Nickel oxide was doped with a wide range of concentrations (mol%) of Aluminum (Al) by solvothermal synthesis;single-phased nano powder of nickel oxide was generated after calcination at 900oC. When the concentration of Al dopant wasincreased, the reduced intensity was confirmed through XRD analysis. Lattice parameters of the synthesized NiO powder weredecreased after treatment of the dopant; parameters were increased when the concentration of Al was over the doping limit(5mol% Al). The binding energy of Ni2+ was chemically shifted to Ni3+ by doping Al3+ ion, as confirmed by the XPS analysis.The tilted structure of the synthesized NiO with 5mol% Al dopant and the polycrystalline structure of the Ni0.75Al0.25O wereobserved by HR-TEM analysis. The electrical conductivity of the newly synthesized NiO was highly improved by Al dopingin the conductivity test. The electrical conductivity values of the commercial NiO and the synthesized NiO with 5mol% Aldopant (Ni0.95Al0.05O) were 1,400s/cm and 2,230s/cm at 750oC, respectively. However, the electrical conductivity of thesynthesized NiO with 10mol% Al dopant (Ni0.9Al0.1O) decreased due to the scattering of free-electrons caused by the largenumber of impurity atoms; the electrical conductivity of Ni0.9Al0.1O was 545s/cm at 750oC.