Structural Analysis of Silicate Anions in Calcium Silicates by Trimethylsilylation Method
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概要
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In order to establish the availability of trimethylsilylation (TMS) method, which was applied to change of silicic acid groups having various structures in the formation process of calcium silicates. The results were compared with those of different techniques of X-ray diffraction and infrared spectroscopy.<BR>The calcium silicates were prepared by heating the mixture of Ca (OH) <SUB>2</SUB> and SiO<SUB>2</SUB>·nH<SUB>2</SUB>O of varying Ca/Si atomic ratios of 1/1, 3/2 and 2/1 at 400-1400°C for 3 hours. In the case of Ca/Si atomic ratio of 1/1, it was found from the results obtained by applying the TMS method to formation of low crystalline calcium silicates consisting in ranges of monomer to cyclic tetramer from temperature at 600°C and especially, to presence of Si<SUB>2</SUB>O<SUB>7</SUB><SUP>6-</SUP> ion due to Ca<SUB>3</SUB>Si<SUB>2</SUB>O<SUB>7</SUB> that did not identified by X-ray diffraction and infrared spectrum. It was confirmed that the heated product above 1100°C must be converted to p-CaSiO<SUB>3</SUB> having low temperature type at room temperature but was stabilized to α-CaSiO<SUB>3</SUB> (Ca<SUB>3</SUB>Si<SUB>3</SUB>O<SUB>9</SUB>) having high temperature type as trimer and existed together Si<SUB>2</SUB>O<SUB>7</SUB><SUP>6-</SUP> ion and SiO<SUB>4</SUB><SUP>4-</SUP> ion due to β-Ca<SUB>2</SUB>SiO<SUB>4</SUB>. In the formation process of Ca/Si atomic ratio of 2/1, the heated product showed the formation of monomer to cyclic tetramer at temperature above 600°C but finally changed to SiO<SUB>4</SUB><SUP>4-</SUP> ion. The above results obtained by Lentz's method were partially compared with those of Masson's method.
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