Spark discharge is widely applied to fabricate the small scale particles. The ultrasound-aided spark discharge process is based on an electrical discharge in liquid media in the electrical discharge machining (EDM). The morphology, element composition, and crystal structure of Nickle particles were observed analyzed by SEM, EDS and XRD, respectively. The EDS and XRD indicated a high purity nickel particle generated in pure water. Plus, the effects of dielectric mediums on the size distribution were investigated. The size distribution of particles in pure water is narrower than in kerosene. This distribution is remarkable after the ultrasound is introduced into the generating process. Based on the attaching and entrapping processes, the formation mechanism of different structural particles was interpreted. The results serve as a guide for the future research on controlling the particle properties such as size and morphology through improving the experimental conditions.