Crosslinking behaviors of acrylonitrile butadiene rubber (NBR)/poly (vinyl chloride) (PVC) alloy, filled with anhydrous copper sulfate (CuSO 4 ) particles, were investigated for the first time by dynamic mechanical analysis (DMA) under hetero and isothermal modes, respectively. In the heterothermal testing, (NBR/PVC)/CuSO 4 compound showed two marked increases in the storage modulus (E 0 ), corresponding to coordination crosslinking of NBR-CuSO 4 and self-crosslinking of NBR and PVC respectively. During the isothermal testing, a dramatic increase in E 0 was found at the initial stage while that of original NBR/PVC alloy was not detected. The marked increase in E 0 of (NBR/PVC)/CuSO 4 compound was mainly due to the crosslinking induced by coordination between À ÀCN and Cu 2þ . The increasing extent of E 0 increased with the rise of CuSO 4 content, suggesting the formation of a greater number of crosslinks. Moreover, the activation energy (E a ) of crosslinking process was about 139 kJ/mol. In this work, fourier transform infrared spectrum (FT-IR) and equilibrium swelling method were also performed for the characterization of the compound.