bluuebunny/crossref_metadata_2025 huggingface dataset:
Advances in Boron Measurement with Wavelength Dispersive XRF
Authors: Adamson B. W. , Juchli K. , Matula G.
Published: March 2019

Over recent years, the availability of man made “crystals“ (Layered Synthetic Microstructures or Multilayers) has led to a significant extension of the capabilities of WD XRF for the lighter elements. In particular, the elements from Atomic Number 5 (Boron) to Atomic Number 12 (Magnesium) have benefitted.

This paper will cover the lower end of this range and show how selection of multilayers is made. It will then consider the optimization of collimation to suit The performance characteristics of the multilayer device. One of many new applications opened up by these advances will be covered in detail (analysis of Boron in BPSG coatings on Silicon Wafers). Finally, a word of warning will be issued to those seeking to apply this newfound performance in routine XRF environments.
Requirement Analysis and Preliminary Design for Energy Dispersive X-ray Fluorescence Analysis Software
Authors: Liu Zhaogui
Published: March 2019

The rapid progress of x-ray fluorescence analysis spectrometers has been closely associated with advances in computers. Due to the power of computers, it is possible to acquire the data automatically and interpret complex information accurately and quickly, so as to provide both qualitative and quantitative analyses. It is now about thirty years that computers have been applied to X-Ray Fluorescence Analysis (XRFA). Few workers have discussed the style of the various approaches, although many different software packages have been used for XRFA. Requirement analysis has been performed for Energy Dispersive (ED) XRFA, and preliminary designs are given for three types of structures: i. Sequence structure, ii. Tree structure, and iii. Net structure.
Fast, High-Resolution X-ray Microfluorescence Imaging
Authors: Carpenter D. A. , Taylor M. A.
Published: March 2019

X-ray micro fluorescence imaging refers to the use of an x-ray beam as a probe to excite XRF in a specimen and produce a spatially resolved image of the element distribution. The advantages of high sensitivity and low background, together with the nondestructive nature of the measurement, have lead to applications of x-ray microfluorescence analysis in biology, geology, materials science, as well as in the area of nondestructive evaluation. Previous reports have described the development of an x-ray microprobe which uses a conventional source of x-rays to produce a 10-μm beam. This paper describes improvements to the microprobe which have increased the beam power and the solid angle of detection. The data collection and display software have also been enhanced.
X-ray Fluorescence and Fire-Assay Collection: Useful Partners in the Determination of the Platinum-Group Elements
Authors: Eddy Basil T , Stuckenberg Belinda L , Pansi Gemot
Published: March 2019

This paper describes the determination of the individual platinum-group elements by X-ray fluorescence after nickel-sulphide fire-assay collection. The platinum-group sulphide residue obtained after the dissolution of the nickel is dissolved in acid, and reduced to the metal by use of sodium borohydride. The finely divided metals are then filtered onto a millipore filter, and measured by X-ray fluorescence spectroscopy. The procedure makes use of gold as an internal standard. Factors affecting the accuracy and precision are investigated.
CCD Based X-ray Detectors
Authors: Tate Mark W.
Published: March 2019

The advent of intense synchrotron radiation sources for X-ray diffraction has made many otherwise difficult experiments feasible. The increased intensity will not he fully utilized, however, unless there are farther developments in detector technology. Improvement in detector characteristics will, of course, aid those using laboratory sources as well. For instance, construction of low noise, high, quantum efficiency detectors will reduce integration times and enable one to detect weak signals.
MATCHDB - A Program for the Identification of Phases Using a Digitized Diffraction-Pattern Database
Authors: Smith Deane K. , Johnson Gerald G. , Hoyle Susan Q.
Published: March 2019

The availability of automated powder diffractometers, APD, has revolutionized the collection of diffraction data and allowed many improvements in the analysis of these data. The biggest change is the ease of digitizing the diffraction trace rather than preparing it as a strip chart on paper from an analog recorder. When the data are collected properly, the trace is a digitized record of intensity versus 2θ. The trace is an accurate representation of the diffraction pattern containing the sample information along with the spectral and instrument aberrations.
The Substructure of Austenite and Martensite Through a Carburized Surface
Authors: Makinaon J. D. , Weins W. N. , De Angelis R. J.
Published: March 2019

The complex relationships among composition, roartensite start and finish temperatures, morphology of the martensite, residual stress distribution, and quenching conditions produce significant microstructural changes through a carburized case. Variations in the amount of retained austenite, the diffracting-particle size, and hardness were measured every 50μm in depth through a one percent carbon case on AISI-SAE 4320 steel. Measurement were made to a total depth of 2 mm. The percent retained austenite decreases from a maximum of 26% near the surface to a few percent in the bulk. It is shown that the x-ray diffracting-particle size of the martenaite phase is a structure parameter that changes when the martensite morphology goes from plate to lath type. The austenite phase diffracting-particle size is controlled hy the deformatioxis induced by the martensite formation.
X-ray Characterization of Thin Diamond Films Deposited by Hot-Filament Chemical Vapor Deposition
Authors: Hamilton Richard F. , Garg Diwakar , Wood Keith A. , Hoover David S.
Published: March 2019

Synthesizing thin diamond films by chemical vapor deposition (CVD) is the most recent and technologically important development in the thin-film field. Thin diamond films are useful in many applications because of their unique physical, chemical, optical, and electronic properties.

To assess thin diamond films’ suitability for support membranes in X-ray lithography, X-ray diffraction was used to characterize the crystal structure and orientation of these films deposited on silicon wafers by hot-filament assisted CVD. X-ray transmission properties of free-standing thin diamond films prepared by selectively etching silicon substrates were characterized by X-ray fluorescence in short and long wavelength regions.

This paper discusses conventional and grazing incidence diffraction techniques used to study the crystal structure of thin diamond films and compares the results with film morphology. It also describes X-ray transmission properties of these films in terms of Beer's Law, the mass absorption coefficient, and the wavelength of attenuated radiation. Finally, it reveals the long wavelength regions for optimum X-ray lithography operations using polycrystalline diamond (PCD) film.
X-Ray Fluorescence Analysis Applied to Small Samples
Authors: Jaklevic J.M. , French W.R. , Clarkson T.W. , Greenwood M.R.
Published: March 2019

We describe an adaptation of photon excited x-ray fluorescence analysis which is optimized for the analysis of small samples. A fine focus x-ray tube is used in conjunction with small diameter detector collimators in order to focus on a small sample volume with as high sensitivity as possible. Sample areas of less than 1 mm diameter can be analyzed with ppm detectability. In applications involving the analysis of human hair samples, a minimum detectable limit of 10 ppm Hg can be realized in a 1 mm long segment of a single hair in a counting time of 200 seconds. Simultaneous measurements of the sample mass can be obtained from the intensity of the incoherent scattering. An automated x-ray fluorescence analysis system using the technique for the scanning of elemental profiles in such hair samples will be described.
Diffrac-at Search: Search/Match Using Full Traces as Input
Authors: Nusinovici Julian , Winter Marcus J.
Published: March 2019

The advantages of using the full trace as input for search/match rather than the traditional list of d/I values are emphasized. These advantages stem from the availability and the logical employment of the whole information of the diffractogram.

The two key features which enable successful identification of minor phases are discussed: (1) the reliable discrimination between background and weak lines and (2) by regarding the actual full widths of major lines as regions where weak lines can, potentially, he obscured.

The user friendliness of the. package will be presented: the graphical user interface, the high level of interactivity, and the speed of the search/match - now less than 8 seconds for searching the current whole ICDD database of 61,993 reference patterns when using an i486/66-based PC.
A New XRD tool for Metallurgical Research: ICDD's Metals & Alloys Indexes
Authors: Dann Jeffrey N. , Huang Ting C. , Mueller Melvin H. , Wallace Peter L. , Weissmann Sigmund , Calvert Larry D.
Published: March 2019

The International Centre for Diffraction Data (1CDD), formally the Joint Committee for Powder Diffraction Standards (JCPDS), recently published a compilation of metal and alloy indexes of powder diffraction and structural data. This compilation is designed to make the identification and characterization of metallic and related materials easier and far more accurate. Systematic searches for chemical analogs and greater use of partial chemical knowledge are now possible.
The Development of a Time-Resolved X-Ray Measurement System Using Imaging Plate
Authors: Sasaki Katsunari , Yamazaki Hideto , Masuda Kenji , Hsiue Ging-Ho
Published: March 2019

A X-ray diffraction system using an Imaging Plate(IP) has been developed for time resolved X-ray measurements. The system consists of a new drum scanning type IP reader which includes a multiple time resolved X-ray exposure mechanism and a simple high temperature sample holder. Both are controlled from a personal computer. The new IP reader also supports 50μm/pixel reading for high resolution type IP (Blue IP), and has a spatial resolution better than 75μm.
High Energy Resolution X-Ray Spectrometer for High Count Rate Xrf Applications
Authors: Rossington C. S. , Madden N. W. , Chapman K.
Published: March 2019

A new x-ray spectrometer has been constructed which incorporates a novel large area, low capacitance Si(Li) detector and a low noise JFET (junction field effect transistor) preamplifier. The spectrometer operates at high count Tates without the conventional compromise in energy resolution. For example, at an amplifier peaking time of 1 p.sec and a throughput count rate of 145,000 counts sec-1, the energy resolution at 5.9 keV is 220 eV FWHM. Commercially available spectrometers utilizing conventional geometry Si(Li) detectors with areas equivalent to the new detector have resolutions on the order of 540 eV under the same conditions. Conventional x-ray spectrometers offering high energy resolution must employ detectors with areas one-tenth the size of the new LBL detector (20 mm2 compared with 200 mm2). However, even with the use of the smaller area detectors, the energy resolution of a commercial system is typically limited to approximately 300 eV (again, at 1 μsec and 5.9 keV) due to the noise of the commercially available JFET's. The new large area detector is useful in high count rate applications, but is also useful in the detection of weak photon signals, in which it is desirable to subtend as large an angle of the available photon flux as possible, while still maintaining excellent energy resolution. X-ray fluorescence data from die new spectrometer is shown in comparison to a commercially available system in the analysis of a dilute muhi-element material, and also in conjunction with high count rate synchrotron EXAFS applications.
Ultra-High Vacuum Grazing Incidence Small Angle X-Ray Scattering Camera for in Situ Surface Analysis
Authors: Parrill Joanne Levine , Cohen Jerome B. , Chung Yip-Wah
Published: March 2019

An ultra-high vacuum chamber designed for in situ grazing incidence small angle x-ray scattering (GISAXS) surface analysis is described. Unique features of this equipment are the precision rotary feedthrough for angular alignment of the sample, the sample heating design, the Be window arrangement, and the compatibility of this chamber with both a rotating anode and a synchrotron beamline. This chamber was used as part of a GISAXS camera utilizing a 18 kW Rigaku rotating anode, pin-hole collimation, and a position sensitive detector. The resolution of this camera was 0.007 A-1 with a 1.4 mm wide beamstop and CuKα
The Use Of Multilayer Structures in the Energy Dispersive X-Ray Fluorescence Analysis of Low Z Elements
Authors: Kanngieβer Birgit , Qeckhoff Burkbard , Scheer Jens , Swoboda Walter , Laursen Jens
Published: March 2019

A toroidal focLising W/Si multilayer and a planar W/Si multilayer were tested for the possible usefulness for the Energy Dispersive X-Ray Fluorescence Analysis (EDXXRF) of low Z elements.
Total Reflection X-Ray Fluorescence Spectroscopy: Analysis Of Gaas And InGaAs
Authors: Filcs-Sesler Leigh Ann , Plumton Don , Kao Yung-Chung , Kim Tae S.
Published: March 2019

This article explores applications of total reflection x-ray fluorescence (TRXRF) to GaAs processes. The applications include determination of surface contamination and InGaAs layer thicknesses. Surface contamination can deteriorate device performance and can occur in starting substrates and in subsequent processing. We demonstrate that TRXRF is a quick, nondestructive method for identifying sulfur contamination on incoming wafers and low levels of metallic impurities from device fabrication. Variable angle TRXRF has been used to determine heterostmeture film thickness, measuring films of InGaAs on GaAs as thin as 4 nm.
Fluorescence Yield Xanes and Exafs Experiments: Application to Highly Dilute and Surface Samples
Authors: Waychunas Glenn A. , Brown Gordon E.
Published: March 2019

The development of intense synchrotron radiation sources during the last twenty years has enabled several types of x-ray spectroscopy and scattering techniques to come into practical use. One of the most significant methods for the characterization of extremely dilute samples is high resolution x-ray absorption-edge spectroscopy. The technique is usually divided into two separate methods according to whether the x-ray absorption near edge structure (XANES) or the extended x-ray absorption fine structure (EXAFS) is analyzed. XANES features are due mainly to bound-state electronic transitions just below, and on the low energy side of the edge, and to multiple scattering resonances on the top of the edge and at somewhat higher energies. EXAFS features are oscillations due to ejected photoelectron back scattering interference processes in the close vicinity of the absorber atom. XANES analysis is used to determine atom valence, atom site distortion from regular geometries, and other details of the atom site. EXAFS features can be analyzed to recover interatomic distances between the absorber atom and its first few shells of neighbors, as well as the number and types of these neighbors. Together these techniques can provide an atomspecific probe of die short-range structure within almost any type of condensed matter.
Sensitivity Improvement and Stabilization For Ultra Light Element Analysis by X-Ray Spectrometry
Authors: Toda K. , Kohno H. , Arai T. , Araki Y. , Haraill G.
Published: March 2019

Many light and ultra-light element analysis problems have been addressed by X-ray fluorescence. Recent innovative features of X-ray spectrometers have extended the applicability of X-ray fluorescence to ultra-light element analysis. Sensitivities have improved through the use of a newly developed end window X-ray tube. Selection of analyzing optics conditions optimize to some degree the sensitivity/resolution/intensity problems. Instrument stability is greatly improved by simply monitoring and controlling the vacuum within the analyzing chamber. Data are presented to illustrate the effects of these novel instrument components as well as describing several new application techniques for ultra-light element analysis.
X-Ray Diffraction of Radioactive Materials
Authors: Schiferl D. , Roof R. B.
Published: March 2019

X-ray diffraction studies on radioactive materials are reviewed. Considerable emphasis is placed on the safe handling and loading of not-too-exotic samples. Special considerations such as the problems of film blackening by the gamma rays and changes induced by the self-irradiation of the sample are covered. Some modifications of common diffraction techniques are presented. Finally, diffraction studies on radioactive samples under extreme conditions are discussed, with primary emphasis on high-pressure studies involving diamond-anvil cells.
Application of Microbeam X-Ray Technique to the Evaluation of the Plastic Zone Size of Fatigued Steels
Authors: Izumiyama Akimasa , Yoshioka Yasuo , Terasawa Masao
Published: March 2019

The microbeam X-ray diffraction technique was used for the evaluation of fracture analysis on the fatigued low carbon steel specimens.

It is possible to evaluate both monotonic and cyclic plastic zone sizes beneath fatigue fracture surface. Thus the stress intensity factor can be estimated.
Quasi-Fundamental Correction Methods Using Broadband X-Ray Excitation
Authors: Quinn A. P.
Published: March 2019

A critical discussion of the equivalent wavelength representation of polychromatic primary radiation as applied to the fundamental parameters method is given. This representation raises problems with appropriate selection of equivalent wavelengths and with accurate calculation of secondary fluorescence. Methods for reducing these difficulties are discussed and have been incorporated into a mini-computer program which achieves reasonable accuracy for alloy test cases.
PDF Search and Match Algorithms for the Cyber 205 Vector Processor
Authors: Winder Dale , Loftis Bruce
Published: March 2019

The CYBER 205 has a number of features applicable to the manipulation of the powder diffraction file (PDF). The FORTRAN language has been extended to include many vector procedures and calls to internal system procedures (e.g., the system clock, is accessible and timing of routines is accurate to a microsecond). A VECTOR is specified by its address and its length. A pointer to a vector, a DESCRIPTOR, can be assigned and then used in arithmetic and relational expressions. A BIT vector is a binary switch such that a bit value (ON or OFF) can control the disposition of a corresponding element of a vector. The maximum size of a vector is 65535 elements.
Experimental Study of Precise Peak Determination in X-Ray Powder Diffraction
Authors: Huang T. C. , Parrish W. , Lim G.
Published: March 2019

The combined derivative method (accompanying paper) was tested with a large number of experimental patterns to illustrate its use in various difficult problems commonly arising in peak search analysis of X-ray diffraction data. Patterns obtained with various step sizes, resolution, counting statistical noise, and profile widths were used. The precision in 2θ determination and overlap resolution are in good agreement with those previously obtained from calculated profiles, raise identification of noise as diffraction peaks was eliminated by using a convolution range proportional to the full width at half maximum. Peak search results (both 2θ and intensity) were also compared to those obtained by profile fitting to illustrate the different characteristics of these two methods.
Residual Stress Relaxation in Cemented Carbide Composites Studied Using the Argonne Intense Pulsed Neutron Source
Authors: Krawitz A. D. , Roberts R. , Faber J.
Published: March 2019

Cemented carbide composites with a WC hard phase and a Co-Ni alloy binder phase have been subjected to monotonic and cyclic deformation and studied using the high resolution General Purpose Powder Diffractometer at the Argonne Intense Pulsed Neutron Source. Upon deformation, relaxation of bulk differential thermal residual stresses, tensile in the binder and compressive in the carbide, is observed to occur as a function of loading mode and plastic strain via shifts in diffraction peak positions. In addition, peak breadth behavior indicates broadening. At low plastic strain this is due primarily to a range of residual stress and at high plastic strain it is attributable to the plastic deformation alone since relaxation is essentially complete. The appropriateness of neutrons is discussed.
Computer-Assisted Alignment of a Guinier X-Ray Powder Diffraction System
Authors: Fitzpatrick J.J. , Pressnall J.S.
Published: March 2019

Digitized data acquisition and subsequent peak-profile fitting are used in aligning and maintaining the Guinier diffraction system in this laboratory. Utilization of a stepping motor driven goniometer along with profile analysis allows rapid and reproducible alignment while providing a means to investigate the types and magnitudes of errors introduced by various misalignments of the optical system.
A Comparison of Trace Metal Determination in Contaminated Soils by XRF And ICAP Spectroscopies
Authors: Kendall Douglas S. , Lowry Joe H. , Bour Edward L. , Meszaros Timothy J.
Published: March 2019

The National Enforcement Investigations Center of the EPA provides support services for the enforcement activities of the Agency. Recently, we have analyzed hazardous wastes as part of efforts to enforce the Resource Conservation and Recovery Act and the Superfund Act. Sample preparation for inorganic elemental analysis is a difficult and time-consuming step. Thus, it would be desirable to be able to use x-ray fluorescence methods which require relatively little sample preparation for the analysis of solid hazardous wastes. A major problem to be overcome is the need to calibrate for a large variety of samples. However, a compensating factor is that the error will be largely determined by the sampling error and the measurement accuracy is not quite so critical.
Determination of Barium and Selected Rare-Earth Elements in Geological Materials Employing a HpGe Detector by Radioisotope Excited X-Ray Fluorescence
Authors: LaBrecque J.J. , Preiss I.L.
Published: March 2019

The laterite material (geological) from Cerro Impacto was first studied by air radiometric techniques in the 1970's and was found to have an abnormally high radioactive background. Further studies showed this deposit to be rich in thorium, columbium, barium and rare-earth elements (mostly La, Ce, Pr and Nd). A similar work (1) has been reported for the analysis of Brazil’s lateritic material from Morro do Ferro to determine elemental compositions (including barium and rare-earth elements) and its relationship to the mobilization of thorium from the deposit using a Co-57 radioisotope source.
Determination of Oxygen and Nitrogen in Various Materials by X-Ray Fluorescence Spectrometry
Authors: Arai T. , Ohara S.
Published: March 2019

Spectrographic analysis for carbon and boron using fluorescent x-rays has been studied over the past few years; principles and applications for using those ultra-soft x-rays were described, based on the combination of total reflection and filtering rather than on the wavelength dispersive method of Bragg reflection (1, 2). However, oxygen and nitrogen, with x-ray wavelengths of 23.7lÅ and 31.60Å, respectively, cannot be detected as easily because of their high absorption by the detector window materials such as polypropylene, polyester or formvar films.
Analysis of Graphite in Caststeels using XRFA
Authors: Wariwoda L. , Mantler M. , Weber F.
Published: March 2019

For carbon analysis in an iron-matrix the C-Kα intensity is not only a function of the amount of graphite. but also of the diameter of the spherolites and, for a given total carbon content, of the graphite/cementite ratio. In order to verify this, steel and caststeel sample surfaces were photographed before and after etching and the images digitized. The arcal fractions covered by graphite, cementite, and iron were used to compute the corresponding individual weight fractions and total carbon contents. Count rates were drawn to the scale of these as well as of the nominal carbon concentrations.
Application of the Fundamental Parameter Method to Analyses of Light Element Compounds Considering the Scattering Effects
Authors: Mori Shigeyuki , Mantler Michael
Published: March 2019

The fundamental parameter (FP) method has been applied to many elemental analysis fields because of the advantage that it does not require standards of the same matrix as the unknown. In most FP software packages only primary and secondary excitations are included in the mathematical models, and hardly any software for routine applications has ever been reported involving the secondary enhancement by scattered radiation (SESR) as well as the scattered primary fluorescent radiation (SPFR). This can lead to errors in the analyses of compounds rich in light elements, like oxides, nitrides, carbides, borides, etc.
O K-V Spectra of Oxides and Superconducting Materials
Authors: Sakai Masahiro , Hayakawa Shinjiro , Kawai Jun , Gohshi Yohichi
Published: March 2019

Oxygen K-V (Kα) X-ray fluorescence spectra of MgO, Cu2O, CuO, La2CuO4, La2-xSrxCuO4, YBa2Cu3O7-x , and GdBa2Cu3O7-x are measured. The local (oxygen) and partial (2p) electron density of states (DOS) of these compounds are calculated by the cluster approximation with the discrete variational (DV) Hartree-Fock-Slater (Xα) method. The calculated O 2p DOS are compared with the measured X-ray fluorescence spectra. It is found that the measured 0 K-V X-ray fluorescence line shapes are well reproduced by the O 2p DOS calculated by a cluster including the second nearest neighbor atoms (oxygen atoms) in the solids. This indicates that the oxygen K-V X-ray emission spectra reflect the oxygen-oxygen orbital hybridization in the solid as well as the oxygen-metal orbital hybridization.
Raw Materials Analysis by XRF in the Cement Industry
Authors: Babikian Sona H.
Published: March 2019

The sources of raw materials used in the manufacture of Portland cement include pure to argillaceous limestones, shale and clay, plus minor quantities of sand, iron ore, fly ash, coal ash and suitable industrial wastes. To ensure a high quality product, rapid - precise - reproducible and practical analytical techniques are required. Quantitative XRF analysis techniques meet those demands.

For this comparative technique, the instrument used is a wavelength dispersive sequential spectrometer. The advantages and the drawbacks of the technique are discussed, along with the procedure of the specimen fused bead preparation. The importance of calibration standards and unknown samples being prepared in an identical manner, and being presented to the instrument under similar conditions, is stressed. International and synthetic standards, concentration ranges for the five major elements, mathematically generated coefficients to correct absorption and enhancement effects, and a summary of the standard error of estimates are examined and discussed.

The accuracy of the method is verified by the analysis of known standard reference materials such as obsidian rock, coal fly ash, argillaceous limestone and blastfurnace slag. The values are compared with the known certified values.
Proposed Methods for Depth Profiling of Residual Stresses using Grazing Incidence X-Ray Diffraction (GIXD)
Authors: Predecki Paul , Zhu X. , Ballard B.
Published: March 2019

Two proposed methods are described for obtaining the depth profiles (τ-profiles) of strains and stresses as a function of the 1/e penetration depth τ, using GIXD in the asymmetric geometry, without the need for layer removal. In the first, the ψ-method: ψ is varied, for a given reflection, while holding τ constant, by varying the wavelength λ and adjusting the incident angle α so as to maintain τ constant. This allows dϕ,ψ vs Sin2ψ plots to be obtained at constant τ. In the second, the ϕ-integral method: interplanar spacings dϕ,ψ are measured for ϕ values from 0 to 2π, at constant ψ and τ by holding α fixed. Two ψ values, i.e. two wavelengths, are needed to obtain the whole strain tensor, but if the sample is quasi-isotropic and the stress state is biaxial, only one wavelength is needed. A direct method is also described for obtaining the profiles as a function of depth z (z-profiles) from the corresponding τ-profiles using inverse Laplace transforms. Application of the method to the residual strain vs τ data of Doerner and Brennan for an Al film on Si is presented.
In Situ High Temperature X-Ray Diffraction Studies of Modified Poly(Ethylene Terephthalate)
Authors: Blanton T. , Seyler R.
Published: March 2019

The effect of dimethyl-5-sodiosulfoisophthalate, SIP, on poly(ethylene terephthalate), PET, crystallization has been studied using in situ high-temperature x-ray diffraction, HTXRD. At low levels of SIP modification, PET-like crystallinity was observed. At high SIP levels, clustering of polyester ionomers was observed and crystallization was significantly suppressed. The HTXRD data along with differential scanning calorimetry, DSC, and small angle x-ray scattering, SAXS, indicate that the change from bulk crystallization to bulk ionomer formation occurred when 8-12 mol% of the diester linkages contained SIP.
Application of Imaging Plate for Polymer Analysis
Authors: Sasaki Katsunari , Kakefuda Kohji , Masuda Kenji , Hsiue Ging-Ho , Hsu Chain-Shu
Published: March 2019

The Fuji Imaging Plate (IP) is a 2-Dimensional X-ray detector on which a latent X-ray image is stored as a distribution of color centers in a photo-stimulable phosphor(BaFBr:Eu) screen. It has excellent characteristics such as a wide dynamic range of five or more digits and an order of magnitude higher sensitivity than X-ray film. Thus it has been actively used in the field of X-ray single crystal structure analysis.

For polymer studies, 2-D information is useful to analyse a sample's orientation or periodic structure, and some system such as 2-D position sensitive detector (PSD) are widely used. But in spite of the superior performance of the IP which will give significant advantages in various measurements, few applications have been reported in this field, because most conventional IP based systems are specialized for the single crystal structure analysis,

Therefore we developed the R-AXIS II D (Rigaku Automated X-ray Imaging System II D), an IP reader for general X-ray diffractometry which has a removable IP in order for exposure with external X-ray optics, and software which converts 2-D data to conventional 2theta-intensity or beta-intensity data for analysis of crystallinity or orientation. In this paper, we report the performance of R-AXIS II D and its applications to polymer studies and thin film analyses.
Determination of the Interaction Strains in Two-Phase Brass with X-Ray Diffraction
Authors: Noyan I.C. , Schadler L.S.
Published: March 2019

Deformation in polycrystalline materials is highly inhomogeneous on a micro scale. This inhomogeneity arises from the anisotropy of the constituent grains, coupled with local configurational parameters such as texture, gram size or proximity to a free surface. In a recent paper, we had outlined a new method that extended the traditional x-ray stress analysis to yield quantitative measures of such inhomogeneous deformation. In this paper, this method is used to study the partitioning of inhomogeneous deformation between the phases of 60-40 brass tensile specimens subjected to applied loads.
Measurements and Prediction of Residual Stress in Metal Matrix Composites
Authors: Ericsson Torsten , Ohlsson Anders , Persson Christer
Published: March 2019

There has been a great interest in metal matrix composites during the last 10-15 years. The reason is their potential to achieve a high strength and good dimensional stability in a large temperature range and to obtain a good stiffness. The interest has particularly been focused on light metals reinforced with a continuous or discontinuous ceramic phase. The reinforcement and the matrix have very different properties such as thermal expansion and elastic modulus, which of course is the point in using this type of reinforcement. These differences between matrix and reinforcement gives rise to residual stresses after temperature changes or after plastic deformation.
RS/hyper: A Hypertext-Based Workstation for Reliable X-Ray Residual Stress Measurements
Authors: Ward A. , Hendricks R. W. , Brauss M.
Published: March 2019

Advances over the last ten years in computer automation and control, compact and portable x-ray sources, and reliable and efficient detector systems have allowed X-Ray Determination of Residual Stress (XRDRS) measurements to become a viable method of evaluating the state of stress in metals, alloys, and ceramics. However, problems associated with incorrect XRDRS equipment operation and poor experimental technique are prevelant in industry, necessitating better operator training and education. Therefore, an interactive computer workstation, called RS/hyper, was developed to lead the operator towards correct operating procedures and reliable experimental technique.

Proper machine setup, machine maintenance, radiation safety, experimental technique, theoretical understanding, and limited data evaluation are presented in RS/hyper. Graphical aids are used extensively to avoid confusion and misinterpretation of theoretical concepts and equipment instructions. RS/hyper is interactive, allowing the user to learn about topics at a comfortable level of explanation. Compared to written texts and references, RS/hyper has been shown to reduce training and problem solving time by a factor of 16.

RS/hyper will train novice users of XRDRS equipment so that the data acquired from such machines will be reliable in an industrial environment. Also, since the software educates the user, data will be more accurately represented before interpretation. The experienced user should find RS/hyper useful as a reference to XRDRS and related information.
X-Ray Elastic Constants of Sintered and HIP'ed ZrO2 Ceramics with Different Chemical Components
Authors: Sasaki Toshihiko , Kuramoto Makoto , Yoshioka Yasuo
Published: March 2019

Mechanical and X-ray elastic constants of four types of ZrO2 were measured for (133) planes with Cr-Kα radiation. The main differences among the specimens were the chemical components, the sintering method and the heat-treatment. It was found that the elastic constants were affected by the heat-treatment, but little by the other factors. The influence of the method of the peak determination on the result was also examined. The residual stresses at the knife edge were determined.
Asymmetric Diffraction with Parallel-Beam Synchrotron Radiation
Authors: Toraya Hideo , Huang Ting C. , Wu Yan
Published: March 2019

In this paper, the advantages and disadvantages of using the asymmetric 2θ scanning technique with a fixed incident angle α are described. Vertical-scan powder diffractometers with long horizontal parallel slits with an aperture of 0.05° and parallel-beam synchrotron radiation with λ = 1.54 Å and α = 10°, 2°, and 1° were used to collect α-Al2O3, silver behenate CH3(CH2)20COOAg, and Si powder diffraction patterns. The synchrotron radiation data were analyzed by profile fitting, and the results were compared with those obtained by the conventional θ-2θ scanning technique. As expected, significantly higher intensities were obtained from the asymmetric diffraction data with α = 10°. At smaller α = 2° and 1°, however, the intensities were reduced because of a smaller effective beam height. The peak positions remained practically unchanged for the data obtained with α = 10°, but displaced toward higher 2θ angles for α = 2° or lower, and, consequently a refractive-index correction was needed. Profile shape was slightly broadened and became more Lorentzian in asymmetric diffraction with highly oblique incidence of the beam. The change in shape was, however, negligibly small. The results showed that intensive and reliable powder diffraction data can be obtained from asymmetric diffraction by fixing the incident beam at a sufficiently large angle to fully illuminate the available sample surface.
Stresses in Thin Films
Authors: Cohen Jerome B.
Published: March 2019

While any subject associated with films evokes immediate thoughts about solid-state devices, there are other much more mature areas where it is important, such as coatings, and yet work on this entire subject is only in its infancy. Residual stresses are not only important because of their well-known effect on corrosion and mechanical properties, they can also lead to other severe problems. For example, it is now believed that stress gradients can lead to void formation and subsequent failure in metallization in electronic devices. Thus, it is not only the level of stress that can be important, but gradients across a surface of a thin stripe, or through the thickness.
Measurement of Relaxation in Strained Layer Semiconductor Structures
Authors: Halliwell Mary A. G.
Published: March 2019

Many advanced semiconductor device designs require the growth of heteroepitaxial layers with lattice parameters differing by up to a few percent with respect to the substrate. X-ray diffraction offers a nondestructive method of determining the extent of relaxation. This paper discusses the sensitivity of x-ray techniques to small amounts of relaxation, describes how relaxation is measured in cubic materials for layer on (001) substrates and suggests nomenclature for the case of asymmetric relaxation.
X-ray Diffraction Analysis of SiGe/Si Superlattices
Authors: Fatemi M. , Prokes S. , Shanabrook B. V. , Wang K. L.
Published: March 2019

It is well known that x-ray diffraction techniques provide one of the most direct means of analyzing superlattice periodicity, layer thickness, strain, and defect structure. This suitability of x-rays is a consequence of the fact that most superlattice periods are in the range of 10 to 50 times the typical wavelength (Cuκα=1.54 Å) and are hence measurable by x-ray diffraction, and also that x-rays are non-destructive within the energy and dosage ranges needed for these studies. Applications of x-ray techniques to supperlattices have been discussed in many publications in the open literature.
Surface and Ultra-Thin Film Characterization by Grazing-Incidence Asymmetric Bragg Diffraction
Authors: Huang T. C.
Published: March 2019

An effective technique using grazing-incidence X-rays and asymmetric-Bragg diffraction (GIABD) for the characterization of crystalline phases on surfaces and structural depth-profiles in thin films is described. The application of the GIABD using both X-ray and synchrotron radiation sources for the analysis of an iron-oxide magnetic thin film previously reported to have an unexpected magnetically-dead layer is discussed. The X-ray diffraction analysis using the GIABD and the conventional θ-2θ scanning techniques detected an anti-ferromagnetic hexagonal α-Fe2O3 on the surface and a ferromagnetic tetragonal γ-Fe2O3 in the bulk of the film, respectively. The synchrotron diffraction analysis using incident angles below and above the critical angle of total reflection quantitatively determined the structural depth-profiles of α-Fe2O3 and γ-Fe2O3 in the film.
XRD Characterization of Titanium/Copper Thin Films Heat Treated in Vacuum and Hydrogen
Authors: Sullivan M. J. , Goldsmith C. , Ficalora P.
Published: March 2019

Thin film metallization is used on integrated circuit chips and ceramic and/or organic substrates for a number of different purposes, On chips the metallization forms Ohmic and Schottky Barrier Diode contact to the semiconductor and the electrical properties of these contacts are strongly influenced by the metals used. Interaction of the metal and semiconductor during processing can result in major variations in the electrical properties of the contacts, Chip metallization is also employed to provide electrical interconnection between devices on a chip. The interconnections can all be made in a single layer, or for more complex chips, a number of layers might be employed using dielectric layers to separate metal layers and via holes through the dielectric for layer-to-layer interconnection. Chip metallization is also used to form the interconnections between the chips and the substrate carrier.
X-ray Examination of Fracture Surfaces of Silicon Nitride Ceramics
Authors: Yajima Zenjiro , Hirose Yukio , Tanaka Keisuke
Published: March 2019

The residual stress left on the fracture surface is one of the important parameters in X-ray fractography. It has been used to analyze fracture mechanisms in fracture toughness and fatigue tests especially of iron and steels.

In the present paper, X-ray fractography was applied to the brittle fracture surface of a silicon nitride ceramics. The first part deals with the determination of the stress constant for diffraction from Si3N4(411) plane by Cr-Kα radiation. The second part describes the effect of the notch-tip radius on the fracture toughness value. In the last part, the plastic zone depth was determined from the residual stress destribution beneath the fracture surface.
X-ray Residual Stress Measurement on Fracture Surface of Stress Corrosion Cracking
Authors: Tsuda Masaaki , Hirose Yukic , Yajima Zenjiro , Tanaka Keisuke
Published: March 2019

X-ray fractography is a new method utilizing the X-ray diffraction technique to observe the fracture surface for the analysis of the micromechanisms and mechanics of fracture. The X-ray residual stress has been confirmed to be a particularly useful parameter when studying the fracture surfaces of high strength steels. The method has been applied to the fracture surface of fracture toughness and fatigue specimens.
The Importance of Consistent 1/d Scans in Determining Size and Strain by Powder Diffraction Profile Analysis
Authors: Zhang Y. , Stewart J. H. , Hubbard C. R. , Morosin B.
Published: March 2019

This paper reports and discusses the results of a computer modeling study on powder diffraction profile analysis for crystallite size and strain of polycrystalline materials. The results of this computer modeling show that if the spans of diffraction profiles in reciprocal space (1/d) are not carefully chosen, an overestimation on size and an underestimation on strain may result in analysis by both the Warren-Averbach and the Hall-Williamson methods. A general way to eliminate such errors based on profile fitting and regeneration is presented and discussed in this paper.
The Use of 2-D Detector Utilizing Laser-Stimulated Luminescence for X-ray Diffraction Studies on Mechanical Behaviour of Materials
Authors: Yoshioka Y. , Shinkai T. , Ohya S.
Published: March 2019

The development of linear position-sensitive detectors (PSD) has resulted in a large reduction of data acquisition times in the field of x-ray stress analysis. However, we also require two-dimensional (2-D) diffraction patterns for material evaluation. Especially, the microbeam x-ray diffraction technique gives valuable information on the structure of crystalline materials and this technique has been applied to fracture analysis by x-rays. Many kinds of 2-D PSD have been developed that have insufficient spatial resolution. So x-ray film has still been used as a 2-D detector, but it requires relatively long exposure times and then the process after exposure is very troublesome.
Design of High Performance Soft X-ray Windows
Authors: Perkins Raymond T. , Allred David D. , Knight Larry V. , Thorne James M.
Published: March 2019

X-ray windows are used in sources and detectors to separate the neighborhood of the x-ray generation or detection from the use environment. While each use has its own requirements, there are some principles that should be used in designing an optimal x-ray window. Because x rays are absorbed to some extent by all materials, minimizing absorption is one criterion in preparing windows. Also, for most uses there is a pressure difference across the window so that ensuring pinhole-free structure and sufficient mechanical strength to support the differential is another criterion for window design. Traditionally, absorption, is minimized by fabricating the window with lower atomic number (low Z) elements such as Be, B or C. However, the wavelength (energy) region of interest becomes a very important complicating factor.
XRF Technique as a Method of Choice for On-Site Analysis of Soil Contaminants and Waste Material
Authors: Piorek Starislaw
Published: March 2019

Recent years were marked by a rapid increase of interest in the ase of x-ray fluorescence for on-site chemical characterization of contaminated soils and waste materials.

The known advantages of the XRF technique, such as capability of simultaneous, multielement analysis, speed of measurement (10 to 100 seconds), little or no sample preparation, wide concentration range, “portability,“ and ease of integration into environmental monitoring station(s), make it specifically suited for this application.

Major difficulties still inhibiting wider use of the XRF for hazardous waste screening stem from the lack of suitable calibration samples and proper protocols, as well as from the low awareness of the industry about the technique.
Screening of Hazardous Waste with an Energy Dispersive X-ray Fluorescence Spectrometer
Authors: Jacobus N.C.
Published: March 2019

“HAZARDOUS WASTE SITE” - What picture do those words bring to mind? Most people visualize a remote area behind a tall chain-linked fence with signs prohibiting entrance and warning of the dangers within. For these sites already identified as hazardous waste sites, access is limited, and all who enter must wear appropriate protective clothing when working on the site. However, a yet to be identified “hazardous waste site” may be as close by as the back lot of a manufacturing facility in your town. Or, it may be a vacant lot in your neighborhood or even your own property, land on which children play and vegetable gardens grow. Thus, those involved in locating hazardous contamination and determining the extent of that contamination are not only with the U.S. Environmental Protection Agency and its contractors, but are also with state and local departments of health as well.
Microvolume Analysis of Fly Ash by Synchrotron Radiation X-ray Fluorescence (SRXRF) and Electron Microprobe X-ray Microanalysis (EPXMA)
Authors: Török Sz. , Sándor Sz. , Rausch H.
Published: March 2019

The assessment of the potential environmental and toxicological effects of particulate material emitted to the atmosphere requires detailed physical and chemical characterization of the particles. One of the most widely studied types of pollutant particles is coal fly ash as a byproduct of coal combustion. These particles are inhomogeneous, highly variable, span a broad range of sizes and have diverse morphologies.

It has been shown that numerous toxic trace elements tend to increase in bulk concentrations with decreasing particle size (1).
Intensity and Distribution of Background X-Rays in a Wavelength-Dispersive Spectrometer. II. Applications
Authors: Omote K. , Arai T.
Published: March 2019

In the spectroscopic analysis of minor and trace elements by fluorescent X-rays, many improvements in the analytical performance of trace element measurements have been made. For the analysis of trace elements, the background intensity governs the analytical accuracy and the lowest detection limit in a sample. A comparison is made between experimental and theoretically calculated background X-ray intensities in a previous paper. It is based on the formula for scattered X-ray intensity, from the estimation of Thomson and Compton scattered X-rays. Also, the asymmetrical peak profiles at the base of the giant intensity peak are discussed and are clearly shown in the skirt part of K beta X-rays, e.g. , Ni-K beta or Fe-K beta X-rays. The purpose of this report is to investigate the intensity of background X-rays, using glass beads and powder samples of iron oxide and quartz, based on the previous fundamental studies and the overlapping correction procedure for cobalt determination in low-alloy and stainless steel.