赵敏,张倩,杨睿,蔺跃龙,边磊,周文清,赵猛.低场核磁共振研究胶黏剂的固化和老化过程[J].装备环境工程,2023,20(10):118-123. ZHAO Min,ZHANG Qian,YANG Rui,LIN Yue-long,BIAN Lei,ZHOU Wen-qing,ZHAO Meng.Curing and Aging of Adhesives by Low-field Nuclear Magnetic Resonance[J].Equipment Environmental Engineering,2023,20(10):118-123.
低场核磁共振研究胶黏剂的固化和老化过程
Curing and Aging of Adhesives by Low-field Nuclear Magnetic Resonance
投稿时间:2023-09-24  修订日期:2023-10-09
DOI:10.7643/issn.1672-9242.2023.10.014
中文关键词:  低场核磁共振  胶黏剂  固化  老化  交联结构  弛豫时间  固化机理中图分类号:O631.6 文献标识码:A 文章编号:1672-9242(2023)10-0118-06
英文关键词:low-field nuclear magnetic resonance (LF-NMR)  adhesive  curing  aging  cross-linked structure  relaxation time  curing mechanism
基金项目:
作者单位
赵敏 清华大学 化学工程系,北京 100084 
张倩 清华大学 化学工程系,北京 100084 
杨睿 清华大学 化学工程系,北京 100084 
蔺跃龙 内蒙动力机械研究所,呼和浩特 010010 
边磊 内蒙动力机械研究所,呼和浩特 010010 
周文清 内蒙动力机械研究所,呼和浩特 010010 
赵猛 内蒙动力机械研究所,呼和浩特 010010 
AuthorInstitution
ZHAO Min Department of Chemical Engineering, Tsinghua University, Beijing 100084, China 
ZHANG Qian Department of Chemical Engineering, Tsinghua University, Beijing 100084, China 
YANG Rui Department of Chemical Engineering, Tsinghua University, Beijing 100084, China 
LIN Yue-long Inner Mongolia Institute of Dynamical Machinery, Hohhot 010010, China 
BIAN Lei Inner Mongolia Institute of Dynamical Machinery, Hohhot 010010, China 
ZHOU Wen-qing Department of Chemical Engineering, Tsinghua University, Beijing 100084, China 
ZHAO Meng Inner Mongolia Institute of Dynamical Machinery, Hohhot 010010, China 
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中文摘要:
      目的 研究胶黏剂的固化程度及在自然贮存和温度循环中的变化。方法 利用低场核磁共振技术,通过测定胶黏剂中氢原子在固化和老化过程中横向弛豫时间T2的变化,反映固化过程中交联结构的发展,以及交联结构在6个月自然贮存和100次高低温循环过程中的变化,阐明胶黏剂的老化机理。结果 光固化胶黏剂的光交联反应在20 min后就进行完全,热固化胶黏剂在60 ℃固化4 h后即达到了较高程度的交联,120 ℃固化对交联程度的影响不大,更多的是对交联结构的完善。经过‒45~75 ℃下100次高低温循环后,胶黏剂的交联结构变化不明显。自然贮存6个月后,胶黏剂不仅发生继续交联,而且结构发生了一定的松弛,这些将对其长期使用稳定性带来影响。结论 低场核磁共振对氢原子的运动能力敏感,而且制样简单,测试速度快,是研究交联结构变化的强有力的工具,对胶黏剂的研制、固化工艺优化、固化机理研究具有重要的应用价值。
英文摘要:
      The work aims to study the curing degree of adhesive and its changes in natural storage and temperature cycle. With the help of the low-field nuclear magnetic resonance (LF-NMR) technology, the change of transverse relaxation time T2 of hydrogen atom in the adhesive during curing and aging was measured to reflect the development of cross-linked structure during curing and the change of the cross-linked structure during 6 months of natural storage and 100 high and low temperature cycles, and clarify the aging mechanism of the adhesive. The results showed that the photo-cross-linking reaction of the light-cured adhesive was completed in 20 min minutes. The thermosetting adhesive reached a high degree of cross-linking after curing at 60 ℃ for 4 h. Curing at 120 ℃ had little effect on the cross-linking degree, but improved the cross-linked structure further. After 100 high and low temperature cycles at ‒45~75 ℃, the cross-linked structure of the adhesive did not change obviously. However, after natural storage for 6 months, the adhesive not only continued to cross-link, but also had a certain relaxation in structure, which would affect its long-term use stability. Low-field nuclear magnetic resonance is sensitive to the mobility of hydrogen atoms, simple in preparation and fast in testing. It is a powerful tool to study the changes of the cross-linked structure, and has important application value in the development of adhesives, the optimization of curing process and the study of curing mechanism.
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