Quasi-isothermal DSC testing of epoxy adhesives using initial fast heating rates

Abstract

Three major factors decrease the accuracy of the cure measurement in standard-isothermal testing using differential scanning calorimetry (DSC). First, cure occurs during the heating step. Second, data are lost during the stabilization period between the dynamic and isothermal step. Third, the baseline selection requires a modification to the protocol. An alternative, which is explored in this study, is the use of fast ramps, which decrease the heating time, but this has been avoided due to overshoot that occurs between the dynamic and isothermal step, which is troublesome for systems with autocatalytic kinetics. By mitigating these factors, a quasi-isothermal protocol was developed. Therefore, more complete cure kinetics were captured with the implementation of fast DSC to decrease the ramp time and through the optimization of furnace parameters to decrease stabilization time and temperature overshoot. The data suggested this quasi-isothermal analysis more accurately measured the isothermal curing kinetics of a commercial epoxy adhesive at 110, 115, and 120 degrees C for fast ramps of 175, 350, and 500 K/min compared to the traditional ramp of 5 K/min. The enthalpy spike at the dynamic to isothermal transition remains an issue; however, an empirical shift can be used to compensate for the enthalpy signal lag.