A new titanate K2ZnTiO4 has been synthesized by solid-state reaction. This compound is isostructural with K2ZnGeO4, space group Pca21, Z=8. Unit-cell parameters were determined: a=11.3352(6) Å, b=5.6352(5) Å, c=16.0125(13) Å, and V=1022.8(3) Å3. Powder diffraction data are reported.

The Debye-Scherrer technique and filtered Cu Kα, radiation were used to obtain powder data for reflections to an angle of 2θ = 155°; a vertical scanning diffractometer was used to obtain intensity data to an angle of 2θ = 99°. The space group is with Z = 4. The lattice parameters of the tetragonal unit cell were measured to be a = 6.189 (1) Å and c = 12.391 (1) Å with c/a = 2.002 The unit cell volume was calculated as U = 474.6 (2) Å3 and the X-ray density as Dx = 6.07 ± 0.003 gm cm−3. By comparing measured and theoretical intensity values, the sublattice distortion parameter x was estimated to be x = 0.227 (12).

The successful synthesis of ZnS hollow microspheres by a solvothermal route is reported. The synthesis was achieved by a proper selection of a sulfur source, i.e., Na2S2O3⋅5H2O or (NH2)2CS, to react with Zn(CH3COO)2⋅2H2O in mixed solvents of ethylene glycol and deionized water. The ZnS products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and photoluminescence spectroscopy. XRD identified the ZnS products to have either zinc blende or wurtzite structure. SEM images revealed hollow ZnS microspheres with 1 to 2 μm diameters and 100 to 200 nm shell thicknesses. TEM images confirmed that the hollow ZnS microspheres were assembled by ZnS crystalline nanocrystallites. The room-temperature photoluminescence spectrum of the zinc blende hollow microspheres showed a strong green emission at 514 nm and weak emission at 379 nm.

An ordered oxygen-deficient tetragonal perovskite compound La1.67Sr0.33Cu205 has been synthesized by solid state reaction. X-ray powder diffraction was used to characterize the material. Unit cell parameters least-squares refined from non-overlapping diffraction peaks are a = 10.8696(9)Å, c = 3.8612(6)Å and V = 456.2(1)Å3. X-ray powder data have been obtained for the experimentally observed peak positions corrected for systematic errors, the relative intensities, values of dexp and the Miller indices of both resolved and overlapping reflections. The experimental diffraction pattern was compared to computer simulated patterns calculated from the neutron crystal structure parameters and the non-oxygen-deficient LaCuO3 compound. The figure of merit is F30 = 33.8 (0.018, 48).

Accurate, digitized, spectral distribution data are given for CuKα radiation, comprising the profiles of CuKα1, CuKα2 and CuKα3,4. Three consistent analytical procedures are detailed for locating the peak of an X-ray emission line and are found to be superior to the conventional graphical centerline method.

The performance of a tapered, monocapillary optic was compared to double-pinhole optics by measuring the intensity and widths of powder diffraction peaks generated using Cr Kα and Cu Kα X-rays (46 kV, 46 mA). A microdiffractometer and curved image-plate system was used to collect diffraction patterns displayed by an alumina intensity standard. A monocapillary optic with a 20 μm beam width (measured at half the maximum intensity, FWHM) was compared to collimating pinhole optics with two apertures: one with 30 μm diameter pinholes and another with 50 μm pinholes. The average, integrated intensity of the diffraction peaks in the patterns collected using the 20 μm monocapillary optic was 6 to 7 times greater than the average diffraction intensity obtained with the 50 μm pinhole collimator and 25 times greater than the intensity obtained with the 30 μm collimator. The average increase in the FWHM of the diffraction peaks in the patterns obtained with the monocapillary optic was ∼2 times greater than the pinhole collimators.

Guided by the dispersion, surface of dynamical theory, we easily obtain evidence of the fact that in asymmetrical surface reflections (Bragg case) of X-rays at a perfect crystal, the angular widths of the incident and reflected beams are different from the same widths in the symmetrical Bragg case. The beam with the smaller glancing angle to the surface is angularly expanded, the other one, contracted (though in cross section, the former is contracted and the latter, expanded). Consequently, if the incident glancing angle is the smaller one (striping incidence, Vreftection), the angular width of the reflected beam is smaller than in the symmetric case (S-reflection), and that of the reflected section out of the primary beam is greater, and vice versa (striping emergence, if-reflection). At striping incidence, a contraction occurs, whereas at striping emergence, expansion of the angular reflection range occurs. These facts offer a number of possibilities for applying asymmetrical reflections to the well-known technique of the two crystal diffractometer—the author proposes the term “diffractometer” instead of the widely used “spectrometer”—in the (nv, −n)-position. These possibilities extend the efficiency of the double diffractometer with multiple effects, and some of them are given below: (1) Realization of rocking curves of extremely small angular width in the (nv, −nR)-position, and consequently increased sensibility of that width to lattice distortions, (2) Use of the extremely small angular width (or more strictly, the sharp θ-λ-coordination) of the beam emerging from a first crystal. This is in V-reflection for scanning the intrinsic diffraction pattern of the second crystal used in S- or V-reflection [(nv, −ns) or (nv, −nv) -position], (3) Increased steepness of the sides of the rocking curves using (nv, −nR) or (nv, −ns)-positions which allows double diffractometric topography (Bond-Andrus, Bonse-Kappler) of increased angular resolving power. (4) Repeated ^-reflections (eventually within a single crystal provided with a suitable groove) leading to further angular contraction of the resulting reflected beam and therefore further increased angular resolving power [(nv, −nv, nR, −nR)- and (nv, −nv, +nS)-positions]. Here the tails of the rocking curve are also suppressed by multiple reflection (Bonse-Hart).

Tissue's two major components: lipid and protein, are of a primary importance, related as they are to the normal life states. Assay of protein and lipid (fat and lean) in vivo is of certain criticality in human disease states, such as wasting, edema, obesity and other dyscrasias involving body mass and fat-lean balance. Since the elemental composition of lipid and protein molecules differ in a significant and regular fashion, their mass absorption coefficients differ when radiation in the x-ray and lower energy gamma ray region is used. Two monochromatic photons, one in the 20 to 30 keV region, another in the 60 to 100 keV region, can be shown to exhibit an absorption ratio in a two component system of fat and lean which provides for a determination of the component mass ratios. Photons from x-ray machines and isotopic x- and gamma ray sources have been proposed for this. The radionuclide offers qualities of stability, small size and weight, portability, zero power consumption and, generally, a certain economy. The electron capture decay of 109Cd provides a gamma ray at 88 kilovolts and a daughter (Ag) Kα doublet at 22 keV. This fortuitous energy combination is advantageous in this differential absorptiometry. The 109Cd source provides for a stable geometry and calls for the simultaneous measurement of both photons by non-dispersive x-ray spectroscopic techniques. Ten mCi of 109Cd was incorporated into a sealed source, filtered for the silver Kβ1 x-ray (at 24. 942 keV) with 0. 1 mm palladium and collimated with a grazing aperture arrangement. Fat-lean tissue simulating standard samples three cm to ten cm in length and of various component ratios were studied. Component weight percent was determined using a function of the transmitted radiation. Determinations on water (the lean simulator) and polyethylene (the fat Simulator) as well as other materials produced absorption ratios concurring favorably with the known make-up of the Simulators.

In vitro dual beam analysis of muscle tissue samples showed a high degree of correlation with the results of ether lipid extractions. Using lipid extraction values as the standard, the x-ray absorptiometric technique produced percentage lipid levels averaging within 0. 5% of the extractions.

In vivo measurements of fat content of the triceps muscle area were compared with skinfold thickness measurements of the same area. Coefficient of correlation was 0. 88.

A new group of ternary carbide phases which are formed by combination of an element of the scandium group (which is taken to include the rare-earth elements) with aluminum and carbon has been found. These phases are related to the series of T3BCx compounds discovered by Stadelmaier (T for a transition element and B for a B subgroup element). Atomic size effects are discussed which show that T3BCx phases behave in a manner similar to many ordered binary phases of AB3 stoichiometry. There is a readjustment in size of the various metallic components which results in effective radii compatible with cubic close packing. An anomaly which appears when the observed lattice parameters of T3BCx are related to the Goldschmidt radii of the component atoms is discussed in this light. Measurements of the intensities of X-ray diffraction peaks are used to show that the carbon atom in these phases occupies the octahedral hole in the center of a Cu3Au-type unit cell. This position is maintained in alloys which contain varying amounts of carbon.

This method for precisely determining the background level of broadened x-ray profiles assumes that the background under the peak can be approximated by a straight line, and the decay in the tails several profile widths from the peak follows a Cauchy-like law. It uses a plot of I(s)s2 vs. s2 where I(s) is the intensity and the scattering vector s = 2cosθo sin(θ-θo)/ƛ where θo is the centroid, θ the Bragg angle and X the x-ray wavelength. The true background is determined by the slope of the linear portion of the plot and its extension to s2=0 gives the rate of decay of the tails. Results on synthesized and experimental profiles show that the method is useful for Warran-Averbach analysis, because it avoids spurious oscillations and the “hook” effect in the plot of the corrected Fourier coefficients, and makes it possible to correct for overlapping tails of adjacent reflections.

Without modifying the General Electric XRD-5 diffractometer accurate lattice parameters of cubic structures may be determined quite simply and precisely. The method is applicable to both solid and powder samples and gives a precision of at least ±0.00025 A. The most important step in the analysis is the alignment of the diffractometer. The specimen must be in the exact center for precise work. However, after the initial alignment, daily alignment is a routine matter. This technique for lattice-parameter determination will also be useful for determining thermal coefficients of expansion and residual-stress measurements.

X-ray diffraction can be used to nondestructively measure residual stress of polycrystalline materials. In x-ray stress measurement, it is important to determine a stress constant experimentally in order to measure the stress accurately. However, every value measured by x-ray diffraction has statistical errors arising from counting statistics. The equations for calculating the standard deviations of the stress constant and elastic constants measured by x-rays are derived analytically in order to ascertain the reproducibility of the measured values. These standard deviations represent the size of the variability caused by counting statistics, and can be calculated from a single set of measurements by using these equations. These equations can apply Lu any meuhud for x-ray stress ifiesuremenL. The variances of the x-ray stress and elastic constants are expressed in terms of the linear combinations of the variances of the peak position. The confidence limits of these constants of a quenched and tempered steel specimen were determined by the Gaussian curve method. The 95% confidence limits of the stress constant were -314 ± 25 MFa/deg.

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.

A method to measure low level iodine concentrations by means of a Total Reflectance X-Ray Spectrometer (TXRF) was presented at the 1986 and 1988 Denver X-Ray Conferences (Ref. 1 and 2.). The optimum set-up of the spectrometer for this purpose was obtained by using a Cu-anode tube. The collimated beam was two times totally reflected: first on the mirror and then on the synsil sample substrate. By these means the undesired high energy bremsstrahlung was almost eliminated. This operational mode is very convenient for iodine measurement by L-lines. The detection limit of iodine was as low as 100 pg.

For simultaneous measurement of several elements (I2<Z<83) it was necessary to change the set-up of the spectrometer.

Metal matrix composites develop residual strains after consolidation due to the thermal expansion mismatch between the reinforcement fiber and the matrix. X-ray and neutron diffraction measured values for the longitudinal residual stress in the matrix of three titanium MMCs are reported. For thick composites (> 6 plies) the surface stress measured by x-ray diffraction matches that determined by neutron diffraction and therefore represents the stress in the bulk region consisting of the fibers and matrix. For thin sheet composites, the surface values are lower than in the interior and increase as the outer rows of fibers are approached. While a rationale for this behavior has yet to be developed, accounting for composite thickness is important when using x-ray measured values to validate analytic and finite element calculations of the residual stress state.

The yttrium-based metal–organic framework, Y(btc) (btc = 1,3,5-benzenetricarboxylate), shows moderate uptake of methane (0.623 mmol g−1) and molecular oxygen (0.183 mmol g−1) at 1 bar and 308 K. Neutron powder-diffraction data for the guest-free, CD4-, and O2-loaded framework reveal multiple adsorption sites for each gas. Both molecular guests exhibit interactions with the host framework characterised by distances between the framework and guest atoms that range from 2.83 to 4.81 Å, with these distances identifying interaction most commonly between the guest molecule and the carboxylate functional groups of the benzenetricarboxylate bridging ligand of the host.

An alternative neutron diffractometer performance, which documents the feasibility of using a high-resolution three-axis neutron diffractometer for elastic and plastic deformation studies of bulk metallic polycrystalline samples, is presented. Contrary to the conventional double-axis setting, the suggested alternative consists of an unconventional three-axis set-up employing a bent perfect crystal monochromator and an analyzer with a polycrystalline sample in between. Though the alternative is, for measurements, much more time-consuming, its sensitivity to the change of the diffraction angle of the sample is, however, substantially higher and permits also plastic deformation studies on the basis of analysis of the diffraction line profiles. Moreover, much larger widths (up to 10 mm) of the irradiated gauge volumes can be investigated when just slightly affecting the angular resolution properties of the experimental setting.

High-temperature X-ray powder photography has proved of great value in many directions in the metallurgical field. Some of the successes achieved and problems encountered by the author and other investigators using an established-type camera (British Unicam) for temperatures up to 1400°C will be discussed. This will be by way of specific case histories, chosen both for their own scientific interest and to illustrate the techniques employed. The applications concern phase transformations and the measurement of coefficients of thermal expansion in iron and steels, as well as in some nonferrous metals and inorganic compounds.

A quantitative x-ray fluorescence (XRF) analytical system has been developed with the emphasis on small sample size. The system employs a two kilowatt tungsten anode x-ray tube, and an 80 mm2 lithium drifted silicon x-ray detector arranged in a compact geometry. Operation at 55 kV and 20 m A give a sensitivity of 153 counts/min/ng at Z=42 (molybdenum). A computer controlled target changer makes it capable of analyzing 32 targets automatically. The sample target is rotated during irradiation, so that the average sample position is defined to 0.2 mm. Several sets of 5 to 9 calibration targets have exhibited a standard deviation of less than 1%.

Uniaxial Plastic Deformation (UPD) has been known to produce anomalies in residual stress measurements based on x-ray diffraction techniques. This study was undertaken to determine the magnitude of the effects, if any, on residual stress calculations from various materials subjected to UPD. An x-ray diffraction study using the two-exposure method ( ψ = 0° and ψ = U5°) was made on several iron, aluminum, and titanium alloys (AISI 4340, 4330M, 4130; 2024-13, 7075-T611; Ti-6Al-4V) before and after these alloys were deformed plastically by bending on a U-bend test fixture. The x-ray peak shifts, Δ2θ0-ψ, were recorded and the x-ray stress factors, Ki, calculated by three different methods. The results indicate that UPD of the calibration specimens will increase or decrease Ki depending on the alloy. These results are discussed together with observations on the additivity of residual and applied stresses, and the per cent differences in the stress measurements based on stress factors calculated by three different methods.