Characterization of the crosslinking reaction in high performance adhesives
In this study, thermal analysis, infrared spectroscopy (near and mid) in conjunction with low field NMR, have been used to characterize the crosslinking reaction involving phenol formaldehyde resin and a crosslinking agent, hexamethylenetetramine (HMTA) used as adhesive in organic-inorganic composit...
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| Veröffentlicht in: | International journal of adhesion and adhesives 2017-10, Vol.78, p.256-262 |
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| container_title | International journal of adhesion and adhesives |
| container_volume | 78 |
| creator | Patel, Jigneshkumar P. Xiang, Zou Guo Hsu, Shaw Ling Schoch, Andrew B. Carleen, Sena Ada Matsumoto, Dean |
| description | In this study, thermal analysis, infrared spectroscopy (near and mid) in conjunction with low field NMR, have been used to characterize the crosslinking reaction involving phenol formaldehyde resin and a crosslinking agent, hexamethylenetetramine (HMTA) used as adhesive in organic-inorganic composites. The strong hydrogen bonds in the resin and the completely crystalline HMTA (Tm = 280°C) severely hamper the crosslinking process. Yet the addition of a small amount of plasticizer can induce an efficient (> 50% increase) crosslinking reaction as compared to the system without plasticizer. The infrared spectroscopy clarifies the dissolution process of the crystalline crosslinker and the specific interactions needed to achieve miscibility of the reactants. The thermal analysis enabled us to follow the reaction as a function of temperature. The low field NMR with the T1 inverse recovery technique allowed us to monitor the crosslinking process directly. For the first time, it is now possible to identify the functionality of the plasticizer and correlate the degree of crosslinking achieved in order to assess the macroscopic cohesive strength needed for high performance adhesives. |
| doi_str_mv | 10.1016/j.ijadhadh.2017.08.006 |
| format | Article |
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The strong hydrogen bonds in the resin and the completely crystalline HMTA (Tm = 280°C) severely hamper the crosslinking process. Yet the addition of a small amount of plasticizer can induce an efficient (> 50% increase) crosslinking reaction as compared to the system without plasticizer. The infrared spectroscopy clarifies the dissolution process of the crystalline crosslinker and the specific interactions needed to achieve miscibility of the reactants. The thermal analysis enabled us to follow the reaction as a function of temperature. The low field NMR with the T1 inverse recovery technique allowed us to monitor the crosslinking process directly. 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The strong hydrogen bonds in the resin and the completely crystalline HMTA (Tm = 280°C) severely hamper the crosslinking process. Yet the addition of a small amount of plasticizer can induce an efficient (> 50% increase) crosslinking reaction as compared to the system without plasticizer. The infrared spectroscopy clarifies the dissolution process of the crystalline crosslinker and the specific interactions needed to achieve miscibility of the reactants. The thermal analysis enabled us to follow the reaction as a function of temperature. The low field NMR with the T1 inverse recovery technique allowed us to monitor the crosslinking process directly. For the first time, it is now possible to identify the functionality of the plasticizer and correlate the degree of crosslinking achieved in order to assess the macroscopic cohesive strength needed for high performance adhesives.</description><subject>Adhesion tests</subject><subject>Adhesive bonding</subject><subject>Adhesives</subject><subject>Bond strength</subject><subject>Bonding strength</subject><subject>Crosslinking</subject><subject>Crystal structure</subject><subject>Crystallinity</subject><subject>Degree of functionality</subject><subject>Hexamethylenetetramine</subject><subject>Hydrogen bonds</subject><subject>Infrared analysis</subject><subject>Infrared spectroscopy</subject><subject>Miscibility</subject><subject>NMR</subject><subject>Nuclear magnetic resonance</subject><subject>Phenol formaldehyde</subject><subject>Phenol formaldehyde resins</subject><subject>Plasticization</subject><subject>Polymer matrix composites</subject><subject>Segmental dynamics</subject><subject>Solubilization</subject><subject>Spectrum analysis</subject><subject>Studies</subject><subject>Thermal analysis</subject><issn>0143-7496</issn><issn>1879-0127</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2017</creationdate><recordtype>article</recordtype><recordid>eNqFkM1OwzAQhC0EEqXwCigS54TdOLXTG6jiT1TiAmfLcdaNQ5sUO60ET49D4Yy00h72m1nNMHaJkCGguG4z1-q6iZPlgDKDMgMQR2yCpZyngLk8ZhPAgqeymItTdhZCCxGEgk_Y86LRXpuBvPvSg-u7pLfJ0FBifB_C2nXvrlslniIyHl2XNG7VJFvytvcb3RlK4mMKbk_hnJ1YvQ508bun7O3-7nXxmC5fHp4Wt8vUFCCGdA614bMyp4prm5tccuKIlTXCVpUUJLSWcsZLrEuDqC23Bee8igjVhnjJp-zq4Lv1_ceOwqDafue7-FLhXAiQBcqREgfqJ4knq7bebbT_VAhqLE616q84NRanoFSxuCi8OQgpZtg78ioYRzFp7TyZQdW9-8_iG7Yfe0Y</recordid><startdate>201710</startdate><enddate>201710</enddate><creator>Patel, Jigneshkumar P.</creator><creator>Xiang, Zou Guo</creator><creator>Hsu, Shaw Ling</creator><creator>Schoch, Andrew B.</creator><creator>Carleen, Sena Ada</creator><creator>Matsumoto, Dean</creator><general>Elsevier Ltd</general><general>Elsevier BV</general><scope>AAYXX</scope><scope>CITATION</scope><scope>7SR</scope><scope>7TB</scope><scope>8BQ</scope><scope>8FD</scope><scope>FR3</scope><scope>JG9</scope><scope>KR7</scope></search><sort><creationdate>201710</creationdate><title>Characterization of the crosslinking reaction in high performance adhesives</title><author>Patel, Jigneshkumar P. ; 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The strong hydrogen bonds in the resin and the completely crystalline HMTA (Tm = 280°C) severely hamper the crosslinking process. Yet the addition of a small amount of plasticizer can induce an efficient (> 50% increase) crosslinking reaction as compared to the system without plasticizer. The infrared spectroscopy clarifies the dissolution process of the crystalline crosslinker and the specific interactions needed to achieve miscibility of the reactants. The thermal analysis enabled us to follow the reaction as a function of temperature. The low field NMR with the T1 inverse recovery technique allowed us to monitor the crosslinking process directly. 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| source | Elsevier ScienceDirect Journals |
| subjects | Adhesion tests Adhesive bonding Adhesives Bond strength Bonding strength Crosslinking Crystal structure Crystallinity Degree of functionality Hexamethylenetetramine Hydrogen bonds Infrared analysis Infrared spectroscopy Miscibility NMR Nuclear magnetic resonance Phenol formaldehyde Phenol formaldehyde resins Plasticization Polymer matrix composites Segmental dynamics Solubilization Spectrum analysis Studies Thermal analysis |
| title | Characterization of the crosslinking reaction in high performance adhesives |
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