Understanding the physical properties associated with the gelation and fusion of a PVC plastisol will help to improve process efficiency. Plastisol gelation and fusion were characterized by using both scanning electron microscopy (SEM) and atomic force microscopy (AFM) and were compared with the tensile properties developed at various temperatures. Both SEM and AFM showed good agreement during the early stages of gelation. However, AFM continued to show particle boundaries during the latter stages of gelation and fusion that provided a more nearly accurate comparison with the resulting tensile properties.