In-situ measurement of chemical shrinkage of MY750 epoxy resin by a novel gravimetric method

Abstract

A novel approach has been developed to measure in-situ chemical shrinkage of epoxy resins at the temperature of cure, during which the epoxy resins pass through liquid, rubbery and glassy states. A small sample of MY750/HY917/DY073 epoxy resin system, sealed in a thin-walled silicone bag, was suspended in a pot of silicone fluid and weighed independently of the silicone bath. The buoyancy of the sample was monitored as its density increases with respect to the constant density fluid during isothermal cures at three different temperatures. The relationship between the chemical shrinkage and degree of cure was deduced from a cure kinetics model for the resin. The good match of the results for the three different cure cycles suggests that chemical shrinkage is only a function of degree of cure regardless of time and temperature. A bi-linear relationship was fitted to the experimental data. The break point is at a degree of cure of about 28%, with corresponding chemical shrinkage of 3%. This point is linked to the gel point of the resin, which was measured as approximately 25% degree of cure in previous work. Total cure shrinkage of 6.9% for the MY750 resin system was obtained by extrapolating the results to a degree of cure of 100%. The method is sensitive, reliable and keeps the resin stress-free; therefore it should be applicable to a wide range of materials.