In this paper, NiO-YSZ composite powder was synthesized via in situ urea combustion method to prepare high homogeneity cathode. Sm0.2Ce0.8O1.9 (SDC) is used as a barrier interlayer between Ba0.5Sr0.5Co0.8Fe0.2O3-δ (BSCF) anode and 8YSZ electrolyte to avoid solid state interaction for high temperature application. The crystal structure and surface morphologies of NiO, YSZ, BSCF and SDC powders were characterized, respectively. The optimization of technological conditions for the synthesis was investigated. The adding amount was calculated by the combustion reaction equation. BSCF-SDC/YSZ/Ni-YSZ single button cells were prepared and the related electrochemical performances were test at 850°C. The research results showed that the products were well crystallized with NiO coating on YSZ particles. The optimized addition of CO(NH2)2 to Ni(NO3)2 was 2:1. A SOEC single cell made from NiO-YSZ with the molar ratio of 2:1 composite powder exhibited better performance than the other samples with the electrolytic voltage of 0.98V and showed excellent durability under the electrolytic currency of 0.33 A/cm2, the input stream of 90%H2O+10%H2. The hydrogen production rate of the single SOEC using BSCF/SDC can be up to 196.6 mL·cm-2h-1, which indicates that it could be a potential candidate for the future application of SOEC technology.