Hitherto it has not been possible to produce a microscopic image with adequate resolution of the high-impact two-phase system poly(vinyl chloride) (PVC)/chlorinated polyethylene (CPE) due to inadequate phase contrast. With the aid of various chemical staining methods and through ion etching, a way has been found for studying the microstructure of the PVC/CPE system by light microscopy and electron microscopy. These independent visualization techniques and scanning electron micrographs of fracture surfaces show, as the morphology with optimal mechanical and rheological properties, networklike distribution of the rubber phase and, imbedded in this, a PVC phase consisting of primary particles.