Abstract
Phosphate-containing silicate materials prepared using sol–gel method from Si(OC2H5) were investigated at the variation of the amount of phosphate modifier from 5 to 50 wt% in term of P2O5. Chemical composition, textural and structural properties of these materials were characterized by FTIR-spectroscopy, TEM, X-ray diffraction and nitrogen adsorption. It was shown that the materials posse monomodal pore size distribution of 5–20 nm for the samples dried at 100 °C and 40–60 nm for the specimens calcined at 600 °C. The mean pore size and surface area depended on the amount of phosphoric acid. Before the stage of high temperature treatment phosphoric acid, introduced into the structure of the materials as a modifying agent, was uniformly distributed inside a porous space of the material and was not chemically bonded with silicate. After high temperature treatment both chemical interaction of silicate with phosphate, providing the formation of silicate-phosphate structures, as well as redistribution of free modifier from the bulk of granules to their surface took place. The polyphosphate layer is formed on the material surface closing the internal porous space. However, in this case a part of the phosphate modifier remains chemically unbound to SiO2 structure.
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Acknowledgments
This work was supported by the Federal Program “Scientific and scientific-educational professional community of innovated Russia in 2009–2013”, was partially supported by the Grant of the Ministry for Education and Science of the Russian Federation (contract No. 13.G36.31.0001 dated 07.09.2010), and was financially supported by the Federal target program «Studies and Development of Russia’s Scientific and Technological Priorities for 2007–2013».
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Epiphanova, A., Magaev, O. & Vodyankina, O. Formation and characterization of phosphate-modified silicate materials derived from sol–gel process. J Sol-Gel Sci Technol 61, 509–517 (2012). https://doi.org/10.1007/s10971-011-2652-z
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DOI: https://doi.org/10.1007/s10971-011-2652-z