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通过高斯加权的1H CPMG弛豫曲线测定橡胶交联密度
引用本文:高鹏飞,褚琳琳,杨翼,江纪锋,王嘉琛,姚叶锋,周兵.通过高斯加权的1H CPMG弛豫曲线测定橡胶交联密度[J].波谱学杂志,2018,35(1):60-74.
作者姓名:高鹏飞  褚琳琳  杨翼  江纪锋  王嘉琛  姚叶锋  周兵
作者单位:1. 华东师范大学 物理与材料科学学院, 上海市磁共振重点实验室, 上海 200062;2. 上海纽迈电子科技有限公司, 上海 200333;3. 双钱集团上海轮胎研究所有限公司, 上海 200237;4. 同济大学 材料科学与工程学院, 上海 201804
基金项目:国家自然科学基金资助项目(21574043;41572103),国家重点基础研究发展计划(“973计划”)资助项目(2013CB921801),上海市科委资助项目(15142200500),华东师范大学科研创新基金
摘    要:CPMG(Carr-Purcell-Meiboom-Gill)回波法是测量橡胶交联密度常用交联点之间的分子量(Mc)表示]的一种常用核磁共振(NMR)技术,但实验发现通过该技术获得的Mc对于CPMG序列中脉冲间隔时间具有较强的依赖性,导致交联密度NMR测量值与橡胶材料硬度的相关性低.为了克服这一缺点,本文对不同脉冲间隔时间下CPMG实验测得的质子横向驰豫曲线进行高斯加权.通过对高斯加权求和后的质子横向驰豫曲线进行处理分析,实现了对橡胶交联密度更加准确地测量,大幅提升了天然橡胶交联密度NMR测量值与材料硬度的相关性.本文方案测量能获得与1H DQ NMR方法相当,或比之更佳的交联密度-硬度相关性.同时,本文方案比1H DQ NMR方法更为高效,整体测量时间缩短为1H DQ NMR实验时间的1/10.

关 键 词:1H  CPMG  高斯加权求和  1H  DQ  NMR  交联密度  橡胶  
收稿时间:2017-07-29

Measurement of Crosslinking Density of Rubbers by Analyzing Gaussian-Weighted CPMG Relaxation Curves
GAO Peng-fei,CHU Lin-lin,YANG Yi,JIANG Ji-feng,WANG Jia-chen,YAO Ye-feng,ZHOU Bing.Measurement of Crosslinking Density of Rubbers by Analyzing Gaussian-Weighted CPMG Relaxation Curves[J].Chinese Journal of Magnetic Resonance,2018,35(1):60-74.
Authors:GAO Peng-fei  CHU Lin-lin  YANG Yi  JIANG Ji-feng  WANG Jia-chen  YAO Ye-feng  ZHOU Bing
Institution:1. Shanghai Key Laboratory of Magnetic Resonance, Department of Physics, East China Normal University, Shanghai 200062, China;2. Shanghai Niumag Electronic Technology Co., Ltd., Shanghai 200333, China;3. Double Coin Group Shanghai Tire Research Institute Co., Ltd., Shanghai 200237, China;4. School of Materials Science and Engineering, Tongji University, Shanghai 201804, China
Abstract:CPMG sequence is widely used to measure crosslink density of rubber.However,the crosslink density obtained by this technique has a strong dependence on the interval times between the pulses in CPMG sequence,and the results measured have only a weak correlation with rubber hardness.To overcome this shortcoming,we proposed in this work to construct a 1H T2 relaxation curve by summing Gaussian-weighted CPMG relaxation curves acquired at by varying the interval time between the pulses in CPMG sequence.Using the multi-echo Gaussian-weighted relaxation curve to calculate the crosslink density gave results that had greatly improved correlation with the rubber hardness.The new method was also fast and efficient,as it took only one-tenth of the experimental time required for the conventional 1H double quantum NMR (1H DQ NMR) experiment.
Keywords:1H CPMG  Gaussian-weighted summation  1H double quantum NMR (1H DQ NMR)  crosslink density  rubber  
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