bluuebunny/crossref_metadata_2025 huggingface dataset:
X-Ray Fluorescence Minor- and Trace-Element Analyses Silicate Rocks in the Presence of Large Interelement Effects
Authors: King B. S. , Espos L. F. , Fabbi B. P.
Published: March 2019

An X-ray fluorescence (XRF) method has been devised for the rapid quantitative determination of 16 minor and trace elements in geological materials. This method, a modification of a direct dilution method (1, 2, 3), uses a sample-to-binder ratio of 85:15 for sample preparation. Pellets prepared by this method are durable and do not deteriorate rapidly when exposed to high X-ray irradiation. Interferences and matrix effects are successfully corrected in actual analyses by employment of multiple linear regression equations.

Accuracy and precision have been improved over the method previously used in this laboratory. Detection limits have been lowered for Zn, Rb, Y and Zn approximately by the factor of 2. When interelement corrections are made, the XRF values are found to be in good agreement with the preferred chemical values for the 19 international silicate-rock standards.
Excitation Efficiencies for K and L X-Ray Fluorescence by a Mo Transmission Tube
Authors: Watson R.L. , Michael M.W. , Hernandez J. , Leeper A.K. , Wendt C.D.
Published: March 2019

The excitation efficiencies for K- and L- x-ray fluorescence by a Mo transmission tube operated at 30 kV have been measured. K x-ray excitation efficiencies for 14 elements ranging from A1 to Y and L x-ray excitation efficiencies for 12 elements ranging from Br to U are presented. The K x-ray excitation efficiencies are compared to those predicted from theoretical photoionization cross sections and empirical fluorescence yields, and the L x-ray excitation efficiencies are used in conjunction with theoretical photoionization cross sections to derive average L-shell fluorescence yields.
A Theoretical Study of the Effects of Dead Layers on Low Energy X-Ray Detectors
Authors: Hight R. , Inskeep C. N.
Published: March 2019

A Monte-Carlo model has been developed to calculate the effect entrance windows, or dead layers, have on the spectral shape and the counting efficiency of semiconductor detectors used in the low energy x-ray region (1 – 5 KeV).
The Effect of Various Pattern Aberrations on Figures of Merit Used With Whole Pattern Recognition Techniques
Authors: Smith D. K. , Hoyle S. Q. , Johnson G. G.
Published: March 2019

The affect of several aberrations on the figures of merit, FOM, used in the identification analysis of diffraction patterns has been examined by generating simulated diffraction traces with mathematically induced errors. Patterns of mixtures with random 20 shifts, intensity variations, and profile broadening were generated for analysis by MATCHDB, and the behavior of three FOMs during the search step was followed. The results have shown that the angle errors are the most serious in degrading the potential for identification of the phases in the mixtures. Intensity errors cause some degradation on the results. Broadening has little affect when using whole-pattern matching methods.
New Developments in PC-Based Powder Data Retrieval Programs
Authors: Jenkins Ron
Published: March 2019

While most contemporary methods of qualitative analysis of multi-phase materials are still based on the classic Search/Match/Identify process developed by Hanawalt, Rinn and Frevel in the 1930s, during the past 10 years or so the personal computer, with associated CD-ROM storage, has made a dramatic impact on the ways in which classical procedures are being implemented. Until recently, most of the commercial mainframe and PC based software packages for qualitative phase identification have been designed to implement a fully automatic search/matching sequence. All of the major instrument suppliers now offer such programs as part of their Automated Powder Diffractometer (APD) packages. While these programs are extremely useful, the success of their application to a specific problem is critically dependent on the quality of both experimental data and reference data. Until the problems arising from comparing variable quality experimental and reference data are completely understood, it appears that there will continue to be an interest in user-inter active (computer-aided) manual methods of search/matching. This paper explores the use of the personal computer in the area of computer-aided search/matching
The Use of a Conventional Powder Diffractometer for Thin-Film Thickness Determination From Reflectivity DATA
Authors: Huang T. C. , Gilles R. , Will G.
Published: March 2019

Precise thin-film thicknesses have been obtained from X-ray specular and off-specular reflectivity data collected with a conventional powder diffractometer. An analysis of the specular reflectivity curve for a 565.9-Å thick pt film showed the results agreed with those determined previously from high-resolution reflectometer data to within 6.6 Å or 1.2%. An analysis of the off-specular reflectivity curves which have well-defined interference fringes showed that the results were insensitive to the surface alignment. Values of Pt thickness for the off-specular reflectivity curves agreed with that of the specular reflectivity curve to within 6.2 Å or 1.1%. The insensitivity in film-surface misalignment makes conventional powder diffractometer attractive for film-thickness determination and opens this techniques to many laboratories.
Complicated Average Stress-Fields and Attempts at Their Evaluation With X-Ray Diffraction Methods
Authors: Ruppersberg H.
Published: March 2019

Conventional X-ray stress analysis is based on the so called "linear sin2ψ" law and yields average two axial stresses in the irradiated surface layer of polycrystalline specimens. Three examples are given in this paper where either strong deviations from the linear law are observed due to stress gradients or where the linear law yields wrong results because of three axial stresses. Special experimental techniques are described and formalisms are given for the evaluation of the corresponding stress fields which are in the described cases more complicated than usual.
Determination of X-Ray Elastic Constants of Isotropic Materials With Non-Linear Sin2ϕ Diagrams
Authors: Sasaki Toshihiko , Hirose Yukio
Published: March 2019

As known well, non-linear sin2ϕ diagrams are observed from materials having either steep gradients of residual stresses paralell to the surface normal of the specimen or tri-axial stress components. Many authors have reported on this problem for several processing such as polishing and grinding etc. The authors also obtained such non-linear data from an electro-plated zinc—nickel alloy. For these cases, the sin2ϕ method is inadequate for the stress evaluation. Much attention has been given to the stress analysis from about 1970s as compared to the X-ray elastic constants for this phenomenon.
X-Ray Stress Measurement of Alloy Steels X-Ray Study of Elastic Deformation for Alloy Steels with Composite Microstructures
Authors: Tsuda Masaaki , Goto Tokimasa , Sasaki Toshihiko , Hirose Yukio
Published: March 2019

Residual stress is inevitably introduced into composites because of the mismatch of the coefficient of thermal expansion, and it is different for each phase. The x-ray method can detect separately the stress in each phase, so will yield useful information for analyzing the toughening mechanisms of composites.
Capillary Optics for X-Ray Analysis
Authors: Dozier C. M. , Newman D. A. , Gilfrich L. V. , Freitag R. K , Kirkland J. P.
Published: March 2019

Capillary collimators have found a number of uses in fluorescence, diffraction and other x-ray fields. Most of these applications are realized with single, straight glass capillaries. Focussing of synchrotron x-radiation beams has been shown with tapered capillaries. In addition, numerous straight and bent capillaries, bundled into lens-like optics, offer experimenters many other possibilities for better use of the x-radiation from tubes, synchrotron radiation, and plasma sources or the x-ray intensity collected from samples.
Toroidally Shaped Hopg Crystals as Strongly Focusing Bragg Reflectors of Characteristic X-Ray Tube Radiation for Edxrf Analysis
Authors: Beckhoff B. , Kanngieβer B. , Scheer J. , Swoboda W. , Laursen J.
Published: March 2019

The characteristic 17.441 keV Mo-Kα tube line yields an exceedingly strong reflection at a Bragg angle of 6.0710 on Highly Oriented Pyrolytic Graphite (IIOPG). Using doubly bent toroidally shaped crystals we were able to concentrate the characteristic radiation from a Mo anode fine focus tube onto a small focal spot area of about 1 mm. FWHM diameter, as was observed by an X-Ray sensitive CCD. The radiation of the Mo anode fine focus tube is emitted at a take-off angle of 60 into a total solid angle with an aperture of 120. About 90 percent of this primary radiation solid angle can be used for the desired Bragg reflection on the designed toroidal crystal surface. This feature ensures the high beam intensity needed for special excitation problems.
Optics for X-ray Microfluorescence to Be Used at the European Synchrotron Radiation Facility
Authors: Vincze L. , Janssens K. , Adams F.
Published: March 2019

Micro-SRXRF (Synchrotron Radiation induced X-ray Fluorescence) is ti microanalytical technique which, utilizes an intense, polarized X-ray micro beam originating from the storage ring to induce X-ray fluorescence in a microscopic volume of the sample under investigation. The emerging fluorescent and scattered radiation is normally detected by an energy-dispersive Si(Li) detector. The recorded fluorescent spectra provide qualitative and quantitative information on the examined material yielding minimum, detection limits in the ppm and in favourable cases in the sub-ppm range at current SRXRF-facilities. Possible applications of synchrotron X-ray microprobes are the mapping of chemical elements in biological tissues, investigation of element migration and partitioning in geological systems, the analysis of individual microscopic particles and a variety of topics in applied research.
Xrf With Tunable Monochromatic Excitation and Variation of the Incidence Angle
Authors: Ebel Horst , Ebel Maria F. , Svagera Robert , Wirth Norbert , Kaitna Roland , Schandl Hartinut
Published: March 2019

The x-ray source of our instrument is a rotating anode system with a silver target. It is flanged to a He-filled monochromator chamber. The photon energy of the x-rays for the excitation of characteristic specimen radiation can be tuned continuously from IkeV to 30 keV. The cross-section of the beam - monochromatic or polychromatic tube radiation - leaving the monochromator chamber is variable within 0.1 and 100mm2. A Be-window separates the evacuable specimen chamber from the monochromator chamber. The specimen holder allows for a linear movement of the specimen in x- and y-direction normal to the beam of incident x-radiation and allows a laterally resolved analysis. A rotation around an axis normal to the incident x-ray beam enables investigations under variable incidence- and take-off angles. X-ray detection is performed by an energy dispersive system.
On-Line Analysis Of Molten Metals Using a Wavelength Dispersive X-Ray Spectrometer
Authors: Creasy Larry E.
Published: March 2019

The electron beam furnace is a nearly ideal tool to conduct on-line analysis of molten metal. In the process of melting the metal with a high intensity electron beam, x-rays are created. A wave-length dispersive x-ray spectrometer, specially designed for this environment, has been used to analyze the composition of the molten metal. This significantly reduces the time required to determine the concentration of critical elements in the melting process.
A New Method Of Graphic Representation Of Sample Analysed By XRF
Authors: Figueroa Rodolfo G. , Caro David G.
Published: March 2019

XRF nondestructive sample analysis is very convenient when applied to samples that should not be altered, for example, works of art or archeological pieces. When one has various similar samples of this characteristic, a good sample comparison method is necessary. There are various comparison methods among which the three component graphic representation allows a comparison in a throe element component. In an XRF analysis, a large number of peaks, representing emissions from K and L lines normally appear. When a well calibrated spectrum is provided, the determination of the elements in the samples is relatively simple. However, accuracy is difficult to acheive when results from many samples are to be compared.
Computer Automation of X-Ray Powder Diffraction
Authors: Lindsey J.S. , Christenson C.P. , Henslee W.W.
Published: March 2019

The interfacing of a Hewlett-Packard 9825 calculator to an Enraf-Nonius microdensitometer and a Philips powder diffractometer provides automated data collection and manipulation on a routine basis. Data is acquired and stored on a floppy disk; background corrections are made; diffraction peak maxima are found, normalized and plotted; a table of approximate d-spacing
(±0.0lÅ) is printed. The analyst designates the internal standard peaks. Corrected d-spacings are then computed, tabulated and printed above the appropriate peak. An accurate d-spacing scale is drawn on the plot. The total time for a scan is approximately twenty minutes with only about five minutes of operator time required. The program is conversational and requires little prior knowledge of the software by the operator. Data interpretation is further aided by supporting programs to calculate patterns from literature, determine lattice constants for observed phases, help index patterns, deconvolute overlapping peaks, carry out crystalline size determinations and perform search/match procedures. Such supporting programs are possible because, even though the system can be used in a “dedicated” manner, it is still a stand-alone computer. Thus, the desired degree of automation in data collection has been obtained without sacrificing flexibility.
Quantitative Phase Analysis of Devonian Shales by Computer Controlled X-Ray Diffraction of Spray Dried Samples
Authors: Smith Steven T. , Snyder Robert L. , Brownell W. E.
Published: March 2019

Spray drying is shown to be an effective and rapid method for preparing samples for quantitative analysis by x-ray powder diffraction. Previously intractable problems like the simultaneous analysis of multiple phases in orientation prone systems can be carried out. Using this method, and a computer controlled diffractometer, five and six phase analyses of Devonian shales can be accomplished in approximately forty minutes. A rapid and convenient method for using the absorption diffraction technique for x-ray quantitative analysis is described.
Comparison of Stress Measurements by X-Rays with Three Different Detectors and a Strongly Fluorescing Specimen
Authors: James M. R. , Cohen J. B.
Published: March 2019

Measurements on the heat affected zone of a weldment are presented using a gas filled position sensitive detector and a normal diffractometer equipped with a scintillation detector and a solid state detector. The sample, a surface ground titanium alloy, provided a difficult application for the X-ray technique from which a test of the real usefulness of the position sensitive detector could be made. The diffraction profile from the Ti alloy is very broad and the fluorescence produces a high background. The fluorescence is easily rejected using a solid state detector; however, the time of analysis is very long. With the position sensitive detector, the combination of increased energy discrimination over the scintillation detector and the simultaneous measurement of many data points over the broad peak enabled the measurements to be made for the same accuracy in much shorter times than for either the solid state detector or the scintillation detector.
A Diffractometer Based Energy Dispersive Elemental Analyser
Authors: Ciccarelli Michael F. , Goehner Raymond P.
Published: March 2019

Instrumentation has been developed which employs standard x-ray diffraction equipment and an energy dispersive analyzer for elemental and phase analysis. A General Electric XRD-6 diffractometer, a sample chamber, a Nuclear Semiconductor energy dispersive analyzer (EDA) with 155 eV resolution, and a Tracor Northern multichannel analyzer are its main components.
Development of the Detector Response Function Approach for the Library Least-Squares Analysis of Energy-Dispersive X-Ray Fluorescence Spectra
Authors: Wielopolski L. , Gardner R. P.
Published: March 2019

A procedure to obtain analytical models for the elemental X-ray pulse-height distribution libraries necessary in the library least-squares analysis of energy-dispersive x-ray fluorescence spectra is outlined. This is accomplished by first obtaining the response function of Si(Li) detectors for incident photons in the energy range of interest. Subsequently this response function is used to generate the desired elemental library standards for use in the least-squares analysis of spectra, or it can be used directly within a least-squares computer program, thus eliminating the large amount of computer storage required for the standards.
Determination of Solids Content in Slurries by X-Ray Scattering
Authors: Farus J. , Kierzek J. , Zóltowski T. , Kuc G. , Ratyński W.
Published: March 2019

Using corrections applied to the XRE analysis of copper ore flotation materials, two methods of determining the ratio of solid to liquid content in slurries are described. Both are based on the use of coherently scattered radiation. In the first method the intensity of Cu, Pb and Fe is normalized using a coefficient defined as a ratio of scattered radiation from the sample and pure diluent. In the second, the regression equations are applied. Satisfactory results have been obtained for solid contents ranging from 10 to 40%.
Improved X-Ray Fluorescence Capabilities by Excitation with High Intensity Polarized X-Rays
Authors: Ryon Richard W. , Zahrt John D.
Published: March 2019

Energy dispersive x-ray fluorescence is an established and versatile tool for measuring major and trace elements in virtually any kind of solid or liquid specimen. The usefulness of the method could he extended even further if the time of analysis for multicomponent samples could he reduced. In other words, we desire to analyze a wide range of elements with detection limits at least as good as obtained when the excitation conditions are optimized for a specific element or narrow range of elements. A major impediment to achieving this goal when analyzing bulk, low-Z materials is the scatter of source radiation into the detector by the specimen being analyzed. The adverse effects of the scattered radiation are its contribution to the background signal (i.e., “noise“) and its overwhelming contribution to the limited counting rate of the system electronics.
Evaluation of Existing X-Ray Powder Diffraction Standards for Phosphate Minerals
Authors: Blanchard Frank N.
Published: March 2019

Of the roughly 3,000 known mineral species over 290 or 10 percent are phosphates. This report deals with a recently initiated project, the purpose of which is to produce better X-ray powder diffraction standards than currently exist for selected phosphate minerals. The project involves evaluation of existing X-ray diffraction standards for phosphate minerals, and collection of new data from species for which current data are judged unsatisfactory.
Data Sets for Evaluation of Powder Diffraction Search/Match Algorithms
Authors: Pfoertsch Diane E. , Hamill Gregory P. , De Camp Wilson H.
Published: March 2019

Among powder diffractionists, there is a concern about establishing criteria for testing existing and new computer methods for searching the Powder Diffraction File (PDF) data base. A large number of papers on this subject have been presented at recent Denver Conferences and at other meetings, such as the American Crystallographic Association.

The PDF now exceeds 42,000 patterns, with an average of about thirty lines per pattern. Thus, it contains approximately 2.5 million numerical values. At its current rate of growth, the PDF will double in less than twenty years.
A Useful Guide for X-Ray Stress Evaluation (XSE)
Authors: Hauk Viktor M. , Macherauch Eckard
Published: March 2019

This paper summarizes experiences available for the measurement of lattice strains in different materials with different wavelengths to evaluate stresses by means of X-rays. The recommendations given are based on previous statements. Some principles of fundamentals of X-ray physics for the recording of interference lines with Ω and ψ-diffractometers are dealt with. Methods applicable for the determination of the peak position of the interference lines, the assessment of linear and non-linear lattice strain distributions, and tine calculation of stresses are outlined. For iron, aluminium, copper, nickel and titanium the constants for practical X-ray stress evaluation (XSE) and the parameters of measurement are tabled.
Small Area X-Ray Diffraction Techniques; Applications of the Micro-Diffractometer to Phase Identification and Strain Determination
Authors: Goldsmith C.C. , Walker G.A.
Published: March 2019

The trend towards smaller devices and packages in the semiconductor industry makes it increasingly important and increasingly difficult to obtain useful X-ray diffraction information from the small areas employed. This study covers applications of a Rigaku micro-diffractometer to measure strain and obtain phase information from areas less than 100μm in diameter. Examples of residual stress mappings between electrical vias only 100μm apart and phase determination on a single electrical via 120μm diameter will be shown.
References Intensity Quantitative Analysis Using Thin-Layer Aerosol Samples
Authors: Davis Briant L.
Published: March 2019

Interest in the reference intensity ratio CRIR) method continues as a result of the potential capabilities of the technique for rapid multi-component quantitative analysis. The theoretical basis for the RIR technique is now well established (Chung, 1974; Hubbard et al., 1976; Davis, 1980, 1981; Davis and Johnson, 1982), Major areas for which the method can still be greatly improved include the methods used for sample preparation, the measurement of accurate intensities, and the use of an internally consistent set of reference intensity constants (designated RIR, or ki). In the methodology developed at the Institute of Atmospheric Sciences (IAS), South Dakota School of Mines and Technology, sample preparation centers about the suspension of the pulverized sample into an aerosol and collection onto filter media. Because of this step, intensities must be corrected from their raw values to intensities representative of “infinite thickness“ and volumetrically constant conditions of normal sample diffraction. The measurement and correction of intensities and sample preparation methodology is the subject matter of the present paper.
Evidence for Stacking Faults in Multiaxial Strained Alpha-Brass
Authors: Roof R. B.
Published: March 2019

As part of a program studying the effects of large strain deformations resulting from multiaxial loading to a variety of materials, a thin walled tube (0.46” O.D. x 0.02” wall thickness) of 70-30 Brass was subjected to strain deformation in the following directions 1) along the tube axis, εz = 0.3393; 2) circumferential around the tube surface, εθ = -0.0121; 3) perpendicular to the wall thickness, εR = 0.3514. This report describes the results of an x-ray examination of the external surface of the tube by the line broadening technique.
Line Broadening Studies on Highly Defective Al2O3 Produced by High Pressure Shock Loading
Authors: Morosin B. , Graeber E. J. , Graham R. A.
Published: March 2019

Enhanced solid state reactivity of materials both during and after shock compression has been attributed to the introduction of large numbers of defects into the crystalline lattices and to reduction in the particle and crystallite size of powders [1,2]. Line broadening of x-ray diffraction profiles provides a means to determine the residual lattice strain resulting from such defect concentrations as well as a means to determine the coherent crystallite size. Various diffraction studies on shock-loaded powder materials have previously been reported and much of this work primarily by Soviet and Japanese scientists has recently been reviewed [2]. Cohen has reported results on shock-loaded copper [3]. In prior work, however, shock, pressures have not typically been quantified and there are few detailed line broadening investigations of refractory inorganic powders [1,4,5]. The present study on shock-loaded alumina powders is a detailed investigation of the influence of shock loading on residual lattice strain and coherent crystallite size.
An Empirical Background Calculation Method for Multi-Channel X-Ray Spectrometers
Authors: Kellogg R. B.
Published: March 2019

Several literature references address the relationship between the reciprocal of the absorption coefficient and the Compton scatter peak, intensity. Most workers use a Compton scattered tube line in the calculation of background; however, use of Bremsstrahlung scatter in the present work is also valid for this calculation. Background calculation for a fixed-angle monochromator is desirable since the background cannot be measured off peak. A method for calculating background for fixed-channel instruments by summing the calculated Rayleigh and Compton scatter intensities is presented in this paper.
Polarization of X-Rays by Scattering from the Interior of a Cylinder
Authors: Zahrt John D. , Ryon Richard
Published: March 2019

It is of interest today to use polarized X-rays in X-ray secondary fluorescence as a means of improving signal to noise ratios in the analysis of trace elements. Current experimental design makes use of two mutually perpendicular scatterings from plane parallel materials. Radiation with the electric field vector in the scattering plane (scattering angle = 90°) will be annihilated. Hence, after the mutually orthogonal, 90° scatterings no source X-rays should reach the detector. In practice source X-rays will only be greatly reduced at the detector due to such things as multiple scatter and collimator divergence. An experimental problem associated with this design however is the reduced intensity of the signal because of the scatterings with concomitant increase in analysis time.
Trace Element Analysis by Synchrotron Radiation Excited XRF
Authors: Davies S.T. , Bowen D.K. , Prins M. , Bos A.J.J.
Published: March 2019

The ability rapidly and quantitatively to detect trace elements in a host matrix is of great importance in many areas of science and engineering. This fact is underlined by the considerable amount of effort that has been put into developing such techniques as electron probe microanalysis, proton Induced x-ray emission (Pixe), the laser microprobe mass analyser (Lamma) as well as conventional x-ray fluorescence methods. Recently the availability of electron storage rings partially or wholly dedicated to producing intense beams of synchrotron radiation has provided a new tpol to complement the above mentioned techniques. This paper reports on work at Daresbury Laboratory on synchrotron x-ray fluorescence (SXRF) fo r quantitative trace element analysis.
The Measurement of Triaxial Residual Stress in Polymer-Coated Aluminum Circuitry in Microchip Modules
Authors: Crowder Cyrus E. , Radler Michael J. , Townsend Paul
Published: March 2019

The development of high density interconnection (HDI) technology in multichip modules (MCM's) will establish a new level in the hierarchy of electronic systems. The modules use organic insulating layers which, because of their low dielectric permittivity and loss, enable circuits with maximum density and speed. However, differences in the coefficients of thermal expansion (CTE's) for the insulating layers, the interconnects, and the substrates, produce residual stresses in the various components during processing. These stresses must be understood to engineer reliable designs for MCM's.
X-Ray Measurement of Triaxial Residual Stress in Ceramic Composites and Coating
Authors: Tanaka Keisuke
Published: March 2019

The X-ray diffraction method was used to measure the triaxial state of residual stresses in each phase in the following four kinds of composites; ZrO2/Al2O3 composite, WC-Co alloy, SiC/Al-alloy composite, and TiC/SiC coating. The residual macrostress and microstress were determined from the phase stresses by using the rule of mixture. The effects of heat treatment and surface finishing on the residual stress were studied. The measured value of the thermal residual stress was compared with the theoretical prediction based on the mismatch of the coefficient of thermal expansion.
Highly Sensitive X-Ray Stress Measurement in Small Areas
Authors: Fujii Nobuyuki , Kozaki Shigeru
Published: March 2019

The authors tried a new measuring method for stresses in small areas of ceramics. This method is characterized by the following.

1)

Applicable to small areas.

2)

High sensitivity.

3)

Stress calculations by measuring the average Debye ring radius in view of spotty diffraction rings.

4)

The use of an imaging processor for (3).

5)

The use of an imaging plate (IP) for reducing the exposure time.

We worked out a computer simulation about errors of the values measured by our method. The result showed a good approximation. With a test piece applied with a certain load, the difference between stresses measured by our method and those by a strain gauge was about 12 percent. We applied this method to the measurement of residual stresses which took place near the silicon nitride (Si3N4)/304 stainless steel brazing point interface. In the case of using an X-ray beam of 100 μm diameter, the exposure time was 90min with a high sensitive X-ray film and 3min with the imaging plate. In the case of an X-ray beam of 40 μm diameter, it was 120 to 190 min with the imaging plate.
Measuring Residual and Applied Stress using X-Ray Diffraction on Materials with Preferred Orientation and Large Grain Size
Authors: Pineault James , Brauss Michael
Published: March 2019

One of the most difficult tasks in applied and residual stress measurement of polycrystalline materials using x-ray diffraction is dealing with preferred orientation and large grain size.

A common solution to large grain size problems has been to choose a larger aperture, but in certain cases this is undesirable and/or impossible. When preferred orientation has been identified as the problem, the common approach has been to choose another diffraction plane or oscillate the x-ray diffraction head during data collection. Remedies such as these can distort the peak breadth and are often not sufficient to totally negate the grain size and preferred orientation effects.

A technique described as the “step scan with virtual window” has been developed jointly at MTL (formerly Canmet) and Proto Mfg. Ltd. to deal specifically with the aforementioned effects of grain size and preferred orientation.

This paper highlights some of the problems that arise in stress analysis of materials exhibiting preferred orientation and large grain size. Subsequently a comparison of the results obtained using standard diffraction technique, oscillation and the “step scan with virtual window” is made.
X-ray Topography of Surface Layers and Epitaxial Films
Authors: Bowen D. Keith
Published: March 2019

The techniques of X-ray topography are reviewed, with special reference to their application to the study of surface layers and thin films. The methods of section topography, white radiation topography and double and triple crystal topography are shown to be the most appropriate, with grazing or glancing incidence methods assuming special importance. Applications to the questions of epilayer mismatch and dislocation content, process-induced defects and surface damage are discussed.
Residual Stresses and Differential Deformation of Electroplated Structures
Authors: Sheikh G. , Noyan I. C.
Published: March 2019

We report the results of a recent study where nickel substrates electroplated with chromium were loaded in-situ on an x-ray diffractometer. This technique allows determination of lattice spacings in the vicinity of the interface for both the film and the substrate as a function of the applied load. We used such lattice parameter data, SEM observations of the surface and x-ray peak breadth data to study the partitioning of deformation between the film and the substrate. The data indicates progressive loss of adhesion between the film and the substrate with increasing deformation. We observe significant effect of electroplating residual stresses on the mechanical behavior of the system. The loss of adhesion between the film and the substrate coupled with the initial residual stress profile causes an apparent 'negative Poisson's ratio' for the film during initial stages of the loading. This effect disappears with cyclic loading and unloading.
Application of Position Sensitive Detectors for Neutron Diffraction Texture Analysis of Hematite Ore
Authors: Will G. , Merz P. , Schäfer W. , Dahms M.
Published: March 2019

Texture means the orientation distribution of the many crystallites in a polycrystalline sample with respect to a reference system on the sample, for example the rolling direction in steel. Texture has to be distinguished from preferred orientation observed in laboratory-made powder samples. Preferred orientation is just a nuissance in the experiment and must be corrected in the ensuing analysis, for example by the formula given by March and published by Dollase Preferred orientation we find commonly in samples containing plate-like crystal flakes. This is again to be distinguished from a non-random particle distribution in the powder samples prepared for diffraction experiments. This effect is always present, also for example in NBS silicon, even if only to a. very small degree (see for example Will et. al). It must and can easily be corrected for in the final least-squares calculation.
Derivation of d-Values from Digitized X-ray and Synchrotron Diffraction Data
Authors: Huang T. C. , Parrish W. , Masciocchi N. , Wang P. W.
Published: March 2019

A precise and practical method for the determination of d-values and lattice parameters from digital diffraction data is described. Systematic errors are corrected mathematically during a d-spacing / lattice-parameter least-Squares refincment process making it unnecessary to use internal standards. X-ray and synchrotron diffraction data of an ICDD alumina plate obtained with a wide variety of experimental conditions and analysis parameters were used to study the precision in the derivation of d-values and the accuracy in the determination of lattice parameters. Results showed that the precision in determining d-values was high with |Δd/d|avg ranging from 2x105 to 4x10-5. Using the results obtained from the high precision XRD analysis as a reference standard, the accuracy in the lattice parameter determinations from the synchrotron diffraction data reached the l-2x10-6] range. Lattice parameters, with an accuracy in the high 10-5 range, were also obtained using parameters commonly used in a routine XRD analysis such as a wide RS (0.11°) for high intensity, peaks only in the front reflection region, no Kα2 stripping, and a Single 2θo parameter for systematic error corrections.
Time-Resolved X-ray Stress Measurement During Cyclic Loading
Authors: Ohya Shin'ichi , Ohta Shozaburo
Published: March 2019

X-ray stress analysis is widely used in the measurement of residual stress or stress under static loading. If it is possible to measure actual stress at any applied stress level during cyclic loading by using x-rays, it will be of much help in investigating dynamical fatigue behavior such as crack closure and change of residual stress distribution.
Determination of Rolling Contact Stress Distribution by X-ray Diffraction
Authors: Milan David L.
Published: March 2019

An investigation was conducted of the potential for detection of the contact stress distribution in tapered roller bearing components made of carburized steel. Various raceway stress distributions were created by control of the profile and alignment of the rolling surfaces. Determination of residual stress in the rolling direction and peak breadth were made using a multiple tilt sin2ψ technique. The measurements were made at the surface and at depths below the surface. It was found that the distribution of residual stress and peak breadth perpendicular to the rolling direction in the layers below the surface of the inner race correlated highly with the imposed contact stress distribution. The correlation was less in the case of the outer race. The residual stress distribution measured on the surface of the inner race was observed to be inversely proportional to the contact stress distribution.
Diffraction Plane Dependence of X-ray Elastic Constants of Alumina
Authors: Kurita Masanori , Ihara Ikuo , Saito Akira
Published: March 2019

The 95% confidence linits of the x-ray elastic and stress constants of α-alumina were detemined from seven kinds of diffraction planes by the Gaussian curve method in order to investigate the diffraction plane dependence of the eonstants. No difference in the elastic constants larger than their 95% confidence intervals was observed for most diffraction planes. Also, the measured elastic constants for most planes were closer to the values calculated from the Voigt model than those from the Reuss model. Since the diffraction line of the (410) plane measured with cobalt Kα radiation by using an automated x-ray stress analyzer locates at the highest diffraction angle of 168.4, the use of this plane will allow the most accurate stress measurement. Also, the measured x-ray elastic constants for the (410) plane almost agreed with both values calculated from the Voigt and Reuss models. Therefore, the (410) plane is the most appropriate plane for x-ray stress measurement of alumina.
Numerical Resolution Enhancement of X-ray Diffraction Patterns
Authors: Ohno Katsumi , Harada Hiroshi , Yamagata Toshihiro , Yamazaki Michio
Published: March 2019

A numerical resolution-enhancement method was developed for x-ray diffraction data measured with a conventional x-ray diffractometer. This method removes the instrumental broadening due to x-ray optics, including the spectral distribution of the x-ray source such as the CuKα doublet. The advantages of this method are to separate the cluster of peaks in x-ray powder patterns into individual peaks without previous knowledge of the number of peaks, and to remove CuKα2 reflection peaks automatically.

The instrumental window function, which was approximated by a modified pseudo-Voigt function, was calculated from the measured diffraction pattern of NBS Standard Reference Materials (640B) by a non-linear least squares method. The simple diffraction patterns, including no CuKα2 peaks, were obtained from the diffraction patterns measured with the conventional x-ray diffractometer by using the window function mentioned above.

The application of the method of determination of the lattice misfit between γ and γ phases in Ni-base superalloys was also described.
Standard Database Format for the Dissemination and Storage of Diffraction Data - Task Group Progress Report on JCAMP-DX
Authors: Hamill G.P. , Jenkins R. , Schreiner W.N.
Published: March 2019

In planning for PDF-3, the International Centre for Diffraction Data's full pattern database of raw diffraction data, it is evident that a standard format for storage and exchange of diffraction data is necessary. An evaluation of the JCAMP-DX protocol by a task group* of the International Centre for Diffraction Data has resulted in a set of format cooes specific to X-ray diffraction. The proposed structure of the data is divided into four parts: the minimal component set required by the JCAMP-DX definition (name, data, owner, sample identification, data type, etc.), a minimum item set required to define the X-ray diffraction data, an open selection of requested but not required information on the sample, its preparation and the instrument, and finally the data itself in one of several specified formats. All information stored in JCAMP-DX format is in ASCII characters. Therefore, these data are printable, easily read by the user and compatible with almost any computer or media storage device. Codes defining the information are primarily in shortened, but readable, English. The task group is completing the work on this project and will be presenting its proposals to JCAMP.
Crystal Chemistry and Phase Equilibria of the BaO-R2O3-CuO Systems
Authors: Wong-Ng Winnie , Paretzkin Boris , Fuller Edwin R.
Published: March 2019

Two important factors, the progressively decreasing size of the lanthanides, which is known as the lanthanide contraction, as well as the stability of different oxidation states of these elements influence the prediction of compound formation in the Ba-R-Cu-O systems. A systematic investigation of these lanthanide systems and comparison with the Y system has revealed a correlation of the effect of the above factors, in particular the size factor, on the trend of phase formation, solid solution formation and phase compatibility diagrams of the Ba-R-Cu-O systems. For example, it has been found that the smaller the size of R3+ or the greater the mismatch betwaen Ba2+ and R3+ in the solid solution series Ba2-ZR1+lCu3O6+x, the smaller the extent of solid solution formation. This differing extent of solid solution formation influences the ternary phase relationships.
An Artificial Intelligence System for XRF Data on a Personal Computer
Authors: Wittig Erland P. , Rechsteiner Carl E.
Published: March 2019

Automation of X-ray fluorescence equipment has proliferated during the last 10 years. However, the focus has been on data collection and data massage. Data presentation has been limited to a few rudimentary formats. These formats ‘ generally involve printing the results in some arbitrary fashion, followed by manual transfer to the client.

This paper describes a system (using rudimentary artificial intelligence techniques) that automates data presentation. It handles data from 14 different methods; evaluates the data against the requirements of the method (i.e. mass balance, detection and reporting limits, and matrix interferences). Further, a data report is generated in a consistent format, including the reporting of significant figures. Additionally, an exception report is printed when the measured results are outside the applicable range of the method or violate quality assurance constraints. In such cases, alternative methods are recommended in the exception report.
SPC Analysis of Optimal Strategies for Restandardization of X-ray Fluorescence Analyses
Authors: DeGroot P. B.
Published: March 2019

Quantitative XRF analyses almost always depend on measurements of x-ray emission intensities of standards of known composition. The usual approach is a careful initial standardization with multiple standards lhat are checked for accuracy, stability, homogeneity, and internal consistency. This is followed by limited periodic restandardization or recalibration with one or two of the initial standards or a reference sample. The frequency and protocol of these periodic restandardizations tend to be rather arbitrary; for example adjustment on the basis of the average of a triplicate measurement of a standard at the beginning of the work day. There are certainly a large number of other possible restandardization strategies. They range all they way from no restandardization at all, through single or n replicate restandardization measurements before analysis of each group of M unknowns, to cumulative or moving averages, again with variable replicate size, frequency, and now averaging range. This paper examines the outcomes of some of these restandardization strategies applied to synthesized, realistic XRF analysis data which incorporate both abrupt and gradual changes in instrument response. SPC (Statistical Process Control) control charts are shown to be a very useful tool for determining optimum restandardization strategies. Optimal strategies (least scatter in calculated concentrations with fewest standards) which emerged from this study included not restandardizing at all except when indicated by an SPC chart of a reference standard intensity run concurrently with each unknown, and a moving range of 3, with standards run every 5 unknowns, coupled with SPC monitoring of the standards used for this restandardization.
Corrections for the Effect of Scattering on XRF Intensity
Authors: Fernandez J. E. , Molinari V. G. , Sumini M.
Published: March 2019

Corrections for scattering on XRF intensity have commonly used integral approaches and isotropic approximations, which give a limited knowledge on this subject. An exact theoretical expression for XRF enhancement due to coherent and incoherent scattering is presented in this paper. It has been obtained as a solution of the Boltzmann transport equation for photons. This equation describes the diffusion of photons in an infinite homogeneous target. Both the excitation and the emission beams have been assumed to be well collimated. The solution accounts for the mixed, scattering and photoelectric interactions. Complete kernels including atomic form factors have been used for both types of scattering. An appropriate kernel has been written for the photoelectric interaction. The correction is computed for several pure elements and is compared with isotropic approximations.
XRFPC: A Program and Data Base for XRF Computations
Authors: Fernandez J. E.
Published: March 2019

XRF intensity computations, for polychromatic x-ray sources and multicomponent samples, need a high number of low speed floating-point operations, making them a hard bone for any computer. The evaluations of the Intensity expression require the computation of complex attenuation coefficients. They involve also a spread quantity of atomic data for a high number of elements. And the users need to insert additional information on the experiment, like the excitation-detection geometry or the x-ray tube spectrum, interactively. Personal computers are an optimum target for this kind of application mainly due to the low cost of the computation time and the possibility to display high-resolution graphics. Moreover the increasing power of microprocessors makes it possible to attack hard computations like this on a PC.
Application of Field Mobile EDXRF Analysis to Contaminated Soil Characterization
Authors: Harding A. R. , Walsh J. P.
Published: March 2019

Effective assessment and remediation of hazardous waste sites dictates that analytical methodologies be developed which assist in the evaluation of site contamination and simultaneously make efficient use of sampling time and resources (1). Optimally, a technique would provide on-site personnel with immediate and accurate information concerning the identity and concentration of inorganic soil contaminants (2).
X-Ray Diffraction Using Synchrotron Radiation - A Catalysis Perspective
Authors: Holyńska B. , Lankosz M. , Ostachowicz J. , Ostachowicz J. , Ostachowicz J.
Published: March 2019

A modern metal-ore flotation process requires a continuous instrumental measurement of the metal content in main flotation streams. X-ray fluorescence technique is most often used for on-stream analysis of metal-ore slurries,1 Especially the radioisotope energy-dispersion XRF (REDXRF) method provides the possibility of using measuring probes immersed in the slurry at the point of analysis. The main advantage of this technique is the elimination of the necessity to transport the slurry to a control laboratory which houses the X-ray spectrometer.