W. Volksen et al., IMIDE-DIMETHYLSILOXANE BLOCK-COPOLYMERS - DESIGN AND SYNTHESIS OF A PERMANENT BURIED OXYGEN-ION ETCH BARRIER, Journal of applied polymer science, 66(1), 1997, pp. 199-208
Imide-siloxane multiblock copolymers were investigated. A key feature
of these copolymers is the preparation of bis(aminopropyl) oligomers v
ia anionic ring-opening polymerization. The molecular weights of the o
ligomers ranged from 1000 to 5000 g/mol. The oligomers were coreacted
with 4,4'-oxydianaline (ODA) and pyromellitic dianhydride (PMDA) dieth
yl ester chloride in a N-methyl-2-pyrrolidone/THF-solvent mixture in t
he presence of N-methylmorpholine. The resulting amic ethyl ester silo
xane copolymers were isolated and washed to remove homopolymer contami
nation. Copolymer compositions, determined by H-1-NMR, ranged from 20
to 65 wt % siloxane content and the measured compositions were close t
o those charged. Solutions of the copolymers were cast and cured (350
degrees C) to effect imidization, producing clear films. The films sho
wed tough ductile mechanical properties with moduli varying with silox
ane content. The copolymers displayed good thermal stability with deco
mposition temperatures in the proximity of 450 degrees C. Multiphase m
orphologies were observed irrespective of siloxane block lengths or co
mpositions. (C) 1997 John Wiley & Sons, Inc.