Developments in X-ray analysis hardware and software have combined to dramatically improve the throughput, speed, and accuracy of formulation analyses. We will focus on a complimentary development, the growth and application of a comprehensive database based on the Powder Diffraction File™ (PDF®). The PDF is an edited and standardized combination of several crystallographic databases with ∼497 000 published entries. The comprehensive nature of this database, combined with phase identification and digital pattern simulations, was used to identify complex formulations with crystalline and noncrystalline ingredients. We will show how these parallel developments enhance the ability to correctly identify complex formularies.

This work introduces a new simple approach to determine experimental X-ray elastic constants (XECs) of thin films by coupling the sin2ψ method and the substrate curvature technique. The approach is demonstrated on polycrystalline Cu thin films with the thickness 200, 800, and 2400 nm deposited on Si(100) substrates. Applying synchrotron radiation, the elastic strains in the films are determined using sin2ψ method while the macroscopic stresses are assessed by measuring the substrate curvature. The stresses are calculated using the Stoney formula from the radius of substrate curvature determined by the rocking curve measurement of substrate 400 reflection at different sample positions. Results show that the magnitude of the macroscopic stress in the films is proportional to the magnitude of the slope in the sin2ψ plots. On the basis of this observation, XECs of the films were calculated showing no dependence on the film thickness. The characterization of the samples was performed at the synchrotron source Hasylab.

Crystal structure of Ca1.1Co1.9(PO4)2 was successfully determined from laboratory X-ray powder diffraction data (Co Kα) using direct methods and the Rietveld refinement. The crystal structure was found to be monoclinic (space group P21∕n, Z=4) with lattice dimensions of a=1.452 67(5) nm, b=0.494 34(1) nm, c=0.867 50(3) nm, β=92.316(1)°, and V=0.622 45(3) nm3. The final reliability indices calculated from the Rietveld refinement were Rwp=3.93%, Rp=3.02%, RB=4.10%, and S=1.48. Both Co and Ca atoms were distributed over the 2a and 2d sites with a preference of Ca at the 2d site. The coexistence of Co and Ca on the 2a and 2d sites is indispensable for stabilizing Ca1.1Co1.9(PO4)2 in the Ca3(PO4)2-Co3(PO4)2 system.

The crystal structure of La2SiO5 was refined from laboratory X-ray powder diffraction data (CuKα1) using the Rietveld method. The crystal structure is monoclinic (space group P21∕c,Z=4) with lattice dimensions a=0.93320(2) nm, b=0.75088(1) nm, c=0.70332(1) nm, β=108.679(1)°, and V=0.46687(1) nm3. The final reliability indices were Rwp=7.14%, RP=5.52%, and RB=3.83%. There are two La sites in the structural model, La1 and La2. La1 is ninefold coordinated to oxygen, forming a tricapped trigonal prism with a mean La1-O distance of 0.263 nm. The La2O7 coordination polyhedron is a distorted capped octahedron with a mean La2-O distance of 0.251 nm. The La1O9 polyhedra share faces and the La2O7 polyhedra share edges, forming two sets of sheets that alternate parallel to the (100) plane. These sheets are linked through SiO4 tetrahedra and non-silicon-bonded oxygen atoms to form a three-dimensional structure. This compound is isomorphous with the low-temperature (X1) phases of R2SiO5 (R=Y and Gd). The volumes of RO9 polyhedra steadily increase with increasing ionic radius of R, from Y3+ to Gd3+ to La3+, which causes substantial volumetric expansion of the crystals.

The crystal structure of cesium ammonium hexachlorotellurate [Cs0.86(NH4)0.14]2TeCl6, has been determined using X-ray powder diffraction techniques. At room temperature, the title compound crystallizes in the cubic space group Fm3m, with a lattice parameter a=10.470(17) Å. The Rietveld refinement of the structure led to final confidence factors Rp=0.0338 and Rwp=0.0487. The structure of [Cs0.86(NH4)0.14]2TeCl6 belongs to the large family of K2PtCl6-related structures. The H atoms of the ammonium group are orientated with its apex toward Te atoms as seen in the related compound (NH4)2SiF6. An IR spectroscopic study was performed to confirm the results of the diffraction method, notably concerning the presence of the ammonium group.

This study examined basal peak irrationalities according to boundary conditions of the hectorite basal diffraction unit (BDU), which were recognized as the total assembly of 2:1 phyllosilicate layer plus interlayer material. The hectorite basal profiles were computer-simulated using the three kinds of BDU settings identified from the middle of octahedral sheets in the nearest neighbor (centrosymmetric model), the middle of interlayers in the nearest neighbor (centrosymmetric model), and a basal oxygen plane to the margin of interlayer in contact with the next phyllosilicate layer (non-centrosymmetric model). In the results of simulations, irrationality and asymmetry of the hectorite basal peaks relied straightforwardly on the BDU scattering modulations for the non-Bragg angles containing information on the synergic scattering events of phyllosilicate layer and interlayer material. Among the concerned BDU boundaries, the non-centrosymmetric model more effectively represented the real hectorite profile than the two previously reported centrosymmetric models.

Detailed structural properties of La1−xBaxCoO3 (LBCO) have been investigated by means of X-ray powder diffraction and Rietveld analysis. A structural phase transformation from R3c to Pm3m at x=0.30–0.35 has been detected based on a comparison between the refinements of R3c and Pm3m. The Co–O bond length of the CoO6 octahedron expanded rapidly with increasing Ba content when x<0.1, and then it leveled off and kept constant at 0.1⩽x⩾0.35, where the Co–O–Co bond angle reaches 180°. The Co–O bond length expansion resumed with increasing Ba content beyond x=0.35.

A study examining the feasibility, and possible necessity, of using transmission data from capillary mounted samples for quantitative analysis of hydrated cement systems was conducted. In order to obtain true quantitative results, the amorphous contents were determined by the addition of an internal standard. The amorphous content of the starting tricalcium silicate was found to be approximately 21–22 wt %, in close agreement with previously published results. The study revealed that the spherical harmonics preferential orientation correction may not be reliable with unmicronized hydrated cement materials in reflection geometry, as chemically unreasonable progressions in Portlandite content with time were observed. The data obtained from capillary measurements, however, exhibited little or no preferential orientation, and appeared to produce the progression of phase contents expected from the reaction. The use of capillaries would appear to be justified in some circumstances to obtain reliable quantitative results from hydrated cementitious materials. In this particular system, a significant fraction of calcium carbonate was present as aragonite, as well as the more usual calcite.

We discuss the impact of strong absorption for thermal neutrons on data analysis and compare absorption corrections in the GSAS and MAUD Rietveld codes for texture and structural parameter refinement. Diffraction data were collected on the neutron powder diffractometer HIPPO at LANSCE from dysprosium and erbium, which are moderate-to-strong absorbers for thermal neutrons with absorption cross sections of 159 barns for Er and 994 barns for Dy at λ=1.8 Å. Both elements have hexagonal-close-packed (hcp) crystal structures, and the samples were various thicknesses of rolled foils. The orientation distribution functions (ODF) were fit to the same neutron time-of-flight data sets using two very different full pattern Rietveld analysis procedures. Spherical harmonics functions were fit to the textured data using GSAS. These data were also analyzed by the modified direct method E-WIMV using MAUD. The resulting pole figures from the ODFs determined by both Rietveld analysis packages are qualitatively similar, and the textures were confirmed by X-ray diffraction. Additionally, data from orthorhombic dysprosium and erbium fluoride powders show that atomic positions are not sensitive to absorption. We address inconsistencies and methodologies in data analysis when strong absorption is present.

Neutron diffraction studies were carried out to ascertain the structural details of the composition Ce0.5Nd0.5O1.750. The structure was unequivocally found to be that of C-type cubic. The refinement on an F-type cubic lattice was found to be unacceptable because of high R values. Selected bond distances are also being reported. In addition, the neutron diffraction studies on a typical defective F-type composition Ce0.75Nd0.25O1.875 were also carried out.

Li0.5M0.25TiOAsO4 (M=Mg,Co,Ni,Zn) oxyarsenates powders were prepared by coprecipitation method from dilute solution of Li2CO3,M(NO3)2×H2O (M=Mg,Co,Ni,Zn), (NH4)H2AsO4 and TiCl4 in ethanol. The resulting powders, obtained after drying at about 60 °C, were heated progressively with intermittent grindings at 200 °C–750 °C in air. These new compounds crystallize in the monoclinic system with space group P21∕c. Their parameters are functions of M2+ ion size.

Improved X-ray powder diffraction data for synthetic PdSn are reported. Powder diffraction data were collected with a laboratory X-ray source (CuKα) for Rietveld refinement. Refined crystallographic data for PdSn (orthorhombic, Pnma) are a=6.1388(4), b=3.89226(3), c=6.3377(4) Å, V=151.43(2) Å3, Z=4, and Dx=9.87 g∕cm3.

Amantadine hydrochloride, p-aminophenol hydrochloride, and methylamine hydrochloride, compounds often studied in pharmacology, were investigated by means of powder diffractometry. The chemical formula of the first compound is C10H17N HCl and crystallizes in the monoclinic system, space group C2∕c (15) with lattice parameters a=2.0279(6) nm, b=1.1171(2) nm, c=9.759(4) nm, and β=109.00(3)°. p-Aminophenol hydrochloride C6H7NO HCl crystallizes in the orthorhombic system, space group P222 with lattice parameters a=0.6619(2) nm, b=0.88461(2) nm, and c=0.6101(2) nm. Methylamine hydrochloride CH5N∙HCl crystallizes in the tetragonal system, space group P4∕nmm (129) with lattice parameters a=b=0.6068(1) nm and c=0.50689(8) nm.

K3Nb3WO9(AsO4)2 has been investigated by means of X-ray powder diffraction. Powder diffraction data were obtained by conventional diffractometer with Kα radiation. Unit-cell dimensions were determined by an indexing program based on variation of parameters by successive dichotomies. An orthorhombic cell (space group Pnma) was found with a=15.001 (1) Å, b=14.814(1) Å, c=7.2374 (8) Å, and V=1608.4 (4) A3. The figures of merit were calculated to be M(20)=35.9 and F(20)=70.8 (0.0055,51).

In this study, we use X-ray diffraction (XRD) and micro-Raman spectroscopy (MRS) to measure internal strains in sensors embedded in polymer matrix composites. Two types of strain sensors embedded in either chopped graphite fiber∕epoxy matrix composite (MRS) or unidirectional graphite fiber∕polyimide matrix composite (XRD) were investigated. For XRD measurements, the sensors were in the form of spherical aluminum inclusions with diameters ranging from 1 to 20 μm. Due to large cross section area of an incident X-ray beam, only average stresses are reported using the XRD approach. Complementary to XRD experiments, MRS was pursued to measure internal strains in Kevlar-49 fibers embedded in chopped graphite fiber∕epoxy matrix composite. In recent years, MRS as an experimental tool for microstrain measurements has drawn considerable attention mostly due to its excellent spatial resolution. The resolution of MRS typically ranges between 1 and 10 μm, which means that strains can be measured in individual sensors. The principle of this method relies on a change of certain molecular vibration frequencies as a result of an applied stress. Several examples are presented and discussed to demonstrate the potential of combining micro and macrostrain measurements and modeling to capture the stress distribution in heterogeneous materials.

Single-phase samples of La1−xCaxMnO3 compounds have been synthesized by solid-state reaction. Detailed Rietveld analysis of powder X-ray diffraction data showed that La1−xCaxMnO3 undergoes a structural phase transformation from R-3c to Pnma at X=0.05–0.075. There is a linear variation of lattice parameters as a function of calcium concentration. The slope of this linear variation changes at X=0.6. A correlation between observed Mn-O bond lengths, corresponding to different compositions, and possible magnetic phases is discussed.

In this study, the effects of growth interruptions on the formation of the interfaces in GaAs∕AlAs multilayers are investigated. For that purpose, a series of different samples has been manufactured with molecular-beam epitaxy. The introduction of growth interruptions of 50 s after the deposition of the layer leads to a change in the morphological properties of the interfaces, in particular their correlation length. These modifications due to the growth interrupt are analyzed with diffuse X-ray scattering. As a result of the measurements, an extension of the lateral correlation length can be proved. By contrast, the vertical correlation of the interfaces is not affected.

Synchrotron X-ray powder diffraction (XRPD) data were collected for the silver(I)-aspartame complex [Ag(C14H17N2O5)]∙1∕2H2O. The complex was obtained from a stoichiometric mixture of aspartame (3-amino-N-(α-carboxyphenethyl)-succinamic acid N-methyl ester, C14H18N2O5), Na2CO3, and AgNO3. Indexing using Crysfire and Chekcell proposed an orthorhombic unit cell with space group P2221. The lattice parameters are a=12.4750(1) Å, b=21.60614(14) Å, and c=4.88888(9) Å.

Crystallographic structures of two new orthophosphates Ca0.50SbFe(PO4)3 and CaSb0.50Fe1.50(PO4)3 obtained by conventional solid state reaction techniques at 900 °C, were determined at room temperature from X-ray powder diffraction using Rietveld analysis. The two compounds belong to the Nasicon structural family. The space group is R3 for Ca0.50SbFe(PO4)3 and R3c for CaSb0.50Fe1.50(PO4)3. Hexagonal cell parameters for Ca0.50SbFe(PO4)3 and CaSb0.50Fe1.50(PO4)3 are: a=8.257(1) Å, c=22.276(2) Å, and a=8.514(1) Å, c=21.871(2) Å, respectively. Ca2+ and vacancies in {[Ca0.50]3a[◻0.50]3b}M1SbFe(PO4)3 are ordered within the two positions, 3a and 3b, of M1 sites. Structure refinements show also a quasi-ordered distribution of Sb5+ and Fe3+ ions within the Nasicon framework. Thus, in {[Ca0.50]3a[◻0.50]3b}M1SbFe(PO4)3, each Ca(3a)O6 octahedron shares two faces with two Fe3+O6 octahedra and each vacancy (◻(3b)O6) site is located between two Sb5+O6 octahedra. In [Ca]M1Sb0.50Fe1.50(PO4)3 compound (R3c space group), all M1 sites are occupied by Ca2+ and the Sb5+ and Fe3+ ions are randomly distributed within the Nasicon framework.

X-ray powder diffraction data for Mo2.85Al1.91Si4.81 are reported. The new Mo2.85Al1.91Si4.81 compound was successfully prepared using the self-propagating high-temperature synthesis (SHS) technique. The starting atomic mixture of reactant powders was Mo+2(1−x)Si+2xAl with x=0.3. The final powder compound obtained by the SHS technique was determined to be Mo2.85Al1.91Si4.81 by ICP-AES. X-ray powder diffraction pattern of Mo2.85Al1.91Si4.81 was recorded using an X-ray powder diffractometer, Cu Kα radiation, and analyzed by automatic indexing programs. Mo2.85Al1.91Si4.81 was found to be hexagonal with a=4.6929(2) Å and c=6.5515(4) Å. The XRD results are in good agreement with those of Mo2.85Ga2Si4.15.