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Effect of isothermal aging on post-imidization and glass transition temperature of LaRC-IA polyimide resin
Authors:Kelvin M Jordan  Jude O Iroh
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.
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