Structure studies were performed on nanocrystalline powder of MgO xerogel prepared by the sol-gel technique, producing high purity, chemically homogeneous materials of relatively high specific surface area. Magnesium methoxide was used as an MgO precursor. The wet gel was dried under conventional conditions, yielding xerogel with periclase phase; the only crystalline form of magnesium oxide. The X-ray diffraction, scanning and transmission electron microcopies were used as the tools of structure analysis. The Toraya PRO-FIT procedure and the Rietveld refinement method were applied for X-ray data analysis. Both techniques apply the Pearson VII function for the description of line profiles. The gamma crystallite size distribution was determined using the FW(1/5)/(4/5)M method proposed by Pielaszek. The obtained values of and ? (measure of polydispersity) of particle size parameters are equal to 7.1 nm and 2.1 nm, respectively, whereas the average crystallite size, estimated by the Williamson- Hall procedure, was equal to 7.5 nm. The Rwp, and S fitting parameters obtained from the Rietveld refinement were equal to 6.4% and 1.8, respectively. This would seem the most satisfactory result, when considering the nanosize of MgO crystallites and a very probable presence of amorphous phase.
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