In this article, a new nitrile-butadiene rubber (NBR) crosslinked composites containing poly(viny chloride) (PVC) and hindered phenol (AO-80 and AO-60) was successfully prepared by melt-blending procedure. Microstruture and dynamic mechanical properties of the composites were investigated using SEM, DSC, XRD, and DMTA. Most of hindered phenol was dissolved in the NBR/PVC matrix and formed a much fine dispersion. The results of DSC and DMTA showed that strong intermolecular interaction was formed between the hindered phenol and NBR/PVC matrix. The NBR/PVC/AO-80 crosslinked composites showed only one transition with higher glass transition temperature and higher tan 6 value than the neat matrix, whereas for the NBR/PVC/AO-60 crosslinked composites, a new transition appeared above the glass transition temperature of matrix, which was associated with the intermolecular interaction between AO-60 and PVC component of the matrix. Both AO-80 and AO-60 in the crosslinked composites existed in amorphous form. Furthermore, the chemical crosslinking of composites resulted in better properties of the materials, e.g., considerable tensile strength and applied elastic reversion. (C) 2008 Wiley Periodicals, Inc.