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Reactive epoxies with functional zeolite fillers: IR spectroscopy and PALS studies

Published online by Cambridge University Press:  10 October 2011

Muhammad Quasim Shaikh
Affiliation:
Faculty of Engineering, Institute for Materials Science, Multicomponent Materials, Christian-Albrechts University at Kiel, 24143 Kiel, Germany
Klaus Rätzke*
Affiliation:
Faculty of Engineering, Institute for Materials Science, Multicomponent Materials, Christian-Albrechts University at Kiel, 24143 Kiel, Germany
Jan Christian Gaukler
Affiliation:
Saarland University, Chair for Adhesion and Interphases in Polymers, D-66041 Saarbruecken, Germany
Wulff Possart
Affiliation:
Saarland University, Chair for Adhesion and Interphases in Polymers, D-66041 Saarbruecken, Germany
Franz Faupel
Affiliation:
Faculty of Engineering, Institute for Materials Science, Multicomponent Materials, Christian-Albrechts University at Kiel, 24143 Kiel, Germany
*
a)Address all correspondence to this author. e-mail: kr@tf.uni-kiel.de
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Abstract

Epoxy–dicyandiamide (Dicy) formulations frequently contain a free accelerator for reducing the curing temperature and the time for network formation, which reduces the shelf life of these adhesives. This study compared the reaction kinetics during the storage at 60 °C for a precured epoxy adhesive (EP = diglycidyl ether of bisphenol A and Dicy, mass ratio 100:6.7, precured at 150 °C for 1 h) mixed either with free accelerator (=EPacc) or with the same concentration of accelerator immobilized in micro- or nanozeolite fillers (EPμ-filled and EPn-filled, respectively). During storage, the infrared (IR) study probed the chemical modifications. They lead to increasing cross-linking density and a loss of free volume as detected by positron annihilation lifetime spectroscopy (PALS). Cross-linking precedes to the chemical vitrification. Additionally, the glass transition and the free-volume parameters were investigated for the three EP’s as a function of temperature by PALS after thermal curing.

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Articles
Copyright
Copyright © Materials Research Society 2011

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