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An instrument has been developed for monitoring cure processes under microwave heating conditions. The main function of the instrument was a calorimeter for performing microwave thermal analysis. A single model resonant cavity was used as the heating cell in the microwave calorimeter. Thermal analysis measurements were obtained by monitoring the variation in the microwave power that was required to maintain controlled heating of the sample. The microwave thermal analysis data were analogous to conventional differential scanning calorimetry measurements. The dielectric properties of the sample, as a function of the extent of cure, have been obtained using perturbation theory from the changes in resonant frequency and quality factor of the microwave cavity during heating. Additionally, remote sensing fibre-optic probes have been employed to measure real time in situ infrared spectra of the sample during the cure reaction. In this paper, we describe the design and operation of the microwave calorimeter. Examples of experimental results are also presented.

The cure of an epoxy resin system, based upon a diglycidyl ether of bisphenol-A (DGEBA) with HY917 (an acid anhydride hardener) and DY073 (an amine-phenol complex that acted as an accelerator), was investigated using a conventional differential scanning calorimeter and a microwave-heated power-compensated calorimeter. Dynamic cure of the epoxy resin using four different heating rates and isothermal cure using four different temperatures were carried out and the degree of cure and reaction rates were compared. The cure kinetics were analyzed using several kinetics models. The results showed different activation energies for conventional and microwave curing and suggested different reaction mechanisms were responsible for curing using the two heating methods. Resins cured using conventional heating showed higher glass transition temperatures than did those cured using microwave heating. Kinetics analysisThe reactions taking place in an uncatalyzed acid anhydride-cured epoxy system include monoester, diester, and ether formation, as seen in Scheme 1. 12Correspondence to: R. J. Day (richard.day@manchester.ac.uk).

ABSTRACT:The cure of a commercial epoxy resin system, RTM6, was investigated using a conventional differential scanning calorimeter and a microwave-heated calorimeter. Two curing methods, dynamic and isothermal, were carried out and the degree of cure and the reaction rates were compared. Several kinetics models ranging from a simple nth order model to more complicated models comprising nth order and autocatalytic kinetics models were used to describe the curing processes. The results showed that the resin cured isothermally showed similar cure times and final degree of cure using both conventional and microwave heating methods, suggesting similar curing mechanisms using both heating methods. The dynamic curing data were, however, different using two heating methods, possibly suggesting different curing mechanisms. Near-infrared spectroscopy showed that in the dynamic curing of RTM6 using microwave heating, the epoxy-amine reaction proceeded more rapidly than did the epoxy-hydroxyl reaction. This was not the case during conventional curing of this resin.