bluuebunny/crossref_metadata_2025 huggingface dataset:
Examination of the Reaction Kinetics at Solder/Metal Interfaces via High Temperature X-Ray Diffraction
Authors: DeHaven P. W. , Walker G. A. , O'Neil N. A.
Published: March 2019

There is a great deal of interest by the electronics Industry in understanding the reactions occurring at the interface between a solid metal and a liquid solder or braze. This is due to the complex nature of current microelectronics Packaging, where soldering or brazing operations often involve complex metallurgies and tightly controlled furnace profiles. However, to date only a few studies have been carried out on the reaction kinetics at a liquid metal-solid metal interface. This is due in part to the difficulty in carrying out such , experiments. In the past, two main techniques have been used to obtain solid-state kinetic data. The first, quantitative metallography, is slow and tedious to perform, and generally of limited accuracy. The second technique involves measuring the change of some property, such as electrical resistivity, that is a function of the concentration of one of the phases. The main disadvantages of these techniques are that absolute values of concentration are not obtained, and that the relationships between a property and constitution are rarely available. In addition, most physical properties are sensitive to factors other than constitution, and interference from these factors can often result in erroneous data.
Using a Microcomputer-Controlled Robot Arm as a General Purpose Sample Changer
Authors: Russ John C. , Christian Russ J. , Leyden Donald E.
Published: March 2019

We have previously reported in these proceedings on the automation of Wavelength-Dispersive X-ray Fluorescence arid X-ray Diffraction Spectrometers using stepping motors, either installed in place of existing synchronous drive motors, or attached to existing gear or belt drive mechanisms that control the theta/two-theta positioning of the spectrometer. This technique is applicable to most types of instruments (successful adaptations to Philips, Siemens, GE/Diano, and Rigaku systems are working routinely at this writing).
A Versatile XRF Analytical System for Geochemical Exploration and Other Applications
Authors: Smith T. K.
Published: March 2019

For more than a decade the Institute of Geological Sciences has carried out large-scale geochemical analysis in pursuit of mineral exploration and regional geochemical reconnaissance programmes for the Department of Industry. Over this period an XRF analytical system has been developed to meet part of this requirement for multielement data. The elements of interest range from the fourth period to uranium, and have become more numerous as exploration and analytical techniques have expanded. In particular, additions have been made of those elements such as arsenic, molybdenum and tungsten which are more difficult of determination by conventional methods.
Quantitative X-Ray Fluorescence Analysis for Fly Ash Samples
Authors: Schlorholtz Scott , Boybay Mustafa
Published: March 2019

The disposal of fly ash from coal burning power plants is rapidly becoming an environmentally complex problem. Recently though, the attitude towards fly ash use has been changing from a disposal oriented point of view to a more rational position which considers fly ash as a resource to be recycled. One major hinderance of fly ash use has been the extreme variability of composition that exists between fly ashes produced at different power plants. This variability makes the analysis of fly ash very important.

The most common methods currently used for fly ash analysis are atomic absorption or wet chemistry methods defined in ASTM C311. Both methods tend to be expensive, time consuming, and sample preparation is both tedious and critical for some elements. In this study X-ray fluorescence (QXRF) is used for the quantitative analysis of the major and minor elements found in “typical” fly ashes. The method, which is computer controlled, is quick, reliable, and requires minimal sample preparation.
Polarization of X-Rays by Scattering from the Interior of a Cylinder
Authors: Zahrt John D.
Published: March 2019

In the previous paper, ZRI, we have discussed the properties of single scatter radiation emanating from a point source, displaced a distance e° from the inside radius r* of a cylinder wall, scattering inside the wall, and reaching a point analyte on a diameter line with the source but removed a distance eA, from the inside radius. Figure 1 shows the instrumental design. It is to be recalled that a triangle inscribed by a circle with two of its verticles defining a diameter is always a right triangle. Thus all such scattering events described above are approximately 90°. This in turn almost annihilates the electric field vector in the scattering plane and creates essentially plane polarized X-rays at the analyte. If the analyte-detector line lies perpendicular to the plane of the cylinder, scattering of the polarized source X-rays by the analyte into the detector Is also a 90° event, and being perpendicular to the first scattering plane, should essentially annihilate the source X-rays at the detector.
Applications of Room Temperature Energy Dispersive X-Ray Spectrometry Using a Mercuric Iodide Detector
Authors: Leyden D.E. , Harding A.R. , Goldbach K.
Published: March 2019

Energy dispensive X-ray spectrometry has been used extensively for the rapid, simultaneous deterninaion of elements in a variety of sample types. Excitation of the analytical sample can be by either X-ray tube, secondary targets, or radioactive isotopic sources. Tube sources have the advantages of convenient control of the excitation conditions, whereas an isotopic source or secondary target must be physically replaced by another to affect an excitation change. The use of primary filters between the sample and X-ray tube can greatly enhance the flexibilitty of the excitation conditions.
A Mathematical Comparison of the Lachance - Traill Matrix Correction Procedure with Statistical Multiple Linear Regression Analysis in XRF Applications
Authors: Klimasara Anthony J.
Published: March 2019

It will be shown that the Lachance-Traill XRF matrix correction equations can be derived from the statistical multiple linear regression model. By selecting and properly transforming the independent variables and then applying the statistical multiple linear regression model, the following form of the matrix correction equation is obtained:

Furthermore, it will be shown that the Lachance-Traill influence coefficients have a deeper mathematical meaning. They can be related to the multiple regression coefficients of the transformed system:

Finally, it will be proposed that the Lachance-Traill model is equivalent to the statistical multiple linear regression model with the transformed independent variables. Knowing these facts will simplify correction subroutines in Quantitative/Empirical XRF Analysis programs. These mathematical facts have already been implemented and presented in a paper: “Automated Quantitative XRF Analysis Software in Quality Control Applications” (Pacific-International Congress on X-ray Analytical Methods, Hawaii, 1991).

This demonstrates that the Lachance-Traill model has a strong mathematical foundation and is naturally justified mathematically.
SUPERXAP- A Personal-Computer-Based Program for Energy-Dispersive X-Ray Spectra Analysis
Authors: Yager D.B. , Quick J.E.
Published: March 2019

SUPERXAP (Super X-ray Analysis Program) enables IBM-compatible personal computers to analyze energy-dispersive spectra using least-squares spectral deconvolution. The program corrects for instrument drift, background, peak overlap, and matrix effects. Pull down menus provide 24 subroutines and functions, that allow spectra to be transferred, stored, viewed, manipulated, and analyzed. Spectral peaks can be identified manually or automatically with color-coded K, L or M lines. Working curves are developed using an interactive routine that creates standard files by least-squares fitting of peak intensities to known elemental abundances. Elemental abundances in unknowns may be determined in a variety of ways including on-line analysis of spectra as they are generated by an energy-dispersive detector and by batch analyses of spectra stored on disk. Standard deviation, based on counting statistics, is reported for each element in each analysis. Written in QuickBASIC 4.5 for interface with a KEVEX 7000 radioactive-source x-ray fluorescence analyzer, SUPERXAP could be adapted, with minor modification, to accept and analyze data from other instruments that produce energy-dispersive spectra.
Areas for Improvement in XRF Analysis of Low Atomic Number Elements
Authors: Vrebos Bruno A.R. , Kuipéres Gjalt T.J.
Published: March 2019

Accurate analysis of the light elements has been, from the early applications of X-ray fluorescence spectrometry a struggle compared to the determination of heavy elements in the same matrices. In contrast, there has been virtually no upper limit to the atomic number of the element that could be determined. The lower limit, however, has been continuously adjusted downward through the years. Clearly, the sensitivity as well as the lower limit of detection for the heavy elements have also been improved, but the effect is Jess striking than the advances made in the region of tight element performance. This paper deals specifically with wavelength dispersive sequential x-ray fluorescence spectrometry, although some of the observations made are equally applicable to energy dispersive spectrometry.
Applications of ED-XRF Technology to On-Line Analysis
Authors: Gunning Geoffrey R.
Published: March 2019

On-line analysis is a valuable tool for many industrial manufacturing processes. Real-time analytical results allow immediate control of a manufacturing process, giving significant improvements in product quality, and reductions in product wastage and labor.
Application of XRF in the Aluminum Industry
Authors: Feret Frank R.
Published: March 2019

X-ray fluorescence analysis has been used in the aluminum industry since the beginning of the 1950's. Initial applications involved predominantly raw materials such as bauxite. During the last decades its use expanded to every stage of aluminum production and today, XRF analysis is a recognized analyticaI technique, applied routinely in exploration, reduction and fabrication processes. Typical XRF applications in the aluminum industry at present are listed in Table 1. The number of determinations given represents usual industrial requirements, and may vary between laboratories. The sample preparation techniques are again the most commonly used for the applications.
X-Ray Diffraction from Multilayers with Different Microstructures
Authors: He Ping , Woolkm John A. , Sequeda Federico O.
Published: March 2019

X-ray diffraction measurements were performed on CoαPt1-α/Pd, Co/Pd, Co/Fe, and Co/W multilayer samples with different structures, such as CoαPt1-α alloy layer composition α, bilayer thickness, and number of bilayers. Multilayer samples were made by magnetron sputtering in a chamber with multi-parallel guns and a position controllable substrate. CoαPt1-α alloy layers were deposited by cosputtering from Co and Pt targets mounted on guns tilted towards a common substrate. Compositions of Co and Pt in CoαPt1-α layers were varied by use of different sputtering power. The thicknesses of magnetic and non-magnetic layers in multilayered samples were also systematically changed to investigate the relationship between x-ray diffraction lines and crystalline structures of multilayered films. It was found that the position of the main diffraction peak from multilayered films was solely determined by the crystalline structures within bilayers rather than bilayer thickness. A model was introduced to calculate microstructural parameters such as the thickness of interfaces and compositions at interfaces.
Residual Stress Measurements on Cr/Ni Pads Evaporated on Polyimide Thin Films
Authors: Goldsmith C. C. , Van Buskirk C.
Published: March 2019

Polyimide films are becoming more important in multi-layer structures, acting as dielectric films to separate conductive layers. High thin film residual stresses can cause problems with the polyimide film, leading to loss of adhesion between the metal film and the polyimide or can cause cracking in the polyimide.

In this paper, we examine the residual stresses in “as deposited” metal films evaporated onto BTDA-APB polyimide films and follow the change in residual stress of the nickel layer during subsequent thermal processing. We will show that the change in residual stresses can be correlated to the glass transition temperature of the polyimide film.
Thin Film Critical Residual Stress for Metal Pads on a Ceramic Substrate
Authors: Goldsmith C. C. , Kamath S. M. , Kumar A. H.
Published: March 2019

Residual stresses present in thin films evaporated on ceramic substrates, can lead to loss of adhesion of the metal features to the ceramic, or, between metal films in multi-level stacks. If the adhesion is good, ceramic cracking may occur around the metal features. Long term one must avoid stress corrosion cracking in the ceramic. These residual stresses are generated by a variety of causes. In general, defect incorporation during the deposition process and thermal expansion mismatch between thin film and substrate play major roles.

In this paper, we describe a method for determining the residual stresses that may be detrimental, or more accurately, the residual stress induced load that may cause reliability problems. This method involves evaporating metal pads or various thicknesses onto the ceramic to the point of failure, and measuring the residual stress loading on the substrate. A direct measure of this loading is the stress intensity factor which takes into account both the residual stress and pad or film thickness. Thus, a critical “load” or stress intensity at which substrate cracking or thin film delamination occurs can be estimated. This approach can be used to select the optimum metal-thickness combination for various substrates.
X-Ray DCD and EPMA Measurements of Al Concentration in Epitaxial AlxGa1-xAs/GaAs Layers
Authors: Macquistan D.A. , Bassignana I.C. , SpringThorpe A.J. , Packwood R. , Moore V.
Published: March 2019

Double Crystal X-Ray Diffraction (DCD) is often used to determine the Al content of AlxGa1-xAs/GaAs epitaxial layers. Assessing composition from a measurement of mismatch is problematic because it invokes a number of assumptions. This study bypasses these difficulties by comparing the measurement of mismatch directly with Al composition measurements made by electronprobe microanalysis. A study of coherent epitaxial AlxGa1-xAs layers showed that mismatch varies linearly with composition. The equation Al (x) = |ΔΘ| / 368 summarizes the relationship over the coherent range, where |ΔΘ| is measured in arc seconds.
Near-Surface-Layer Analysis by Critical Takeoff-Angle X-Ray Fluorescence Detection
Authors: Hayakawa Shinjiro , Sasaki Satoshi , Gohshi Yohichi
Published: March 2019

Near-surface-layer analysis by x-ray fluorescence critical takeoff-angle detection was examined theoretically and experimentally. The takeoff-angle dependence of Cr K-L x-ray fluorescence from Cr thin films was measured with practical analyzed depth varying from several thousand to less than one hundred angstroms. Comparison of Cr K-L and K-M takeoff-angle dependence shows the analyzed depth depends on the observed x-ray energy even with identical takeoff angles. The potential of nondestructive depth profiling is also discussed.
Phase Identification using Whole-Pattern Matching
Authors: Smith D. K. , Hoyle S. Q. , Johnson G. G.
Published: March 2019

The use of whole-pattern matching techniques for phase identification provides increased confidence in the phases determined compared with d-I matching and enhances the potential for determining the existence of phases present in low concentrations. Reference patterns from a database of selected phases were compared with the experimental pattern obtained from an unknown, and the results were ranked using figures-of-merit designed to distinguish the best pattern matches. Several different figures-of-merit have been evaluated, all of which proved successful in recognizing the strongest phase but varied with respect to the other phases.

Low-concentration phases are revealed when the patterns of the more abundant phases are stripped from the experimental trace using the best-fit scaled reference traces. Pattern stripping is improved by pattern shifting and profile shape matching which are provided for in the matching program.
An Algorithm for Correction of Intensity Aberrations in Bragg-Brentano X-Ray Diffractometer Data; Its Importance in the Multiphase Full-Profile Rietveld Quantitation of a Montmorillonite Clay
Authors: Matulis C.E. , Taylor J.C.
Published: March 2019

Intensity aberrations in Bragg-Brentano X-ray diffractometers reduce the measured intensities at low angles relative to higher angles, and the correction factor can be large at low 2θ angles. Aberration-free data is of great importance in full-profile Rietveld quantitative analysis or structure refinement. An algorithm is given which corrects the intensity aberrations for particular instrument dimensions and sample absorbance, with a fixed divergence slit. Variable divergence slits increase the Bragg-Brentano aberrations and skew the data. The importance of an aberration correction curve produced with the computer program BBCCURV is described in the multiphase Rietveld quantitation of a montmorillonite clay with the SIROQUANT quantitative analysis program system; good quantitation of the montmorillonite can only be obtained if the aberration corrections are applied.
Phase Analysis of Portland Cement by Full Profile Standardless Quantitative X-Ray Diffraction - Accuracy and Precision
Authors: Taylor J.C. , Aldridge L.P.
Published: March 2019

The multiphase Rietveld method has been used in the determination of phase abundance in six standard Portland cements, using the SIROQUANT personal computer software package for XRD quantitative analysis. Because of the extreme amount of line superposition and weakness of the cement patterns care must be taken in the selection of standard XRD profiles and in the refinement of unit cell dimensions and linewidths. Comparison with round-robin microscope assays of the same cements shows r.m.s. deviations of assays between the two methods of 2.1% for alite, 3.1% for belite, 1.7% for aluminate and 1.3% for ferrite. Precision, studied by repeated SIROQUANT analyses of nine XRD patterns from the same Australian cement show esd's of 1.3% for the alite assay, 0.8% for belite, 0.5% for aluminate and 0.5% for ferrite.
XRD Pattern Fitting as a Tool to Control Plating Parameters in Zinc Nickel Electroplates
Authors: Hammond Lloyd , Wright Don
Published: March 2019

Rietveld X-ray powder diffraction (XRD) and uniaxial stress measurement procedures are being evaluated as a means of correlating the crystalline structure properties of zinc-nickel electroplate with observed plating properties. The study is being performed on a suite of six samples of varying composition (6 to 20%Ni) electrodeposited on mild steel. Rietveld refinement of the XRD data (Rietveld, 1969) has been performed on a specially prepared ingot (9%Ni:91%Zn) to determine the structural parameters and relative abundances for the γ(Ni4Zn22), δ(Ni3Zn22) and η(Zn) phases which could possibly be present in the electroplate. Relative phase abundances were verified by Atomic Absorption Spectrometry (AAS) and electron probe microanalysis (EPMA) image mapping techniques.

The structural parameters for the ingot zinc-nickel phases were subsequently used as initial parameters in Rietveld calculations for the six electroplate samples. Structure refinement of the electroplate XRD data was hampered by extremely high preferred orientation and the corresponding lack of quality diffraction peaks. However, Rietveld refinements produced accurate cell dimensions (which correlate linearly with nickel composition), a means of quantifying the degree of preferred orientation, and crystalline phase verification. For residual stress determination, d-sin2ψ plots were produced for each electroplate sample. The plots were found to be linear for Ni < 12%, allowing calculation of residual stress, and distinctly curved for Ni > 12%.
An Advanced Technique for High Temperature X-Ray Elastic Constant and Stress Investigations
Authors: Liu Chun , Lebrun Jean-Lou , Sibieude François
Published: March 2019

A high temperature in situ X-Tay diffraction (HTXRD) instrument was devised for residual stress (RS) and X-ray elastic constant (XECs) investigations. The aim was to gain a better understanding of the stresses developed during high temperature oxidation, which is essential for the lifetime improvement of refractory alloys. The investigators use sin2ψ method to survey the stress evolution during oxidation in both the scale and the substrate, and differential method to determine the XECs that relate the measured/measurable deformation to the stress state of the materials studied. The stresses on the Ni/NiO system are measured in situ. The XECs are determined on XC75 steel samples. This paper presents the theories of stresses and XECs determined by HTXRD and briefly discusses the experimental results.
Humidity Controlled Diffractometry and its Applications
Authors: Kühnel Radko A. , van der Gaast Sjerry J.
Published: March 2019

Humidity sensitive mineral phases change their structure when humidity varies resulting in X-ray pattern changes in intensity, position, and shape of lines. These structural changes in hydrous minerals are induced by dehydration and rehydration, which can lead to phase transformations or to steady depletion which may result in a total structure collapse. By means of X-ray diffraction with a special attachment, such reactions can be followed. The controlled relative humidity is provided in situ, in a closed cell, by a flow of moistened helium gas which is flushed through the cell during the XRD analysis. Humidity diffractometry allows studies of reaction rates of dehydration-rehydration reactions and their reversibilities, as well as effects of additives and impurities on these reactions. Potential applications in basic research and in industry are demonstrated using montmorilionite, ettringites, sodium carbonates and calcium sulfates.
Measurement of Atomic Elastic Constants by Pulsed Neutron Powder Diffraction
Authors: Lawson A. C. , Kwei G. H. , Goldstone J. A. , Cort B. , Sheldon R. I. , Foltyn E. , Vaninetti J. , Eash D. T. , Martinez R. J. , Archuleta J. I.
Published: March 2019

We have developed a technique for determining the atomic elastic constants from measurements of the Debye-Waller factors. The Debye-Waller factors are obtained by Rietveld refinement of time-of-flight neutron diffraction data and interpreted in terms of an atomic Debye-Waller temperature. The method is applicable to powders and to materials that must be encapsulated for safety or environmental reasons. We will illustrate our technique with applications to actinide metals, to metallic hydrides and to high-temperature superconductors.
X-Ray Diffraction Study of Shock-Modified Tetragonal Phases of SnO2 and MnO2
Authors: Newcomer P. , Morosin B. , Graham R. A.
Published: March 2019

X-ray diffraction line-profile analysis on tetragonal forms of SnO2 (cassiterite), MnO2 (pyrolusite), and previously studied TiO2 (rutile), which were subjected to high pressure shock loading, show that residual lattice strain and coherent “crystal” size are a function of shock parameters. An interesting observation on a sample of MnO2 concerns the recovery of cubic Mn2O3 (bixbyite) in the material subjected to 22 GPa, indicating a shock-induced chemical synthesis.
Peak Broadening in Asymmetric Powder Diffraction
Authors: Dragoi Danut
Published: March 2019

In the case of asymmetric X-Ray powder diffraction, usually used for stress analysis, the peak broadening is a function of the following instrumental parameters: divergence angle of incident and diffracted X-Ray beams (equatorial divergence), divergence angle of Soller slits (axial divergence), tilt angle ψ, and the intrinsic parameters of the sample (Bragg angle, size and mosaicity of the microcrystals, crystallographic imperfections due to atom impurities). This effect of peak broadening is discussed quantitatively, independent of the form of the peak, by using an approximation of a constant distribution of the intensities of diffracted X-Ray beams. The broadening effect due only to the ψ tilt of the sample surface is studied in this work. The results are compared with experimental data obtained on ceramic composite material: α-Al2O3/SiC(whisker).
An Experimental Examination of Error Functions for Bragg-Brentano Powder Diffractometry
Authors: King H.W. , Payzant E.A.
Published: March 2019

A single function for the elimination of errors in precision lattice parameter determination has not been developed for the Bragg-Brentano x-ray diffractometer method, because of the different angular dependencies of the systematic errors. A review of the error functions shows that all but one can be calculated from the instrumental settings and known properties of a sample under investigation. The residual sample displacement error can be then be eliminated by using extrapolation plots or computer methods to correct the data to cosθcotθ plots. The slopes of cosθcotθ plots can also be used to align high temperature furnaces and low temperature cryostats mounted on x-ray diffractometers.
The Detection of Superlattice Lines in Cu-Zn Alloys using a Solid State Detector
Authors: Payzant E.A. , King H.W.
Published: March 2019

Using a high purity germanium solid state detector with sufficiently high energy resolution to discriminate between copper Kα and Kβ radiation, the superlattice reflections of the ordered Cu-Zn β′ brass structure have be detected by the anomalous dispersion effect. By coupling the high purity germanium solid state detector to a multichannel analyser, the superlattice reflections of the β′ brass structure were also detected by energy dispersive x-ray diffraction. Other applications for this combination of high resolution detector, electronic energy discriminator and multichannel analyser are indicated.
Effects of Refraction and Reflection on Analysis of Thin Films by the Grazing-Incidence X-ray Diffraction Method
Authors: Takayama Toru , Matsumoto Yoshiro
Published: March 2019

The grazing-incidence X-ray diffraction (GIXD) method was employed to analyze two-layer thin films, which were the samples of Å lOO Å Au/500Å Cu/Si02(substrate) and 250Å Cu/500Å Au/SiO2(substrate), which were prepared by the evaporation technique under the condition that the SiO2substrate was at room temperature. Diffraction profiles were obtained at various glancing angles ( α ) and the data were analyzed as a function of α. The results were as follows : 1) Diffraction peaks were shifted to larger diffraction angles, because of the refraction of the incident X-ray beam. The angular shift has been approximated by the equation, α - α2- αc2)1/2, where αcis the total ref reflection critical angle of the material. 2) As a result of the correction of angular shift, the stress of the evaporated films was estimated to be null. 3) The broadening of the Cu diffraction peak and the enhancement of the Cu diffraction intensity occurred at angles near αcof Cu, due to the reflection of the X-ray beam at the Cu/Au interface.
A Comparative Study of Stress Determination Techniques in Polycrystalline Thin Films
Authors: Noyan L. C. , Goldsmith C. C.
Published: March 2019

A review of the literature has shown that two major techniques are used to determine stress/strain in thin film structures: curvature measurement technique and internal stress measurement by the traditional sin2ψ technique. However, to date, there is no published comparison of the results from both techniques when they are applied to a given specimen.

In this paper we compare both methods theoretically and experimentally. We show that, while in some cases similar information is obtained from both techniques, there are cases where the two measurements give different results. We will show that, in such cases, the two methods can be complementary. Thus, they can be used to yield a more complete description of the total stress/strain tensor in the material.
Characterization of Thin Films Using XRF
Authors: Willis James E.
Published: March 2019

Thin film samples represent ideal samples for analysis using X-ray fluorescence in that they tend to be flat, smooth and homogeneous. However, before a sample can be characterized using XRF, several questions must be answered.
Basic Studies of Multi-Layer Thin Film Analysis Using Fundamental Parameter Method
Authors: Kataoka Y. , Arai T.
Published: March 2019

X-ray fluorescence analysis is the most suitable method, for the characterization of the thickness and the chemical composition of thin film samples. It is non-destructive, rapid, precise, and accurate for both metal and oxide samples.
Measurement of the Phase Composition of Partially Stabilized Zirconia (PSZ) Test Parts by X-Ray Powder Diffraction
Authors: Wewman R. A.
Published: March 2019

Zirconia(ZrO2) is one of a number of ceramic materials under development both at Dow and other companies for high cost, low-volume applications under severe corrosion/wear conditions. To improve the physical properties of zirconia, much work has been done worldwide in recent years developing partially stabilized zirconia, or PSZ. This is zirconium oxide which has been “stabilized” in the tetragonal form, typically by the addition of calcium or yttrium oxide. The term “partially stabilized” is given to these materials because the proper amount of oxide stabilizer will cause the zirconia to crystallize almost entirely in the tetragonal form under the proper processing conditions. However, the PSZ fabricated part is not completely stabilized, because it will undergo a tetragonal to monoclinic (T → M) phase transformation when subjected to an applied stress.
An Overview of the Use of XRD as a Tool in the Total Analysis of Powdered Household Laundry Detergents
Authors: King Margaret M. , Sabino Evelyn M.
Published: March 2019

Manufacturers of household laundry products and laundry detergent builders want to know the exact formularies used in prospective customers' and competitive product lines. No convenient source exists for this information because published formularies are numerous and differ widely, (See Table 1.)
Intensity and Distribution of Background X-rays in Wavelength Dispersive Spectrometry III
Authors: Arai Tomoya , Shoji Takashi
Published: March 2019

In the spectroscopic analysis of composite elements by x-ray fluorescence (XRF), it is the fundamental feature of this method that the background x-ray intensity is lower than that with electron excitation. However, the background x-rays of this method, which consist of Thomson (Rayleigh) and Compton scattered x-rays from the primary radiation, impair the analytical performance at the ppm level. In order toinvestigate the intensity of the background x-rays precisely,the study was conducted in two parts. The first part compared the measured and theoretically calculated x-ray intensities for Rh Kα and Rh Kβ peaks from various materials. The second part examined the determination of low concentrations of lead,arsenic and colonium in steel samples. The variation in the background x-ray intensities of the analyzed elements was found to be caused by the variation of the major elements and a correction equation for it is derived.
Analytical Errors from Electronic Instability in the Counting Chain of a Wavelength-Dispersive XRF Spectrometer
Authors: Smith T. K. , Ingham M. N.
Published: March 2019

Sporadic displacements of substantial magnitude were observed during routine analysis in the concentration intercepts for some trace elements, together with a similar change in the sensitivity (slope) for magnesium when determined using a synthetic multilayer. These effects were traced to the electronic circuit providing correction for pulse amplitude shift with intensity.
Theoretical Estimation of the Fourth-Order XRF Intensity
Authors: Fernandez J. E. , Molinari V. G.
Published: March 2019

A theoretical expression for the fourth-order XRF-intensity has been found using the transport theory. An exact solution of the Boltzmann equation for the photon flux in a semi-infinite homogeneous medium has been applied iteratively to find the intensity, XRF emission has been isolated from the scattering processes by considering only the photoelectric effect in the interaction kernel. The incident and emitted beams have been assumed as well-collimated.

Fourth-order intensity computations for a multicomponent material are reported as an example. Results show that the fourth-order intensity remains below a tenth of the tertiary and therefore may be neglected in most cases.
The Use of Field-Portable X-ray Fluorescence Technology in the Hazardous Waste Industry
Authors: Raab G. A. , Kuharic C. A. , Cole III W. H. , Enwall R. E. , Duggan J. S.
Published: March 2019

As the Environmental Protection Agency adds ever more sites to the National Priorities List for Superfund clean-up, there is a tremendous need for a fast method of screening for contaminants. In the case of inorganics, we can apply field-portable X-ray fluorescence technology.

With commercially available field-portable X-ray fluorescence equipment using in-situ measurements we can quickly screen a site (hundreds of measurements), input the data to a portable computer, process it, and print a colored concentration isopleth map of the contaminant of interest, all in realtime.

The in-situ measurement approach pioneered by Lockheed is the key to rapid screening capability. Problems arising from particle size distribution, soil heterogeneity, and bulk density are minimized by employing site-specific standards in the construction of our calibration curves. Inherent in these site-specific standards are all the matrix problems which occur in the routine samples.

The strength of field-portable X-ray fluorescence technology is the accuracy of analysis above the quantitation limits. The difficulty in measuring low concentrations near the detection limit is the weak point of field-portable units.

NOTICE: Although this research was funded in part by the U.S. EPA through Contract 68-03-3249 to Lockheed Engineering & Sciences Company, it has not undergone Agency review and does not necessarily reflect Agency policy.
X-ray Fluorescence Analysis of Zeolites for the Determination of Silica: Alumina Ratio and Soda: Alumina Ratio
Authors: Gokhale P. A. , Wuensche M. R.
Published: March 2019

Zeolites-based fluid cracking catalysts are used in petroleum refining. Zeolites are crystalline alumina silicates with a framework based on extensive three-dimensional network of oxygen, and cations which occupy nonframework positions. The distribution of silicon and aluminum atoms within the framework determines many important properties of zeolites, most notably catalytic, absorptive capacity, acidity, stability, etc. For the zeolite scientist, information obtained from the determination of silca:alumina ratio (SAR) and soda:alumina ratio (NAR) during crystallization, dealumination and cationic exchange is important for the optimization of preparative techniques and development of new products.
Applications of On-Line XRF and XRD Analysis Techniques to Industrial Process Control
Authors: Hietala Mattt , Kalnicky Dennis J.
Published: March 2019

Temperature, pressure, and flow measurements are considered standard for process control purposes. It is vital that they be made on-line in real-time and not manually in the laboratory. Chemical assays should be done as fast and continuous as temperature measurements in order to be useful for process control. Until recently, this has not been the case because the assay methods have been difficult to automate.
What Can Data Analysis Do for X-Ray Microfluorescence Analysis?
Authors: Zahrt John D.
Published: March 2019

In 1985 Nichols and Ryon [1] first demonstrated their x-ray microfluorescence analysis (XRMF) system. By 1986 Nichols et al. [2] Boehme [3] and Gurker [4] provided us with spectacular photographs of x-ray images of geological materials, wire grids, and semiconductor chip carriers. During the delivery of the paper by Nichols et al. [2] the present author realized that a higher degree of spatial resolution could be accomplished by analysis of the raw data.
Micro X-Ray Fluorescence Analysis with Synchrotron Radiation
Authors: Hayakawa Shinjiro , Iida Atsuo , Aoki Sadao , Gohshi Yohichi
Published: March 2019

A synchrotron radiation X-ray micro analyzer(SRXMA) was developed at Photon Factory in Japan. The present SRXMA combines a double crystal monochromator and mirror optics and either a white or a monochromatic microbeam can be used. Micro X-ray fluorescence analysis was carried out, and a minimum detection limit of 1 ppm for Mn was obtained for 100 sec measurement with the white beam. With monochromatic beam excitation, micro X-ray spectroscopies are now feasible.

The obtained beam size was 1.6 μ;m - 34 μm* The beam was blurred in one direction by the scattered X-rays caused by the surface irregularities of the focusing mirror. Improvements in the mirror quality will ensure a beam spot of just a few microns with sufficient intensity.
Chemical State Analysis by X-Ray Fluorescence Using Absorption Edges Shifts
Authors: Sakurai Kenji , Iida Atsuo , Yohichi Gohshi
Published: March 2019

Recently synchrotron radiation (SR) sources have been extensively used for the study of materials science. The high intensity of tunable monochromatic X-rays from SR facilitates many types of spectroscopic/ diffraction studies which have otherwise not been possible. Regarding the X-ray fluorescence technique, significant improvement of the minimum detection limit has been performed and has enabled trace element analysis in the order of tens of ppb or 10-12 g.3-8 SR microanalyzers and near surface analysis using grazing incidence geometry are also attractive applications of synchrotron X-ray fluorescence technique. From a point of materials characterization, chemical state analysis is not less important than ordinary element analysis.
High Resolution X-Ray Fluorescence Si Kβ Spectra: A Possible New Method for the Determination of Free Silica in Airborne Dusts
Authors: Purton J , Urch D S , West N G
Published: March 2019

High resolution x-ray emission spectroscopy (HRXES) has been used to record the Si Kβ spectra of a variety of minerals. Distinct changes in peak profile can be related to mineral typo. Representatives spectra were chosen and incorporated, into a computer programme to allow the determination of free silica in binary and quaternary mixtures. The potential of HRXES for the analysis of airborne dust samples is discussed.
X-ray Diffraction Analysis of High Tc Superconducting Thin Films
Authors: Huang T. C. , Segmuller A. , Lee W. , Lee V. , Bullock D. , Karimi R.
Published: March 2019

X-ray diffraction techniques have been used for the structure characterization of Y-Ba-Cu-O and Tl-Ca-Ba-Cu-O thin films. A powder diffraction analysis of Y-Ba-Cu-O films showed that the films deposited at 650°C on Si are polycrystalline and have an orthorhambic structure similar to that of the YBa2Cu3O7 bulk superconductors. In addition to the conventional powder diffraction technique, both the rocking curve and the grazing incidence diffraction methods were used to characterize a YBa2Cu3O7 film on (110) SrTiO3 substrate. Results showed that the film was epitaxially grown and aligned with its substrate in a true epitaxy. Phase identification and line broadening analyses of Tl-Ca-Ba-Cu-O films showed that the films are comprised of one or more superconducting phases and probably contain stacking faults.
Texture Analysis of Thin Films and Surface Layers by Low Incidence Angle X-ray Diffraction
Authors: Heizmann J. J. , Vadon A. , Schlatter D. , Bessières J.
Published: March 2019

It is necessary to know the orientation of thin surface layers for the electronic industry as well as for different studies on interphases (epitaxy, topotaxy, phase transformation, reactivity of solids).

It is difficult to obtain information with a conventional Schulz goniometer (Bragg-Brentano geometry) because of the insufficient amount of diffracting material.
Fast Thickness Measurement of Thin Crystalline Layers by Relative Intensities in XRPD Method
Authors: Kimmel G. , Shafirstein G. , Bamberger M.
Published: March 2019

In this work a continuous wave CO2 laser was used for melting a layer of amorphous alumina obtained by anodizing 6061 aluminum plates. Melting the surface of the anodized plates led to the formation of a new uniform corundum layer at the expense of some of the amorphous coating, resulting in a double layer coating of crysta11ine on amorphous.

The characterization of the corundum layer is essential for process optimization study. Among the non-destructive methods X-ray diffraction is useful, because it provides us with selected data on the crystalline layer.
Separation of the Macro- and Micro-Stresses in Plastically Deformed 1080 Steel
Authors: Winholtz R. A. , Cohen J.B.
Published: March 2019

The stress tensors were measured with x-ray diffraction in both the ferrite and cementite phases of a 1080 steel specimen deformed in uniaxial tension. The macro- and micro-stresses were separated for all the components of the stress tensors. All the components except the hydrostatic components of the micro-stresses could be determined without an accurate value of the unstressed lattice parameter. Tensile stresses were found in the cementite and compressive stresses in the ferrite along the deformation direction. The tensile stresses in the cementite were quite large.
Taking into Account the Texture Effect in the Measurement of Residual Stresses by Using the Vector Method of Texture Analysis
Authors: Tidu Albert , Vadon Albert , Heizmann Jean-Julien
Published: March 2019

Crystallographic texture induces an anisotropic mechanical behavior of the poly-crystal, so that the current analysis of the macro residual stress by X-ray diffraction cannot be used, because the lattice-stram distribution versus sin2(φ) presents a non-linear behavior. In order to take into accountthe influence of the texture, several authors have proposed theoretical explanations using the orientation distribution function. Many of them use the ODF to calculate the X-ray elastic constants, another one uses Bunge's texture representation to obtain analytical expressions of the strain for textured specimens.
X-Ray Diffraction Studies on Shock Modified Y Ba2 Cu3 O7 Superconductors
Authors: Lowry Lynn E. , Lawson Daniel D. , Phillips Wayne M.
Published: March 2019

Y.Ba2Cu3O7, a high TC superconductor powder, was shock compacted and explosively welded inside a copper matrix using the explosive fabrication methods described by Murr, Hare and Eror. The shock compression fabrication technique provides the ability to process the superconductor powders into useable structures that will minimize environmental degradation and will not negatively affect the physical or mechanical properties. Additionally, the introduction of shock induced defects are known to increase solid-state reactivity in ceramic materials. For this reason, shock compression fabrication of the superconductor/copper system offers the possibility of enhancing the superconducting properties of the YBa2Cu3O7 powders.
The Characterization of a Solid Sorbent with Crystallite Size and Strain Data From X-Ray Diffraction Line Broadening
Authors: Briden Frank E. , Natschke David F.
Published: March 2019

EPA's Air and Energy Engineering Research Laboratory is currently investigating the injection of dry calcium hydroxide [Ca(OH)2] into coal fired electric power plant burners for Che control of sulfur dioxide (S02) emissions.
Parallel Beam and Focusing X-ray Powder Diffractometry
Authors: Parrish W. , Hart M.
Published: March 2019

Comparison of results using synchrotron radiation and X-ray tubes requires a knowledge of the fundamentally different profile shapes inherent in the methods. The varying asymmetric shapes and peak shifts in focusing geometry limit the accuracy and applications of the method and their origins are reviewed. Most o f the focusing aberrations such as specimen displacement, flat specimen and θ-2θ mis-setting do not occur in the parallel beam geometry. The X-ray optics used in synchrotron parallel beam methods produces narrow, symmetrical profiles which can be accurately fit with a pseudo-Voigt function, They have the same shape in the entire pattern. Only the width increases as tanθ due to wavelength dispersion but with higher resolution systems dispersion can be eliminated. The constant instrument function contribution to the experimental profile shape is an important advantage in studies involving profile shapes, e.g., small particle sizes and microstrains, and accurate integrated intensities. The absence of systematic errors leads to more precise lattice parameter determinations.
Optimizing the Calculation of Standardless Quantitative Analysis
Authors: Jinsheng Lu , Ronghou Xie , Xiaoqun Tan , Nieuwenhuizen C.
Published: March 2019

A method for quantitative phase analysis without standards (QPAWS) has been published in 1977 and has gained considerable interest, as the calibration for quantitative XRD may sometimes be difficult. Standards for quantitatative XRD are not generally available, and in many cases even the pure phases cannot be obtained.

The QPAWS method is based on (i) analysis of all phases present in the samples, (ii) foreknowledge of mass absorption coefficients (MAC)(iii) measuring samples which contain all phases in varying concentrations. In this method the number of samples used is equal to the number of phases to be analysed.
A Reference Database Retrieval System: Information as a Tool to Assist in XRD Phase Identification
Authors: Alam S.O. , Edmonds J.W. , Hom T. , Nicolosi J.A. , Scott B.
Published: March 2019

A common analytical problem in a X-ray diffraction laboratory is the phase identification of an unknown sample. Presently, most phase identification is either performed manually or through computer search-match programs, as found on automated powder diffraction systems. Whether phase identification is performed manually or with computer search-match, often, the diffractionist wishes or needs to be able to make use of more sample information in the phase identification process than just d-I data. Additional information may be in the diffractionist's possession or can be readily obtained. The types of additional information which can be used in computer search-match programs are currently limited to information in the Powder Diffraction File-1 (PDF- 1) (1), formerly Level I, database (ie., JCPDS sub-files, elemental and functional groups). The use of other information is not possible. Users of manual search procedures are not able to make optimum use of additional information.
X-ray Diffraction Studies of Solid Solutions of Pentaglycerine-Neopentylglycol
Authors: Chandra D. , Barrett C. S. , Benson D. K.
Published: March 2019

An array of molecules that is anisotropic in the extreme has been discovered in certain thermal-energy storage materials and is reported here: neopentylglycol (NPG) and NPG-rich solid solutions with pentaglycerine (PG) have a crystal structure, stable at room temperature, that consists of bimolecular chains of molecules that are all unidirectionally aligned throughout a crystal. There are hydrogen bonds between every molecule in one chain and its neighbors in that chain, but none between molecules of one chain and any molecules of the neighboring parallel chains. Thus there are strong intermolecular bonds along each chain and only weaker bonds between the chains. The structure has been determined by using modern single crystal techniques with 529 independent reflections from a crystal of NPG (C5H12O2). The structure is monoclinic with space group P21/c - C2h5. This anisotropic structure transforms to a cubic structure at higher temperatures.