The E-beam curable BMI resin systems and phenylethynyl terminated AFR-PEPA-4 oligomer together with an imide model compound N-phenyl-[4-(phenylethynyl) phthalimide] were synthesized and characterized.
E-beam exposure cannot propagate the polymerization of BMI system until the temperature goes up to 100oC. However, a small amount of oligomers may be generated from solid-state cure reaction under low E-beam intensity radiation. Higher intensity E-beam at 40 kGy per pass can give above 75% reaction conversion of BMI with thermal cure mechanism involved.
NVP is a good reactive diluent for BMI resin. The cure extents of BMI/NVP increase with the increase of the dosage and applied dosage per pass. The reaction rate is much higher at the beginning of the E-beam cure and slows down after 2 dose passes due to diffusion control. Free radical initiator dicumyl peroxide can accelerate the reaction rate at the beginning of E-beam cure reaction but doesnÂt affect final cure conversion very much. According to the results from FT-IR, 200 kGy total dosage E-
beam exposure at 10 kGy per pass can give 70% reaction conversion of BMI/NVP with the temperature rise no more than 50oC. The product has a Tg of 180oC.
The predicted ultimate Tg of cured AFR-PEPA-4 polyimide is found to be 437.2oC by simulation of DSC Tg as a function of cure. The activation energy of thermal cure reaction of AFR-PEPA-4 oligomer is 142.6 ± 10.0 kJ/mol with the kinetic order of 1 when the reaction conversion is less than 80%.
The kinetics analysis of the thermal cure of N-phenyl-[4-(phenylethynyl) phthalimide] was determined by FT-IR spectroscopy by following the absorbance of the phenylethynyl triple bond and conjugated bonds. The thermal crosslinking of N-phenyl-[4-(phenylethynyl) phthalimide] through phenylethynyl addition reaction has a reaction order of 0.95 and an activation energy of 173.5 ± 8.2 kJ/mol. The conjugated bond addition reactions have a lower reaction order of 0.94 and lower activation energy (102.7 ± 15.9 kJ/mol). The cure reaction of N-phenyl-[4-(phenylethynyl) phthalimide] can be described as a fast first-order reaction stage followed by a slow second stage that is kinetically controlled by diffusion.
| Identifer | oai:union.ndltd.org:tamu.edu/oai:repository.tamu.edu:1969.1/3075 |
| Date | 12 April 2006 |
| Creators | Li, Yuntao |
| Contributors | Sue, Hung-Jue, Morgan, Roger J. |
| Publisher | Texas A&M University |
| Source Sets | Texas A and M University |
| Language | en_US |
| Detected Language | English |
| Type | Book, Thesis, Electronic Dissertation, text |
| Format | 1705183 bytes, electronic, application/pdf, born digital |
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