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Diphenyldiphenylethynylsilane monomer (DPDPES) was synthesized with ethyl bromide, diphenyldichlorosilane and phenylacetylene by Grignard reaction. The molecular structure was characterized by FTIR and ¹H-NMR spectroscopy. The polymer of polydiphenyl(diphenylethynyl)silane (PDPDPES) was also prepared by thermal polymerization. Non-isothermal thermal decomposition process of PDPDPES was studied with TG-DTG technology <i>via</i> model method to get thermal decomposition function and the corresponding mechanism which was further verified by model-free method. Results show that the apparent activation energy and the pre-exponential factor are about <i>E</i><i>_a</i>=245.37kJ/mol and lg<i>A</i>=13.78s^-1 obtained by six different kinetic methods, respectively. The mechanism of functions are <i>f</i>(<i>α</i>)= 10/23 &#183;(1-<i>α</i>)&#183;[-ln(1-<i>α</i>)]^-1.3 and <i>g</i>(<i>α</i>)=[-ln(1-<i>α</i>)]^2.3。