Poly(vinyl chloride) (PVC)/acrylonitrile-butadiene rubber (NBR) blends with different types of partitioning agent were obtained through melt blending. The samples were characterized according to the viscosities properties, torque rheometry and mechanical resistance as tensile testing, tear strength, and hardness. The morphology and phase imaging were studied using an atomic force microscopy operating in tapping mode (TMAFM). It was observed that the PVC/NBR blends with PVC as partitioning agent showed an increase in the tensile stress and Young's modulus compared to the PVC/NBR blends with calcium carbonate as partitioning agent. The morphology of the blends examined by TMAFM evidenced the effect of the partitioning agent as obtained with other techniques.