Crystal structure and microstructure of synthetic hexagonal magnesium–cobalt cordierite solid solutions (Mg2−2xCo2xAl4Si5O18)

Co2+-containing cordierite glasses, of nominal compositions (Mg1−xCox)2Al4Si5O18(withx= 0, 0.2, 0.4, 0.6, 0.8 and 1), were prepared by melting colloidal gel precursors. After isothermal heating at 1273 K for around 28 h, a single-phase α-cordierite (high-temperature hexagonal polymorph) was synthesized. All materials were investigated using X-ray powder diffraction and field-emission scanning electron microscopy. The crystal structure and microstructure were determined from X-ray diffraction patterns. Rietveld refinement confirmed the formation of magnesium–cobalt cordierite solid solutions. The unit-cell volume increased with the increase of cobalt content in the starting glass. The crysta…

Microstructural evolution of mullites produced from single-phase gels

The crystalline microstructure of mullites obtained by heating monophasic gels has been investigated. Gels with alumina to silica molar ratio of 3:2 (as in secondary mullite) and 2:1 (as in primary mullite) were prepared by gelling mixtures of aluminium nitrate and tetraethylorthosilicate. Phase transformations were induced by heating the gel precursors, with different final treatment temperatures between 1173 and 1873 K. The mullites formed as a result of thermal treatment were studied by means of X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The crystalline structure (unit-cell parameters) and microstructure were determined from X-ray diffraction pa…

X-ray diffraction microstructure analysis of mullite, quartz and corundum in porcelain insulators

Abstract The X-ray diffraction microstructure analysis has been performed on commercial samples of the silica and alumina porcelain insulators obtained at 1300 °C, with the same time of firing. The study was carried out on mullite, corundum and quartz by applying several integral breadth methods (i.e. the Williamson–Hall analysis, the Langford method and the Halder–Wagner approximation) and the Fourier analysis (Warren–Averbach method). The apparent crystallite sizes determined for the mullite are direction-dependent (anisotropic) and within each group of samples, on average, the greatest values are obtained along the direction [0 0 1]. With regard to the microstructure of the corundum and …

X-ray diffraction line broadening on vibrating dry-milled Two Crows sepiolite

A reference sample of sepiolite and products of its comminution by vibrating dry-milling have been studied using X-ray diffraction (XRD) line-broadening analysis, complementary field emission scanning electron microscopy (FESEM) images and surface area measurements. The apparent crystallite sizes determined via XRD are in agreement with observations on FESEM images. The sepiolite aggregates consist of lath-shaped agglutinations of prisms and pinacoids elongated along [001], each lath including several crystallites in that direction. The surface area magnitudes are in the range of previous experimental measurements of other sepiolites. The results obtained show the effectiveness of vibro-mil…

Crystalline microstructure of sepiolite influenced by grinding

The crystalline microstructure of ground sepiolite has been investigated. A reference sample of sepiolite and products of its comminution by dry grinding were studied through X-ray diffraction pattern analysis, specific surface measurements by nitrogen adsorption and complementary analysis of field emission scanning electron microscope images. A statistical model of polycrystals was applied to describe and determine the crystalline microstructure of the studied specimens. The model parameters characterizing the microstructure were prevalent crystallite shape, volume-weighted crystallite size distribution and second-order crystalline lattice strain distribution, and they were determined for …

X-ray diffraction line-broadening study on two vibrating, dry-milling procedures in kaolinites

Due to the great technological importance of the microstructure of kaolinite, characterizing its evolution during dry milling of kaolin and analyzing the microstructural information obtained from different methods were the main aims of this work. The microstructural alteration of kaolinite is evaluated by X-ray diffraction and electron microscopy methods, comparing the results obtained and analyzing the correlations between them. The Warren-Averbach and Voigt-function methods of X-ray diffraction microstructural analysis have been applied successfully to the study of the effects of two different, vibrating-cup dry-milling configurations in the microstructure of kaolinite from the reflection…

X-ray diffraction Warren–Averbach mullite analysis in whiteware porcelains: influence of kaolin raw material

ABSTRACTCompositional and microstructural analysis of mullites in porcelain whitewares obtained by the firing of two blends of identical triaxial composition using a kaolin B consisting of ‘higher-crystallinity’ kaolinite or a finer halloysitic kaolin M of lower crystal order was performed. No significant changes in the average Al2O3 contents (near the stoichiometric composition 3:2) of the mullites were observed. Fast and slow firing at the same temperature using B or M kaolin yielded different mullite contents. The Warren–Averbach method showed increase of the D110 mullite crystallite size and crystallite size distributions with small shifts to greater values with increasing firing temper…

Crystalline Microstructure of Corundum Fillers Determined from Powder X-Ray Diffraction Patterns

Sizes and Shapes of Crystallites in Mullites Produced by Thermal Treatment of Kaolin - Alumina Mixture

Comparative X-ray diffraction study of the crystalline microstructure of tetragonal and monoclinic vanadium–zirconium dioxide solid solutions produced from gel precursors

The microstructural characteristics of solid solutions, prepared by heating dried gel precursors with nominal compositions VxZr1−xO2(0 ≤x≤ 0.1) at 723 and 1573 K, were determined from X-ray diffraction patterns. The crystalline microstructure of the resulting specimens, characterized by a prevalent crystallite shape, a volume-weighted crystallite size distribution and a second-order lattice strain distribution, was found to depend on the vanadium content. A characteristic feature of all size distributions was their bimodality, explained as a result of transformations between tetragonal and monoclinic phases during thermal treatment. A comparative study of the microstructure of both zirconia…

An X-ray powder diffraction study of the microstructural evolution on heating 3:2 and 2:1 mullite single-phase gels

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…

Crystalline microstructure of boehmites studied by multi-peak analysis of powder X-ray diffraction patterns

Nanocrystalline boehmite (gamma-aluminium-oxyhydroxide) is a material of industrial importance, the functionality of which follows from its crystalline microstructure. A procedure for preparing boehmite nanoparticles, comprising the formation of a precipitate by the alkalization of an aqueous solution of aluminium nitrate and subsequent hydrothermal aging, was previously elaborated. The application of an additive (maltitol or tartaric acid) to control the sizes and shapes of crystallites in the produced polycrystalline powder of boehmite was developed. The aim of this work is a study of the effect of the hydrothermal treatment time on nanocrystalline characteristics of boehmite, both in abs…

Solubility and microstructural development of TiO2-containing 3Al2O3·2SiO2 and 2Al2O3·SiO2 mullites obtained from single-phase gels

Abstract The interdependence of the titanium oxide amount and the anisotropic growth of mullites prepared from single-phase gels were investigated. Gels with stoichiometries 3(Al2−xTixO3)·2(SiO2) and 2(Al2−xTixO3)·(SiO2), with 0 ≤ x ≤ 0.15 were prepared by the semialkoxide method. Gels and specimens heated at temperatures between 1200 and 1600 °C were characterized by using infrared spectroscopy (IR), X-ray diffraction (XRD) and transmission and field emission scanning electron microscopies (TEM and FESEM). Al2TiO5 as minor impurity was detected in both series of mullites for gel precursor compositions x = 0.10 and x = 0.15, obtained at temperatures between 1200 and 1600 °C. Variations of l…