Ni/YSZ composites for a cathode that can be used in high temperature electrolysis were prepared by ball milling of Ni and YSZ powder. Ball milling was performed in a dry process and in ethanol. The microstructure and electrical conductivity of the composites were examined by XRD, SEM, TEM and a 4-point probe. XRD patterns for both the dry and wet ball-milled powders showed that the composites were composed of crystalline Ni and YSZ particles. The patterns did not change with increases in the milling time up to 48 h. Dry-milling slightly increased the average particle size compared to starting Ni particles, but little change in theparticle size was observed with the increase in milling time. On the other hand, the wet-milling reduced the average size and the increasing milling time induced a further decrease in the particle size. After cold-pressing and annealing at 900 oC for 2 h, the dry-milled powder exhibited high stability against Ni sintering so that the particle size changed little, but the particle size increased in the wet-milled powder. The electrical conductivity increased after sintering at 900 oC. Particles from the dry and wet process became denser and contacted closer after sintering, providing better electron migration paths.