The polymerization process of bisphenol-A dicyanate (BADCy) has been studied using a positron-annihilation lifetime technique (PAL). The polymerization was conducted at 150°C, and the process was followed by PAL. Seven kinds of samples with different curing times were also formed at 150°C, and the relation between the period of the curing time and the degree of polymerization was studied. It has been shown that theo-Ps lifetime increases in samples with a higher polymerization than 85%, which is consistent with measurements of the specific volume of BADCy.