Search results for "Powder diffraction"
showing 10 items of 243 documents
Effect of additives on the crystallization of cordierite-based glass-ceramics as glazes for floor tiles
2003
Abstract The effect of several additives such as fluxes and/or nucleants on a parent glass with composition located in the primary field of cordierite within the quaternary system CaO–MgO–Al 2 O 3 –SiO 2 has been examined. Crystallization path of glasses was determined by differential thermal analysis (DTA) and X-ray powder diffraction (XRD). Pressed pellets of powdered glasses containing different additives were submitted at thermal treatments up to 1200 °C. The microstructural development at several temperatures was followed by field emission scanning electron microscopy and energy-dispersive X-ray analysis. The results shown that additions of TiO 2 as nucleant and/or B 2 O 3 as flux to a…
Crystallization behaviour and microstructural development in ZrSiO 4 and V-ZrSiO 4 solid solutions from colloidal gels
2000
Abstract Zircon and vanadium-doped zircon blue pigments were prepared by heat treatment of gel precursors. Gels with nominal compositions Vx-ZrSiO4 with x=0.0, 0.002, 0.004, 0.02 and 0.2 were prepared by formation of a silica coating on zirconia colloidal particles previously obtained. The crystallization behavior and microstructural evolution were studied using X-ray powder diffraction (XRD), energy dispersive X-rays microanalysis (EDX), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and selected area electron diffraction (SAED). The results indicated that the vanadia loading in the precursor gels speeds up the crystallization of the vanadium-co…
Precursor-based synthetic pathways to nanometer NdNiO3−x particles
1993
Abstract The oxygen deficient neodymium nickel perovskite, NdNiO3−x, has been obtained by different low temperature-low oxygen pressure synthetic procedures. Besides a solid-matrix based route, both ordered and disordered chemical-precursors have been used as starting products. X-ray powder diffraction shows that the structure of this defective perovskite is orthorhombic. The study of the grain morphology of the products as resulting from the different synthetic procedures indicates that the main parameter determining the average particle size, which is in the nanometer range, is the maximum temperature achieved in the synthesis. Resistivity and DSC measurements show the existence of a meta…
Low-temperature Ti-containing 3:2 and 2:1 mullite nanocrystals from single-phase gels
2007
Abstract TiO 2 -containig single-phase gels with (Al 2 O 3 + TiO 2 )/(SiO 2 ) molar ratios 3/2 and 2/1 were prepared by gelling mixtures of aluminium nitrate, tetraethylorthosilicate and titanium isopropoxide. Gels were fast heated at several temperatures up to 1100 °C. Dried and heated gels were characterized by differential thermal analysis (DTA), magic angle spinning nuclear magnetic resonance (MAS-NMR), X-ray powder diffraction (XRD), and scanning and transmission electron microscopies (SEM and TEM). Coupled DTA and XRD results of gels fast heated at 900 °C showed the crystallisation of two mullites as well as a small amount of alumina-silica spinel. 27 Al NMR spectra showed the format…
An X-ray powder diffraction study of the microstructural evolution on heating 3:2 and 2:1 mullite single-phase gels
2006
Single-phase gels with compositions 3Al2O3·2SiO2 and 2Al2O3·SiO2 were prepared by gelling mixtures of aluminium nitrate and tetraethylorthosilicate. Gels were fast heated at different temperatures between 900°C and 1600°C. The phase transformation and microstructural changes of both mullite precursor gels over the temperature range were followed by X-ray powder diffraction (XRD), lattice parameter determination (LP), and scanning and transmission electron microscopies (SEM and TEM). The distribution of crystallite sizes and strains were determined by linewidth refinements of X-ray diffraction patterns using the integral breadth method of Langford and the Warren-Averbach analysis. XRD of bot…
Structure and properties of CoMnSb in the context of half-metallic ferromagnetism
2006
Although its X-ray powder diffraction patterns show a superstructure, the compound CoMnSb, like the well-known half-Heusler alloy NiMnSb, is often referred to the category of half-metallic ferromagnets with $C{1}_{b}$ structure. Our study assigns CoMnSb to space group $Fm\overline{3}m$. The crystal structure of CoMnSb can be represented as an alternation of ${\mathrm{Co}}_{2}\mathrm{Mn}\mathrm{Sb}$ and MnSb structural units, and, in contrast to NiMnSb, displays three Mn and two Sb positions in the elementary cell. The presence of nonequivalent antimony and manganese positions was verified using NMR and M\"ossbauer spectroscopic measurements. Band-structure calculations based on a proposed s…
Template-free synthesis and structural evolution of discrete hydroxycancrinite zeolite nanorods from high-concentration hydrogels.
2017
We report the synthesis and characterization of hydroxycancrinite zeolite nanorods by a simple hydrothermal treatment of aluminosilicate hydrogels at high concentrations of precursors without the use of structure-directing agents. Transmission electron microscopy (TEM) analysis reveals that cancrinite nanorods, with lengths of 200-800 nm and diameters of 30-50 nm, exhibit a hexagonal morphology and are elongated along the crystallographic c direction. The powder X-ray diffraction (PXRD), Fourier transform infrared (FT-IR) and TEM studies revealed sequential events of hydrogel formation, the formation of aggregated sodalite nuclei, the conversion of sodalite to cancrinite and finally the gro…
Electronic excitations in ZnWO4 and ZnxNi1−x WO4 (x = 0.1 − 0.9) using VUV synchrotron radiation
2011
The photoluminescence spectra and luminescence excitation spectra of pure microcrystalline and nano-sized ZnWO4 as well as the Zn x Ni1−x WO4 solid solutions were studied using vacuum ultraviolet (VUV) synchrotron radiation. The samples were also characterized by x-ray powder diffraction. We found that: (i) the shape of the photoluminescence band at 2.5 eV, being due to radiative electron transitions within the [WO6]6− anions, becomes modulated by the optical absorption of Ni2+ ions in the Zn x Ni1−x WO4 solid solutions; and (ii) no significant change in the excitation spectra of Zn0.9Ni0.1WO4 is observed compared to pure ZnWO4. At the same time, a shift of the excitonic bands to smaller en…
Total-scattering pair-distribution function of organic material from powder electron diffraction data.
2014
AbstractThis paper shows that pair-distribution function (PDF) analyses can be carried out on organic and organometallic compounds from powder electron diffraction data. Different experimental setups are demonstrated, including selected area electron diffraction and nanodiffraction in transmission electron microscopy or nanodiffraction in scanning transmission electron microscopy modes. The methods were demonstrated on organometallic complexes (chlorinated and unchlorinated copper phthalocyanine) and on purely organic compounds (quinacridone). The PDF curves from powder electron diffraction data, called ePDF, are in good agreement with PDF curves determined from X-ray powder data demonstrat…
Structure characterization of hard materials by precession electron diffraction and automatic diffraction tomography: 6H-SiC semiconductor and Ni1+xT…
2012
Using a combination of automated diffraction tomography and precession electron diffraction techniques, quasi-kinematical electron diffraction data sets were collected from intermetallic Ni1+xTe1 embedded nanodomains and ion-thinned specimens of 6H–SiC semiconductor. Cell parameters and space groups were found automatically from the reconstructed 3D diffraction volume. The extracted intensities were used for fast ab initio structure determination by direct methods.