SYNOPSISThe feasibility of using remote FT-IR spectroscopy to monitor the gelation reaction of an epoxy resin used in advanced composite materials has been studied. The commercial epoxy resins MY720 and MY721, consisting mostly of tetraglycidyl4,4'-diaminodiphenyl methane (TGDDM) were cured with diaminodiphenylsulfone (DDS) in a microcapillary cell connected to an FT-IR spectrometer by single silica fiber optics. By operating in the near-IR, direct measurement of the consumption of epoxide and primary amine and growth in hydroxyl groups was possible. It was found that the primary amine band a t 5067 cm-' was the most sensitive for rapid and accurate real-time monitoring of the cure reaction up to gelation. The temperature dependence of amine consumption from 135 to 180°C gave an activation energy of 70 kJ mol-' for the cure reaction in agreement with DSC. Several artefacts involved in using fiber optic FT-IR in this way have been identified.
An infrared (IR) emission cell which is capable of operation up to 1500°C is described. The cell is based on an atomic absorption graphite furnace and is coupled to a Fourier transform infrared spectrometer. The spectrometer has been used to measure the emission spectrum of quartz from 200 to 1400°C, and the changes in the spectrum occurring with temperature can be related to the formation of cristobalite; transitions between low and high forms (alpha and beta forms) can also be monitored. Aragonite has also been analyzed through the temperature range 100 to 600°C, and the aragonite/calcite transition is clearly evident. The transformation of kaolinite to metakaolinite and through to mullite and cristobalite has also been studied with this in situ technique. The formation of mullite is evident in the spectrum at temperatures as low as 900°C, and the formation of cristobalite is clearly seen at 1200°C.
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