Dynamic vulcanization is a mixing process employed in the melt state of elastomers with thermoplastics. This process may result in the formation of thermoplastic vulcanized (TPV) materials with improved properties such as mechanical strength, Young's modulus, hardness, and abrasion fatigue. In this study, a vulcanized thermoplastic was obtained by the dynamic vulcanization of poly(vinyl chloride)/acrylonitrile butadiene rubber (PVC/NBR) blends using a curative system based on sulfur (S)/tetramethylthiuram disulfide (TMTD) and mercaptobenzothiazyl disulfide (MBTS). The formation of crosslinks was characterized by differential scanning calorimetry (DSC) and Fourier transform infrared (FTIR) spectroscopy. The mechanical properties were analyzed by tensile tests and the phase morphology was investigated using atomic force microscopy (AFM) operating in the tapping mode-AFM. The phase images of the dynamically vulcanized blends showed an elongated morphology, which can be associated to the formation of crosslinks that give the material its excellent mechanical properties.