The room temperature X-ray powder diffraction pattern of Fe2GeSe4, a II2 □ IV VI4 semiconducting compound, has been recorded and evaluated. This material was found to be orthorhombic, a=13.069(1), b=7.559(1), c=6.2037(6) Å, V=612.83(9) Å3, Z=4, Dx=5.42 gcm−3. The structure refinement carried out using the Rietveld method indicated that this material crystallizes in space group Pnma (No. 62) with an olivine type of structure. The refinement of 33 parameters led to RWP=15.3%, RP=10.2% for 5251 step intensities and RB=9.44% and RF=9.36% for 913 reflections.

Phases of general formula (RE, A)2M3O7 (RE=lanthanide, A=Ca, Sr, Ba; M=Ga, Al) are of interest for their nonlinear optical properties and have potential as solid state lasers. Their structures have been refined using X-ray and neutron diffraction data and are related to gehlenite, Ca2Al2SiO7, with M cations occupying Al and Si sites and RE and A cations sharing the Ca site with no evidence for ordering, although they occur in the ratio 1:1 because of stoichiometry; the M cations are tetrahedrally coordinated. (RE, Ba)2M3O7 compounds cannot be synthesized for M=Al or for RE cations smaller than Sm; this limitation is believed to be due to size mismatch between cations within the structure.

The X-ray powder diffraction patterns for two new synthetic calcium uranium (VI) silicate hydrate phases are reported. Ca1.5U6(OH)7O16·7H2O is orthorhombic, space group P*a*, with unit cell a=13.8949(14), b=12.0776(12), c=15.228(3) Å. The structure appears to be related to that of becquerelite. Ca2(UO2)2(Si2O5)3·10H2O was also indexed on an orthorhombic unit cell, a=12.075(3), b=15.406(6), c=26.043(6) Å. The Powder Diffraction File coverage of uranium-containing minerals which could, on the basis of their chemical formula, form in U-containing cements is also reviewed.

The following fifteen reference patterns of boride, silicide and oxide ceramics represent the first group of ceramic phases measured at the National Bureau of Standards under the project “High Quality Reference Patterns and Total Digital Powder Patterns of Technologically Important Ceramic Phases”. The support and interest of the JCPDS-ICDD in this project is gratefully acknowledged.

The general methods of producing these X-ray powder diffraction reference patterns are described in this journal, Vol. 1, No. 1, pg. 40(1986).

Recent developments in the Rietveld method for the analysis of powder diffraction data have seen the method evolve from its original purpose of crystal structure refinement to nclude the determination of phase abundance in polycrysalline mixtures and the estimation of crystal size and strain parameters. However, the Rietveld method is not easy to use and may deter many powder diffractionists, who are not inerested in structure refinement per se, from using the method in its non-structural applications.

In order to overcome the difficulties in using the Rietveld method, a program, QPDA (for Quantitative Powder Diffraction Analysis), has been written that sets the conditions necessary for a single or multi-phase refinement, runs the Rietveld program and extracts phase abundance and size/strain information from the refined parameters. The program comprises a user-friendly, default-driven system of subroutines, written initially in VAX Fortran, and operates from a database of inorganic materials frequently encountered in a wide range of minerals and materials science industries.

Equations (3) and (5) should be corrected to read as follows:

Powders of Al and Ti were blended and compacted, the compact then melted in an attempt to produce single phase Al3Ti. Optical microscopy of the cast and homogenized specimen revealed an almost single phase microstructure with minor amounts of a second phase. The composition of the matrix was measured using fully quantitative energy dispersive X-ray analysis. By use of X-ray diffractometry, the interplanar spacings and the associated integrated peak intensities were experimentally measured for the binary DO22 compound, Al3Ti. Using standard structure factor equations, the intensities were calculated for the various reflections. Good agreement was obtained between calculated and observed intensities.

After regeneration, the catalyst UOP-R-62 was used for conversion of reforming benzine. The percentage of conversion benzine fraction was considerably smaller than that of the new catalyst sample. To determine the cause of catalyst deactivation, in addition to standard methods of analysis, X-ray diffraction and scanning electron microscopy were used. Real and model samples of UOP-R-62 were analysed. Real samples were prepared with the new catalyst, a used and regenerated catalyst with good activity and a deactivated catalyst. Model samples were prepared from the new catalyst by heating at 400–1100 °C in a porcelain crucible in a muffle furnace for 1 h. Prepared samples were measured in a Philips diffractometer system and examined in a scanning electron microscope. The obtained diffractometer patterns, FWHM value of the 440 reflection of γAl2O3, electron micrographs and images of emitted characteristic X-rays were mutually compared. Only the values obtained from the deactivated catalyst differed from the others. Besides reduced broadening of the 440 line the material exhibited new X-ray diffraction lines, a change in phase composition, and modifications in morphology and microstructure. These changes are an indication that overheating of individual spheres of catalyst UOP-R-62 to a temperature of 700—1100 °C or higher caused their deactivation.

Indexed X-ray powder diffraction data derived from Rietveld crystal structure refinements are reported for synthetic potassium-richterite (KRC: K[CaNa]Mg5Si8O22(OH)2), nickel-potassium-richterite (NIKRC:K[CaNa] Ni5Si8O22(OH2) and cobalt-potassium-richterite (COKRC:K[CaNa]Co5Si8O22 (OH2). The following dimensions were obtained: KRC: a = 10.0547(8), b = 17.997(1), c = 5.2746(4)Å, β = 104.832(5)°; NIKRC: a = 10.0297(7), b = 17.942(1), c = 5.2576(4)Å, β = 104.982(5)°; COKRC: a = 10.1166(9), b = 18.066(1), c = 5.2752 (4)Å, β= 104.846(6)°.

X-ray powder diffraction data and refined unit cell parameters for SrTi3Nb4O17, SrTi5Nb4O21, SrTi7Nb4O25, SrTi9Nb4O29, SrTi11Nb4O33, SrTi13Nb4O37, and SrTi15Nb4O41 are reported here. The powder patterns for these oxides suggest that they form a homologous series SrM2n+1O4n+5 (M=Ti, Nb; n=3→9), which is isostructural with the orthorhombic “chemically twinned rutile” series found previously in the K2O-TiO2-Ta2O5 and BaO-TiO2-Nb2O5 systems. The structures are built of corner-sharing slabs of the rutile structure; successive members are generated by adding 2TiO2 to the slab thickness of the previous member. The series crystallizes in space group Cmcm (No. 63), with members exhibiting similar a-, b-dimensions (∼6.6, ∼8.9 Å; respectively), and c-dimensions that linearly increase (by ∼4.4 Å per member) from 20.8 Å for n=3 to 47.1 Å for n=9.

A nonlinear optical material, o–chlorobenzol–benzoyl thiourea (C14H11ClN2OS), has been characterized by X-ray powder diffraction. Experimental values of 2θ corrected for systematic errors, relative peak intensities, values of d, and the Miller indices of 78 observed reflection with 2θ up to 72° are reported. The powder diffraction data have been evaluated, and the figures-of-merit are reported. The unit cell parameters least-squares refined from 28 nonoverlapping peaks of the monoclinic compound with a P2 space group are a=13.2797(4) Å, b=12.4058(8) Å, c=8.1561(2) Å, β=95.398(1)°, V=1337.7(4) Å3, Z=4, Dx=1.444 g/cm3. © 1997 International Centre for Diffraction Data.

The Metals and Alloys Indexes, published by the International Centre for Diffraction Data, contain four indexes. These are: (a) the alphabetical formula index (AFI); (b) the Pearson symbol code index; (c) the common name index; and (d) the Strukturbericht symbol index. These indexes (which contain metals, alloys, and related phases in the Powder Diffraction File) have been designed to be used independently or in conjunction with the Powder Diffraction File to facilitate the characterization of materials. All data in these indexes have been critically reviewed. The organization, selection of materials, and use of alphabetical formulas are similar to those of standard metallurgical references such as Pearson or Villars and Calvert. The arrangement of the AFI promotes systematic searches for chemical analogs and assists users in locating possible matches when only partial chemical information is available. The structural indexes aid in characterization by correlations to prototype and related structures. Some applications of the indexes are given here.

Ab initio structure determination of new compound (Pb0.6Cu0.4)Sr2PrCu2O7−x was obtained at 300 and 100 K from X-ray powder diffraction data and refined by Rietveld technique. (Pb0.6Cu0.4)Sr2PrCu2O7−x has an isotypical structure with TlBa2CaCu2O7 (1212) at both 300 and 100 K. At 300 K, crystal data: (Pb0.522Cu0.4)Sr2PrCu206.53, Mr=681.293, tetragonal system, space group P4/lmmm, a = 3.8631(5)Å, c= 11.9134(2)Å, V= 177.79Å3, Z= 1, Dx, = 6.3631 g/cm3, μ=1036.549 cm−1 (λ=1.54051 Å), F(000) = 299.6, the structure was refined with 31 parameters to Rwp = 4.02%, Rp=2.96% for 3379 step intensities and Rb = 4.80%, Rf=5.17 for 143 reflections, “goodness of fit” S = 2.20. At 100 K, crystal data: (Pb0.547Cu0.4)Sr2PrCu2O6.89, Mr=692.232, tetragonal system, space group P4/mmm, a = 3.8580(2) Å, c= 11.8898(5) Å, Z=1, Dx = 6.4953 g/cm3, μ= 1053.235 cm−1 (λ=1.54051 Å), F(000) = 304.6, the structure was refined with 32 parameters to Rwp = 5.53%, Rp=4.22% for 2574 step intensities and Rb = 6.11%, Rf=5.31% for 111 reflection, “goodness of fit” S= 1.79. Moreover, the composition of Pb was refined to 0.522 at 300 K and to 0.547 at 100 K as compared with the stoichiometric composition 0.6.

Fourier transform methods of smoothing and interpolation are applied to X-ray diffraction data. It is shown that, frequently, too small a step size is used. Major gains are to be expected by selection of the optimum step size and use of these methods.

A comparison of Fourier transforms of diffractograms of quartz measured between 67 and 69° 2θ, collected at varying step intervals (0.1 to 0.01° 2θ) was used to illustrate these applications. By examining the Fourier transform of the diffractogram and noting where it decays to die baseline, a reasonable estimate of the optimal step interval can be obtained. In addition, Fourier interpolation can be used to enhance the appearance of the diffractogram, approximating a continuous plot.