FORMED BY PLANAR WAVEGUIDE-RESONATOR WITH SPECIFIC ELEMENT COMPOSITION REFLECTORSV.K. Egorov, E.V. Egorov…There was tested the features alteration of X-ray spectrum generated by tube with Co-anode in result of the beam formation by the specific planar radiation guide equipped by reflectors with surface layers contained Fe atoms great quantity. The m…
FACTORS AFFECTING IN-LINE PHASE CONTRAST IMAGING WITH A LABORATORY MICROFOCUS X-RAY SOURCEK.L. Kelly, B.K. Tanner…The effect of source size is considered, and by introducing water into the imaging path the influence of water on the phase contrast is determined. The results confirm that good phase contrast images can be achieved using a polychromatic laborat…
FULL SPECTRUM CALCULATIONS OF EDXRF SPECTRAW.T. Elam, B. Shen, B. Scruggs, J. Nicolosi…To evaluate the utility of such methods, we have calculated the full spectra of several compounds covering a wide range of compositions. The calculated spectra are compared directly with measured spectra. They include scattering of the X-ray tub…
FUNDAMENTAL PARAMETER METHOD USING SCATTERING X-RAYS IN X-RAY FLUORESCENCE ANALYSISY. Kataoka, N. Kawahara, S. Hara, Y. Yamada, T. Matsuo, M. Mantler…The concept of substituting a compound matrix by a single element of average atomic number has been efficiently applied to the analysis of biological samples, polymers, liquids, and powders where the non-measuring elements were unknown. It was f…
FUNDAMENTAL PARAMETER PROGRAMS: ALGORITHMS FOR THE DESCRIPTION OF K, L AND M SPECTRA OF X-RAY TUBESH. Ebel…The measurements were performed on 23 elements and acceleration voltages from 5kV to 30kV. Continuous spectra are described by a modified Kramers cross section. For absorption correction of continuous and characteristic spectra in the target Lov…
HIGH-RESOLUTION PARALLEL-BEAM POWDER DIFFRACTION MEASUREMENT OF SUB-SURFACE DAMAGE IN ALUMINA-SILICON CARBIDE NANOCOMPOSITEB.K. Tanner, H.Z. Wu, S.G. Roberts…ABSTRACT The sub-surface damage in ground and subsequently annealed alumina/silicon carbide nanocomposite has been studied by analysis of the x-ray diffraction line width as a function of incidence angle. Bragg peak broadening fell as the depth …
IDENTIFICATION OF PAINTING MATERIALS USED FOR MURAL PAINTINGS BY IMAGE ANALYSIS AND XRFS. Shirono, Y.Hayakawa…In this study, we investigated the materials used for the mural paintings in this tumulus directly and non-destructively using a combination of X-ray fluorescence (XRF) analysis for inorganic materials, and image analysis for organic materials. …
IN-SITU OBSERVATION OF CREEP DAMAGE IN AL-AL2O3 MMCS BY SYNCHROTRON X-RAY TOMOGRAPHYA. Pyzalla, B. Camin, B. Lehrer, M. Wichert, A. Koch, K. Zimnik, E. Boller, W. Reimers…Reconstructions of the gauge volume of the creep samples show the particle delamination, particle fracture, void formation and growth at 340°C at various stages of the creep process. KEYWORDS MMC, tomography, creep, damage, X-ray INTRODUCTION Co…
INFLUENCE OF GROWTH INTERRUPTION ON THE FORMATION OF SOLID-STATE INTERFACESI. Busch, M. Krumrey, J. Stümpel…For that purpose a series of different samples has been manufactured with molecular beam epitaxy (MBE). The introduction of growth interruptions of 50 s after the deposition of the layer leads to a change in the morphological properties of the i…
INVESTIGATING THE NATURE OF LINE BROADENING IN ELECTROCHEMICALLY DELITHIATED LI-XMMNRXWNIRX8CORX-OMP.S. Whitfield, S. Niketic, Y. Le Page, I.J. Davidson…Previous hypotheses attributing the phenomena to stacking faults can not explain all of the broadening features, as some of them (e.g. 003) disobey the selection rules expected of stacking faults in a cubic close-packed system (H-K = 3N ± 1). An…
INVESTIGATION OF LATERAL STRUCTURED INTERFACES WITH DXRS AND SPMI. Busch, G. Dai, J. Stümpel…The reciprocal scattering image (space map) contains the morphological structure of the interfaces of the system and provides statistical values of the critical parameters, such as the roughness σ and the correlation length ξ. With the measureme…
LABORATORY SYSTEM FOR X-RAY NANOTOMOGRAPHYA. Sasov…This spatial resolution in the volume terms is equal or better than can be achieved in synchrotron tomography, 5 orders better than in existing laboratory instruments and 10-12 orders better in comparison to clinical CT. The instrument is built …
LOBSTER EYE OPTICS FOR COLLECTING RADIATION OF A LASERPLASMA SOFT X-RAY SOURCE BASED ON A GAS PUFF TARGETA. Bartnik, H. Fiedorowicz, R. Jarocki, J. Kostecki, R. Rakowski, M. Szczurek, L. Pína, L. Švéda, A. Inneman…Soft X-rays in the wavelength range from about 3 nm to 20 nm were produced as a result of irradiation of a double- stream gas puff target with laser pulses of energy 0.8 J and time duration of about 3 ns. The spectra and absolute energies of sof…
MEASUREMENT AND MODELING OF INTERNAL STRESSES AT MICROSCOPIC AND MESOSCOPIC LEVELS USING MICRO RAMAN SPECTROSCOPY AND X-RAY DIFFRACTIONB. Benedikt, M. Lewis, P. Rangaswamy…Two types of strain sensors embedded in either chopped graphite fiber/epoxy matrix composite (MRS) or unidirectional graphite fiber/polyimide matrix composite (XRD) were investigated. For XRD measurements, the sensors were in the form of spheric…
MEASUREMENT OF STRAIN AND LATTICE TILT AT THE MARGINS OF THIN FILM ISLANDS ON SINGLE-CRYSTAL SUBSTRATES BY DOUBLE-CRYSTAL X-RAY TOPOGRAPHYP.M. Adams…Strain and deformation are concentrated along the film edges and were recorded as contrast in double-crystal X-ray topograph (DXRT) images. The contrast in the DXRT images was measured and was related to lattice deformation by means of the X-ray…
MEDICAL X-RAY IMAGING, CURRENT STATUS AND SOME FUTURE CHALLENGESE.L. Ritman…Major technical advances over the years, culminating in helical scanning, multi slice, x-ray computed tomography, can now provide ~ 0.5 mm3 resolution 3D images of the spatial distribution of tissue attenuation coefficients of an entire adult hu…
MICROTOMOGRAPHY OF AMORPHOUS METAL DURING THERMO-PLASTIC FOAMINGJ.C. Hanan, C. Veazey, M.D. Demetriou, F. DeCarlo, S. Thompson…A new method to produce metallic foam through a thermo-plastic expansion process has been discovered and characterized with microtomography. The new foaming process enables porosities unachievable through traditional metallurgical processes. The…
MONTE-CARLO MODELING OF SILICON X-RAY DETECTORSB. Cross, G. Bale, B. Lowe, R. Sareen…ABSTRACT A new 3-D Monte-Carlo code, X-Tracker, was developed to model internal events that occur as X-ray photons are absorbed within Si(Li) detectors. The goal was to model the performance of state-of-the-art detectors, including peak shapes, …
MULTI-MODE X-RAY STUDY OF SODIUM AND MAGNESIUM SULFATE ATTACK ON PORTLAND CEMENT PASTEN.N. Naik, A.C. Jupe, S.R. Stock, A.P. Wilkinson, P.L. Lee, K.E. Kurtis…However, despite over six decades of study, considerable uncertainty remains in optimally selecting and proportioning materials for sulfate resistance, and current understanding of the actual mechanisms of degradation in sulfate environments rem…
MULTI-SPECTRAL XRF COUNTING: SQUEEZE TWICE AS MUCH INFORMATION FROM YOUR DETECTORW.K. Warburton, P. Grudberg, J. Harris, G. Roach, B. Cross…Improving energy resolution ΔE helps by increasing peak/background ratio and providing a more accurate estimate of the background but also reduces counting statistics due to increased pileup losses. Time variant filtering techniques have not bee…
NEW OBSERVATIONS ON LIBR RELEASING AGENT LAYER IN FUSION BEADSF. Claisse…The composition of the layer is not pure LiBr but a mixture of bromides of Li and metallic ions from the sample. A small quantity of bromides are present inside the bead as droplets. Introduction For years, XRF analysts add lithium bromide (and …
OPTIMAL DESIGN OF TRANSMISSION GRATING FOR X-RAY TALBOT INTERFEROMETERW. Yashiro, A. Masada, A. Momose…Shape parameters of an amplitude grating used in XTI strongly affect the effi- ciency. We calculated efficiencies assuming rectangular and trapezoidal patterns for an ab- sorption grating. As a result, a rectangular absorption grating of a duty …
PARAMETER STUDIES FOR AN OPTIMIZED XRF-DETERMINATION OF PB IN BONEN. Cernohlawek, P. Wobrauschek, C. Streli, N. Zoeger…The intention of this work was to study the feasibility of in vivo L-shell XRF measurements of Pb in bone using X-ray tubes as excitation sources. Parameter studies using direct tube excitation with various anode materials (Mo and W) and filters…
PHASE IMAGING WITH AN X-RAY TALBOT INTERFEROMETERA. Momose, W. Yashiro, Y. Takeda, Y. Suzuki, T. Hattori…JASRI/SPring-8,Mikazuki, Hyogo 679-5198, Japan. dLaboratory of Advanced Science and Technology for Industry, University of Hyogo, 3-1-2 Kouto, Kamigori, Hyogo 678-1205, Japan. ABSTRACT X-ray Talbot interferometry (XTI) is described as a novel ph…
POWDER X-RAY DIFFRACTION DETECTION OF CRYSTALLINE PHASES IN AMORPHOUS PHARMACEUTICALSB.A. Sarsfield, M. Davidovich, S. Desikan, M. Fakes, S. Futernik, J.L. Hilden, J.S. Tan, S. Yin, G. Young, B. Vakkalagadda, K. Volk…Materials in the amorphous phase are less thermodynamically stable than any crystalline form, leading to a tendency for the amorphous materials to transform to a known or potentially unknown crystalline phase. The time scale for any transformati…
QUANTITATIVE ENERGY-DISPERSIVE ELECTRON PROBE X-RAY MICROANALYSIS OF INDIVIDUAL PARTICLESC.-U. Ro…The low-Z particle EPMA allows the quantitative determination of concentrations of low-Z elements such as C, N, and O, as well as higher-Z elements that can be analyzed by conventional energy- dispersive EPMA. The quantitative determination of l…
QUANTITATIVE RIETVELD ANALYSIS OF HYDRATED CEMENTITIOUS SYSTEMSL.D. Mitchell, P.S. Whitfield, J.C. Margeson…In order to obtain true quantitative results, the amorphous contents were determined by the addition of an internal standard. The amorphous content of the starting calcium trisilicate was found to be approximately 21-22 wt%, in close agreement w…
QUANTITATIVE TRANSPORT PROPERTIES OF GRANULAR MATERIAL CALCULATED FROM X-RAY PCT IMAGESM.A. Knackstedt, C.H. Arns, F. Bauget, A. Sakellariou, T.J. Senden, A.P. Sheppard, R.M. Sok…To enhance and add predictive power to the collected data, various analysis techniques have been developed. In this paper, transport properties calculated directly from the pore space morphology are presented for 36 porous granular specimens. Re…
RESIDUAL STRESS DISTRIBUTIONS IN GTA SPOT WELDED TI6AL4V DISKSJ. Sariel, I. Dahan, R. Reuven, M. Szanto, A. Stern…Disks of three thicknesses, 6.5, 8.5 and 10.5 mm were welded using several currents. The results were also compared to those obtained by the Hole- Drilling (HD) method, and by numerical simulations. The distributions obtained by all three method…
RESIDUAL STRESS MEASUREMENT OF CEMENTITE PHASE IN PLASTICALLY DEFORMED CARBON STEELSY. Horimoto, L. Che, M. Gotoh, Y. Hirose…For globular structure specimens, X-ray stress measurements of cementite were realized after pretreatments on them; Compressive residual stresses were observed in ferrite and tensile residual stresses in cementite; The residual stress in cementi…
RIETVELD TEXTURE ANALYSIS BY NEUTRON DIFFRACTION OF .HIGHLY ABSORBING MATERIALSH.M. Volz, S.C. Vogel, C.T. Necker, J.A. Roberts, A.C. Lawson, D.J. Williams, L.L. Daemen, L. Lutterotti, J. Pehl…Diffraction data were collected on the neutron powder diffractometer HIPPO at LANSCE from dysprosium and erbium, which are moderate to strong absorbers for thermal neutrons with absorption cross-sections of 159 barns for Er and 994 barns for Dy …
TEMPERATURE DEPENDENCE OF RESIDUAL STRESS IN TITANIUM NITRIDE COATINGS ON HAYNES 188 SUPERALLOYS.H. Ferguson, H.W. King…In the as-coated condition the TiN films have a pronounced [111] orientation texture and a compressive room temperature stress of -10.5 GPa. After heating for periods of 1h between 450 and 800 °C, the compressive residual stress was irreversibly…
THERMAL LATTICE EXPANSION IN EPITAXIAL SRTIO3(100) ON SI(100)D.E. McCready, Y. Liang, V. Shutthanandan, C. Wang, S. Thevuthasan…The SrTiO3 layer thickness (~400 Å) was determined a priori by ex situ X-ray reflectivity (XRR). In addition, the SrTiO3(100) film was further characterized before and after thermal treatment by Rutherford backscattering spectroscopy in channeli…
TIME-RESOLVED X-RAY IMAGING IN STUDIES OF ADVANCED ALLOY SOLIDIFICATION PROCESSESR.H. Mathiesen, L. Arnberg…These self-assembly solidification structures evolve in complex processes determined by the transport of heat and mass to and from the different constituents. The transport processes are also influenced and complicated by interacting mechanisms …
TIME-RESOLVED Μ-XRF AND ELEMENTAL MAPPING OF BIOLOGICAL MATERIALSK. Tsuji, K. Tsutsumimoto, K. Nakano, K. Tanaka, A. Okhrimovskyy, Y. Konishi, X. Ding…Xin Jie Kou Wai Da Jie; Beijing 100875; China Telephone: 62207171; E-mail: xld@ht.rol.cn.net Abstract We have developed a micro-XRF instrument using a polycapillary x-ray lens. In addition, a time-resolved MCA (multi channel analyzer) was instal…
UNTANGLING CATION ORDERING IN COMPLEX LITHIUM BATTERY CATHODE MATERIALS – SIMULTANEOUS REFINEMENT OF X-RAY, NEUTRON AND RESONANT SCATTERING DATAP.S. Whitfield, I.J. Davidson, L.M.D. Cranswick, I.P. Swainson, P.W. Stephens…Combining the information in X-ray and neutron data in simultaneous refinements has historically been a powerful tool. However, increasingly complex compositions require more information and element contrast than two datasets can provide. This p…
USE OF THE MONTE CARLO SIMULATION CODE CEARXRF FOR THE EDXRF INVERSE PROBLEMR.P. Gardner, F. Li, W. Guo…Then the Monte Carlo – Library Least-Squares (MCLLS) approach is used. This approach consists of using a forward Monte Carlo code (CEARXRF) that is capable of simulating the complete non-linear pulse-height spectral response of any EDXRF system….
X-RAY AND NEUTRON DIFFRACTION OF ERDK POWDERS B FILMSM.A. Rodriguez, J.F. Browning, C.S. Frazer, R.G. Tissot, S.C. Vogel, D.J. Williams, A. Llobet…Rietveld refinement results demonstrated sensitivity to deuterium site occupancy and distribution within the fluorite-type lattice. Powder refinements showed that the presence of 10% D at the octahedral site caused detectable contraction in the …
X-RAY BACKSCATTER IMAGING: PHOTOGRAPHY THROUGH BARRIERSJ. Callerame…In contrast to more commonly used transmission images, backscatter imaging involves positioning both source and detection apparatus on only one side of a target object. This presents the user with inspection opportunities in situations that may …
X-RAY MICROTOMOGRAPHIC IMAGING AND ANALYSIS FOR BASIC RESEARCHJ.H. Dunsmuir, S. Bennett, L. Fareria, A. Mingino, M. Sansone…Recent advances in source and detector design have produced conventional x-ray source instruments with comparable spatial resolution but with lower throughput and without element specific imaging[2]. Both classes of instrument produce 3D images …
X-RAY PHYSICS IN PLASTICS: LOW ABSORPTION KEEPS PHOTON IN PLAYJ.-C.A. Lee, P.J. Ramadge, B. Hubbard-Nelson, D.I. Feinstein…Because polymers are mainly composed of light elements, the x-ray mass attenuation depth is deeper. Polymer analysis requires a physical model with greater fidelity than Sherman’s model: 1) infinite sample thickness is no longer valid, 2) the inci…

2004 – VOL48

A MONTE CARLO CODE FOR SIMULATION OF PULSE PILE-UP SPECTRAL DISTORTION IN PULSE-HEIGHT MEASUREMENTW. Guo, R.P. Gardner, F. Li…Experimental verification was carried out by measuring an Fe-55 spectrum with a Si(Li) X-ray spectrometer. Based on the spectrum measured at low counting rate, which is considered to be the “true” spectrum with no pulse pile-up distortion, the p…
AN IN SITU HIGH-TEMPERATURE X-RAY DIFFRACTION STUDY OF PHASE TRANSFORMATIONS IN SILVER BEHENATET.N. Blanton, S. Zdzieszynski, M. Nicholas, S. Misture…In the absence of development chemistry silver behenate exhibits four phase transformations when heated from room temperature to 200 ºC. Combining XRD and differential scanning calorimetry (DSC) results, the phase transformation temperatures and…
BAYESIAN ANALYSIS OF CERIA NANOPARTICLES FROM LINE PROFILE DATAN.Armstrong, A. Dowd, J.P. Cline, W. Kalceff…The analysis is in general agreement with transmission electron microscopy results, while demonstrating the impor- tance of appropriate a priori information needed in the method. The analysis also identifies other microstructural effects, such a…
CHANGES IN ELASTIC-STRAIN PROFILES AROUND A CRACK TIP DURING TENSILE LOADING AND UNLOADING CYCLESY. Sun, H. Choo, P.K. Liaw, Y.L. Lu, B. Yang, D.W. Brown…Spatially-resolved strain measurements were performed on a 316 LN stainless steel to determine the in-plane (parallel to the loading direction) lattice-strain profiles ahead of the crack tip under a constant tensile load. The strain scanning was…
DEVELOPMENT OF A MONTE CARLO – LIBRARY LEAST-SQUARES (MCLLS) CODE PACKAGE FOR THE EDXRF INVERSE PROBLEMR.P. Gardner, W. Guo…It consists of a linear library least-squares (LLS) code and a comprehensive Monte Carlo code named CEARXRF that is capable of calculating the unknown sample spectrum, all the elemental library spectra in the sample, and the differential operato…
DEVELOPMENT OF XRD IN EL SALVADORE. de Henriquez…Interpretations of permeability and temperature have given a broader outlook of the geothermal system. XRD technique was not limited to the geothermal industry. Samples from different industries are being accepted, such as solid particles in air…
DIFFRACTION STUDIES OF ORDER-DISORDER AT HIGH PRESSURES AND TEMPERATURESJ.B. Parise, S.M. Antao, C.D. Martin, W. Crichton…European Synchrotron Radiation Facility, B. P. 220, F-38043 Grenoble, France BSTRCT Recent developments at synchrotron X-ray beamlines now allow collection of data suitable for structure determination and Rietveld structure refinement at high pr…
DISLOCATION DENSITIES AND CHARACTER EVOLUTION IN COPPER DEFORMED BY ROLLING UNDER LIQUID NITROGEN FROM X-RAY PEAK PROFILE ANALYSISI. Dragomir-Cernatescu, M. Gheorghe, N. Thadhani, R.L. Snyder…The crystallite size distribution and defects evolution were determined as a function of different reduction levels (e.g. 67%, 74%, 87%, and 97%). By using the Multiple Whole-Profile (MWP) fitting procedure the Fourier transforms of the experime…
ELEMENTAL IMAGING FOR PHARMACEUTICAL TABLET FORMULATION ANALYSIS BY MICRO X-RAY FLUORESCENCET. C. Miller, G.J. Havrilla…Recently imaging techniques, such as Raman, near-IR, and fluorescence imaging, have become popular for “visualization” of pharmaceutical formulations, allowing for spatial and chemical composition information to be obtained simultaneously. These…
ELEMENTAL MAPPING IN SLICES OF HUMAN BRAIN BY SR MU-XRFN. Zoeger, C.Streli, P. Wobrauschek, C. Jokubonis, G. Pepponi, P. Roschger, S. Bohic, W. Osterode…To determine the local distribution of lead (Pb) and other trace elements, X-Ray Fluorescence Spectroscopy (XRF) measurements have been performed, using a microbeam setup and highest flux synchrotron radiation. Experiments have been carried out …
ETCHING METHODS FOR IMPROVING SURFACE IMPERFECTIONS OF DIAMONDS USED FOR X-RAY MONOCHROMATORSJ.A. Maj, A.T. Macrander, G.J. Waldschmidt, S.F. Krasnicki, Y. Zhong, R. Khachatryan, Y.S. Chu, R. Erck, J. Woodford…However, due to imperfections in the diamond, the rocking curves of diamond crystals are wider (e.g, 30%) than the theoretical values. Proper etching of the diamond can reduce the effects of imperfections. We explore four etching techniques usin…
FAST IN-SITU X-RAY DIFFRACTION ANALYSIS DURING QUENCHING OF A BALL BEARING STEELT.K. Hirsch, A. da S. Rocha…Sample temperatures up to 900°C were reached with a specially-designed furnace, in which fast cooling of sample is executed by gas quenching. Stress development during quench- ing followed the expected transformation behavior for an AISI 52100 b…
FATIGUE-INDUCED PHASE FORMATION AND ITS DEFORMATION BEHAVIOR IN A COBALT-BASED SUPERALLOYM.L. Benson, T.A. Saleh, P.K. Liaw, H. Choo, D.W. Brown, M.R. Daymond, X.-L. Wang, A.D. Stoica, R.A. Buchanan, D.L. Klarstrom…Metals and Ceramics Division, Oak Ridge National Laboratory, Oak Ridge, TN 37831, USA 3. Los Alamos Neutron Science Center, Los Alamos National Laboratory, Los Alamos, NM 87545, USA 4. Department of Mechanical and Materials Engineering, Queen’s …
FIELD DEPLOYMENT OF A PORTABLE XRD/XRF INSTRUMENT ON MARS ANALOG TERRAINP. Sarrazin, D. Blake, S. Feldman, S. Chipera, D. Vaniman, D. Bish…A portable CheMin prototype was built to test the capability of the instrument for remote in-situ mineralogical characterization of geological materials. The instrument was successfully deployed at a variety of Mars analog sites in Death Valley,…
GETTING THE HOT STRUCTURESK.F. Kelton, A.K. Gangopadhyay…These studies have led to new insights into the liquid state and have revealed how local order in the liquid can dictate phase formation. In this article, levitation techniques are briefly discussed, focusing most on electrostatic levitation. Re…
IMPROVING ENERGY STABILITY IN THE NIST MICROCALORIMETER X-RAY DETECTORT. Jach, J.A. Small, D.E. Newbury…We report on some sources of energy scale drift in microcalorimeter X-ray detectors and the manner in which they have been addressed. Previously observed drifts of >10 eV/h have been reduced to 1-2 eV/h. This improved stability has resulted in t…
INVESTIGATION OF THE MICRO STRUCTURE OF ENERGETIC CRYSTALS BY MEANS OF X-RAY POWDER DIFFRACTIONM. Herrmann, H. Fietzek…Therefore an approach is made to quantify and characterize of the ener- getic powders RDX and HMX using X-ray diffraction. The mechanical properties of these cyclic nitramines are supposed to be dominated by different defect mechanisms – deform…
MEASUREMENT OF THE SILICON DIOXIDE CONCENTRATION IN HAFNIUM SILICATE GATE DIELECTRICS WITH A TXRFC.M. Sparks, P. Lysaght, T. Rhoad…This allows for the introduction of a physically thicker film with lower leakage current and with capacitance equivalent to a thinner (1.0 nm and below) SiO2 layer [1-3]. Although binary metal oxide films such as HfO2 and ZrO2 exhibit higher per…
MICRO XRF OF LIGHT ELEMENTS USING A POLYCAPILLARY LENS AND AN ULTRA THIN WINDOW SILICON DRIFT DETECTOR INSIDE A VACUUM CHAMBERP. Wobrauschek, B. Frank, N. Zoeger, C. Streli, N. Cernohlawek, C. Jokubonis, H. Hoefler…Though for some applications (e.g.: biological- and geological samples, samples from art and archeology) the extension to light elements is of great interest. Therefore µ-XRF measurements using a polycapillary lens mounted inside a vacuum chambe…
MICRO-XRF INSTRUMENT DEVELOPED IN COMBINATION WITH ATOMIC FORCE MICROSCOPEK. Tsuji, T. Emoto, Y. Matsuoka, Y. Miyatake, T. Nagamura, X. Ding…Xin Jie Kou Wai Da Jie, Beijing 100875, China ABSTRACT A new micro-XRF instrument was developed in combination with an atomic force microscope (AFM). A small pinhole of 5 or 10 µm was made on the AFM cantilever. The center of the micro X-ray bea…
MINIATURE X-RAY TUBES UTILIZING CARBON-NANOTUBE-BASED COLD CATHODESA. Reyes-Mena, C. Jensen, E. Bard, D.C. Turner, K.G. Erdmann, Q. Qiu, B. Gao, J. Lu, O. Zhou…MINIATURE X-RAY TUBES UTILIZING CARBON-NANOTUBE- BASED COLD CATHODES A. Reyes-Mena, Charles Jensen, Erik Bard, D. Clark Turner and K. G. Erdmann MOXTEK, Inc., Orem, UT 84057 Qi Qiu, Bo Gao, Jianping Lu and Otto Zhou XINTEK, Inc., Chapel Hill, NC…
NEW CORRECTION PROCEDURE FOR X-RAY SPECTROSCOPIC FLUORESCENCE DATA: SIMULATIONS AND EXPERIMENTJ.M. Ablett, J.C. Woicik, C.C. Kao…In the dilute limit, and for thin films, the X-ray fluorescence signal is directly proportional to the atomic sub-shell absorption coefficient. However, for concentrated samples, the well-documented self-absorption effect often leads to the seve…
NON-LINEAR 2 THETA-SIN2 PSI DIAGRAM BY SHOTPEENING ON SPRING STEELT. Sakakibara, Y. Sato…It is commonly known that a material under directional deformation exhibits non-linear 2θ-sin2ψ diagram (ψ-split ) due to the triaxial stress state. In this study, the residual stress distributions of spring materials deformed by shot peening at…
ON THE INFLUENCE OF GENERATOR AND DETECTOR SETTINGS IN X-RAY POWDER DIFFRACTOMETRYM.J. Fransen…With the introduction of photon-counting, 1- and 2-dimensional X-ray detectors, this effect has become more prominent than with the traditional diffraction geometry. In this paper, the influence of generator and detector settings on the fluoresc…
POWDER DIFFRACTION ANALYSIS OF HYDRAULIC CEMENTS: ASTM RIETVELD ROUND ROBIN RESULTS ON PRECISIONP. Stutzman…The ASTM C01.23 Compositional Analysis subcommittee developed test method C 1365 Standard Test for ‘Determination of the Proportion of Phases in Portland Cement and Portland-Cement Clinker Using X-Ray Powder Diffraction Analysis.’ A round-robin …
QUANTITATIVE ANALYSIS OF CALCIUM OXIDE DESICCANT CONVERSION TO CALCIUM HYDROXIDE USING X-RAY DIFFRACTIONT.N. Blanton, C.L. Barnes…When exposed to water, CaO converts to Ca(OH)2. X-ray diffraction techniques have been developed to study the conversion process and quantify the amount of CaO/Ca(OH)2 in powder and dispersed samples using the reference intensity ratio (RIR) met…
RESIDUAL STRESS MEASUREMENTS OF CAST ALUMINUM ENGINE BLOCKS USING DIFFRACTIOND.J. Wiesner, T.R. Watkins, T.M. Ely, S. Spooner, C.R. Hubbard, J.C. Williams…Materials Science and Engineering, Ohio State University, Columbus, OH 43210 ABSTRACT Residual stresses and strains in as-cast and annealed aluminum engine blocks were mapped in the main web area above the bearing split using diffraction. Automa…
RIETVELD PROCESSING OF PHASES IN HIGHLY TEXTURED REFRACTORY STEELSJ.L. Garin, R.L. Mannheim…These kinds of alloys usually contain strong preferred orientations due to dendritic solidification of the austenitic and ferritic solid solution phases, which must be taken into account whether accurate processing of powder diffraction data is …
SMALL-ANGLE X-RAY SCATTERING TO DISCERN MICROSTRUCTURE OF SEMICRYSTALLINE POLYANHYDRIDES FOR DRUG DELIVERYM.J. Kipper, S. Seifert, P. Thiyagarajan, B. Narasimhan…Cass Ave., Argonne IL, 60439. 3Intense Pulsed Neutron Source, Argonne National. Cass Ave., Argonne IL, 60439. ABSTRACT Polyanhydride copolymers based on 1,6-bis(p-carboxyphenoxy)hexane (CPH) and sebacic acid (SA) are bioerodible, semicrystalline…
SPATIALLY-TRANSIENT STRESS EFFECTS IN THIN FILMS BY X-RAY DIFFRACTIONC.E. Murray, C.C. Goldsmith, I.C. Noyan…For cases in which the material properties and/or the stress state are not homogeneous, traditional approaches may yield erroneous stress results. On the other hand, with proper care, relevant mechanical information about the system can be obtai…
STRESSES IN SHAPE MEMORY POLYMER-MATRIX NANOCOMPOSITES FOR BIOMEDICAL APPLICATIONSD. Balzar, G. Stefanic, K. Gall, M.L. Dunn, Y. Liu…After 50% compression of the composite material at 25 °C, the SiC particles exhibit a compressive stress, which is almost completely released during heated recovery at 120 °C. The residual stresses in SiC hexagonal (6H) phase were estimated thro…
TEMPERATURE EXPERIMENTS FOR IMPROVED ACCURACY IN THE CALCULATION OF POLYAMIDE-11CRYSTALLINITY BY X-RAY DIFFRACTIONP. Ricou, E. Pinel, N. Juhasz…Rilsan® Polyamide-11 (PA-11), produced by Arkema Inc., is a semi-crystalline polymer with an eleven-carbon repeat unit belonging to the general class of Nylon polymers. This material presents the peculiarity of having a smectic phase along with …
THE DIRECT DETERMINATION OF X-RAY DIFFRACTION DATA FROM SPECIFIC DEPTHSA. Broadhurst, K.D. Rogers, T.W. Lowe, D.W. Lane…A series of traditional data collections with varying angles of incidence are required, and the X-ray diffraction data arising from specific depths will be calculated by the transformation of these measured, angle-dependent spectra. These may th…
THE X-RAY RESPONSE OF SILICON DRIFT DETECTORST. Eggert…The calculations are in good agreement with the measurements for secondary electron charge cloud widths σsec of (85±7) nm below and (128±10) nm above 1.83 keV. The main background contribution arises from thermalized electrons escaping the activ…
TOWARDS FAST RECIPROCAL SPACE MAPPINGJ.F. Woitok, A. Kharchenko…The quality of the data benefits from the detector’s unique properties such as a high local linearity range and high dynamic range. This paper describes maps of symmetri- cal and asymmetrical reflections taken on different kinds of samples. A qu…
TRACE ELEMENT ANALYSIS USING A BENCHTOP TXRF-SPECTROMETERH. Stosnach…By analysing various heavy metals in raw and digested sewage as well as mercury in recycling glass, the suitability of the TXRF system for these kinds of applications could be proven. Based on this data, the benefits, disadvantages, and restrict…
TWO-DIMENSIONAL MAPPING OF RESIDUAL STRAINS IN 6061-T6 ALUMINUM ALLOY FRICTION STIR WELDSW. Woo, H. Choo, D.W. Brown, Z. Feng, P.K. Liaw, S.A. David, C.R. Hubbard…Three different weld specimens were prepared from a 6061-T6 aluminum alloy with the purpose of separating the effects of the frictional heat and plastic deformation on the residual strain distribution and the angular distortion in the weld plate…
VIBRATING SAMPLE HOLDER FOR XRD ANALYSIS WITH MINIMAL SAMPLE PREPARATIONP. Sarrazin, S. Chipera, D. Bish, D. Blake, D. Vaniman…The technique relies on vibrations generated in a sample holder to create movement of the powdered sample in the absence of macroscopic movement of the sample holder itself. The major benefits over conventional sample handling strategies are: 1)…
X-RAY DIFFRACTOMETRY STUDIES AND LATTICE PARAMETER CALCULATION ON KNO3-NH4NO3 SOLID SOLUTIONSW.-M. Chien, D. Chandra, J. Franklin, C.J. Rawn, A.K. Helmy…Ammonium nitrate (AN) is of great use for gas generators of automobile air bag systems. The X-ray diffraction results showed the single (AN) phase III from 5% to 20% KNO3 in NH4NO3 and up to 373 K, which is the important temperature range for th…
XRF ANALYSIS OF HARMFUL METALS COLLECTED ONTO FILTERS AS THIN LAYERS FROM WORKPLACE AIR: INTER-LABORATORY EXERCISER.D. Foster…Sets of prepared filter standards were used to “transport” a master calibration established on an X-ray spectrometer at the Health and Safety Laboratory (HSL) to a wide range of makes and types of X-ray spectrometers in over 20 participant labor…

2003 – VOL47

1- AND 2-DIMENSIONAL DETECTION SYSTEMS AND THE PROBLEM OF SAMPLE FLUORESCENCE IN X-RAY DIFFRACTOMETRYM.J. Fransen…In this paper, the influence of the chosen X-ray optical geometry on the fluorescent background is determined experimentally from diffractograms recorded on a series of 10 samples with elements ranging from Ti to Ga. The samples were measured wi…
A PHOTONEUTRON SOURCE FOR BULK MATERIAL STUDIESM.A. Reda, J.F. Harmon…We suggest a photonuclear-based neutron source, using an electron linear accelerator, which may provide an inexpensive method to perform neutron scattering and diffraction experiments. This paper reports the results of calculations using Monte C…
A BEHAVIOR OF ELASTIC AND PLASTIC STRAIN FOR (A + G) DUAL PHASE STAINLESS STEELS IN ROTATING BENDING TESTH. Hirose, M. Gotoh, T. Yano, T. Sasaki…It has good resistance to corrosion and oxidation. Therefore, this material should be use for the shaft of a car, the screws holding a ship together, and so on. In this study, the effect of residual stress and plastic deformation on fatigue stre…
A CLOSE LOOK AT ELECTROLYTIC MANGANESE DIOXIDE (EMD) AND THE G-MNO2 & E-MNO2 PHASES USING RIETVELD MODELINGD.E. Simon, R.W. Morton, J.J. Gislason…However, a Transmission Electron Microscopy (TEM) study of EMD observed only γ- MnO2 structure as revealed by atom planes with a 0.4 nanometer spacing along with crystal twinning. Rietveld refinement results of EMD x-ray diffraction patterns ind…
A NEW ANALYSIS METHOD FOR TWO-DIMENSIONAL X-RAY DATAJ.C. Hanan, E. Ustundag, J.D. Almer…One challenge is obtaining strain results from Debye-Scherrer rings originating from a few grains of material. In addition, results are typically desired from multiple rings over hundreds or thousands of exposures. Current two-dimensional analys…
A PLUG-IN PROGRAM TO PERFORM HANAWALT OR FINK SEARCH-INDEXING USING ORGANICS ENTRIES IN THE ICDD PDF-4/ORGANICS 2003 DATABASEJ. Faber, C.A. Weth, J. Bridge…The plug-in provides an adjustable search window and match window to account for experimental errors. Both Hanawalt [1,2] and Fink [3] search methods are incorporated. In this paper, we report search-indexing results obtained with the new PDF-4 …
ACCURACY OF STANDARDLESS FP ANALYSIS OF BULK AND THIN FILM SAMPLES USING A NEW ATOMIC DATABASEW.T. Elam, R.B. Shen, B. Scruggs, J. Nicolosi…The database is a recent compilation by Elam, Ravel, and Sieber that is intended for X-ray spectroscopy. We have extended this work to thin films and multiple layer coatings. Significant improvements in accuracy are obtained with the use of upda…
ADVANCES IN QUANTITATIVE XRD ANALYSIS FOR CLINKER, CEMENTS AND CEMENTITIOUS ADDITIONSG. Walenta, T. Fullmann…Thanks to the development of stable-functioning software and the use of high-performance detectors, a quantitative phase analysis by X-ray, including sample preparation, measurement and evaluation, can be performed in fewer than ten minutes. Thi…
ANALYSIS OF ART OBJECTS AND OTHER DELICATE SAMPLES: IS XRF REALLY NON-DESTRUCTIVE?M. Mantler, J. Klikovits…This study is related to paintings and illuminated manu- scripts, where the analytes are often inorganic pigments embedded into organic matrices such as fabrics (canvases), paper or parchment, binders, and varnish. We found that a typical measur…
APPLICATIONS OF X-RAY DIFFRACTION IN CONSERVATION SCIENCE AND ARCHAEOMETRYM.-C. Corbeil…Jordan; the yellow compound pararealgar (As4S4), which was identified for the first time in a painting; and magnesium cobalt arsenate, a violet pigment found in numerous paintings. X-ray diffraction also helped answer questions related to degrad…
APPLICATIONS OF X-RAY STRESS MEASUREMENT FOR INTERFACE AREA OF NI3AL SYSTEM INTERMETALLIC COMPOUND COATINGT. Murotani, T. Yano, H. Hirose, A. Ikenaga…China **Graduate School of Kanazawa University, Kakumamachi Kanawzawa Ishikawa 920-1192, Japan *** Kinjo University Research Center, Kasamamachi 1200, Matto Ishikawa 924-8511, Japan **** Graduate school of Engineering Osaka Prefecture University…
CARBON-NANOTUBE FIELD EMISSION X-RAY TUBE FOR SPACE EXPLORATION XRD/XRF INSTRUMENTP. Sarrazin, D. Blake, L. Delzeit, M. Meyyappan, B. Boyer, S. Snyder, B. Espinosa…Existing miniature X-ray tubes are limited by inefficient thermionic electron sources. We have investigated the potential of carbon nanotube (CNT) field emitters for improving the efficiency and durability of miniature X-ray tubes. CNT field emi…
CHARACTERIZATION OF THE EVOLUTIONARY ASPECTS OF GREAT WHITE SHARK TEETH BY X-RAY DIFFRACTION METHODS AND OTHER SUPPORTING TECHNIQUESM. Kesmez, J. Lyon, D.L. Cocke, J. Westgate, H. McWhinney, T.L. Grady…Grady# ABSTRACT In a research program to explore evolutionary aspects of structural changes in elasmobranch teeth, a natural composite material, dentine and enamel sections of fossilized Great White shark teeth (ranging in age from 4, 12 and 40 …
CHARACTERIZATION TECHNIQUES FOR MINIATURE LOW-POWER X-RAY TUBESA. Reyes-Mena, M. Moras, C. Jensen, S.D. Liddiard, D.C. Turner…The use of this chamber is an innovative approach that allows rapid imaging of the electron beam spot on the anode, as well as the spectral characterization of the tube. The beam- spot dimensions and location can be measured at several high-volt…
COINCIDENCE X-RAY FLUORESCENCE (CXRF) SPECTROMETRY FOR IN VIVO QUANTITATIVE MEASUREMENT OF BONE LEADW. Guo, R.P. Gardner…Based on the physics of atomic transition, certain fractions of the characteristic K-series X-rays and L-series X-rays are in true coincidence. With an advanced CAMAC data acquisition system, experimental results are presented and preliminary qu…
COMBINED X-RAY/NEUTRON RIETVELD REFINEMENT OF LN-DOPED PZT PEROVSKITESM.A. Rodriguez, T.J. Boyle, B.A. Tuttle…Resulting refined structural parameters indicated that the lattice parameters and volume changes in the tetragonal perovskite unit cell were consistent with A and/or B-site doping of the structure. Ce doping is inconsistent with respect to its r…
DESIGN OF EDXRF EQUIPMENT FOR THE NONDESTRUCTIVE STUDY OF PRINTSM. Ardid, J.L. Ferrero, C. Roldan, D. Juanes, J.L. Lluch, R. Vives, P. Punter…Parque Tecnológico. CEEI-Valencia. Centro de Negocios. C/ Benjamin Franklin, 12 E-46980 Paterna (Spain) 3Departament de Física Aplicada. Escola Politècnica Superior de Gandia. Universitat Politècnica de València.Cra. Nazaret-Oliva s/n. E-46730 (…
DETERMINING OPERATING LIFETIME OF LANDING WHEEL HUBS WITH PRD PORTABLE DIFFRACTOMETRA.V. Lutsao, B.N. Kodess, A.V. Kotelkin, S.A. Kononogov, D.B. Matveev, V. Mozalyov, A.D. Zvonkov…The example of residual stress determination in the landing wheel hubs with different service life (take-off-landing numbers) are presented. The assessment of the durability is based on the results of residual stress determination. INTRODUCTION …
DETERMINING X-RAY DIFFRACTION DATA AT VARYING DEPTHS – A PRELIMINARY THEORETICAL APPROACHA. Broadhurst, K.D. Rogers, T.W. Lowe, D.W. Lane…The method is non-destructive and requires only a series of traditional data collections, where the incident angle is varied. The measured spectra are transformed to give calculated X-ray diffraction data arising from different depths. This is i…
DEVELOPMENT AND APPLICATION OF LABORATORY X-RAY FLUORESCENCE HOLOGRAPHY EQUIPMENTY. Takahashi, K. Hayashi, E. Matsubara…Synchrotron radiation (SR) has been mainly used for the measurements because of extremely weak signals which are about 0.3 % of isotropic fluorescent radiation. The measurements limited to the use of a SR source clearly hinder from increasing th…
DEVELOPMENT OF A NEW POSITRON LIFETIME SPECTROSCOPY TECHNIQUE FOR DEFECT CHARACTERIZATION IN THICK MATERIALSF.A. Selim, D.P. Wells, J.F. Harmon, J.R. Williams…In those measurements, the residual stresses were reflected in the line shape parameters of the 511 keV annihilation peak. However, since positron lifetime spectroscopy is a powerful tool to distinguish between different types of defects, such a…
DEVELOPMENT OF AN ASTM STANDARD TEST METHOD ON X-RAY POWDER DIFFRACTION ANALYSIS OF HYDRAULIC CEMENTSP. Stutzman…The ASTM C01 (Cement) Committee formed a task group to investigate quantitative X-ray powder diffraction analysis that resulted in the ASTM C 1365 standard test for X-ray powder diffraction of portland cement clinker and portland cement. Estimat…
EVALUATING EXPERIMENTAL METHODS AND TECHNIQUES IN X-RAY DIFFRACTION USING 280,000 DATA SETS IN THE POWDER DIFFRACTION FILET.G. Fawcett, S.N. Kabekkodu, J. Faber, F. Needham, F. McClune…The PDF is available in two products, PDF-4/Full File and PDF-4/Organics, which allow users to access and query over 150 million filled entry fields. An editorial database is used to generate the commercial products that contain tables of experi…
FINDING DESCRIPTORS USEFUL FOR DATA MINING IN THE CHARACTERIZATION DATA OF CATALYSTSC.K. Lowe-Ma, A.R. Drews, A.E. Chen…For X-ray data to be successfully included in statistical or data mining methodologies that examine contributions to a response function, sufficient pieces of information of the right kind must be extracted from the X-ray data. Traditional X-ray…
GRAZING INCIDENCE IN-PLANE X-RAY DIFFRACTION IN THE LABORATORYB.K. Tanner, T.P.A. Hase, T.A. Lafford, M.S. Goorsky…Low resolution, high intensity measurements are illustrated in the study of the in-plane lattice parameters and texture of a thin polycrystalline ZnO film on glass, the in-plane order in Cd arachidate Langmuir-Blodgett films, and the depth depen…
IMPROVEMENTS IN LOW POWER, END-WINDOW, TRANSMISSION-TARGET X-RAY TUBESC. Jensen, S.M. Elliott, S.D. Liddiard, A. Reyes-Mena, M. Moras, D.C. Turner…Several recent improvements have been achieved to make these tubes considerably brighter, with better output stability and even smaller size and lower power consumption for handheld instrumentation. Areas of the tube that have been improved incl…
IMPROVEMENTS IN XRF SPECIMEN PREPARATION USING THE DRIED RESIDUE METHOD: GALLIUM IN PLUTONIUM METALC.G. Worley, L.P. Colletti…Several modifications were made to a dried residue specimen preparation method for quantifying gallium in plutonium metal in order to improve the method accuracy and precision. Ion exchange chromatography was utilized to remove the plutonium pri…
IN SITU MEASUREMENT OF GROWTH STRESS IN ALUMINA SCALEE.D. Specht, P.F. Tortorelli, P. Zschack…ISSN 1097-0002IN SITU MEASUREMENT OF GROWTH STRESS IN ALUMINA SCALE E.D. Specht and P. F. Tortorelli etals and Ceramics Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA P. Zschack University of Illinois at Urbana-Champaign, Arg…
IN-SITU HIGH TEMPERATURE PHASE TRANSFORMATIONS IN RARE EARTH NIOBATESK. Jurkschat, P. Sarin, L.F. Siah, W.M. Kriven…So far these phase transformations have mainly been studied either at low temperatures (for instance in LaNbO4) or in specimen that have been quenched after heat treatment. Here, high temperature phase transformations of rare earth niobates have…
INVESTIGATION OF THE EFFECT OF USING VARIOUS OPTICS CONFIGURATIONS WITH PROPORTIONAL AND POSITION-SENSITIVE DETECTORSM.J. Kirkham, S.A. Speakman, C.J. Rawn…Incident beam optics used for data collection consisted of a polycapillary X-ray lens, a graded multilayer parabolic X-ray mirror, and programmable divergence slits. Peak position, width, and intensity were studied with respect to the different …
MATERIALS CHARACTERIZATION USING A NOVEL SIMULTANEOUS NEAR INFRARED/X-RAY DIFFRACTION INSTRUMENTT. Blanton, C. Barnes, J. Putrelo, A. Yeboah, S. Switalski…Though convenient to use in a laboratory setting, XRD is not easily adapted to in situ monitoring of synthetic chemical production applications or thin film depositions. Near- infrared spectroscopy (NIR) can be adapted to in situ manufacturing s…
MEASURING SOME ENVIRONMENTALLY SENSITIVE ELEMENTS USING WAVELENGTH DISPERSIVE X-RAY SPECTROMETRYD.L. Wertz, A. Winters, T. Craft, D. Bratton, H. Williams, D. Patrick, R.A. Lemire…At each firing point, a grid of 13 sample sites has been selected. Special attention has been given to measuring the abundances of aluminum and of chloride at these sample sites. INTRODUCTION Certain artillery units of the United States Army and…
MINIMIZATION OF ERRORS DUE TO MICROABSORPTION OR ABSORPTION CONTRASTB.M. Pederson, K.J. Schaible, R.S. Winburn…One of these is microabsorption. Microabsorption has historically been accounted for using the Brindley correction or mainly ignored. This correction has come under much debate in recent years. This study focuses on examining factors that will a…
MIRROR-BASED X-RAY FLUORESCENCE MICROPROBES AT THE ADVANCED PHOTON SOURCE AND THE NATIONAL SYNCHROTRON LIGHT SOURCES.R. Sutton, M. Newville, P. Eng, M. Rivers, A. Lanzirotti…Kirkpatrick-Baez mirrors are being increasingly utilized for production of X-ray microbeams (~ µm) because of their achromaticity, photon density gains in excess of 104, and long working distances (centimeters). Two such instruments reside at th…
ON-STREAM XRF ANALYSIS OF HEAVY METALS AT PPM CONCENTRATIONSG. Roach, J. Tickner…The accuracy of the analyser has been determined to be ±2 ppm (1 sigma). Improvements are planned that will significantly increase the speed and accuracy of the analyser and facilitate its adaptation to online / byline monitoring of mineral proc…
PORTABLE XRF ANALYSIS OF JAPANESE HISTORICAL OBJECTSB. Newbury, B. Stephenson, J. Almer, M. Notis, G.S. Cargill, III, G.B. Stephenson, D. Haeffner…In order to meet this problem, a portable XRF has been recently developed and enables elemental analysis for any object at any place. The instrument is based on energy dispersive XRF, and consists of a body approximately five-kilograms for X-ray…
QUANTITATIVE ANALYSIS BY X-RAY INDUCED TOTAL ELECTRON YIELD (TEY) COMPARED TO XRFAH. Ebel…Whereas the sampling depth of XRFA is determined by photoelectric absorption, for TEY the escape probability of electrons reduces this quantity to values of less than 100 nm. Thus, TEY is practically a surface analytical method with sampling dep…
RESIDUAL STRESS DISTRIBUTION IN GRAIN-ORIENTED SILICON STEELM. Imafuku, T. Suzuki, H. Suzuki, K. Akita…Dotted cavity lines were formed by Nd:YAG laser with a power density of 3.3 mJ/pulse for the laser- irradiated sample. By using a newly developed X-ray stress measurement method for a single crystal, the tensile residual stresses of 70-160 MPa w…
RESIDUAL-STRAIN DETERMINATION BY LEAST-SQUARES REFINEMENT OF TOF NEUTRON-DIFFRACTION MEASUREMENTS OF DEFORMED URANIUMN. C. Popa, D. Balzar, G. Stefanic, S. Vogel, D. Brown, M. Bourke, B. Clausen…The strain tensor was determined by the least-squares refinement of interplanar spacings for 19 Bragg reflections, as determined from the neutron TOF measurements at LANSCE. An annealed uranium plate was used as a reference sample, thus providin…
RETRACTABLE KNIFE-EDGE FOR XRD COMBINATORIAL SCREENINGB.B. He, F.F. Jin, U. Preckwinkel, K.L. Smith…The knife-edge can control the size of the viewed diffracting sample surface, so as to improve diffraction resolution and eliminate cross contamination between adjacent cells in the materials library. It also reduces the background by blocking o…
RIETVELD REFINEMENT OF XRD AND ND: ANALYSIS OF METASTABLE QANDILITE-LIKE STRUCTURESG. Kimmel, J.W. Richardson, R. Xu, P. Ari-Gur, E. Guncharov, J. Zabicky…Metastable phases, produced between 873 and 973 K from xerogels with Mg/Ti atomic ratios in the range ~1.1 < r ≤ 2, were studied by XRD and ND. XRD analysis showed crystal structures similar to that of Mg2TiO4 (qandilite), an inverse spinel of c…
SHOCK-INDUCED DEFORMATION OF TUNGSTEN POWDERD.W. Richards, R.J. DeAngelis, M.P. Kramer, J.W. House, D.A. Cunard, D.P. Shea…Samples of the tungsten powder were recovered and investigated to characterize the structural effects of detonation. Broadened X-ray diffraction profiles obtained from the shocked tungsten powder were analyzed employing double order and single o…
SILICON DRIFT DETECTORS FOR HIGH RESOLUTION, HIGH COUNT RATE X-RAY SPECTROSCOPY AT ROOM TEMPERATUREP. Lechner, C. Fiorini, A. Longoni, G. Lutz, A. Pahlke, H. Soltau, L. Struder…Vinci 32, I-20133 Milano, Italy ABSTRACT An advanced Silicon Drift Detector (SDD) for X-ray spectroscopy designed and fabricated at the MPI semiconductor laboratory has the input transistor of the amplifying electronics integrated on the detecto…
SIMULTANEOUS MEASUREMENT OF X-RAY DIFFRACTION (XRD) AND DIFFERENTIAL SCANNING CALORIMETRY (DSC) DATA UNDER CONTROLLED HUMIDITY CONDITION: INSTRUMENTATION AND APPLICATION TO STUDIES ON HYDRATION, DEHYDRATION AND RE-HYDRATION PROCESSES OF PHARMACEUTICAL COA. Kishi, H. Toraya…Examples of application to studies on hydration, dehydration and re-hydration processes of pharmaceutical compounds under various humidity conditions are presented. Usefulness of the present XRD-DSC system will be demonstrated. INTRODUCTION Hydr…
STATE-OF-THE-ART SILICON DETECTORS FOR X-RAY SPECTROSCOPYP. Lechner, R.Hartmann, P. Holl, G. Lutz, N. Meidinger, M. Porro, R.H. Richter, G. Schaller, F. Schopper, H. Soltau, L. Struder, J. Treis…Vinci 32, I-20133 Milano, Italy ABSTRACT The semiconductor laboratory of the Max-Planck-Institutes for physics and for extraterrestrial physics develops and fabricates silicon sensors for scientific experiments in astronomy and high- energy phys…
STRAIN EFFECTS IN THIN FILM / SI SUBSTRATES REVEALED BY X-RAY MICRODIFFRACTIONC.E. Murray, I.C. Noyan, B. Lai, Z. Cai…Residual tensile stress in 1 µm thick, 190 µm diameter Ni dots of 990 MPa imparted an average compressive stress in the underlying Si substrate. Ni Kα fluorescence scans, acquired simultaneously with Si (333) diffraction data, allow for a precis…
STRESS ERRORS ASSOCIATED WITH MINIATURIZATION OF PSI ASSEMBLY X-RAY STRESS ANALYZERST. Goto…As a concluion, it was found that stress errors increase with decreasing goniometer size, and it is believed that the goniometer size could be optimized by the approach adopted in this study. INTRODUCTION There are many mechanical parts whose un…
STRUCTURAL CHARACTERIZATION OF SIGE AND SIGE:C HETEROSTRUCTURES USING A COMBINATION OF X-RAY SCATTERING METHODSJ.F. Woitok…One main focus of the analysis is to derive a sample model that sufficiently describes all experimental data sets. In addition, the reliability of parameters extracted by just one single method is discussed. It turned out that XRR is more sen- s…
STUDY ON MEASUREMENT TECHNIQUE FOR LATTICE SPACING AT STRAIN FREE BY NEUTRON DIFFRACTION METHODT. Saito, N. Minakawa, Y. Morii, Z. Xiao, T. Sasaki, Y. Hirose…China ** Japan Atomic Energy Research Institute, Tokai-mura, Ibaragi, 319-1195, Japan ***Dept. of Materials Science and Engineering, Kanazawa University, Kakuma-machi, Kanawzawa, Ishikawa, 920-1192, Japan ABSTRACT For precise stress analysis of …
SYNCHROTRON APPLICATIONS IN ARCHAEOMETALLURGY: ANALYSIS OF HIGH ZINC BRASS ASTROLABESB. Newbury, B. Stephenson, J. Almer, M. Notis, G.S. Cargill, III, G.B. Stephenson, D. Haeffner…Argonne National Laboratory, Argonne, IL, USA ABSTRACT Synchrotron X-rays were used to perform non-destructive transmission diffraction and fluorescence experiments on a group of 24 European and Islamic astrolabes dated between 1350- 1720 A.D. i…
TEXTURE AND MICROSTRUCTURE ANALYSIS WITH HIGH-ENERGY SYNCHROTRON RADIATIONH.J. Bunge…In order to achieve extremely high angular- combined with very high lateral resolution a continuous sweeping technique with an area detector was employed. This technique “images” three different types of two-dimensional sections and projections …
TEXTURE MEASUREMENTS USING THE NEW NEUTRON DIFFRACTOMETER HIPPO AND THEIR ANALYSIS USING THE RIETVELD METHODS.C. Vogel, C. Hartig, L. Lutterotti, R.B. Von Dreele, H.-R. Wenk, D.J. Williams…The orientation distribution function (ODF) is extracted from multiple neutron time-of-flight histograms using the full-pattern analysis first described by Rietveld. Both, the well-established description of the ODF using spherical harmonics fun…
THERMALLY-INDUCED STRESSES IN THIN ALUMINUM LAYERS GROWN ON SILICONE. Eiper, R. Resel, C. Eisenmenger-Sittner, M. Hafok, J. Keckes…The films with a thickness of 2 µm were deposited by magnetron sputtering at different temperatures, and XRD measurements were carried out with the heating stage DHS 900 mounted on a Seifert 3000 PTS diffractometer. The strains were characterise…
ULTRA-TRACE SPECIATION OF NITROGEN COMPOUNDS IN AEROSOLS COLLECTED ON SILICON WAFER SURFACES BY MEANS OF TXRF-NEXAFSS. Torok, J. Osan, B. Beckhoff, G. Ulm…The aerosol samples of different size fractions were deposited on silicon wafer surfaces in a May impactor. Using a thin window Si(Li) detector, TXRF detection limits for nitrogen are in the upper fg and lower pg range. Taking advantage of the t…
USE OF XRD PATTERNS TO EVALUATE COMPRESSIVE STRENGTH OF STABILIZED AGGREGATESN.N. Khoury, M. Zaman, J.G. Laguros…Two commonly used aggregates in Oklahoma: (1) Meridian, a limestone aggregate, and (2) Hanson, a rhyolite aggregate, were utilized in this study. Cylindrical specimens were compacted and cured for 1 hour, 3, 28, and 90 days prior to unconfined c…
USING XRF ANALYSIS TO DEVELOP A HIGH-TECH BUSINESSD.L. Wertz, G. Schnaubelt, D. Bratton, V. Viner, T. Craft, K. Vigour, C.D. Deaton…Each of the products is produced from WOMBAT tire-derived powder, whose production is monitored by WDXRF on a day-to-day basis. Currently, the most important product is a low polluting fuel which is co-blended from tire-derived powder and biomas…
X-RAY EXAMINATION OF FRACTURE SURFACE OF DENTAL MATERIALA. Umeda, H. Hirose, M. Gotoh, T. Saito…Mechanical Engineering, Dalian Institute of Light Industry Qinggog Yuan, Ganjinzi District, Dalian, P.R. 116034, China ABSTRACT X-ray diffraction observation of metal fracture provides fracture analysis with useful information on the mechanics a…
X-RAY MICRODIFFRACTION STUDY OF THE HALF-V SHAPED SWITCHING LIQUID CRYSTALK.Takada, T.Noma, T.Togano, T.Mukaide, A.Iida…The HV-FLC is a FLC that has cholesteric – chiral smectic C (Ch – SmC*) phase transition sequences. X-ray microdiffraction measurements revealed that the SmC* phase in the HV-FLC was composed of asymmetric chevron and inclined-bookshelf structur…
X-RAY POWDER DIFFRACTION DATA FOR NA8(ALSIO4)6(REO4)2D.E. McCready, S.V. Mattigod, J.S. Young, B.P. McGrail…Rietveld refinement shows this compound adopts the primitive cubic structure of sodalite (S.G. #218) with a = 9.1528 (1) Å [3]. The calculated value of the reference intensity ratio (I/Ic) is 7.54. The experimental density (Dm) is 2.98 (1) g/cm3…
X-RAYS IN ART AND ARCHAEOLOGY ? AN OVERVIEWM. Schreiner, B. Fruhmann, D. Jembrih-Simburger, R. Linke…X-ray radiography e.g. is a standard technique widely used and accepted by art historians, archaeologists, curators and conservators as this method enables information about the manufacturing process and the condition of an object without “touch…
XRD AND XAFS STUDIES OF CARBON SUPPORTED PT-RU ELECTROCATALYST IN A POLYMER-ELECTROLYTE-FUEL-CELLH. Yashiro, K. Hoshino…XRD analysis identified a face-centered-cubic (fcc) alloy structure for Pt-Ru. XAFS analysis revealed that Pt and Ru atoms were, however, not randomly distributed in the Pt-Ru fcc lattice. A Pt atom was more likely surrounded by Pt atoms, wherea…

2002 – VOL46

A HIGH-TEMPERATURE POWDER DIFFRACTION FURNACEM.D. Dolan, S. Zdzieszynski, S.T. Misture…This paper will describe the technical specifications of the new instrument, and will present temperature calibration with standard reference materials and measurement of phase evolution in an industrial glass batch as illustrations of instrumen…
A NEW SMALL ANGLE X-RAY SCATTERING TECHNIQUE FOR DETERMINING NANO-SCALE PORE/PARTICLE SIZE DISTRIBUTIONS IN THIN FILMY. Ito, K. Omote, J. Harada…In order to avoid strong specular reflection, we used offset scan (2θ / θ+δθ) for measuring scattering data. To deal with reflection and refraction at surface and interfaces, we calculated X-ray wave field in the film based on Distorted Wave Bor…
ACCURATE QUANTIFICATION OF RADIOACTIVE MATERIALS BY X-RAY FLUORESCENCE: GALLIUM IN PLUTONIUM METALC.G. Worley…The steps necessary to handle such materials safely will also be discussed. Quantification of plutonium samples by a well- established aqueous specimen preparation method resulted in relative precision and accuracy values of well less than 1%. A…
ANALYSIS OF GEOLOGIC MATERIALS USING RIETVELD QUANTITATIVE X-RAY DIFFRACTIONR.M. Gonzalez, T.E. Edwards, T.D. Lorbiecke, R.S. Winburn, J.R. Webster…To assess the success of the RQXRD method, the bulk mineralogy of the dacite was determined through a combination of optical study of phenocrysts (plagioclase, augite, orthopyroxene, and Fe-Ti oxide) and detailed study of the groundmass using a …
ANALYSIS OF THE SURFACE MORPHOLOGY OF CVD-GROWN DIAMOND FILMS WITH X-RAY DIFFRACTIONM.J. Fransen, J. te Nijenhuis, J.H.A. Vasterink, R.L. Stolk, J.J. Schermer…Phase identification showed the presence of crystalline molybdenum carbide at the interface, as well as the incorporation of a small amount of non-diamond carbon throughout the diamond layer. The pole figures revealed a change in texture with in…
ANISOTROPIC STRAIN-LIKE LINE BROADENING DUE TO COMPOSITION VARIATIONSA. Leineweber, E.J. Mittemeijer…A nearly Gaussian purely strain-like broadening was observed. The broadening is strongly orientation dependent. For each direction of the diffraction vector relative to the crystallographic axes the width of the reflections varies proportional t…
ANNEALING STUDIES OF PURE AND ALLOYED TANTALUM EMPLOYING ROCKING CURVESD.W. Richards, M.P. Kramer, J.W. House, R.J. De Angelis…In this investigation X-ray rocking curves were employed to characterize the microstructure and further the understanding of the mechanisms of annealing. Plate material produced from the alloyed tantalum demonstrated annealing stages 300ºC highe…
APPLICATION OF SYNCHROTRON EDXRD STRAIN PROFILING IN SHOT PEENED MATERIALSI. Zakharchenko, Y. Gulak, Z. Zhong, M. Croft, T. Tsakalakos…The near surface compression, induced by shot peening, has made it a classic industrial technique to extend the loading limits and fatigue lives of materials. We have measured the detailed depth variation of the strain, in high carbon spring ste…
APPLICATION OF THE BACKSCATTER FUNDAMENTAL PARAMETER METHOD WITH SIMULTANEOUS EXCITATION BY 55FE AND 109CD RADIOISOTOPE SOURCESD. Wegrzynek, A. Markowicz, E. Chinea-Cano, S. Bamford, P.J. Potts…Mickiewicza 30, 30-059 Krakow, Poland 3) Department of Earth Sciences, The Open University, Walton Hall, Milton Keynes, MK7 6AA, United Kingdom ABSTRACT The backscatter fundamental parameter (BFP) method has been applied for determination of ele…
APPLICATIONS OF X-RAY DIFFRACTION IN THE IMAGING INDUSTRYT.N. Blanton…Silver halide grains precipitated as multicomponent AgBr1-xIx phases were found to be comprised of a core with three shells. The composition of the core and shells was determined using lattice constant measurements. Nanocomposites for photograph…
CALIBRATION OF DIFFRACTOMETERS II: INTERNAL CONSISTENCY AND THE BALANCEG. Berti, M. D’Acunto, U. Bartoli, F. De Marco…Reproducibility, repeatability, and accuracy increased when calibration procedures are taken into account. The evaluation of internal consistency is required for a good quality calibration process, a good check of the optical alignment, and accu…
CHARACTERIZATION OF THE SOLIDS WASTE IN THE HANFORD WASTE TANKS USING A COMBINATION OF XRD, SEM AND PLMR.W. Warrant, G.A. Cooke…Approximately 330,000 metric tons of sodium-rich radioactive waste originating from separation of plutonium from irradiated uranium fuel is stored in 177 underground tanks at Hanford. Current plans call for much of this waste to be vitrified and…
COMPARISON BETWEEN CONVENTIONAL AND TWO-DIMENSIONAL XRDB.B. He, U. Preckwinkel, K.L. Smith…A two-dimensional XRD system for combinatorial screening in transmission mode is introduced. IINTRODUCTION A two-dimensional X-ray diffraction (XRD2) system has both the capability of acquiring diffraction patterns in 2D space simultaneously, an…
CRYSTAL STRUCTURE DETERMINATIONS OF THREE-LAYER AURIVILLIUS CERAMICS USING A NEW PARALLEL BEAM X-RAY POWDER DIFFRACTOMETERM.S. Haluska, S. Speakman, S.T. Misture…The intent of this study was to determine the feasibility of parallel beam data in a research environment. These results were compared to those previously obtained using a typical divergent beam diffractometer. In general, the refinement results…
CURVATURE MEASUREMENTS OF STRESSED SURFACE-ACOUSTIC-WAVE FILTERS USING BRAGG ANGLE CONTOUR MAPPINGP.M. Adams…The performance of these devices is critically dependent on the spacing and geometry of the interdigitation. Any manufacturing process errors that affect the geometry of the transducers and/or the surface acoustic wave speed will affect the devi…
DEVELOPMENT OF MEASURING SYSTEM FOR STRESS BY MEANS OF IMAGE PLATE FOR LABORATORY X-RAY EXPERIMENTK. Hiratsuka, T. Sasaki, K. Seki, Y. Hirose…An image plate (IP) was used in this study as an area detector. A stress measuring system using an X-ray two-dimensional detector was developed. This was designed in order to be used in the authors’ X-ray laboratory. The background and the purpo…
DEVELOPMENT OF WAVELENGTH DISPERSIVE X-RAY FLUORESCENCE SPECTROMETER USING A MULTI-CAPILLARY X-RAY LENS FOR X-RAY DETECTIONY. Horino, Y. Mokuno, T. Narusawa, S. Kuwabara, S. Shibata, H. Soejima…We installed a MCX into the X-ray detection side (ie. the crystal spectrometer side) of a conventional WD-XRF machine (Shimadzu XRF-1800). The MCX collects fluorescent X-rays from a selected sample area of diameter 0.1 mm or less and collimates …
DIAGNOSIS OF LN-DOPED PZT FILMS VIA MICRODIFFRACTION: CORRELATION OF PROPERTIES TO OBSERVED FWHMM.A. Rodriguez, G. Brennecka, B. Tuttle, R. Tissot…Additionally, an un-doped film, and a 4 mol% Y-doped film were also investigated. Loss of switchable polarization (fatigue) showed a correlation to increased FWHM of the (222) PZT peak. Careful, systematic profile-fitting and decomposition of th…
EFFECT OF REINFORCEMENT PARTICLE FRACTURE ON THE LOAD PARTITIONING IN AN AL-SIC COMPOSITEH. Choo, B.S. Majumdar, P. Rangaswamy, M.A.M. Bourke…ESA-DE, Los Alamos National Laboratory, Los Alamos, NM 87545 4. MST-8, Los Alamos National Laboratory, Los Alamos, NM 87545 ABSTRACT We studied load partitioning during tensile loading of a 7093 Al alloy reinforced with 15 volume percent SiC par…
EFFECT OF THE RESIDUAL STRESS ON THE MECHANICAL STRENGTH OF THE THIN FILMSM. Gotoh, S. Takago, T. Sasaki, Y. Hirose…TiN and TiCN thin films were deposited by the physical vapor deposition (PVD) on JIS-SKH55 steel (equivalent to AISI M35). Subsequently, the specimens were heated to 573, 798, 843, and 893K. The texture states in thin films were evaluated from t…
HEAVY MINERAL ANALYSIS OF SANDSTONES BY RIETVELD ANALYSISJ.R. Webster, R.P. Kight, R.S. Winburn, C.A. Cool…Heavy minerals were separated from three size fractions covering the range of 0.18 to 0.30 mm. Polished grain mounts prepared from each size fraction were used to identify and measure the size of 1,517 grains by optical microscopy. Mineral compo…
HIGH TEMPERATURE ELASTIC STRAIN EVOLUTION IN SI3N4- BASED CERAMICSG.A. Swift, E. Ustundag, B. Clausen, M.A.M. Bourke, H.-T. Lin, C.-W. Li…The deep penetration of neutrons facilitated these in-situ studies. In particular, the hkl-dependent strains were measured and the results interpreted by Eshelby-based modeling for the Si3N4-SiCp sample. The diffraction data also provided inform…
HIGH TEMPERATURE X-RAY DIFFRACTION STUDY OF REACTION RATES IN CERAMICSM.S. Peterson, C.A. Say, S.A. Speakman, S.T. Misture…Current research has shown that in order to make phase pure materials via solid-state synthesis, over 100 hours of heat treatment are necessary. A custom high temperature X-ray diffractometer (HTXRD) was utilized to observe in-situ formation rea…
HIGH TEMPERATURE X-RAY STUDY OF PHASE EVOLUTION OF BA2YCU3O6+X FILMS USING THE “BAF2 CONVERSION PROCESS”W. Wong-Ng, I. Levin, M. Vaudin, R. Feenstra, L.P. Cook, J.P. Cline…ABSTRACT In-situ high-temperature x-ray diffraction (HTXRD) was used to study the phase formation and reaction kinetics of the Ba2YCu3O6+x (Y-213) phase using the ex-situ “BaF2 conversion process”. Three sets of films on single crystal SrTiO3 su…
IDENTIFICATION OF FORGED WORKS OF ART BY PORTABLE EDXRF SPECTROMETRYM. Ardid, J.L. Ferrero, D. Juanes, C. Roldyn, M. Crespo, M.E. Pernett, M. Marzal, M. Burke, S. Rovira, R. Vives…Pintura, Universitat de Barcelona, BARCELONA (Spain) ABSTRACT The study of patrimonial works by non-destructive techniques allow the analysis of unique and historic pieces without compromising their integrity. The Archaeometry Unit of the Instit…
IN-SITU, IN AIR, HIGH-TEMPERATURE STUDIES OF OXIDE SYSTEMS USING THE THERMAL-IMAGING TECHNIQUEL.F. Siah, J. Schneider, W.M. Kriven…Although the thermal radiative properties of the materials under study dictate their thermal behavior in the image hot-spot, this may be modified through a suitable co-existent coating material which absorbs in the wavelength range of the lamps …
INVESTIGATION OF LOCAL TEXTURES IN EXTRUDED MAGNESIUM BY SYNCHROTRON RADIATIONH.-G. Brokmeier, A. G†nther, S. Yi, W. Ye, T. Lippmann, U. Garbe…Our experiments were carried out at the high-field wiggler beam line BW5 (HASYLAB at DESY in Hamburg, Germany). The penetration power of 100 keV synchrotron radiation was sufficient to study extruded rods of 14 mm in diameter in transmission mod…
LASER-COMPTON SCATTERING AS A POTENTIAL BRIGHT X-RAY SOURCEK. Chouffani, D. Wells, F. Harmon, G. Lancaster, J. Jones…Sharp monochromatic X-ray lines were observed which result from the interaction of the electron beam with the laser optical photons. The back-scattered photons are kinematically boosted to keV X-ray energies. The X-rays were generated by collidi…
LATTICE DILATION IN A HYDROGEN CHARGED STEELG.L. Nash, H. Choo, P. Nash, L.L. Daemen, M.A.M. Bourke…LANSCE-12, Los Alamos National Laboratory, Los Alamos, NM 87545 5. MST-8, Los Alamos National Laboratory, Los Alamos, NM 87545 ABSTRACT The effect of hydrogen charging on the lattice dilation in an ASTM A710-HSLA steel specimen was studied using…
MANAGING BACKGROUND PROFILES USING A NEW X’CELERATOR DETECTORR.W. Morton, D.E. Simon, J.J. Gislason, S. Taylor…This paper discusses the instrument configuration necessary to obtain a satisfactory background profile useful for Rietveld modeling as well as other analytical applications. INTRODUCTION The new Philips X’Celerator [1] detector provides for rap…
MCSHAPE: A MONTE CARLO CODE FOR SIMULATION OF POLARIZED PHOTON TRANSPORTJ.E. Fernandez, V.G. Molinari, M. Bastiano, V. Scot…A B S T R A C T MCSHAPE, a new Monte Carlo code based on the recent analytical solution of the vector transport equations in plane geometry including polarization effects, was developed to provide a proper description of the polarization state e…
METHODOLOGY OF SYNCHROTRON EDXRD STRAIN PROFILINGI. Zakharchenko, Y. Gulak, Z. Zhong, M. Croft, T. Tsakalakos…Extremely tight incident/diffracted b!”#$ %&”(#”)(&*$ +,-.$ /#0$ is used to define a fixed micro-scattering-volume, through which the specimen is scanned to produce the profiling. Exhaustive theoretical modeling of the experiment provides outst…
MINIMIZATION OF MICROABSORPTION EFFECTS IN COMPLEX MIXTURESB.M. Pederson, R.M. Gonzalez, R.S. Winburn…One of these is microabsorption. Microabsorption has historically been ignored or accounted for using the Brindley correction. This correction has come under much debate in recent years. A recent Round Robin study on quantitative analysis includ…
MONOCAPILLARY OPTICS DEVELOPMENTS AND APPLICATIONSD.H. Bilderback, R. Huang, A. Kazimirov, I.A. Kriksunov, K. Limburg, E. Fontes…The optics come in two forms: 1) multibounce condensing capillaries for making submicron diameter beams and 2) one-bounce imaging capillaries with working distances of 20 to 50 mm from the tip of optic to the focal spot. The preliminary results …
PERFORMANCE OF A YB66 DOUBLE-CRYSTAL MONOCHROMATOR FOR DISPERSING SYNCHROTRON RADIATION AT SPRING-8M. Kitamura, H. Yoshikawa, T. Mochizuki, A.M. Vlaicu, A. Nisawa, N. Yagi, M. Okui, M. Kimura, T. Tanaka, S. Fukushima…Spring – 8. The YB, crystal has a large d – spacing of 0.586 nm for the (4 0 0) reflection and is useful as a soft X – ray monochromator for dispersing synchrotron radiation, since there is no intrinsic absorption edge and it is more durable tha…
POLARIZATION FOR BACKGROUND REDUCTION IN EDXRF – THE TECHNIQUE THAT DOES INDEED WORKR.W. Ryon…The general implementation of polarization to X-ray analysis had to await the fixed geometry of energy- dispersive systems. The means of optimizing these systems is shown in this review paper. Improved detection limits are the result. INTRODUCTI…
PULP AND PAPER PLANT MATERIALS ISSUES ADDRESSED BY X-RAY AND NEUTRON DIFFRACTION METHODSC.R. Hubbard, R.A. Peascoe, J.R. Keiser…Both monetary and environmental concerns demand that the inorganic chemicals and the organic byproducts are recycled. Currently recovery boilers are the standard means to recycle the inorganic chemicals and organic waste to produce a large fract…
REEL-TO-REEL TEXTURE ANALYSIS OF HTS COATED CONDUCTORS USING A MODIFIED GADDS SYSTEMJ.L. Reeves, V. Selvamanickam, R.L. Snyder…One way to achieve the high degree of texture is with the coated conductor architecture. The coated conductor is comprised of the HTS layer epitaxially grown on a textured oxide buffer layer on a metal tape which gives flexibility and strength t…
RENDERING OF CRYSTALLOGRAPHIC ORIENTATIONS, ORIENTATION AND POLE PROBABILITY DENSITY FUNCTIONSH. Schaeben, K.G. van den Boogaart…The familiar crystallographic “pole figures” are actually the sum of two spherical X–ray transforms which associate with a real–valued function f defined on a sphere its mean values Xf along one–dimensional circles with centre O, the origin of t…
RESIDUAL STRESS DETERMINATIONS USING PARALLEL BEAM OPTICST.R. Watkins, O.B. Cavin, J. Bai, J.A. Chediak…Utilization of parallel beam optics can experimentally remove/minimize diffraction peak shifts due to such displacements. Data collected from a cylindrical sample (diameter ~ 6 mm) at ambient temperature and flat alumina coatings at elevated tem…
RIETVELD ANALYSIS OF COMPLEX MIXTURES. WHAT CAN WE DO?R.S. Winburn…The recent report on the IUCR Round Robin study on quantitative analysis indicates that accurate results may not always be obtained when using RQXRD, even with simple three-phase mixtures. What can we do when we have samples with many phases and…
RIETVELD REFINEMENT OF 2-THETA SPLIT RANGES – A METHOD FOR REDUCING ANALYSIS TIMEK. Laursen, T. White…The approach taken here is that phases in general show peak broadening as well as a loss of intensity with increasing 2-theta. Thus, by splitting the full analyzed 2-theta range into regions and adjusting the step-size and counting time to an ap…
SPECTRAL INTERFERENCE IN X-RAY FLUORESCENCE ANALYSIS OF COMMON MATERIALSF.R. Feret, H. Hamouche, Y. Boissonneault…Most attention over the past two decades or so was focussed on inter-element interactions and their mathematical corrections using various fundamental-parameters methods. However, spectral interference plays a role, which is very often not prope…
STRESS ANALYSIS USING BREMSSTRAHLUNG RADIATIONF.A. Selim, D.P. Wells, J.F. Harmon, J. Kwofie, A.K. Roy, T. White, T. Roney…Box1625 – 2802, Idaho Falls, ID 83415 ABSTRACT Diffraction methods are the most reliable nondestructive methods of measuring residual stress. X-ray diffraction is restricted to penetration depths of some 10 µm, whereas neutron diffraction can pr…
STRUCTURE OF NANOCRYSTALLINE MATERIALS BY THE ATOMIC PAIR DISTRIBUTION FUNCTION TECHNIQUEV. Petkov…We find that V2O5.nH2O is an assembly of almost perfect bi-layers of VO5 units encapsulating the water molecules. Inside the nanopores of ITQ-4 the cesium ions are found to assemble in short-range ordered zig-zag chains. INTRODUCTION Nanocrystal…
THE INFLUENCE OF SURFACE ROUGHNESS ON THE REFRACTION OF X-RAYS AND ITS EFFECT ON BRAGG PEAK POSITIONSMichael H. Ott, Detlef Löhe…A set of brass samples with different surface roughnesses was used to measure the Bragg peak positions of {111} lattice plane in asymmetric Ω-mode with a constant incidence angle α. In a set of measurements with different incidence angles α the …
THE USE OF X-RAY DIFFRACTION MEASUREMENTS TO DETERMINE THE EFECT OF AGING ON RESIDUAL STRESSES IN UNIDIRECTIONAL AND WOVEN GRAPHITE/POLYIMIDE COMPOSITESB. Benedikt, M. Gentz, L. Kumosa, P.K. Predecki, D. Armentrout, M. Kumosa, J.K. Sutter…Cleveland, OH 44135 ABSTRACT The purpose of this study is to evaluate the effect of aging in either air or nitrogen on the residual interlaminar strains and stresses in unidirectional and woven graphite/polyimide composites. In order to accompli…
THERMAL FATIGUE PROPERTIES OF LASER PEENED HOT WORK DIE STEEL (H13)K. Yatsushiro, M. Sano, M. Kuramoto…Prior to the test, residual stress on the specimen of laser peened surface was approximately -1000 MPa, and the depth of the created compressive stress was approximately 1800µm. During the test, compressive residual stress of laser peened area w…
THREE-DIMENSIONAL MAPPING OF FATIGUE CRACK POSITION VIA A NOVEL X-RAY PHASE CONTRAST APPROACHK. Ignatiev, W.-K. Lee, K. Fezzaa, G.R. Davis, J.C. Elliott, S.R. Stock…Bioeng. & Nanosci. in Adv. Medicine, Northwestern Univ., Chicago, IL 60611 USA ABSTRACT X-ray absorption microtomography loses considerable sensitivity when it is applied to samples with high-aspect-ratio cross-sections, e.g. plates or compact t…
TIME-RESOLVED X-RAY DIFFRACTION STUDIES OF THE TEXTURE FORMATION KINETICS IN THE C49-C54 TISI2 PHASE TRANSFORMATIONA.S. Ozcan, K.F. Ludwig, Jr., C. Lavoie, C. Cabral, Jr., J.M.E. Harper…In previous work we identified three dominant C54 orientations in TiSi2 thin films on Si(001) substrates using X-ray pole figure analysis. In the current study the evolution of the three prominent C54 texture components was further examined usin…
UNDERKARAT JEWELRY: THE PERFECT CRIME? INVESTIGATIONS AND ANALYSIS OF JEWELRY USING XRFD. Kloos…It has become increasingly common in the last 15 years for XRF to be used in a preemptory fashion by jewelry manufacturers for process control and by industry oversight organizations for checking for compliance to karat fineness regulations. XRF…
USE OF X-RAYS IN THE UNITED KINGDOM FORENSIC SCIENCE SERVICED.F. Rendle…The complementary techniques of XRD and XRF are used mainly in trace analysis. Traces may consist of drugs, paint flakes, glass fragments, hair and fibres (natural and man-made), slivers of metal, soils, building materials, stains of any descrip…
VACANCY FORMATION DURING LOW-TEMPERATURE AG(001) AND AG(111) HOMOEPITAXYC.E. Botez, K. Li, E. Lu, W.C. Elliott, P.F. Miceli, E. Conrad, P.W. Stephens…For both orientations, our specular reflectivity data show that a large surface-normal compressive strain is uniformly distributed in the films deposited at T<200K. We attribute the strain to the incorporation of a considerable vacancy concentra…
VORTEX(TM) – A NEW HIGH PERFORMANCE SILICON DRIFT DETECTOR FOR XRD AND XRF APPLICATIONSS. Barkan, J.S. Iwanczyk, B.E. Patt, L. Feng, C.R. Tull…The Vortex™ design allows for a relatively large active area while still maintaining a very low anode capacitance (~ 60 fF). This very small detector capacitance results in a reduction of the series- noise component and hence a reduction of the …
WAVEGUIDE-RESONANCE MECHANISM FOR X-RAY BEAM PROPAGATION: PHYSICS AND EXPERIMENTAL BACKGROUNDV.K. Egorov, E.V. Egorov…It is experimentally shown that the high intensity of its emergent beam is not connected with the mechanism of free radiation propagation and with multiple total reflection of the beam. This type of X-ray passing we associate with the waveguide-…
X-RAY DIFFRACTION ANALYSIS IN THE FORENSIC SCIENCE: THE LAST RESORT IN MANY CRIMINAL CASESW. Kugler…They are often the only methods that allow a further differentiation of materials under laboratory conditions. Smears, minute contact traces, small sample quantities, or tiny sam- ple areas can be successfully analyzed as well as large quantitie…
X-RAY STRESS ANALYSIS OF DAMAGE EVOLUTION IN TI-SIC UNIDIRECTIONAL FIBER COMPOSITESJ.C. Hanan, E. Ustundag, I.J. Beyerlein, G.A. Swift, J.D. Almer, U. Lienert, D.R. Haeffner…Through the use of high energy X-ray microdiffraction, the elastic lattice strains of both phases in a Ti-SiC composite were revealed providing the in-situ load transfer under applied tensile stress at the scale of the microstructure. To underst…
ZINC/IRON PHASE TRANSFORMATION STUDIES ON GALVANNEALED STEEL COATINGS BY X-RAY DIFFRACTIONS. Wienstroer, M. Fransen, H. Mittelstadt, C. Nazikkol, M. Volker…A novel X-ray detection system enables an extreme reduction of measuring time, which allows XRD techniques to be an alternative fast analytical method for surface investigations. In combination with a heating chamber, fast surface phase transfor…

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