Abstract: | A novel high‐resolution thermogravimetry (TG) technique in a variable heating rate mode that maximizes resolution and minimizes the time required for TG experiments has been performed for evaluating the thermal degradation and its kinetics of Kevlar fiber in the temperature range ∼ 25–900°C. The degradation of Kevlar in nitrogen or air occurs in one step. The decomposition rate and char yield at 900°C are higher in air than in nitrogen, but the degradation temperature is higher in nitrogen than in air. The initial degradation temperature and maximal degradation rate for Kevlar are 520°C and 8.2%/min in air and 530°C and 3.5%/min in nitrogen. The different techniques for calculating the kinetic parameters are compared. The respective activation energy, order, and natural logarithm of preexponential factor of the degradation of Kevlar are achieved at average values of 133 kJ/mol (or 154 kJ/mol), 0.7 (or 1.1), and 16 min−1 (or 20 min−1) in air (or nitrogen). The technique based on the principle that the maximum weight loss rate is observed at the minimum heating rate gives thermal degradation results that were in excellent agreement with values determined by traditional TG experiments. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 71: 565–571, 1999 |