In-situ cure monitoring of epoxy/graphene nanocomposites by several spectroscopic techniques
Cure protocols of thermoset resins usually comprise two isothermal steps where resins undergo molecular cross-linking processes. The cure conditions are crucial to ensure a consistent and reliable manufacturing of the piece and have been the subject of an important body of research. While most studi...
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| Published in | Polymer testing Vol. 80; p. 106114 |
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| Main Authors | , , , , |
| Format | Journal Article |
| Language | English |
| Published |
Elsevier Ltd
01.12.2019
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| Subjects | |
| Online Access | Get full text |
| ISSN | 0142-9418 1873-2348 |
| DOI | 10.1016/j.polymertesting.2019.106114 |
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| Abstract | Cure protocols of thermoset resins usually comprise two isothermal steps where resins undergo molecular cross-linking processes. The cure conditions are crucial to ensure a consistent and reliable manufacturing of the piece and have been the subject of an important body of research. While most studies have been carried out by traditional calorimetry or infrared spectroscopy under dynamic conditions, the development of new sensors and in-situ characterization techniques has resulted on a renewed interest on the subject under industrial isothermal protocols. Here, we monitor the curing reaction of both un-filled and nanofilled epoxy resin using broadband dielectric spectroscopy (BDS) and correlate the results with in-situ FT-IR and Raman spectroscopy. Hence, the proposed methodology provides complementary information on the chemical reactions and molecular dynamics associated to the cure cycle and can be an efficient tool for real-time monitorization of thermoset composites manufacturing.
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•Understanding the cure cycle of thermosets provides quality control and avoids potential structural failures.•Industrial curing and post-curing settings are simulated.•Broadband dielectric spectroscopy (BDS) is used to monitor in real-time the cure cycle of TRGO filled epoxy nanocomposites.•BDS procedure is correlated with in-situ FT-IR and Raman spectroscopy.•Chemical reactions and molecular dynamics associated to the cure cycle are correlated. |
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| AbstractList | Cure protocols of thermoset resins usually comprise two isothermal steps where resins undergo molecular cross-linking processes. The cure conditions are crucial to ensure a consistent and reliable manufacturing of the piece and have been the subject of an important body of research. While most studies have been carried out by traditional calorimetry or infrared spectroscopy under dynamic conditions, the development of new sensors and in-situ characterization techniques has resulted on a renewed interest on the subject under industrial isothermal protocols. Here, we monitor the curing reaction of both un-filled and nanofilled epoxy resin using broadband dielectric spectroscopy (BDS) and correlate the results with in-situ FT-IR and Raman spectroscopy. Hence, the proposed methodology provides complementary information on the chemical reactions and molecular dynamics associated to the cure cycle and can be an efficient tool for real-time monitorization of thermoset composites manufacturing.
[Display omitted]
•Understanding the cure cycle of thermosets provides quality control and avoids potential structural failures.•Industrial curing and post-curing settings are simulated.•Broadband dielectric spectroscopy (BDS) is used to monitor in real-time the cure cycle of TRGO filled epoxy nanocomposites.•BDS procedure is correlated with in-situ FT-IR and Raman spectroscopy.•Chemical reactions and molecular dynamics associated to the cure cycle are correlated. |
| ArticleNumber | 106114 |
| Author | Verdejo, Raquel Yuste-Sánchez, Vanesa Hernández Santana, Marianella Ezquerra, Tiberio A. López-Manchado, Miguel Angel |
| Author_xml | – sequence: 1 givenname: Vanesa surname: Yuste-Sánchez fullname: Yuste-Sánchez, Vanesa organization: Institute of Polymer Science and Technology (ICTP-CSIC), Juan de La Cierva 3, 28006, Madrid, Spain – sequence: 2 givenname: Marianella surname: Hernández Santana fullname: Hernández Santana, Marianella email: marherna@ictp.csic.es organization: Institute of Polymer Science and Technology (ICTP-CSIC), Juan de La Cierva 3, 28006, Madrid, Spain – sequence: 3 givenname: Tiberio A. surname: Ezquerra fullname: Ezquerra, Tiberio A. organization: Institute for the Structure of the Matter (IEM-CSIC), Serrano 121, Madrid, 28006, Spain – sequence: 4 givenname: Raquel surname: Verdejo fullname: Verdejo, Raquel organization: Institute of Polymer Science and Technology (ICTP-CSIC), Juan de La Cierva 3, 28006, Madrid, Spain – sequence: 5 givenname: Miguel Angel surname: López-Manchado fullname: López-Manchado, Miguel Angel organization: Institute of Polymer Science and Technology (ICTP-CSIC), Juan de La Cierva 3, 28006, Madrid, Spain |
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| Keywords | Epoxy resin Broadband dielectric spectroscopy In-situ curing Nanocomposite Graphene |
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