NiO nanoparticle was synthesized by a sol-gel method with three different pH values namely pH=1, 7 and 11, and then calcined at temperature of 450 ᵒC. The influence of different pH values on the physical properties of NiO nanoparticles were investigated by a particle size analyzer (PSA), field emission scanning electron microscope (FESEM) and X-ray diffractometer (XRD). Structural analysis confirmed that a cubic structure of NiO nanoparticle was obtained without any secondary phase for NiO powders prepared with pH=1, while the peak of secondary phase (Ni) appeared for NiO powders prepared with pH= 7 and 11. Morphological observation showed that the NiO nanoparticles prepared with pH=7 and 11 tend to form more agglomerates compared to one prepared with pH=1. The average diameter of NiO nanoparticles with pH 1, 7 and 11 were approximately in the range of 19-26 nm, 21-28 nm, and 24-30 nm, respectively. NiO powder that was synthesized with pH=1 was further used to prepare composite anode of NiO Nps-BaCe0.54Zr0.36Y0.1O2.95 (BCZY) powder. Unfortunately a composite of NiO Nps-BaCeO3-BaZrO3 was obtained instead of BCZY and governed by agglomerates with size in the range of 70-300 nm.