Crystalline microstructure of sepiolite influenced by grinding

Abstract

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 each sample by modelling a selected part of the X-ray diffraction pattern and fitting the simulated pattern to a measured one. A strict correlation of microstructure parameters with grinding time and with specific surface magnitudes was observed. A parallelepiped with edge-length ratios almost independent of grinding time (for longer times) was found to be the predominant crystallite shape. The crystallite size distributions were found to be close to logarithmic normal ones, with the mean values decreasing with increasing grinding time and the standard-deviation-to-mean-value ratios approximately constant. The second-order crystalline lattice strain distributions were found to be close to some simple function with the mean value equal to zero, the mean deviation increasing with increasing grinding time and the standard-to-mean-deviation ratios approximately constant. It was demonstrated that the specific surface can be calculated on the basis of the microstructure characteristics. Some details of the relation between crystallites and crystalline grains were explained by comparing the results of analysesviaX-ray diffraction and scanning electron microscopy.