Polymethylsilane (PMS) modified with titanium chloride (TiCl
4) or molybdenum chloride (MoCl
5) was pyrolyzed at various temperatures to enable a detailed investigation of stable phases formed during pyrolysis. The existence of TiSi
2 in PMS-TiCl
4 precursor and β-MoSi
2 in the PMS-MoCl
5 precursor below 1273 K suggested a strong interaction between Si-H and the metal chlorides during mixing. During pyrolysis of the PMS-10 mass% TiCl
4 precursor, a silicon rich Si-Ti-C state was obtained below 973 K, which simultaneously formed crystalline Si, TiSi
2, and SiC phases at relatively low temperatures below 1273 K. During pyrolysis of the PMS-MoCl
5 precursors, however, formation of crystalline Si and SiC phases were not accelerated, while the crystalline β-MoSi
2 or α-MoSi
2 phase was formed rapidly.
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