In this research paper, synthesis and characterization of bulk nanostructured Al(Zn) solid solution and Al(Zn)/Al2O3 nanocomposite were investigated. For this purpose, fully dense Al(Zn) solid solution and Al(Zn)/Al2O3 nanocomposite were produced by spark plasma sintering method. Consolidated samples were characterized by nanoindentation and nanoscratch tests. Differential thermal analysis revealed that the reaction temperature between Al and zinc oxide in the as-blended and as-milled conditions and hence formation of Al(Zn)/Al2O3 is in the range of 600 to 700 °C. Uniform dispersion of alumina nanoparticles in the Al(Zn) matrix increased the hardness and modulus of elasticity of the Al(Zn)/Al2O3 nanocomposite, significantly. In addition, it was found that the plasticity index of Al(Zn)/Al2O3 nanocomposite was lower than that of nanostructured Al(Zn) solid solution while the wear resistance of nanocomposite sample was noticeably larger than that of solid solution sample.