Methyl-di(m-ethynylphenyl-amino)silane (MEAS) is a new kind of silazane with ethynylphenyl groups in the end of the molecule. The studies about the curing reaction kinetics and curing reaction mechanism are important for its application and performance. In this article, differential scanning calorimeter was used to study the curing reaction kinetics of MEAS. The results showed that both of the apparent activation energy (E_a) and the reaction order (n) that were evaluated with the method of Kissinger (113.4 kJ/mol, 0.93) agreed well with those using the method of Ozawa (116.1 kJ/mol, 0.95). According to structural changes during curing characterized using Fourier-transform infrared spectra, it was inferred that MEAS resin underwent the main four kinds of cross-linking reaction under the condition of heating. Thermogravimetric analysis was used to characterize the heat-resistance of MEAS thermoset. The results showed that the temperature of 5% weight loss based on the initial weight (T_d5) of the thermoset was 632.4°C and the residue yield at 900°C was 86.4% in nitrogen. The thermoset sintered at 1450°C in argon transformed into a ceramic with yield of 71%, which was studied by scanning electron microscopy and X-ray diffraction. The sintered products were smooth and hard solid and its chemical composition was made up of β-SiC, α-Si₃N₄ ceramic and free carbon. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012