Journal of Applied Polymer Science, Vol.53, No.13, 1805-1812, 1994
In-Situ Cure Monitoring of Epoxy-Resins Using Fiberoptic Raman-Spectroscopy
Fiber-optic Raman spectroscopy was used to monitor the curing of epoxy resins in situ for eventual application to polymer composite processing. A 200-mu m diameter quartz fiberoptic sensor immersed in liquid resin was used to obtain Raman spectra for a concentration series of diglicidyl ether of bisphenol-A in its own reaction product with diethylamine using an 820 nm continuous-wave diode laser excitation. A Raman peak at 1240 cm(-1) was assigned to a vibrational mode of the oxirane (epoxide) ring and its normalized intensity was found to be linearly related to the concentration of epoxide groups in the resin mixtures. Raman peaks at 1112 and 1186 cm(-1) associated with phenyl and gen-dimethyl resin backbone vibrations, respectively, did not change in intensity due to the curing reaction and were used as internal references to correct the Raman spectra for intensity changes due to density fluctuations and instrumental variations during the experiments. Fiber-optic Raman spectroscopy was used to monitor the extent of reaction in situ for the room-temperature cure of phenyl glicidyl ether with diethylamine. The extent of reaction of the epoxide groups calculated from the Raman spectra were in excellent agreement with kinetic data from Fourier transform near-infrared absorbance measurements made under the same conditions.