Curing and Aging of Adhesives by Low-field Nuclear Magnetic Resonance
Received:September 24, 2023  Revised:October 09, 2023
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DOI:10.7643/issn.1672-9242.2023.10.014
KeyWord:low-field nuclear magnetic resonance (LF-NMR)  adhesive  curing  aging  cross-linked structure  relaxation time  curing mechanism
                    
AuthorInstitution
ZHAO Min Department of Chemical Engineering, Tsinghua University, Beijing , China
ZHANG Qian Department of Chemical Engineering, Tsinghua University, Beijing , China
YANG Rui Department of Chemical Engineering, Tsinghua University, Beijing , China
LIN Yue-long Inner Mongolia Institute of Dynamical Machinery, Hohhot , China
BIAN Lei Inner Mongolia Institute of Dynamical Machinery, Hohhot , China
ZHOU Wen-qing Department of Chemical Engineering, Tsinghua University, Beijing , China
ZHAO Meng Inner Mongolia Institute of Dynamical Machinery, Hohhot , China
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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.
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