The point of zero charge(PZC) of SiC nanoparticles was determined by means of standard potentiometric titration method, while the influences of the main technological parameters on the microstructure of electrodeposited Ni-SiC composite film were studied and optimized. The results show that high bath pH value favors SiC nanoparticles negatively charged and high bath temperature promotes them positively charged. Under the experimental conditions, sodium dodecyl-glycol is proven to be an effective surface modification anionic surfactant for SiC nanoparticles. The results also show that the optimized Ni-SiC composite film is composed of the nanoparticles with the average grain size in the nanometer range (100 nm), and SiC nanoparticles disperse into the nickel matrix uniformly.