Without experimental or predicted literature crystal structures for succinonitrile at low temperature, structure solution was attempted from powder diffraction data taken at 173 and 90 K from a solid sample. Its room-temperature plastic-crystal state makes production of a sample with good particle statistics and random orientation almost impossible. Combining constrained models, simulated annealing, and careful application of second-order spherical harmonic corrections nevertheless produced viable-looking structures at 90 and 173 K, yielding two distinct structure models with the same projection down c. VASP optimization of atom coordinates in the experimental cell agreed well with the 90 K model but poorly with the model derived from the 173 K data. The refined 90 K structure changed little on optimization and fitted all datasets from 85 to 225 K. Plots of cell data, torsion angles, and isotropic displacement parameters against temperature suggest possible phase transitions around 100, 120, and 180 K. Cell data at 90 K: monoclinic P21/a, a=9.0851(5) Å, b=8.5617(5) Å, c=5.8343(3) Å, β=79.295(2)°, and Z=4. Succinonitrile has gauche conformation, in agreement with literature spectroscopy data.

It is demonstrated that a complex X-ray characterization of semiconductor films epitaxially grown on metal oxide buffer layers and Si(111) substrates is possible using laboratory-based equipment. This is demonstrated with epi-germanium on Pr2O3 as buffer material. Pole figure measurements prove that epi-Ge layers are nearly single crystalline with exactly the same in-plane orientation (type A) as the Si(111) substrate, while the lattice of the oxide layer is 180° rotated around the [111] surface normal (type B). Only a small fraction (less than 0.6 vol %) of the epi-Ge exhibits type B rotation twins. The main structural defects are microtwin lamellas lying in {111} planes 70.5° inclined to the wafer surface. The different in-plane orientation of the Si substrate and epi-Ge on one side and the Pr2O3 buffer layer on the other side allows a very sensitive analysis of strain and defects even for a 10-nm oxide layer buried under a 100-nm Ge. The epi-Ge layers are nearly fully relaxed and the Pr2O3 buffer layer is compressively strained. Due to the existing defects the Ge (111) planes are tilted in a characteristic pattern relative to the Si substrate.

This study focuses on characterization of an (Al,Cr)3Ti alloy processed together with titanium powder by reactive mechanical milling (RMM) to produce an ultrafine grained intermetallic alloy matrix with in situ carbide and hydride phases formed during processing. Observations of X-ray scattering as RMM processing time increases show severe broadening of matrix diffraction peaks, accompanied by the appearance of diffraction peaks resulting from the formation of very small crystallites of TiC and TiH1.92 phases with increasing volume fractions, and finally, increasing background intensity as the crystallite size of the matrix phase decreases to ∼2 nm. Estimates of phase volume fractions were made by the direct comparison method, along with crystallite sizes by Warren–Averbach peak profile analysis. The general increase in background intensities has been attributed to random static displacements of the large fraction of atoms located within the grain boundary regions. Further, it has been concluded that the matrix material with a crystallite size of a few nanometers has about half the atoms in statically displaced positions defining the boundary regions. The results argue that background intensity changes should not be ignored and are useful in interpreting scattering from these nano-scale materials.

The ICDD sponsored a round robin on the quantitative Rietveld phase analysis of pharmaceuticals. 11 participating laboratories from the pharmaceutical community submitted both raw data and processed quantitative results. The purpose of the round robin was to evaluate current practices in laboratories, so procedures and methods were not specified, but they were recorded. Cluster analysis tools were applied to all the data sets and their use helped identify the root causes of several types of errors in specimen preparation, data treatment, and Rietveld analysis. The authors considered this round robin to be difficult. Sample homogeneity was an issue and molecular orientation was observed in many data sets. Each material studied has structural polymorphs so the selection of starting parameters and their refinement was nontrivial. Similar to prior round robins on inorganic materials and minerals, this round robin identified operator errors as the major contributor to poor results. Four laboratories achieved excellent results on all phases in all three samples, with accuracy within relative errors of 5% to 10%.

The crystal structure of the mullite in a commercial material was refined by the Rietveld method using laboratory X-ray powder diffraction data. In this one refinement, most of the common challenges—including variable stoichiometry (partially occupied sites), multiple impurity phases, amorphous material, constraints, restraints, correlation, anisotropic profiles, microabsorption, and contamination during grinding—are encountered and the thought processes during the refinement are described step-by-step. Interpretation of the refinements includes bulk chemical analysis, chemical composition of the mullite, assessment of the geometry, bond valence sums, the displacement coefficients, crystallite size and microstrain, comparison to similar structures to assess chemical reasonableness, and the nature of the amorphous phase.

A specially designed specimen holder employing a beryllium dome has been fabricated for collection of X-ray diffraction (XRD) data from highly reactive materials. The specimen holder has a robust O-ring type seal (<10−9Torr) and no observed intensity artifacts in the 1° to 150° 2θ range. The design also minimizes specimen displacement errors and allows for analysis of both powders and bulk specimens (i.e., pellets). The simple design makes for straightforward assembly of the holder within the confines of a glove box. XRD analysis of hygroscopic LaBr3 powders collected with this holder are suitable for Rietveld structure refinement, yielding unit cell lattice parameters of a=7.9703(6) Å and c=4.5122(6) Å; cell volume=248.44(6) Å3; Rp=7.70%.

The evolution of internal stresses in oxide scales growing on polycrystalline Fe3Al alloy in atmospheric air at 700 °C was determined using in situ energy-dispersive synchrotron X-ray diffraction. Ex situ texture analyses were performed after 5 h of oxidation at 700 °C. Under these conditions, the oxide-scale thickness, as determined by X-ray photoelectron spectroscopy, lies between 80 and 100 nm. The main phase present in the oxide scales is α-Al2O3, with minor quantities of metastable θ-Al2O3 detected in the first minutes of oxidation, as well as α-Fe2O3. α-Al2O3 grows with a weak (0001) fiber texture in the normal direction. During the initial stages of oxidation the scale develops, increasing levels of compressive stresses which later evolve to a steady state condition situated around −300 MPa.

X-ray powder diffraction data, unit cell parameters, and space group for alaptide are presented (a=21.136(4) Å, b=7.212(4) Å, c=6.126(3) Å, space group P212121, cell volume=933.8(8) Å3, and Z=4). All measured lines were indexed and are consistent with the P212121 space group. No detectable impurities were observed.

K2Zn3(P2O7)2 was synthesized by solid state reaction and its crystal structure was determined by ab initio method from powder X-ray diffraction (XRD) data. The title compound was determined to be orthorhombic with space group P212121, Z=4, and lattice parameters a=12.901(8) Å, b=10.102(6) Å, and c=9.958(1) Å. Values of lattice parameters from 303 to 573 K were measured by temperature-dependent XRD. Thermal expansion coefficients α0, lattice parameters, and cell volume at 0 K were determined to be α0(a)=1.62327×10−4/K, a0=12.855(4) Å, α0(b)=1.17921×10−4/K, b0=10.070(8) Å, α0(c)=2.62364×10−4/K, c0=9.880(4) Å, and α0(V)=6.599×10−2/K, V0=1278.967(0) Å3. The specific heat equation as a function of temperature was determined to be Cp=0.77115+0.00231T−1241.60027T−2−1.4133×10−6T2 (J/K g), for temperatures from 198 to 710 K. The melting point estimated from the μ-DTA heating curve is 795 °C.

CaMnO3 is a parent compound for numerous multicomponent manganese perovskite oxides. Its crystallographic data are of primary importance in the science and technology of functional CaMnO3-based materials. In the present study, data were collected for a CaMnO3 sample at 302 K. The crystal structure refinement yields accurate absolute values of lattice parameters, a=5.281 59(4) Å, b=7.457 30(4) Å, and c=5.267 48(4) Å, leading to orthorhombic distortion of (c/a, √2c/b)=(0.997 33,0.998 95). The orthorhombic distortion of the CaMnO3 structure is discussed on the basis of comparison of our unit-cell size with data already published. At a graphical representation of the distortion, it is observed that there is a considerable scatter of the distortion values among the literature data but, interestingly, a considerable fraction of experimental results (including the present one) for stoichiometric samples are grouped around the distortion (c/a, √2c/b)=(0.9973,0.9990), which lies close to a maximum in the extent of orthorhombicity. The influence of off-stoichiometry on the orthorhombic distortion is discussed on the basis of available experimental data. Simulations, employing a mean-field approach for low temperatures, predict an increase in cell volume and structural distortions with the concentration of oxygen vacancies when the additional electrons are localized on the manganese. A simple model of delocalization produced the opposite effect, which is expected to combine with lattice vibrations to recover the cubic phase at high temperatures.

Dislocation model of strain anisotropy is presented. The dislocation theorem of strain broadening is suggested which means that strain broadening can only be caused by dislocation-type lattice defects. Based on this theorem strain anisotropy is modeled and accounted for by assuming that strain broadening is caused by dislocations or dislocation-type lattice defects. The effect of strain anisotropy is summarized in hkl dependent dislocation contrast factors, which can be either averaged over the permutations of hkl indices or are different for each different reflection. The dislocation model of strain anisotropy provides a powerful tool to analyze slip activity, Burgers vector populations, and plasticity on the basis of line profile analysis.

The solvent-free conversion of N-carbamoyl-L-proline to hydantoin-L-proline by direct heating at 470 K is reported. A reaction mechanism is proposed based on a nucleophilic intramolecular substitution reaction involving both the lone pair of the NH2 group and the carboxylic acid group of the N-carbamoyl-L-proline. The DSC and TGA experiments show rising of the baselines of the curves prior to melting and decomposition given evidence of the onset of the thermal reaction. NMR experiments were used to identify the product of the reaction, hydantoin-L-proline, whose crystal structure was obtained from X-ray synchrotron powder diffraction data collected on the solidified melt. This compound displays a crystal packing directed by hydrogen bonds forming a layered structure pile up along the c direction.