Vinyltri(phenylethynyl)silane ((ph-C:C) 3 -Si-C=CH 2 ; VTPES) and phenyltri(phenylethynyl)silane ((ph-C:C) 3 -Si-ph; PTPES) were synthesized by Grignard reaction. Their molecular structures were characterized by means of 1 H NMR, 13 C NMR, 29 Si NMR, and FT-IR spectroscopy. Their nonisothermal thermal curing processes were characterized by DSC, and the corresponding kinetic data, for example activation energy (E), pre-exponential factor (A), and the order of the reaction (n), were obtained by the Kissinger method. The results showed that the melting points of VTPES and PTPES were 84 and 116°C, respectively. Their curing reaction rates were consistent with first-order kinetic equations. VTPES monomer had a lower activation energy and curing temperature as a result of coordination between reactive groups.