ZrSiO
4 fine powders were prepared from zirconium oxychloride (ZrOCl
2) and colloidal silica (SiO
2). Effects of the concentration of ZrOCl
2, calcination temperature, heating rate and size of secondary particles after hydrolysis on the preparation of ZrSiO
4 fine powders have been studied. The ZrSiO
4 precursors having Zr-O-Si bond were found in all the solutions after hydrolysis, and the formation rate of ZrSiO
4 was influenced significantly by the concentration of ZrOCl
2. Also the rate in the case of other concentrations than 0.4M was affected remarkably by heating rate, and there was a marked tendency for crystallization of ZrO
2 and SiO
2 to proceed preferentially and creation of ZrSiO
4 nucleus to be obstructed when the heating rate was slow. It is shown that ZrSiO
4 fine powders of the single phase were prepared at a relatively low temperature such as 1300°C by forming the ZrSiO
4 precursors having Zr-O-Si bond and by controlling the secondary particle size after hydrolysis.
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