In recent years, silicon carbide has attracted more and more attention since it has advantages such as lightweight, high strength and hardness, low thermal expansion coefficient, excellent wear resistance, high chemical stability, outstanding thermal conduction ability. Therefore, silicon carbide has been utilized in many industries, especially applications in harsh environments including aerospace, astronomical, and semiconductor instruments. In this study, we develop a surface metallization process for single-crystalline silicon carbide substrate by electroless deposition of nickel. We also investigate the effect of annealing process for the as-deposited Ni-coated silicon carbide substrate. The annealed Ni-coated silicon carbide substrate undergoes electrochemical analysis to evaluate its corrosion resistance. Images from electron microscopes (SEM) confirm the formation of uniform Ni film on silicon carbide surface. X-ray diffraction (XRD) pattern indicates the existence of NixSiy phases after annealing. In addition, the cross-hatch test is carried out to test the adhesion between Ni film and SiC substrate. As a result, the cross-hatched area presents adhesive level of 5B which represents an excellent adhesion between Ni film and SiC substrate.