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Simultaneous Monitoring of Curing Shrinkage and Degree of Cure of Thermosets by Attenuated Total Reflection Fourier Transform Infrared (ATR FT-IR) Spectroscopy

Volume 67, Number 12 (Dec. 2013) Page 1427-1436

XAVIER FERNÀNDEZ-FRANCOS,* SERGEI G. KAZARIAN, XAVIER RAMIS, and ÀNGELS SERRA


We present a novel methodology to simultaneously monitor of the degree of cure and curing shrinkage of thermosetting formulations. This methodology is based on the observation of changes in the infrared absorption of reactive functional groups and the groups used as a standard reference for normalization. While the optical path length is exact and controlled in transmission infrared spectroscopy, in attenuated total reflection Fourier transform infrared (ATR FT-IR), the exact determination of volume changes requires the measurement of the refractive indices of the studied system throughout the curing process or at least an indirect parallel measurement of this property. The methodology presented here allows one to achieve quantitative measurements of the degree of cure and shrinkage for thermosets using in situ ATR FT-IR spectroscopy.



Index Headings: Thermosets; Epoxy; Methacrylate; Fourier transform infrared; FT-IR; Attenuated total reflection; ATR; Polymer; Swelling; Shrinkage.