Advances in Polymer Science 89 by Andreis Kulicke

By Andreis Kulicke

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67), probably due to the effects of chain entanglements in these particular networks u 9 ) . However, it was noticed that in the 13C spectra of swollen gels not all of the carbons in the polymers contribute to the high resolution spectra. 1 and 1 mole% of crosslinking, respectively139). A decrease in signal area of the cross- Application of NMR to Crosslinked Polymer Systems 113 linked PS aliphatic resonances relative to the aromatic area, as well as to the internal standard is also observed. Since this change is not a consequence of increases in T of the aliphatic carbon atoms, it was concluded that the crosslinking limited the motion of some of the backbone carbon atoms so that they were dipolar-coupled and the resulting broad signals were not distinguishable from the spectral base line 140).

11. 86)) M. Andreis and J. L. Koenig 94 dose as the sol fraction. Although the NMR measurements give a slightly lower (5-10%) sol content as compared to the extraction method, the NMR data fit very well to the Charlesby-Pinner equation over a wide range even close to the gel point. The T2L component in the sol fraction at 10 °C is found to be related to the numberaverage molecular mass Mn, while in the separated gel fraction T2S is directly proportional to the average molecular mass between crosslinks (or entanglements) Mc74>: T2S = 6 • 10- 7 Mc (23) The studies of model SBS systems show that the T2L component (corresponding to the PB chain between PS blocks) increases proportionally to the number of mobile protons until the critical molecular weight for the formation of entanglement of the rubber segment (40000) is reached; then the two T2s are observed for a linear PB 95).

The dependence of both diffusion constants on the curing time is shown in Fig. 19. The accuracy for D r data is less pronounced than for the polymer D(Mn), because only the first few data points are relevant for its determination. 0 lo O O 9DMn : -85 0 2 8 O a o ê— g _-g-Hi-s8 24 48 96 144 192 *cure> s Fig. 19. Results for the 63 °C curing study for R-45-M containing 8% ( • ) , 11% (O) and 16% (A) of curing agent IPDI. Diffusion of IPDI (top) and polymer molecules of weight Mn (bottom) is shown as function of curing time (abscissa scale is distorted).

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