Search results for "POWDER"

“Ab-initio” structure solution of nano-crystalline minerals and synthetic materials by automated electron tomography

2012

Most of the newly discovered mineral phases, as well as many new synthesized industrial materials, appear only in the form of nano crystals, with a size not sufficient for single-crystal x-ray structure analysis. The development of techniques able to investigate the structure of nano crystalline materials is therefore one of the most important frontiers of crystallography. The most widespread technique providing relatively fast and well consolidated routes for structure analysis of bulk materials is x-ray powder diffraction (XRPD). Nevertheless, XRPD suffers from intrinsic 1-dimension reduction of information that greatly limits its applicability in presence of peak broadening and overlappi…

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…

Effects of Thermal Treatment on the Structure of Eu:YAG Nanopowder

2007

Eu:YAG nanopowder precursors were obtained by co-precipitation of aluminium, yttrium and europium nitrates solution with ammonia. The hydroxides precursors were calcined at different temperatures from 900 to 1200°C as a function of holding time (1, 2 and 6 hours). The presence of Eu3+ ions in the matrix was confirmed by Energy Dispersive X-rays analysis. X-Ray Diffraction investigation by the Rietveld method shows that the sample treated at 900°C for 1 hour is essentially the garnet phase with the minor presence of hexagonal and monoclinic metastable phases. The Eu3+ ions are incorporated into the garnet phase, as is suggested by the lattice parameter value being larger than that in literat…

From nanostructured powders to dense nanostructured materials: Mechanically activated powder metallurgy

2003

Mechanical Activation as a New Method for SHS

2006

The use of mechanical activation (the elemental powder mixture is milled for a short time at given frequency and impact energy) as a precursor to self-propagating high-temperature synthesis (SHS) results in the formation of nanostructured porous materials. The mechanical activation step was found necessary (i) to modify the thermal parameters of the combustion front (i.e. combustion front velocity, thermal heating rate…) in the cases of Mo-Si, Fe-Al, Ni-Si (ii) to initiate a combustion front in the case of systems having a low exothermicity. Nevertheless, the control of the mechanically activated mixture characteristics and, the understanding of the mechanical activation role on the SHS par…