Aluas Mihaela, Filip Claudiu
Department of Physics, Martin-Luther University, 06110 Halle, Germany.
Solid State Nucl Magn Reson. 2005 May;27(3):165-73. doi: 10.1016/j.ssnmr.2004.10.001.
A novel approach for solid-state NMR characterization of cross-linking in polymer blends from the analysis of (1)H-(13)C polarization transfer dynamics is introduced. It extends the model of residual dipolar couplings under permanent cross-linking, typically used to describe (1)H transverse relaxation techniques, by considering a more realistic distribution of the order parameter along a polymer chain in rubbers. Based on a systematic numerical analysis, the extended model was shown to accurately reproduce all the characteristic features of the cross-polarization curves measured on such materials. This is particularly important for investigating blends of great technological potential, like thermoplastic elastomers, where (13)C high-resolution techniques, such as CP-MAS, are indispensable to selectively investigate structural and dynamical properties of the desired component. The validity of the new approach was demonstrated using the example of the CP build-up curves measured on a well resolved EPDM resonance line in a series of EPDM/PP blends.
介绍了一种通过分析(1)H-(13)C极化转移动力学对聚合物共混物交联进行固态核磁共振表征的新方法。它通过考虑橡胶中聚合物链上序参量更实际的分布,扩展了通常用于描述(1)H横向弛豫技术的永久交联下残余偶极耦合模型。基于系统的数值分析,扩展模型被证明能准确再现在此类材料上测得的交叉极化曲线的所有特征。这对于研究具有巨大技术潜力的共混物(如热塑性弹性体)尤为重要,在热塑性弹性体中,诸如CP-MAS等(13)C高分辨率技术对于选择性研究所需组分的结构和动力学性质是不可或缺的。以在一系列EPDM/PP共混物中一条分辨率良好的EPDM共振线上测得的CP累积曲线为例,证明了新方法的有效性。