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首页> 外文期刊>Polymer: The International Journal for the Science and Technology of Polymers >Measurement of the C-13 spin-lattice relaxation time of the non-crystalline regions of semicrystalline polymers by a cp MAS-based method
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Measurement of the C-13 spin-lattice relaxation time of the non-crystalline regions of semicrystalline polymers by a cp MAS-based method

机译:通过基于cp MAS的方法测量半结晶聚合物的非晶态区域的C-13自旋晶格弛豫时间

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摘要

The non-crystalline C-13 spin-lattice relaxation times of atactic and isotactic polypropylene and those of an ethylene-l-octene copolymer of low crystallinity have been measured by classical inversion and saturation recovery methods as well as by a cp MAS-based pulse sequence. The latter is a saturation recovery-type sequence that involves cross-polarization. It samples preferentially the soft non-crystalline regions of semicrystalline polymers. The method is found to be useful in determining T-1C of the amorphous regions of semicrystalline iPP at room temperature. It is found that the atactic PP molecule and the non-crystalline iPP regions have the same average segmental relaxation rate. The T-1C of some of the carbons investigated was
机译:已通过经典的反演和饱和恢复方法以及基于cp MAS的脉冲测量了无规和等规聚丙烯的C-13自旋晶格弛豫时间以及低结晶度的乙烯-1-辛烯共聚物的非晶态C-13自旋晶格弛豫时间顺序。后者是涉及交叉极化的饱和恢复类型序列。它优先采样半结晶聚合物的软非结晶区域。发现该方法可用于测定室温下半结晶iPP非晶区的T-1C。发现无规PP分子和非晶iPP区域具有相同的平均节段弛豫率。所研究的某些碳的T-1C小于T-1H,实验回收曲线显示,瞬态核Overhauser效应(NOE)对C-13磁化的贡献具有复杂的指数行为。此外,实验数据装有通过求解所罗门方程获得的双指数函数。拟合得出的T-1C与经典反演或饱和度恢复序列获得的值非常吻合。当在延迟期间通过质子磁化的饱和消除瞬态NOE时,基于cp的序列获得了相同的T-1C值。与线性聚乙烯链的那些相比,乙烯共聚物的己基分支导致非晶区中平均主链C-C分子间距离增加,从而导致更高的主链亚甲基节段迁移率。 (C)2002 Elsevier ScienceLtd。保留所有权利。 [参考:32]

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