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Time-resolved method for the measurement of volume changes during polymerization



A new laser scanning dilatometer, based on a simplified capillary-type dilatometer using a laser scan micrometer for the detection of changes of the sample dimension, is described. The method can be applied to time-resolved measurements of volume changes for transparent and nontransparent samples. The time resolution of the setup is below 1 s, the absolute error in determining the volume change is below 0.0004 cm3, and the accuracy of the measured shrinkage is better than 0.2 vol. %. The operation temperature ranges from room temperature to 160 °C. The setup has been applied to the investigation of the volume shrinkage during the curing of epoxy resins [diglycidyl ether of bisphenol A (DGEBA)] without and with fillers. Furthermore, the effect of a phase transformation on the volume has been demonstrated by the melting of a crystalline phase (succinic anhydride) dispersed in a DGEBA matrix due to the heat of reaction. © 2005 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 43: 2314–2325, 2005