Differential scanning calorimetry, Fourier transform infrared (FTIR) spectroscopy, and C-13-NMR were used to characterize the Curing kinetics and structural changes of a copolymer of di[(N-m-acetenylphenyl) phthalimide] ether (DAIE) and [(methyl) diphenylacetylene] silane (MDPES). The results show that the apparent activation energy (E) and reaction order (n) calculated according to the Kissinger method were nearly the same as those calculated according to the Ozawa method. F was 160.4 kJ/mol and n was 0.96 with the Kissinger method, and E was 1.58.1 kJ/mol and n was 0.95 with the Ozawa method. The FTIR and solid-state C-13-NMR results also indicate that with increasing curing temperature, the peaks assigned to Si-H and C C bonded to phenylene carbons decreased, broadened, and finally vanished, whereas the peaks assigned to the C=C carbons and phenyl carbons increased and broadened. Crosslinking reactions in the curing of the DAIE/MDPES copolymer were possible due to the hydrosilylation reaction and the Diels-Alder reaction. (c) 2006 Wiley Periodicals, Inc.