bluuebunny/crossref_metadata_2025 huggingface dataset:
Development of Instrument Control Software for the SRS/300 Spectrometer on a VAX/730 Computer Running the VMS Operating System
Authors: Rokosz M. J. , Artz B. E.
Published: March 2019

It Is not practical to connect each controllable function of a WDXRF (Wavelength Dispersive X-Ray Fluorescence) spectrometer separately to the laboratory computer. Therefore, a spectrometer controller is used to interface with the hardware control actuators which operate the selectable or settable components of the spectrometer system. The basic function of a controller is to receive sequences of orders from the computer and transmit the data which has been collected. More advanced controllers, such as the one used in the Siemens SRS-300 spectrometer, may perform many additional functions. In addition to handling spectrometer-to-lab computer communication, the SMP (Siemens Microprocessor controller) is capable of monitoring the state of the instrument, resolving conflicts in external or internal requests for action, and terminating spectrometer action which can be seen as hazardous or damaging to the instrument.
Instrumentation and Applications for Total Reflection X-Ray Fluorescence Spectrometry
Authors: Tada Y. , Sako Y. , Iwamoto K. , Gonsui S. , Arai T.
Published: March 2019

X-ray fluorescence spectrometry has been used in a broad spectrum of applications. These include elemental analysis, both qualitative and quantitative, based on wavelength dispersive (WDXRF) or energy dispersive (EDXRF) methods. In these methods the detection limit of analyte elements is mainly in the one to ten ppm range in solid samples. Therefore, improvement of these limits is desirable for many useful applications. In this context it is essential to remember that the excitation efficiency for fluorescent X-rays is very low when compared with electron or proton excitation. In the case of WDXRF, the dominant factor is the low reflectivity from the analyzing crystal.
X-Ray Microprobe Studies Using Multilayer Focussing Optics
Authors: Thompson A.C. , Underwood J.H. , Wu Y. , Giauque R.D. , Rivers M.L. , Futernick R.
Published: March 2019

The availability of intense x-rays from synchrotron radiation sources permits the elemental analysis of samples in new ways. An x-ray microprobs using these sources allows the analysis of much smaller samples with greatly improved elemental sensitivity. In addition to the higher x-ray intensity obtained at synchrotron sources, the development of high efficiency x-ray reflectors using multilayer coated optical mirrors permits the achievement of spot sizes of less than 10 μm x 10 μm with enough x-ray intensity to simultaneously measure femtogram quantities of many elements in less than one minute. Since samples to be studied in an x-ray microprobe do not have to be placed in a vacuum, almost any sample can be conveniently analyzed. With an x-ray microprobe it is possible to obtain elemental distributions of elements in one, two or even three dimensions.
Quantitative Analysis of Fluorine and Oxygen by X-ray Fluorescence Spectrometry Using a Layered Structure Analyzer
Authors: Takemura Momoko , Ohmori Hirobumi
Published: March 2019

Recently, layered structure analyzers (called LSA for short) or layered synthetic microstructures (called LSM) with d spacing of several tens of Å, have been developed for use as X-ray analyzing devices in wave-length dispersive spectrometers. The lower detection limit for light elements of atomic numbers lower than 13 , such as aluminum, sodium, fluorine, oxygen, carbon and so on, has been greatly improved.

There have been several reports published regarding LSA (or LSM) applications to light element analyses.
The Viability of XRF Determination of Gold in Mineral Reconnaissance
Authors: Smith T. K. , Ingham M. N.
Published: March 2019

Commercial interest in gold is persistent and resurgent, and there is a consequent need for reappraisal of its methods of analysis. Because its modes of occurrence often manifest themselves in irregular dispersion and low concentration, special care must be taken in sampling and analysis. A sufficient amount of the initial sample must be taken to ensure adequate representation, and preconcentration is often necessary to elevate the metal content to a confidence level high enough above the detection limit for the analytical technique.
Modern Alloy Analysis and Identification with a Portable X-ray Analyzer
Authors: Piorek Stanislaw
Published: March 2019

The combination of an improved resolution, gas proportional detector with advanced microprocessor technology provides a new and unique solution to the problem of alloy analysis.

A field portable, microprocessor controlled, fully user-programmable x-ray analyser is described for fast, reliable, on-site, positive alloy identification and assay. The radio-isotope based analyser employs a modified Lueas-Tooth and Price model of intensity corrections for quantitative, multielement analysis. Applications are reviewed and include examples to show the superior performance of the instrument in such difficult eases as sulfur in carbon steels, and titanium and nickel in stainless steels.

Discussion of the unique alloy identification scheme and its underlying principles is followed by examples of applications illustrating the capabilities of the instrument in distinguishing, in 5 seconds, alloys of closely similar compositions such as stainless steels 303, 304 and 321, and 410 and 416.
Density Measurement of Thin Sputtered Carbon Films
Authors: Gorman G. L. , Chen M.-M. , Castillo G. , Perera R. C. C.
Published: March 2019

The densities of sputtered thin carbon films have been determined using a novel X-ray technique. This nondestructive method involves the measurement of the transmitivity of a characteristic soft (low energy) X-ray line through the carbon film, and using the established equation I1 = I0eμpt where I1/I0 is the transmitivity, fi the photo absorption cross section, t the independently measured thickness, the density p can be easily solved for. This paper demonstrates the feasibility of using this simple technique to measure densities of carbon films as thin as 300 Å, which is of tremendous practical interest as carbon films on this order of thickness are used extensively as abrasive and corrosive barriers (overcoats) for metallic recording media disks. The dependence of the density upon film thickness for a fixed processing condition is presented, as also its dependence (for a fixed thickness) upon different processing parameters (e.g., sputtering gas pressure and target power). The trends noted in this study indicate that the sputtering gas pressure plays the most important role, changing the film density from 2.4gm/cm3 at 1 mTorr to 1.5gm/cm3 at 30 mTorr for 1000 Å thick films.
Determination of Ultra-Thin Carbon Coating Thickness by X-ray Fluorescence Technique
Authors: White R. L. , Huang T. C.
Published: March 2019

A tcchniquc for high-precision measurement of carbon thin-film thickness using X-ray fluorescence (XRF) is described. A quadratic calibration procedure is used for carbon thin films on silicon. Measurement of carbon-film thickness in a double-layer structure of carbon and CoCrX alloy is complicated by interference effects from the underlying layer. The dependence of the relative precision in measuring thickness (σT/T) on the counting time has been derived. It shows that a precision of 2% for a 25-nm carbon coating can be obtained using a W/C crystal and counting time of 4 minutes. Intensity and resolution advantages provided by the recently developed Ni/C and V/C multilayer synthetic crystals are also described.
Effect of Plastic Deformation on Oscillations in "d" vs. sin2ψ Plots a FEM Analysis
Authors: Noyan I. C. , Nguyen L. T.
Published: March 2019

Oscillations jn "d" vs. sin2ψ plots are due to the inhomogeneous partitioning of strains within the diffracting volume. In polycrystalline specimens, such inhomogeneity can be caused by the elastic incompatibility of neighboring grains or by the inhoniogeneous partitioning of plastic deformation within the diffracting volume. There is, however, little work on the degree of inhomogeneity required to cause a given oscillation, and the relative contribution from the elastic and plastic deformation components to a given oscillation.
X-ray Measurement of Grinding Residual Stress in Alumina Ceramics
Authors: Yoshida Hiroyuki , Hanayama Yukio , Morimoto Yoshitaka , Hirose Yukio , Tanaka Keisuke
Published: March 2019

Machine parts made of ceramics are usually finished by grinding. Residual stresses as well as defects introduced by grinding will influence the fracture strength and the function of ceramics parts. Although several investigations used the X-ray diffraction method to measure the grinding residual stresses, their grinding conditions were rather limited.

In the present study, sintered alumina ceramics of 99% purity were ground with a resinoid diamond wheel (#140 grain size number) under various grinding conditions. The effects of depth of cut and stock removal on the residual stress was measured with the X-ray method.
Shadow: A System for X-ray Powder Diffraction Pattern Analysis
Authors: Howard Scott A.
Published: March 2019

The Shadow system consists of a set of programs and files, the relation of which is illustrated in Figures 1 and 2. Of the three programs in the system, Shadow and XRDPLT are used routinely. The third, INSCAL, is used in the determination of various parameters characterizing the instrument. Two files, Shadow.DFT and XRDPLT.DFT, contain default values for parameters controlling the reduction and display of data. A third file, WSGDAT, contains the instrument parameters.
Specific Data Handling Techniques and New Enhancements in a Search/Match Program
Authors: Caussin P. , Nusinovici J. , Beard D. W.
Published: March 2019

A Search/Match program using digitized X-ray powder diffraction Scans as inputs was presented in 1987 at the Denver Conference. This program has been rewritten to take full advantage of ttie newest capabilities of high end personal Computers. Software improveraents combined with the faster processing speed make it possible to search the 53,791 pattern data base in less than 16 seoonds typically (Compaq Deskpro 386/30 with 9 MB of RAM and 80387-20 numerioal processor), This can be compared to the 90 seconds one year ago. A specific program allows the user to create and, if desired, customize the searoh data base directly from the CD-ROM PDF-2, making Updates much easier. Praotiaal examples are given to illustrate the Operation of the proprietary pattern-recognition algorithm used in the search program.
Results of the JCPDS-ICDD Intensity Round Robin
Authors: Schreiner Walter N. , Jenkins Ron
Published: March 2019

Last year at this conference we submitted a preliminary report on an X-ray powder diffraction round robin sponsored by the JCPDS-ICDD. This round robin was designed primarily to study the intensities of diffraction lines found by users in routine work. At that time only a portion of the data had been analyzed, and we reported initial findings on the α-Al2O3, and Zn0 /CaCO3 samples. These included studies on counting statistics, resolution, and the effect of software on intensity precision. Since that time, all the data from the round robin has been entered into Lotus 1-2-3 (*) spread-sheets and numerous additional tests have been carried out. This paper discusses some of the more interesting findings. A complete paper on all of the tests performed is in preparation for submission to the "Methods and Practices Manual" published by the JCPDS-ICDD.
Automatic Computer Measurement of Selected Area Electron Diffraction Patterns from Asbestos Minerals
Authors: Russ J. C. , Taguchi T. , Peters P. M. , Chatfield E. , Russ J. C. , Stewart W. D.
Published: March 2019

Conventional selected area diffraction patterns as obtained in the TEM present difficulties for identification of materials such as asbestifonn minerals, although diffraction data is considered to be one of the preferred methods for making this identification. The preferred orientation of the fibers in each field of measurement, and the spotty patterns that are obtained, do not readily lend themselves to measurement of the integrated intensity values for each dspacing, and even the d-spacings may be hard to determine precisely because the true center location for the broken rings requires estimation. To overcome these problems, we have implemented an automatic method for diffraction pattern measurement. It automatically locates the center of patterns with high precision, measures the radius of each ring of spots in the pattern, and integrates the density of spots in that ring.
Microtomography Detector Design: It's Not Just Resolution
Authors: Deckman H. W. , D'Amico K. L. , Dunsmuir J. H. , Flannery B. P. , Grunert Sol M.
Published: March 2019

The design of an x-ray detector suitable for use in tomography must be optimized for the intended application. Recently, we have developed microtomography applications that require resolution of -1 micron in three spatial dimensions and -1% statistical accuracy in the reconstruction of attenuation coefficients for each cubic micron volume element in a .1 cubic mm specimen. X-ray detector design for these applications must take into account much more than just the demanding micron spatial resolution requirement. The detector must be optimized to take into account the physical properties of the specimen to be measured, the characteristics of the x-ray beam available to probe the specimen, signal to noise ratios needed in the reconstructed image and requirements of the data processing algorithm. In addition, the detector design should be sufficiently flexible to allow significant variation in the kinds of specimens that can be examined.
LM-ACT for Imaging RAM Devices in X-ray Diffraction Topographs
Authors: Beard Warren T. , Armstrong Ronald W.
Published: March 2019

Analysis of serai conductor material and associated integrated circuits (IC) is imperative for ensuring quality products. Currently, routine circuit testing is dominated by measurement of the optical and electrical material/device properties through final device performance and parametric testing.

Characterization of the crystal microstructure still is not considered a routine process test. Structural characterization usually is based on double-crystal rocking curves, x-ray topography, or a combination of these techniques.
XRF in North America
Authors: Leyden Donald E.
Published: March 2019

X-ray fluorescence, or X-ray spectrometry, is a dynamic analytical method; it undergoes constant change and improvement. Because of the early successes for the analysis of difficult samples such as metals, minerals and other solid materials, the technique was widely accepted in industrial applications. This occurred prior to the onset of large government funding to develop instrumental methods such as was provided for the development of inductively coupled plasma emission spectrometry. As a result, many of the important developments in XRF in North America have resulted from research and development by the instrumentation vendors and developments from Industrial and mission oriented government laboratories. There are exceptions, of course.
Personal Observations
Authors: Jenkins Ron
Published: March 2019

Like most instrumental methods of analysis, X-Ray Fluoresence (XRF) has progressed through the various stages of Innovation, Frustration, Application and Consolidation. My own association with the method dates back to the late 1950's which would correspond to the transition period between the innovation and frustration stages alluded to above. At that time, there were probably less than 500 XRF spectrometers in the whole world and to myself, as a young analyst with a limited background in x-ray diffraction methods, the potential power which the XRF method seemed to offer far outweighed any problems from the ‘matrix effects' that people were starting to talk about. This talk covers my own impressions of the highlights of the 20 year period of frustration and application which were to culminate with the general acceptance of the XRF method, in the mid-1970's, as a versatile and reliable analytical tool.
Personal Observations on Trends in XRF
Authors: Gilfrich John V.
Published: March 2019

Over the past many years, x-ray fluorescence analysis (XRF) has developed into a very mature field. The Plenary Session at this, the 35th Annual Denver Conference on Applications of X-Ray Analysis, deals with an evaluation of developments around the world, as viewed by experts from the three major areas, North America, Europe and the Far East. In this brief report, I would like to convey that which I consider to be the state-of-the-art at the present time, and make some prognostications, which may or may not be dignified as predictions. Many of the specifics that I mention will refer to work in which we, at the Naval Research Laboratory, have been involved. To be fair, I will also deal with some areas in which others have worked. In my mind, the field divides itself naturally into four areas: Sources, Dispersion Devices, Detectors and Data Reduction, I would like to deal with each of these in turn.
X-Ray Microanalysis for Alloy Design
Authors: Ohno Katsumi , Yamazaki Michio
Published: March 2019

The characterization of alloys is strongly requested from metallurgists as basic data for computer aided alloy design systems for duplex type alloys such as α-γ type stainless steels, γ-γ’ type Ni-base superalloys, α-β type Ti alloys, etc. The characterization falls into the following three categories.

1)

Determination of entire average composition of bulk specimens.

2)

Identification and the determination of phases including deleterious phases in the alloys.

3)

Determination of the composition of all phases in the alloys and the accuracy of the evaluation of the results obtained without standards.
High Spatial Resolution in X-Ray Fluorescence
Authors: Zahrt John D.
Published: March 2019

During the past eight years or so there has been growing interest in using a polarized x-ray source in energy dispersive x-ray fluorescence spectrometers (1,2,3,4). The effect is to annihilate the source x rays before they scatter into the detector, thus significantly increasing the signal to noise ratio.

Both characteristic or Bremsstrahlung radiation can be polarized by 90° scattering from crystals (Bragg angle = 45°) or from amorphous materials respectively. This 90° polarizing scatter event greatly reduces the incident source radiation on a sample. In an effort to regain some intensity use is made of concave surfaces to utilize a manifold of beams (5,6,7).
Layered Synthetic Microstructures in Sequential and Simultaneous X-Ray Spectrometry
Authors: van Eenbergen Ad , Volbert Bernd
Published: March 2019

For many years Layered Synthetic Microstructures (LSM's) have been used successfully as dispersive devices. The commercial variety introduced in 1984 offered significantly greater stability and diffracted intensity characteristics over Thallium Acid Phthalate (TAP) crystals. These devices offer superior sensitivity for fluorine, sodium and magnesium in all but a few applications where resolution is very critical. Subsequently, a variety of these devices have been optimised for analysis of the lower atomic number elements.

Recently, several industrial applications have required the development of LSM's with 2d spacings optimised to enable quantitative analysis of oxygen, nitrogen, carbon and even boron. In these applications, the large incremental difference in characteristic wavelength per atomic number step limits the dynamic range of elements over which the LSM can be optimised. These considerations are discussed as they relate to routine analyses of very low atomic number elements by sequential Wavelength Dispersive Spectrometry (WDS).

Newly developed fabrication techniques are used to produce curved LSM's for use with the focusing optics of simultaneous WDS. Application of these curved devices for the analysis of Mg in steel, Na in slags and F in glass will be discussed.

Finally, an application which requires the analysis of thin films on semiconductor devices will be described. In this method, characteristic K-spectra and L-spectra of low and high atomic number elements, respectively, are selected for optimum sensitivity to the surface composition.
X-Ray Fluorescence Analysis of Sulphur and Trace Elements in Coal and Oil Tar Pitches, Asphalts and Other Bituminous Compounds
Authors: Kocman Vladimir
Published: March 2019

A novel windowless sample preparation method is described which allows for X-ray fluorescence analysis of light elements (Z = 13 to 20) in coal or oil-tar pitches, asphalts and other bituminous compounds. The article also discusses blending and spiking of pitches with suitable organometallic compounds in order to prepare a range of trace-element calibration standards. The general instrumental conditions, recommended peak counting times and detection limits are also discussed.
Multielement Preconcentration of Rare Earth Elements for Their Determination at ppm-Levels in Geological Samples
Authors: Wolf Eva , Wegscheider Wolfhard , Kolmer Hans
Published: March 2019

A preconcentration procedure is reported for rare earth elements suitable for concentration levels generally found in rocks. This method is of geochemical interest because the abundance of rare earth elements gives important clues to the origin of rock formations.

The procedure is based on an anion-exchange separation step followed by a precipitation of rare-earth elements chelates onto a membrane filter. For the investigation of recovery a combined radionuclide tracer and X-ray sensitivity method was used. Detection limits in the sub-μg/g-range are reported.
Applications For X-Ray Fluorescence Scans of Single Strands of Hair: Actual and Potential
Authors: Toribara Taft Y.
Published: March 2019

Quantitative utilization of energy dispersive X-ray fluorescence spectrometry has been made for many years, and the development of instruments for this purpose have arisen from needs which can be met by the sensitivity of the technique. In a need to get information which could be obtained only by scanning single strands of hair to obtain the profile of the mercury levels along the hair, a unique X-ray fluorescence energy dispersive spectrometer was built. The prototype of this instrument was described at the Denver Conference of 1977, and published in the subsequent publication (1). The present instrument is described in a later publication (2).
The Use of Mass Absorption in Quantitative X-Ray Diffraction Analysis
Authors: Davis Briant L. , Johnson L. Ronald
Published: March 2019

The mass absorption coefficient is perhaps the most under-utilized parameter in x-ray diffraction analysis. Mass absorption measurements are often avoided in quantitative analysis by resorting to calibration curves of internal standards (e.g., Kung and Alexander, 1974, Sec. 7-2.1). However, Leroux et al. (1953) and Frevel and Roth (1982) directly utilized the mass absorption coefficient in multicomponent analysis, and suggested a "substrate diffraction" procedure for directly measuring the sample mass absorption coefficient. The reference intensity procedure of quantitative multicomponent analysis originally formulated by Frank Chung (1974) requires no explicit use of the mass absorption coefficient because all reference intensity ratios are determined relative to an "external" standard, generally corundum (Al2O3).
On-Stream X-Ray Diffraction Analyzer for Mineral Concentrators
Authors: Sipilä Heikki , Koskinen Jouko
Published: March 2019

On-stream X-ray fluorescence analyzers have been available for about 20 years. They have been used with great success and they have made an effective process control possible in many concentrators. They have, however, one severe drawback. Normally the sample that ought to be measured is in slurry form and it would be difficult and expensive to prepare it into more conventional form used in ordinary laboratory practice. The main constituent of slurry is water and normally some kind of plastic film is needed to keep slurry apart from the measuring system at least when the slurry system is malfunctioning. Already these two things are sufficient to set a limit to the lightest element that can be measured with reasonable accuracy and precision. This means that minerals that contain only such low atomic number elements as e.g. Mg, Al, Si and P remain out of reach. Difficulties arise also in cases where the interesting element is not only in the solid material but also in the solution part of the slurry. In great many cases the interesting element occurs in several minerals at the same time which causes certain problems with the accuracy. Fortunately this problem does not set such a basic limitation as a too low Z does unless only one of these minerals is of interest, which may make the whole method worthless.
Lattice Parameter Determination Using Synchrotron Powder Data
Authors: Parrish W. , Hart M. , Huang T. C , Bellotto M.
Published: March 2019

A method for using synchrotron-radiation parallel-beam X-ray diffractometry for precision measurement of scattering angles and lattice parameters is described. The important advantages of the method are the high P/B made possible by wavelength selection and high source intensity, the symmetrical profiles and the absence of most systematic errors making it unnecessary to use standards. Profile fitting with a pseudo-Voigt function is used to determine 2θ to 0.0001º. The zero-angle correction and lattice parameter were determined from least-squares refinement and the average accuracy of observed-calculated 2θs was 0.0020°. Average values of ∆d/d = ∆a/a directly calculated from the individual hkl measurements ranged from 2x 10-5 to 5.7 x 10-5. The precision estimated from the standard deviation of the mean is in the 10-6 range and 1 ppm precision was obtained for Si. The determination of the exact wavelength selected remains to be solved, but ratios of lattice spacings to standards such as NBS SRM 640a can be determined.
Synchrotron Radiation Applied to Computer Indexing
Authors: Smith Gordon S. , Johnson Quintin C. , Cox David E. , Snyder Robert L. , Smith Deane K. , Zalkin Allan
Published: March 2019

Synchrotron radiation was used to obtain a high-resolution powder diffraction pattern of the high-density form of BeH2, a material whose unit-cell dimensions have not previously been determined. The observed d-spacing values were presented to three different computer indexing programs. All three programs returned as best solution a body-centered orthorhombic unit cell with a = 9.082, b = 4.160, c = 7.707 Å and V = 292 Å3. Interpretation of the three-dimensional Patterson led to 12 BeH2 molecules per unit cell; thus, the theoretical density is 0.755 g/cm3. The molecular structure is based on a network of corner-sharing BeH4 tetrahedra rather than flat, infinite chains with hydrogen bridges previously assumed.
Design of a Real-Time Two-Dimensional Residual Stress Analyzer
Authors: Borgonovi G. M.
Published: March 2019

Measurements of residual stress by X-ray diffraction are usually carried out with diffractometers or with one-dimensional position sensitive detectors. The stress is determined from the displacement of the peak that results from intersecting a diffraction cone at high angle with the line scanned by the detector. If a two-dimensional flat detector is used, the intersection of the diffraction cone with the detector plane is a ring, or section of a ring, which is also slightly displaced by the stress. The suggestion has been made use a two-dimensional detector to determine the surface state of stress.
Controlling Laboratoey Conditions: Preventing the Problem, The Health Physicist's Viewpoint
Authors: de Castro Ted
Published: March 2019

After having heard about the magnitude of the problem of safety in the use of analytical x-ray equipment and then learned of the consequences of exposure to these x-rays, it is hard not to be convinced that a problem exists. Also being aware of the degree of responsibility in the event of an accident, it is clear that steps must be taken to prevent such occurrences. Controlling laboratory conditions is the key to prevention and, therefore, the solution to the problem.

Controls may be imposed administratively or with hardware. Administrative controls are easy and inexpensive to impose. Enforcement, however, is time consuming and difficult, since such controls need only be ignored to be compromised. Hardware controls are more positive and difficult to ignore. The bypassing of hardware controls is usually invasive on the equipment and leaves evidence.

When imposing controls it is necessary not to lose sight of the operational needs which brought the x-ray unit into your organization to begin with. Analytical x-ray machines are safest during massive power failures—but not very useful. Administrative and hardware controls which hobble the use of the equipment will be violated. Cooperation between the health physicist and the x-ray users can bring together the requirements of safety and Utility to create controls which will work.
Microstructoral and Chemical Analysis Using Electron Beams: The Analytical Electron Microscope
Authors: Romig A. D.
Published: March 2019

This plenary paper is intended to be an introduction to the capabilities and limitations of analytical electron microscopy (AEM). The description to be given assumes no prior knowledge of AEM or any other electron microscopy, scanning or transmission. However, a basic understanding of x-ray generation and detection will be assumed.
X-ray Imaging of Surface and Internal Structure
Authors: Russ John C.
Published: March 2019

The most familiar result from X-ray analysis is a spectrum (on a chart recording or on film), or perhaps a short list of values (concentrations, d-spacings, etc.) taken from such a spectrum. X-ray pictures are usually associated in our minds with the hospital emergency room or the dentist's office. But images formed by X-rays are also an important tool to study materials' structures. Both conventional and unconventional uses of X-rays to study structural and compositional inhomogeneities find widespread application to materials. Applications include characterization of surface topography and composition variation, as well as internal structure. The methods make use of all types of X-ray interaction with materials, including Bragg diffraction and the fluorescence of characteristic X-rays, as well as simple X-ray attenuation due to absorption and scattering.
X-Ray Microscopy Using Collimated and Focussed Synchrotron Radiation*
Authors: Jones K. W. , Kwiatek W. M. , Gordon B. M. , Hanson A. L. , Pounds J. G. , Rivers M. L. , Sutton S. R. , Thompson A. C. , Underwood J. B. , Giauque R. D. , Wu Y.
Published: March 2019

X-ray microscopy is a field that has developed rapidly in recent years. Two different approaches have been used. Zone plates have been employed to produce focussed beams with sizes as low as 0.07 pm for x-ray energies below 1 keV. Images of biological materials and elemental maps for major and minor low Z have been produced using above and below absorption edge differences. At higher energies collimators and focussing mirrors have been used to make small diameter beams for excitation of characteristic K— or L-x rays of all elements in the periodic
table.
Imaging With Spectroscopic Data
Authors: P. Engler  , Barbour R. L. , Gibson J. H. , Hazle M. S. , Cameron D. G. , Duff R. H.
Published: March 2019

Spectroscopic data from a var iety of analyt ical techniques such as x-ray diffraction (XRD), infrared (IR) and Raman spectroscopies, secondary ion mass spectrometry (SIMS) and energy dispersive X-ray analysis (EDX) can be obtained from small areas of samples (< 1 mm2) through the use of microscope sampling accessories. If provisions are made to scan or translate the sample, then a spectrum that is characteristic of each region of interest can be obtained. Alternatively, selective area detectors eliminate the requirement for scanning the sample. Extract ion of information about a specific energy band from each spectrum allows elucidat ion of the spatial distribution of the feature giving rise to that band. For example, the distribution of a compound could be imaged by extracting the intensity of an IR band or XRD peak due to that compound. Peak posit ion and peak width are other parameters that can be extracted as a function of posit ion. Similarly, elemental distributions could be obtained using SIMS and EDX.
An Automated X-Ray MicroFluorescence Materials Analysis System
Authors: Wherry David C. , Cross Brian J. , Briggs Thomas H.
Published: March 2019

Recently there has been a growing interest in the field of X-Ray MicroFluorescence (XRMF) for analyzing small areas (with sizes greater than about 10 microns diameter). Several recent papers have described prototype systems for this kind of analysis, with particular emphasis on the elemental imaging applications. However, the technique of small-area XRF analysis is not new. For example, Bertin gives an excellent review of much of the earlier work (up to the late 1960s), which used a variety of focusing (with curved crystals) or collimation techniques. Several wavelength dispersive spectrometer systems were modified for small-spot analysis. One of the earliest spectrometers was the X-ray Milliprobe developed by Adler and Axelrod, which employed curved crystals.
Pre-Cracking Technique and its Application to X-Ray Fractography of Alumina Ceramics
Authors: Mishima Tadao , Yoshida Hiroyuki , Hirose Yukio , Tanaka Keisuke
Published: March 2019

X–ray fractography is a new method utilizing the X–ray diffraction technique to observe the fracture surface for the analysis of the micromechanisms and mechanics of fracture.

In the present study, X–ray fractography was applied to brittle fracture of alumina ceramics. The first part deals with our new method of pre–cracking of ceramics. Pre–cracking was introduced to a singleedge notched specimen by longitudinal compression. Then the fracture toughness tests were conducted with pre–cracked specimens as well as notched ones. The effect of the notch radius on the fracture–toughness value was determined. The second part describes the result of X–ray fractography.
X-Ray Fractography of Stress Corrosion Cracking in Aisi 4340 Steel Under Controlled Electrode potential
Authors: Tsuda Masaaki , Hirose Yukio , Yajima Zenjiro , Tanaka Keisuke
Published: March 2019

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

In the present paper, the distribution of residual stress beneath the fracture surface made by stress corrosion cracking was measured by the X-ray diffraction method. Stress corrosion cracking tests were conducted by using compact tension specimens of 200°C tempered AISI steel in 3.5% NaCl solution environment under various electrode potentials. The effect of electrode potential on the growth kinetics of stress corrosion cracking is discussed on the basis of residual stress distribution.
Preliminary Results From a Powder Diffraction Data Intensity Round-Robin
Authors: Schreiner Walter N. , Jenkins Ron
Published: March 2019

For many years the International Centre for Diffraction Data has sponsored round robins covering various aspects of X-ray powder Diffraction with the objective of illuminating and understanding current practices and problems associated with, the analysis of diffraction data. As computer analysis of diffraction data becomes ever more sophisticated, analytic capabilities are extended and the performance, not only of the instrumentation must be checked, but also that of the software which converts the measured data into useful results. In recent years, therefore, we have personally participated in a cell parameter round-robin, a d-spacing round-robin, a peak hunting round-robin, and, most recently, the present intensity round-robin and a line profile round-robin. Still others are in progress or being planned.
Defining and Deriving Theoretical Influence Coefficients in XHF Spectrometry
Authors: Lachance Gerald R.
Published: March 2019

The concepts underlying the definition and calculation of fundamental influence coefficients and their role in the computation of derived coefficients in alpha-type algorithms are examined. The fundamental-parameter method initiated and continues to provide the basis for the steady progress in giving influence coefficients a sound theoretical status. New definitions of fundamental influence coefficients as the prorating of monochromatic coefficients on the basis of the intensities of each elementary contributions as a function of the total fluorescence intensity and of the intensity of the pure analyte are compared to the presently used approach of defining coefficients as a function of total absorption only.
Multi-Capillary and Conic Optical Elements for Parallel Beam Production
Authors: Dozier C. M. , Newman D. A. , Bell M. I. , Xiao Qi-Fan , Espy S. L.
Published: March 2019

Large area, parallel beams of x-rays are potentially useful in many diffraction, imaging and other x-ray analysis applications. Diffraction, in typical experiments, uses only a small portion of the incident beam that is within a limited “rocking curve” of the crystal capable of diffracting, although the whole crystal may be illuminated by the incident beam. Signal intensity can be increased if the ”whole” crystal can be made to diffract simultaneously. Similarly for imaging, improved results also are possible if divergent beams are replaced with nearly parallel ones. Production of parallel beams of large areal extent has not been simple. Often this meant that the source had to be placed at great distances from the sample, reducing the incident intensity. Sometimes, asymmetric cuts of crystals can be used to increase beam cross-sectional areas.

Production of parallel beams of large area! extent has not been simple. Often this meant that the source had to be placed at great distances from the sample, reducing the incident intensity. Sometimes, asymmetric cuts of crystals can be used to increase beam cross-sectional areas.
Generation of 1-10 Ps Hard X-Rav Pulses for Time Resolved X-Ray Diffraction
Authors: Chen P. , Tomov I.V. , Rentzepis P. M.
Published: March 2019

We present a further improvement of our experimental system for the generation of hard x-ray pulses in the range 1-10 ps, A laser system based on a cw mode locked Nd:YLF laser is utilized for the emission of deep UV pulses at 193 nm with duration 1.5 ps and repetition rate of 300 Hz, This UV radiation is used to pump an x-ray diode which produces CuKa x-ray pulses with a duration shorter than 10 ps at 300 Hz.
Residual Stress of Aluminum Thin Films Sputtered on Silicon Wafers Measured by X-Ray Diffraction
Authors: Tanaka Keisuke , Ishihara Keisaku , Akiniwa Yoshiaki
Published: March 2019

A new method of the X-ray stress measurement was proposed for measuring the residual stress in Al thin films having the [111] fiber texture with the fiber axis perpendicular to the film surface. The strain was measured from Al 222 and 311 diffractions obtained by Cr-Kα radiation. The values of in-plane residual stresses σ11, σ22 and σ12, and out-of-plane normal residual stress, σ33 were determined from the measured strains by using the fundamental formulae derived on the basis of Reuss and Voigt models. The measured residual stress in the thin films was nearly equi-biaxial tension. The magnitude of the tensile residual stress decreased with increasing film thickness.
Visualization of Errors in Residual Stresses
Authors: Hendricks R. W. , Allison H. D.
Published: March 2019

Although it is widely known that small errors in d0 produce large errors in calculated components of the triaxial stress tensor, the magnitude and sign of errors in the elastic constants and do has not, thus tar, been visualized. In this study, the combined and isolated effects of errors on the resultant stress calculation is shown via three-dimensional, topographical, and onedimensional graphics. It has been found that stress is most sensitive to errors in d0, and least sensitive to S1. In most cases, errors lead to calculated stresses that differ from the true values by more than 20%, and in the worst cases change the magnitude by more than 200% and may even change the sign.
Residual Stress in Thin Films of Rf-Sputtered Aluminum by X-ray Multtaxial Stress Measurement
Authors: Ejiri Shoukhi , Lin Zheng , Sasaki Tosihiko , Hirose Yukio
Published: March 2019

Residual stress in thin films of RF-sputtered aluminum coated on substrate of glass was measured by X-ray multiaxial stress measurement. The films were manufactured under the various conditions such as temperature of substrate ranged from 473K to 573K, and pressure of argon gas range from 0.0093Pato 13.3Pa respectively. These results brought comprehension that residual stress existed in tri-axial and that was influenced by temperature of substrate and pressure of argon gas. Residual stresses were unstable in range of less than 1.33Pa of pressure of argon gas.
Accurate Measurement of Lattice Misfit Between γ And γ' Phases in Nickel-Base Superalloys at High Temperatures
Authors: Yokokawa Tadaharu , Ohno Katsumi , Murakami Hideyuki , Kobayashi Toshiharu , Yamagata Toshihiro , Harada Hiroshi
Published: March 2019

Accurate measurement of the lattice misfit between the γ and γ phases in Ni-base single crystal superalloys at high temperatures has successfully been achieved using a parallel beam mode X-ray diffractometer with a high temperature specimen stage. The superalloys have γ' precipitates, an ordered FCC structure based on Ni3Al, in a γ-matrix having a disordered FCC structure (LI2). The parallel beam mode, the optics of which is made from a Ge (111) channel cut crystal, generates a superior monochromatic and parallel CuKα1 beam, which makes it possible to resolve a cluster peak in Ni-base superalloys into individual γ and γ ‘ peaks. This peak separation was almost impossible using the CuKα1+2 doublet beam from the standard type para-focusing mode, due to the very small difference in lattice parameters between the two phases.
Modeling and Optimization Algorithm to Analyse Xrpd Data Via Modulation and Pseudo-Voigt Functions
Authors: Berti Giovanni
Published: March 2019

The composition of the sample related-effects with those from the instrument, has been carried out by convolution of involved terms. The sample-related effects have been modelled via the modulation function accounting for packed parallel planes, named here “layers”, and other structure-related parameters. The instrumental parameters have been determined using DISVAR93, a softawre package allowing the diffraction profiles to be represented in the more convenient shape of a pseudo-Voigt function. A constrained optimization process is the basis for determining these instrumental parameters; their calibration is typically carried out by adopting an external standard sample. The comparison of the modeled intensity distribution with the experimental one is performed via minimization of χ2 where the convolutor and minimizator are embedded engines of the algorithm.
Analysis of X-Ray Diffraction Scans of Poorly Crystallized Semrcrystallkve Polymers
Authors: Sanjeeva Murthy N.
Published: March 2019

X-ray diffraction (XRD) scans of many semicrystalline polymers, in which noncrystalline (amorphous) phases with varying degrees of order coexist with more than one crystalline phases, are usually not well resolved. Resolution of such data can be enhanced by deconvolving the effect of size broadening using maximum entropy methods. The use of resolution-enhanced XRD scans for studying the order in the noncrystalline (amorphous) domains and for studying small differences in the crystalline regions in poorly crystallized polymers is illustrated with examples from polyamides and polyesters. Crystallinity in poorly crystallized polymers is determined using an amorphous template obtained by analyzing highly crystalline polymers. The degree of order in the noncrystalline regions is evaluated from the changes in the shape and the position of the amorphous scattering. It is suggested that these procedures can be a part of the documentation of laboratory procedures required for ISO (International Organization for Standards) certification.
Composition of Coal Dusts and Their Cytotoxicity on Alveolar Macrophages
Authors: Lee C. Y. , Lee S.L , Sheehan C. E. , Wang Yinghua
Published: March 2019

Coal mine dust is produced from complex materials which consist of organic sedimentary phases, inorganic minerals, and trace elements. The dust varies in its chemical compositions and is capable of causing lung injury when inhaled. The purpose of this study was to perform scanning electron microscopy combined with energy dispersive spectrometry, wavelength dispersive spectrometry and X-ray diffraction analyses of three coal dusts and examine their effects on rat lung alveolar macrophages (AM) in cell culture. The coal dusts were obtained from coal surfaces of anthracite, meager and fat coal mines. AM were harvested by bronchoalveolar lavage from adult male Wistar rats and were cultured in Eagle's medium at 37°C.
Rietveld Refinement of YBa2Cu3-xNixOy Prepared by Quenching and Oxygen Gettering
Authors: Rodriguez Mark A. , Eatough Michael O. , Licci Francesca
Published: March 2019

We have refined the structures for YBa2Cu2.94Nio.O6Oy (2% Ni) and YBa2Cu2.8ONio.20Oy (6.67% Ni) at y ∼ 6.95 and y ∼ 6.5 contents. Oxygen was reduced by two independent methods: quenching from 690 °C and oxygen gettering at 450 OC, Cu-O bond lengths were calculated based on Rietveld structure refinements for the various samples; they indicate the likely occupancy of Ni in the plane (Cu2) site of the 123 superconductor.
Determination of Thickness of Multiple Layer Thin Films by X-ray Diffraction Technique
Authors: Chaudhuri J. , Hashmi F.
Published: March 2019

In this study, the equations based on x-ray diffraction theory were developed to determine the thickness of multiple layer thin films. The kinematical expression of the integrated reflected intensity from the substrate and films was corrected for the primary and secondary extinction effects assuming a mosaic crystal model. As an example of the application of the method, thicknesses of a double heterostructure system, namely AlAs/AIGaAs/GaAs, were determined. Good agreement was obtained between the results from the x-ray measurement and scanning electron microscopy data demonstrating high precision of this technique.
Energy Dispersive Grazing Incidence X-ray Diffraction Study on Organic Thin Films EpitaxiaHy Grown on Crystalline Substrate
Authors: Ishida Kenji , Kita Akinori , Hayashi Kouichi , Horiuchi Toshihisa , Kal Shoichi , Matsushige Kazumi
Published: March 2019

Thin film technology is rapidly evolving today, and the characterization of the thin film and its surface have become very important issue not only from scientific but also technological viewpoints. Although x-ray diffraction measurements have been used as suitable evaluation methods in crystallography studies, its application to the structural evaluation of the thin films, especially organic one having the low electron densities, is not easy due to the small amounts of scattering volume and the high obstructive scattering noise from the substrate. However, the x-ray diffraction measurements under grazing incidence will aid not only in overcoming the such problems but also in analyzing in-plane structure of the thin films. Therefore, so-called grazing incidence x-ray diffraction (GIXD) has been recognized as one of the most powerful tools for the surface and thin film studies.