화학공학소재연구정보센터
Journal of Polymer Science Part A: Polymer Chemistry, Vol.32, No.2, 203-217, 1994
NMR-Study of PMR-15 Prepolymerization Steps
Variations in PMR-15 composites properties could be due to differences in their chemical compositions occurring during the curing cycle. Variations in the composition of the PMR-15 resin were studied for four different curing cycles, to determine the influences of parameters such as the heating rate or the presence of a temperature stage. The resin mixture was sampled at the same four different temperature points in each cycle and analyzed mainly by H-1- and C-13-NMR. Quantitative analysis of the different chemical species were realized by deconvolution of NMR spectra. At a given temperature, the resin contains the same molecules but in proportions which depend on the curing conditions and which reflect differences in the chemical reactivity of the monomeric species. We have precisely defined the temperature ranges at which each of the key reactions (amidization, imidization, exoendo isomerization) occurs. An imine condensation product of NE and MDA has been identified and shown to be present in the resin mixture even at low temperature. As a result of this study, two possible causes of resin alteration during ageing can be put forward : the presence of nonimidized BTDE moieties and the endo-exo isomerization reaction which will result in deformation and, possibly, microcracking, if reticulation of the end-capped nadimides is not total.