Algorithms are presented to correct intensities affected by divergence slit attenuation in the low 2θ region of Bragg–Brentano powder diffractometers with rectangular sample holders. The intensity loss below a limiting angle 2θ1 occurs when the X-ray beam cross section exceeds the sample surface at decreasing angles. For identification purposes, the observed intensities can be scaled up to values comparable with intensities unaffected by divergence slit effects.

The Rietveld method based on X-ray diffraction (XRD) technology has been commonly applied for the quantitative analysis of crystalline minerals in organic-rich rocks. The presence of organic matter, however, has interference in varying degree to the quantitative result. In this work, the mixed samples of organic matter and crystalline minerals at given proportions were prepared to investigate the effect of organic matter on the Rietveld quantitative analysis of crystalline minerals in coal gangue. The relative standard deviation (RSD) and absolute error (AE) were used to evaluate the precision and accuracy of the quantitative result. The results showed that the presence of organic matter led to a reduction in the precision and accuracy. It was attributed in part to the presence of organic matter, which can produce a background noise in the XRD pattern, especially in the region of 5–30° (2θ). Further results showed that the interference in this region increased with the increase in the organic matter content. The RSD and AE were within the range of 10% and 2%, respectively, when the organic matter content is <30 wt%. Based on this, an approximate method for the Rietveld quantitative analysis of crystalline minerals in coal gangue was established.

In this work a detailed X-ray powder diffraction study of the reversible temperature transformation has been undertaken in several rare earth niobates MNbO4 M being lanthanum, cerium, neodymium, gadolinium, holmium, thulium, ytterbium, and yttrium. Both high-temperature diffractometer and film techniques were used. It was shown for the substances investigated that the low-high transformation is a continuous transition over the wbole temperature range from monoclinic at room temperature to tetragonal at the transition temperature. It was found that the rate of the overall transition is rapid, and also that the transition between any intermediate state occurs reversibly within minutes or seconds. The continuous transition and the rapid rate of attainment of equilibrium in the solid, even between intermediate states of the transformation, support the earlier assumption that it is a displacive-type order-disorder transition.

A method of Fourier analysis of x-ray line broadening is presented whereby microstrain, incoherent particle size, and fault probability can be calculated using only first-order peaks. This method can thus be used in studies of catalysts, vapor- and electrodeposits or heavily textured specimens for which second-order peaks are too broad or weak, in cases where the effect of particle size is not the same for all orders of a peak, or for multiphase specimens where overlap of peaks sometimes occurs. Examples of deformed FCG and BCC metals and alloys are presented, with comparisons to the method of multiple orders.

One part of the procedure, first demonstrated by Pines and Sirenko, provides for reducing the effects of truncation on the Fourier coefficients. As a result, larger particle sizes can be analyzed and the integrated intensity can be determined more precisely. Application to determinations of volume fraction are given.

We have developed a convenient and effective XRF analysis procedure for trace amount of K, Ca, V, Mn, Fe, Ni, Cu, Zn, Cd, and Pb in environmental waters by using a preconcentration using the natural polymer (agar). The thin agar film was prepared by drying a homogeneous agar gel after mixing the aqueous sample solution with the agar powder. XRF analysis of the preconcentrated thin agar films containing trace metals showed a good repeatability because agar films were homogeneous enough. SB (signal to noise) ratios of the XRF intensity of the analytes were improved drastically. The linear calibration curves of K, Ca, V, Mn, Fe, Ni, Cu, Zn, Cd, and Pb showed a good linearity within the calibration ranges. The lower limits of detection (LLD) were 1.4 μg/mL for K, 0.26 μg/mL for Ca, 0.088 μg/mL for V, 0.029 μg/mL for Mn, 0.11 μg/mL for Fe, 0.016 μg/mL for Ni, 0.030 μg/mL for Cu, 0.017 μg/mL for Zn, 0.20 μg/mL for Cd, and 0.066 μg/mL for Pb, respectively. The proposed preconcentration method was applied to several environmental water samples.

The neutron diffraction technique was applied to measure strain distributions in a rebar in a reinforced concrete. At first, absorption coefficients of several kinds of concrete with different compounding ratios of water, cement, and aggregate were measured, and it was confirmed that the absorption coefficient of concrete was affected by the amounts of water and aggregate. In addition, it was also clarified by measuring strain change of the rebar under tensile loading that accuracy of the strain measurement in the rebar in the reinforced concrete was not affected by the neutron absorption by the concrete. Second, the size of the anchorage zone was evaluated by measuring strain distributions in the rebar under pull-out loading. The length of the anchorage zone measured by neutron diffraction was shorter than that measured by strain gauges. Moreover, detailed strain distributions in the rebar around cracks in the concrete were measured under tensile loading, and it was confirmed that the bond condition between rebar and concrete around cracks could be evaluated using the neutron diffraction technique.

A study has been conducted with gibbsite specimens, on the use of Rietveld X-ray powder diffraction (XRPD) pattern fitting for quantitating preferred orientation in powders. This study has shown that an earlier formula gives results which correlate closely with an empirical measure of morphology proposed recently for gibbsite powders, viz., the ratio of the XRPD intensities for the (002) line and the (110, 200) doublet lines. A method is proposed on the basis of this correlation for the correction for preferred orientation of line intensities in gibbsite powder patterns. The correction method appears to have excellent potential for XRPD quantification of gibbsite levels in mixtures, and could have general application for coping with preferred orientation effects in the quantitation of other phases.

In situ deformation studies of polycrystalline materials using diffraction are an established method to understand elastic and plastic deformation of materials. Studies of active deformation mechanisms, the interplay of deformation with texture, and ultimately the development of predictive capabilities for deformation modeling are an active field of research. Parameters studied by diffraction are typically lattice strains and texture evolution, which coupled with the macroscopic flow curve allow for improved understanding of the micro-mechanics of deformation. We performed a study of the uniaxial deformation of Zircaloy-2 at 2 GPa at the 13-BM-D beamline at the Advanced Photon Source. The deformation-DIA apparatus generates a confining hydrostatic pressure using a cubic anvil setup. Two differential rams allow an increase (compressive load) or decrease (tensile load) of the uniaxial straining in the vertical direction, allowing studies of plastic deformation at high pressures. In this paper, we describe how macroscopic strains, hydrostatic pressure, and uniaxial strains are derived and present some brief results.

Synthesis and structural characterization of a novel palladium Pd(II) complex with the amino acid L-citrulline (Cit, C6H13N3O3) are presented in this paper. Elemental analysis indicates a 1:2 metal/ligand molar composition for the complex, with the molecular formula PdC12H24N6O6. The compound was also characterized by infrared (IR) spectroscopic measurements and the crystal structure has been solved by powder X-ray diffraction data with simulated annealing strategy in real space. The Pd(II) complex crystallizes in the triclinic system with space group P-1 and cell parameters a = 4.6493(4) Å, b = 5.222(4) Å, c = 18.040(2) Å, α = 77.41(6)°, β = 94.72(7),° and γ = 101.45(7)°. The crystal structure confirms the presence of Pd(II) ions in a nearly square planar environment and the molecular formula with deprotonated citrulline as proposed by analytical and spectroscopic data.

The X-ray powder pattern of the Pb-free 110 K superconductor phase Bi2Sr2Ca2Cu3Oz has many lines which belong to an incommensurate supercell. Using electron diffraction photographs as a guide, an indexing scheme for the powder pattern has been obtained. The unit cell has a geometrically orthorhombic subcell a = 5.411 (2), b = 5.420(2), c = 37.29(2) Å. Supercell reflections have indices that are derived from the subcell k, l indices by addition of ± q, where q = nδb + nεc: n = 1,2 …; ε = 0.211(2); ε = −0.78(1).

The change in the orthorhombic structure of PbZrO3 was studied as a function of the La substitution for Pb and Ti substitution for Zr. Two types of changes can occur: (1) a change in the atom coordinates toward the positions for a perfect cubic perovskite lattice; and (2) a change of orthorhombic unit cell parameters so that ao, bo, and co exactly fit with the cubic cell parameter ac. Therefore, ao=ac√2, bo=ac.2√2, and co=ac.2, where ao, bo, and co are the orthorhombic cell parameters, and ac is the cubic cell parameter. Substitution of Pb by La in the orthorhombic PLZT leads to both a change in atom coordinates and a change in unit cell parameters toward the perfect cubic structure, especially for La≥4. Substitution of Zr by Ti in the orthorhombic PLZT leads to similar atom coordinate changes, but the unit cell parameters do not change. The composition 0/92.5/7.5 contains a major tetragonal phase and a minor orthorhombic phase. There are only small differences in the orthorhombic structure between the A and the B composition of PLZT. The A composition has a structure closer to the cubic structure than the B composition.

Coatings of plasma sprayed hydroxyapatite (HAp), incubated in simulated body fluid for periods varying from 1 to 56 days, were characterized using conventional laboratory X rays. Quantitative phase analysis, employing TOPAS software, showed an opposite trend in the two main phases of the coating, viz., HAp and tetracalcium phosphate (TTCP). The former increased within the first 7 days of incubation whilst the latter decreased during the same period; both phases stabilized with further incubation. The crystallinity of the coatings exhibited a trend similar to that of HAp i.e., an increase in the early stages of incubation stabilization with further incubation. Results of residual stress determined with Bruker’s D8 Discover and analyzed with LEPTOS software, showed both the normal stress tensor components, σ11 and σ22, to be tensile, relaxing significantly in the early stages of incubation before stabilizing with further incubation.

A series of LiFe1−xZnxPO4 (0.0 ≤ x ≤ 1.0) compounds were prepared by solid-state reaction. Effects of the substitution of Zn for Fe on crystal structure and electrochemical properties of LiFe1−xZnxPO4 were investigated. The results show that single-phase regions of LiFe1−xZnxPO4 with orthorhombic (space group Pmna) and monoclinic (Cc) structures were found for the compounds with low Zn (or high Fe) contents of 0.0 ≤ x ≤ 0.30 and high Zn (or low Fe) contents of 0.90 ≤ x ≤ 1.0, respectively. The LiFe1−xZnxPO4 compounds with medium Zn (or Fe) contents of 0.35 ≤ x ≤ 0.80 are two-phase mixtures containing both the orthorhombic and the monoclinic phases. Systematic variations of unit-cell parameters a, b, c, and volume V with the Zn content determined by X-ray diffraction have also been obtained. Our electrochemical study show that the conductivity of LiFe1−xZnxPO4 increases by almost 2 orders of magnitude from 2.13 × 10−9 to 1.27 × 10−7 Scm−1 as the Zn content increasing from x = 0 to 0.3. The initial specific capacity decreases and the cycle performance increase with increasing Zn-doping content in the four orthorhombic LiFe1−xZnxPO4 compounds. Among the four LiFe1−xZnxPO4 compounds, LiFe0.8Zn0.2PO4 has the highest capacity retentions after 6 to 20 cycles and the capacity retention is 93.7% after 20 cycles, even though the initial discharge specific capacity of LiFe0.8Zn0.2PO4 is lower than those of LiFeZnPO4 and LiFe0.9Zn0.1PO4. LiFe0.7Zn0.3PO4 has the highest capacity retention of 97% after 20 cycles.

Ceramics of Sr2CaFe2WO9 and Sr2PbFe2TeO9 double perovskites have been prepared in polycrystalline form by solid-state technique, in the air. The crystalline structure was analyzed using X-ray powder diffraction (XRPD) at room temperature. Rietveld analysis of XRPD patterns show that both compounds adopt a tetragonal structure with space group I4/m, with unit cell parameters a = 5.5453(1) Å, c = 7.8389(1) Å for Sr2CaFe2WO9, and a = 5.5994(15) Å, c = 7.8979(30) Å for Sr2PbFe2TeO9. A certain degree of anti-site disordering of W and/or Te and Fe on the B –sites have been detected, indicating the presence of a partial amount of W and/or Te at Fe positions and vice versa.

The synthesis at 850 °C and the structural characterization of the elpasolite structure compound Cs2NaCeCl6 is reported space group Fm3m, a = 10.943(2) Å, V = 1310.4 (Å)3, Z = 4, M = 641.64, Dx = 3.252, and Dexp = 3.21. Powder diffraction data from a Rietveld structure refinement, are reported.

LiCu2O2 crystals grown by spontaneous crystallization from the fluxed melt were studied by powder X-ray diffraction. The phase analysis shows that the applied growth conditions are suitable for preparation of a single-phase compound. The as-grown crystals contain only traces of foreign phases (Li2CuO2, CuO, Cu2O) typical for preparation of the LiCu2O2 compound. Attempts to anneal or quench the as-grown crystals led to two-phase samples containing LiCu2O2 and LiCu3O3. X-ray powder diffraction pattern of a LiCu2O2 crystal is reported and compared with literature data. The crystal structure is orthorhombic, space group Pnma, in agreement with literature data. Lattice parameters of the studied sample are a=5.7286(2) Å, b=2.8588(1) Å, and c=12.4143(3) Å. Time evolution of a diffraction pattern illustrates a slow increase of the secondary-phases contribution assumed to be due to interaction of the powdered crystal with humid air. A brief summary of compounds known in the Li–Cu–O system is included

Indexed X-ray powder diffraction data are reported for two energetic materials, oxalylhydroxamic acid and 2-diazo-4, 6-dinitrophenol (DDNP). For these two compounds, powder diffraction data calculated from single-crystal structure determinations are also presented and compared to the experimentally observed powder diffraction data. To evaluate the reliability of the experimentally obtained intensities, an intensity figure of merit, IX(N), based on an average percent difference between observed and calculated intensities for a limited number of strong and moderately-strong lines is proposed as a more useful measure of agreement than R1. For N lines with Icalc > X% relative intensity, IX(N) is defined as

This is compared to

which involves a summation over all lines.

A new variety of ammonium lanthanum sulfate, β-(NH4)La(SO4)2, was synthesized hydrothermally. The crystal structure was solved ab initio from powder diffraction data collected using a conventional X-ray source. The powder diffraction pattern was indexed by the successive dichotomy method: The symmetry is monoclinic, space group Pn, cell dimensions a=6.9365(4) Å, b=9.0055(5) Å, c=5.4541(4) Å, β=90.672(8)°, V=340.68(3) Å3 and Z=2 [M20=65, F30=124(0.0071,34)]. Direct methods were used for structure solution, and refinement of the atomic coordinates was carried out by the Rietveld method (RF=0.061, Rwp=0.099). The structure contains anionic layers built from lanthanum atoms ninefold coordinated to monodentate and bidentate sulfate oxygen atoms. Ammonium groups, which provide hydrogen bonds, are located between the layers. The crystal structure contrasts with that of the α phase, which is less dense by a factor of 4.4%.

Synthetic analogues of the minerals natisite and for the first time of paranatisite were prepared hydrothermally at 200 °C in the system Na2O–TiO2–SiO2–H2O. The obtained powder x-ray diffraction (XRD) patterns were interpreted by the Powder Data Interpretation (PDI) software package. As a result improved indexing and unit cell parameters refinements of these two phases were achieved. Synthetic natisite is tetragonal, space group—P4/nmm, a=0.649 67(8) nm, c=0.508 45(11) nm, V=0.214 50(10) nm3, Z=2, Dcal=3.13 g.cm−1, F30=37.48, M20=52.79. Synthetic paranatisite is orthorhombic, space group—Pmma, a=0.983 86(29) nm, b=0.919 23(19) nm, c=0.481 84(12) nm, V=0.435 78(19) nm3, Z=1, Dcal=3.01 g.cm−1, F30=16.42, M20=29.21.

A new Matlab-based software suite called Tilt-A-Whirl has been applied to XRD data from textured gold films electro-deposited onto nickel substrates. The software routines facilitate phase identification, texture analysis via pole figure visualization, and macrostrain determination. The use of principal component analysis with multivariate curve resolution (PCA/MCR) revealed the extraction of texture components. The unusual hardness properties of one Au film (deposited from a 30% gold depleted BDT-200 bath) were found to be dependent on the (210) out-of-plane preferred orientation of the polycrystalline gold film. The progressive nucleation of Au crystallites during electro-plating has been tied to improved hardness properties of this film.