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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
【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20min后就进行完全,热固化胶黏剂在60℃固化4h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。
【Abstract】 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.
【Key words】 low-field nuclear magnetic resonance (LF-NMR); adhesive; curing; aging; cross-linked structure; relaxation time; curing mechanism;
- 【文献出处】 装备环境工程 ,Equipment Environmental Engineering , 编辑部邮箱 ,2023年10期
- 【分类号】O657.2;TQ430
- 【下载频次】2