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Aluminum borate (9Al2O3·2B2O3) whiskers were chemically synthesized in potassium sulphate flux by using the starting chemicals of aluminum sulphate and boric acid. The synthesis temperature of 1075 °C was found to be the optimum with respect to whisker morphology. A tentative X-ray diffraction (XRD) pattern was suggested for the whiskers produced after heating at 1150 °C. The product purity, phase composition, and whisker morphology were investigated by XRD, energy dispersive X-ray spectroscopy, and scanning electron microscopy, respectively.
In recent years, grazing incidence angle attachments have been shown to be very useful in the phase identification of thin polycrystalline films. These devices are sold commercially as attachments to standard powder diffractometers. The attachment normally consists of a long soller slit assembly and a flat crystal monochromator. The soller slit with or without the monochromator is mounted on the diffracted beam side. In this paper we discuss the effects of different configurations from collimator to monochromator on diffraction data. An understanding of these effects is essential in order to obtain more reliable information on phase transformations, crystallite size, microstrain, and residual stress studies.
A more accurate X-ray diffraction pattern for the high speed steel carbide Fe3W3C is presented. This pattern includes the low angle reflections omitted from previous studies. A wider homogeneity range for the M6C carbide phase at 1200° C is suggested.
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
A chemical and mineralogical investigation of a Moroccan pyrophyllite is presented. X-ray powder diffraction has been largely used for phase identification and crystal symmetry determination. It is shown that this mineral has a triclinic symmetry with cell parameters: a=5.160 Å, b=8.993 Å, c=9.360 Å, α=90.77°, β=100.57°, and γ=89.71°.
X-ray powder diffraction data for clemizole hydrochloride (1-p-chlorob-enzyl-2-pyrrolidin-1′-ylmethyl-benziminazole hydrochloride, C19H20ClN3.HCl) and cyclizine hydrochloride (1-benzhydryl-4-methylpiperazine hydrochloride, C18H22N2.HCl) are reported. Crystals of clemizole hydrochloride are monoclinic, space group P21/n with a = 29.940(5) Å, b = 10.963(2)Å, c = 5.515(2)Å, β = 90.98 (3)°, Z = 4 and Dx = 1.330g cm−3. Crystals of cyclizine hydrochloride are orthorhombic, space group Pna21 (or Pnam), with a = 11.816(1)Å, b = 13.609(2)Å, c = 9.999(1 )Å, Z = 4 and Dx = 1.251g cm−3.
Rietveld analysis of X-ray powder diffraction data was performed on SmBa4Cu3O8.5+δ, which was synthesized from precursors Sm2O3, BaO2, and CuO at 1000 °C in an oxygen atmosphere. SmBa4Cu3O8.5+δ has a cubic perovskite-related structure that is isostructural with YBa4Cu3O8.5+δ, and a doubled perovskite unit cell parameter of 8.177 90±0.000 04 Å.
A new occurrence of the poorly characterized mineral, yukonite, (Ca6.44K0.13Mg0.23)(Fe14.68Al0.36)(AsO4)9O15.78·25.5H2O, is described. New powder X-ray diffraction and electron microprobe data are provided for type material from Tagish Lake, Yukon Territory, Canada, and that from the new locality, Saalfield, Thuringen, Germany. New chemical formulae are proposed. The strongest reflections are at 14.1(100), 2.79(60), 3.25(57), 5.58(37), 2.61(20), 1.63(20), and 2.24(11) Å.
Cadmium hydroxide nitrate dihydrate, Cd5(OH)8(NO3)2·2H2O, and zinc hydroxide nitrate diammoniac, Zn5(OH)8(NO3)2·2NH3, have been investigated by means of X-ray powder diffraction. Their unit cell dimensions were found by an indexing program and confirmed by single crystal studies. Precise data collected with strictly monochromatic radiation are reported. The figures of merit are F30=118 (0.0071,36) for the cadmium compound and F30=53 (0.015,38) for the zinc compound. A short discussion of the unit cell parameters compared to those of a related zinc hydroxide nitrate dihydrate is presented.
The subsolidus phase relations in the ternary system La2O3–Bi2O3–CuO at 900 °C were investigated by X-ray powder diffraction. A new binary compound, Bi2La4O9, was found, as well as a binary and a ternary solid solution series, Bi1−xLaxO1.5 (0.16≤x≤0.33) and La2−xBixCuO4 (0≤x≤0.11), respectively.