Effect of isothermal aging on post‐imidization and glass transition temperature of LaRC‐IA polyimide resin

Abstract The isothermal aging of partilly imidized NASA Langley Research Center, LaRC‐IA polymide resin containing 70 wt% N‐methyl pyrrolidone, NMP was performed in a vacuum oven at 65, 95, 135, 165 and 200°C for 0.5, 1.0, 1.5 and 2 h. The weight loss and chemical changes that occurred during aging was determined gravimetrically and by FTIR spectroscopy, respectively. The imide absorption peak at 1778 cm⁻¹, increased in intensity as the aging temperature was increased from 65 to 200°C. The expulsion of NMP (70 wt%) was completed after ∼2.5 h of aging at 135°C. Additional weight loss ≤4 wt%, after the expulsion of NMP, was attributed to post‐imidization. The imide carbonyl peak absorption at 1721 and 1778 cm⁻¹, respectively, were broadened after aging at 200°C. The broadening of the imide absorption peaks was marked by the disappearance of the amide peak near 1660 cm⁻¹ and is attributable to post‐imidization of the partially imidized polyamic‐acid. Dissolution of the polyimide aged at T ≥ 165°C in dimethyl formamide, DMF, was unsuccessful even after long times of stirring (∼12 h) at elevated temperature (T ∼ 85°C). The DSC thermogram for the LaRC‐IA resin showed a series of broad endothermic peaks between 150–180°C and narrow endothermic peaks at 210°C. The low temperature endotherm disappeared after aging at T ≥ 135°C for t ≥ 1 h. The high temperature endotherm decreased with increased aging temperature and time. The glass transition temperature of the polyimide increased with increased aging temperature and time.