Abstract Si‐containing mono‐ and disubstituted polyacetylenes([CMeC(SiMe 3 )] n , [CHČH( n C 5 H 11 )SiMe 3 ] n , etc.) underwent degradation in air; many of them exhibited relatively high yields of main‐chain scission ( G s > 1). The G s values for the polymers having a long n ‐alkyl group were usually large (ca. 2). In contrast, no polymer degradation occurred in vacuum, indicating that oxygen is necessary for the radiolysis. The polymers irradiated in air contained CO and SiO groups, and dissolved in polar solvents, which are nonsolvents of the starting polymers. From the radiation sensitivity and thermal degradability of these polymers, it is concluded that disubstituted polymers with high Si contents ([CMeC(SiMe 3 )] n , [CMeC(SiMe 2 CH 2 SiMe 3 )] n , etc.) are not only radiation‐sensitive but also thermally stable.
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