Room temperature crystalline structures of La2-xSrxCuO4 samples with uncommonly high hole concentrations (p) up to p=0.4, annealed under 1 and 100 bars of oxygen pressure have been analyzed by X-ray diffraction. Results show that the x=0 sample with p=0.09 and superconducting below 20K is orthorhombic at room temperature. The orthorhombic distortion at 300K decreases with increasing x and becomes tetragonal when x reaches 0.08. This orthorhombic-to-tetragonal phase transformation is consistent with previous work. Samples with x≥0.28 and p≥0.31 remain tetragonal but are nonsuperconducting down to 5K. Lattice dimension anomalies have also been observed and are correlated with the sudden appearance of oxygen vacancies, as seen by the hole concentration measurements. Initially, the value of the lattice dimension a decreases and c increases monotonically with increasing x. A sudden increase in a and decrease in c begins when x reaches 0.28 for samples prepared under 1 bar of oxygen indicating a sudden loss of oxygen from the structure. This sudden reversal in lattice dimensions a and c is not present in samples annealed under 100 bars of oxygen pressure suggesting essentially no oxygen vacancies. The increase in c with x of the La2-xSrxCuO4 samples with no oxygen vacancies can be attributed mainly to the result of substituting smaller La+3 ions by larger Sr+2 ions. A study of the variation of c with the hole concentration reveals that the c lattice dimension drops sharply with no change in the hole concentration when oxygen is continuously removed from the lattice caused by an increase of the Sr content in La2-xSrxCuO4.

A new method for the quantification of montmorillonite by full-profile Rietveld analysis of the XRD profile is presented. A measured standard XRD pattern of Algerian bentonite was used to construct a universally applicable montmorillonite (hkl) file for use with a P.C. based Rietveld XRD quantitative analysis system, SIROQUANT. “Universal” means that the standard file can be used for montmorillonites from other localities. The validity of the montmorillonite standard profile was tested with weighed mixtures of quartz and different standard montmorillonites. The results show the montmorillonite observed (hkl) file is generally applicable (i.e., universal), and can be used to quantify montmorillonite in any mineral without modification or chemical treatment of the sample. Two halfwidth functions were used for the montmorillonite, corresponding to the sharp (hk0) and broad (hkl) classes of reflections. A March preferred orientation parameter for montmorillonite was also refined.

A new quantitative X-ray powder diffraction (QXRPD) method has been developed to analyze polyphase crystalline mixtures. The unique approach employed in this method is the utilization of the full diffraction pattern of a mixture and its reconstruction as a weighted sum of diffraction patterns of the component phases. To facilitate the use of the new method, menu-driven interactive computer programs with graphics have been developed for the VAX series of computers. The analyst builds a reference database of component diffraction patterns, corrects the patterns for background effects, and determines the appropriate reference intensity ratios. This database is used to calculate the weight fraction of each phase in a mixture by fitting its diffraction pattern with a least-squares best-fit weighted sum of selected database reference patterns.

The new QXRPD method was evaluated using oxides found in ceramics, corrosion products, and other materials encountered in the laboratory. Experimental procedures have been developed for sample preparation and data collection for reference samples and unknowns. Prepared mixtures have been used to demonstrate the very good results that can be obtained with this method.

A comparison of X-ray powder diffraction and electron probe microanalyses on samples of Na- and K-doped Bi4V2O11 (BIMEVOX) solid electrolytes indicates some of the problems associated with using XRD to assess phase purity, especially in materials of variable composition such as BIMEVOXes. In this study both the Na- and K-doped materials appeared phase pure by XRD. EPMA indicated the Na-doped materials to be single phase with their expected compositions while the K-containing materials were not phase pure with very little K present in the main BIMEVOX phase.

An environmentally controlled sample stage for Scintag's six-position XRD sample changer is described. Unlike the commercial environmental stages for Scintag XRD units which require removal of the sample changer, and installation and alignment of the sample stage, the stage described herein is designed to fit directly on the sample changer with no realignment. Such a stage provides for more convenient operation for an X-ray diffractometer with multiple users in both routine (ambient environment) and nonroutine (nonambient temperatures up to 250 °C and varying relative humidities) modes. In addition, the new stage uses a window made of a material that is safer to machine compared to beryllium (which is toxic).

Synthesis and unit cell parameter refinement of 25 ferroelectric compounds with the tungsten bronze structure are reported. A general chemical formula for these compounds is (A1, A2, C) B10 O30, where specifically A1 and A2 = K, Na, Ba, Sr, Pb, La, Eu, Sm, Y, Bi; C = Li; and B = Nb, Ta, Ti, W. All compounds were prepared by solid state sintering at temperatures ranging from 1100°C to 1380°C. Refined cell parameters (tetragonal with space group P4bm[100]), I/Icor values, calculated densities and Z values are included for the 25 compounds.

Observed powder diffraction data for two tetracyclines were interpreted with the aid of calculated patterns based upon the crystal structures determined from a single crystal of the same batch for each compound. The results consist of high quality standard powder patterns with the usual supporting data.

The “hook effect” observed in the Warren-Averbach analysis of X-ray diffraction peaks from multiple layer thin films of copper has been investigated theoretically and experimentally. The strengths of the “hook effect” for films of different layer thicknesses were analyzed. The results showed definite correlation between the strengths of the “hook effect” and the grain size distributions in 1, 4, and 19-layer copper films.