There are 39 CRYSTMET® entries in the hexagonal space group P-3m1 (164) reporting both distinct pure phase compounds and atomic coordinates. Having the same Wyckoff positions in the same space group as the C6 structure type, all are isopointal with it. The range of observed c/a values extends from about 0.65 to 1.83. Three types are distinguished: Layered materials with CdI2 type, the CeCd2 type which is a slight distortion of the hexagonal AlB2 type, and the intermediate EuGe2 type made of the materials AuTe2, BaSi2, EuGe2, and SrGe2. Ab initio modeling of the 26 entries with CdI2 and EuGe2 type and atomic coordinates reproduces convincingly both their c/a axial ratios and z coordinates. For CoO2 and SiTe2, both c/a and z deviate to a degree from the reported values, indicating that those materials should be reexamined for superstructures, stoichiometry, etc. Ab initio modeling of the 11 cell-and-type entries with CdI2 type and no coordinates in CRYSTMET reproduced convincingly their reported axial ratios. The X-ray cell data and the ab initioz coordinates were then used in the production of reliable calculated powder patterns for CoTe2, CrSe2, HfS2, HfSe2, HfTe2, NbTe2, SnSe2, VS2, VTe2, ZrS2, and ZrTe2. All 11 patterns have been inserted in the intense diffraction line search system of CRYSTMET operated under the Materials Toolkit. Comparison of calculated patterns for SnSe2 and ZrTe2 with experimental entries in the PDF exposes the complementarity of calculated and experimental powder patterns and suggests that JCPDS pattern #15-223 should be reinterpreted in terms of the CdI2 structure type. The CeCd2⇔AlB2 type transformation is modeled and discussed on YCd2 using both ab initio methods and a hard-sphere model. For z<0.45, the ab initio solution is identical with that from the hard-sphere model while a quantum regime is predicted in the small region 0.45<z<0.467 beyond which YCd2 abruptly transforms to the AlB2 type. In spite of the new understanding gained, this modeling fell slightly short of allowing calculation of z values and powder patterns for the materials CaHg2, DyHg2, ErCd2, GdHg2, HoCd2, HoHg2, LuCd2, NdCd2, SmHg2, TbCd2, and TbHg2 with no coordinates in CRYSTMET.

Three phosphates, MIBaIn2(PO4)3 with MI=Na, K, Cs, isostructural to the langbeinite structure, have been studied from powder diffraction data collected with monochromatic radiation obtained from a conventional X-ray source. Precise powder data are reported, as well as cell parameters, i.e., a=10.026 08(9) Å, a=10.121 57(13) Å and a=10.226 94(9) Å for MI=Na, K and Cs, respectively. A Rietveld refinement has been carried out (space group P213), with final RF factors, 0.061, 0.041 and 0.027, and Rwp factors, 0.196, 0.142 and 0.129, for MI=Na, K and Cs, respectively. There are two octahedrally coordinated In3+ ions in the asymmetric unit and the final refinements suggest disorder on the two sites of the MI/Ba sublattice.

An analysis of the microstructure of nanocrystalline yttrium oxide produced by thermal decomposition of a double oxalate yttrium and ammonium, at temperatures in the range 600 °C to 900 °C, is described. The study is based on line broadening analysis carried out with the (Voigt/Langford) integral breadth and Fourier methods combined with the pattern decomposition technique. Due to the line overlap arising from the density of diffraction lines, the whole pattern refinement method (pattern matching and Rietveld approaches) is also applied. No marked line broadening anisotropy is observed in the patterns. It is shown that for the two samples prepared at the highest temperatures the results are similar whatever the method used and the material can be considered as strain free. For the two lowest temperatures only the whole pattern refinement method is applied. The results suggest that a small amount of lattice microdistortion is present in these two last samples. It is shown that the crystallite growth varies exponentially with temperature. The results obtained from line broadening analysis are compared to those observed with scanning electron microscopy, from which a good accordance is noted between the two techniques.

Polycapillary optics are utilized in a wide variety of applications and are integral components in many state of the art instruments. Polycapillary optics operate by collecting X-rays and efficiently propagating them by total external reflection to form focused and parallel beams. We discuss the general parameters for designing these optics and provide specific examples on balancing the interrelations of beam flux, source size, focal spot-size, and beam divergence. The development of compact X-ray sources with characteristics tailored to match the requirements of polycapillary optics allows substantial reduction in size, weight, and power of complete X-ray systems. These compact systems have enabled the development of portable, remote, and in-line sensors for applications in industry, science and medicine. We present examples of the utility and potential of these optics for enhancing a wide variety of X-ray analyses.

A recently developed Rigaku parallel-beam X-ray diffraction system equipped with a parabolic graded-multilayer mirror in the incident beam and a parallel-slits analyzer in the diffracted beam was used for precision high-temperature diffraction studies. The lattice parameters a and c of α-Al2O3 at room temperature and up to 1473 K were determined with precision in the range of 0.6–7.3×10−5. The thermal expansion coefficients for a and c agreed with literature values to better than 3%. The system was used successfully also to determine the Debye characteristic temperature of Si and to study structural phase transition of LaCoO3 from rhombohedral at room temperature to cubic at 1700 K.

X-ray diffraction methods have been used successfully for the analysis of platinum silicide films of 100 Å or less in thickness. Conventional X-ray diffraction was utilized for phase identification, planar orientation, and crystalline size determination. Low-angle X-ray specular reflectivity analysis measured film thickness. As the nominal film thickness approached 100 Å, it was observed that the deposited platinum film thickness was larger than expected and longer anneal times would be required to ensure homogeneous platinum silicide phase composition.

X-ray powder diffractograms from fcc crystals containing high concentration (more than 1%) of planar defects [deformation stacking faults (SF), double deformation SF, twin boundaries (TB)] have been simulated by Monte Carlo method in kinematic approach. It was shown that the characteristics of powder diffraction peak profiles (except peaks with indexes H00) dependent nonmonotonically on PD concentration, during which peak maximums stay in Bragg positions. An addition point to emphasize is that an appearance of TB only in the crystal not affects on position of all peaks. Several types of PD to be occurred simultaneously in the crystal influence on powder diffractograms additively. Peculiarities of the powder diffraction pattern inherent in different types of PD have been revealed to permit predominant PD type to be found with a high degree of accuracy based on experimental data.

Multilayer optics is one of the widely applied optics for conditioning an X-ray beam in the region of X-ray diffraction. Multilayer optics offers a well-balanced performance. The beam conditioned by a multilayer optic is characterized by low divergence, good spectrum purity, and high intensity. This article will start with a short historical note of the development of X-ray multilayer and a summary on the basic performance characteristics of X-ray multilayer, then move on to the discussion on the design principle of one- and two-dimensional optics. Both parallel beam optics and focusing optics will be addressed. As examples, selected applications of multilayer optics are also briefly discussed. Finally, the main problems associated with the application of multilayer optics are identified and the future developments are discussed.

The existence of glass or amorphous component in Portland cement clinker has been questioned for a long time. However, besides the crystalline phases, there are reports in the literature of noncrystalline material in cement clinker, which is considered to be the residue of the melt that has failed to crystallize. Absolute phase abundances were determined in this study by Rietveld refinements with laboratory X-ray data, using both internal and external phase composition standards. The results clearly demonstrate the existence of an amorphous component in Portland cement clinker. The presence of an amorphous component was also apparent from diffraction data for clinker from which the silicate phases had been chemically removed, using both laboratory X-ray and synchrotron radiation patterns.

In this work we report the synthesis and structural characterization of the elpasolite Cs2NaTbCl6, belonging to the space group Fm3m. The synthesis is by solid state reaction, in controlled atmosphere. By means of thermal analysis (DTA/TGA), the best crystallization temperatures were obtained: 772.2 °C for 2 hours. Structural studies are carried out by means of DRX-powder diffraction and application of the Rietveld profiles refinement method, for the 32 diffraction lines analyzed. The following crystallographic parameters are obtained: a0=10.7636 (Å), Z=4, M=660.44, V=1247.0 (Å)3, Dx=3.519, and Dexp=3.52±0.01.

Samples of amorphous Se, SSe40, SSe30, and SSe20 were synthesized and were then crystallized by annealing at 373 K for 5, 20, and 120 mins. The results showed that the changes in the structural and microstructural parameters for samples SSe40, and SSe30 are different from those of sample SSe20. These discrepancies are being discussed in terms of the peak shifts in both the amorphous and crystalline state, the percentage of sulfur compositional variations, and finally in terms of the probable site occupancy of the sulfur atoms in the selenium structure.

It was seen during the phase relation studies on the CeO2–YO1.5 system that the ceria is able to accommodate a large anion deficiency caused by aliovalent substitution. A neutron powder diffraction study has been carried out at room temperature for the titled solid solution, Ce1−xYxO2−x/2 with x=0.32, which is an anion-deficient variant of the ideal fluorite structure. The structure has been found to be face centered cubic. No superlattice reflections have been observed indicating that the vacancies occupy the random positions in this highly defective solid solution. The bond distances and angles are also being reported.

An experimental X-ray diffraction (XRD) study of calcium salts of four carboxylic acids is presented. Calcium salts of propionic, butyric, valeric, and caproic acids were synthesized mixing in a mortar Ca(OH)2 with the liquid acids. Measuring the thermogravimetric analysis curves it was determined that the salts were actually monohydrates. The densities of the synthesized samples were measured using a density gradient column. The measured values for the densities were as follows: Dm(propionate)=1.38 g/cm3, Dm(butyrate)=1.30 g/cm3, Dm(valerate)=1.26 g/cm3, Dm(caproate)=1.22 g/cm3. The XRD analysis revealed that these compounds have monoclinic cells with symmetry described by the P21/a space group. Calcium propionate hydrate has cell parameters: a=2.437 51(5) nm, b=0.681 24(1) nm, c=0.591 43(1) nm, β=95.320(2)°. For calcium butyrate hydrate the cell parameters are: a=2.966 84(8) nm, b=0.680 74(2) nm, c=0.589 29(2) nm, β=95.442(3)°. The cell parameters for calcium valerate hydrate are: a=3.566 36(4) nm, b=0.682 49(1) nm, c=0.592 77(1) nm, β=107.280(1)° and for calcium caproate hydrate a=4.180 30(5) nm, b=0.682 61(1) nm, c=0.592 13(1) nm, β=110.230(1)°. The calculated density values from the XRD results, taking into account that the number of chemical formulas in the unit cell equals four, agree very well with the measured ones. It was established that the unit cell parameter a grows with the increase of the number of carbon atoms in the aliphatic chain, while parameters b and c remain almost constant. This is an indication of the stacking layer character of the structure as has been suggested for calcium stearate monohydrate. This fact points to the possibility of the refinement of the crystalline structures taking as the starting point the reported structure for calcium stearate monohydrate.

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.

Doubly curved crystal (DCC) X-ray optics provide an enabling technology for new portable, remote, and in situ applications of monochromatic X-rays for composition and structure analysis of amorphous, polycrystalline, and crystalline solids. Femtogram sensitivity for surface contamination, parts-per-billion (ppb) impurity levels for solids, and composition, structure and uniformity of thin films with compact, low power (20–50 W) source optic combinations are possible.

Fluorellestadite, Ca10(SiO4)3(SO4)3F2, has been synthesized as single phase. This compound crystallizes in the apatite type structure, s.g. P63/m, with parameters a=9.4417(1) Å, c=6.9396(1) Å and V=535.76(1) Å3. The refinement of its crystal structure converged to RWP=12.33% and RF=4.58%. The atomic parameters have been used to analyze the phase content of mineralized white Portland clinkers. These clinkers contain Ca3SiO5, Ca2SiO4, Ca12Al14O32F2 and Ca10(SiO4)3(SO4)3F2. The agreement between the elemental composition inferred from the Rietveld phase analysis and that measured by XRF is noteworthy. This comparison does not take into account the presence of amorphous phases and unmodeled elemental substitutions in crystalline phases. Similar Rietveld studies on commercial white Portland clinkers are also shown to be feasible.

The phases developed upon annealing of ZnSe, CdSe, and CdS semiconductors in air are investigated applying X-ray qualitative and quantitative phase analysis. The compositions of the thermally grown oxides over the 373–773 K temperature range are found to be ZnO and ZnSeO3 for ZnSe, CdSeO3 for CdSe and CdSO4 and Cd3O2SO4 for CdS. The percentage phase abundance of each phase is determined at each temperature applying a standardless method. At all temperatures, the oxides are predominantly ZnO with about 10% ZnSeO3 at 773 K in case of ZnSe and CdSO4 with about 9% Cd3O2SO4 at 773 K in case of CdS. The rate of oxidation with temperature is found to be nonlinear for the three chalcogenides. CdS is found to be more resistible for oxidation than CdSe and ZnSe.

Methods of chemical preparation and crystallographic data are reported for four new condensed phosphates: one hydrated cyclotriphosphate MnAg4(P3O9)2·6H2O and three long-chain polyphosphates: MnAg2(PO3)4, NiAg4(PO3)6 and NiNa4(PO3)6. Two of these new condensed phosphates, associated with manganese, belong to previously investigated structure types.