Metal matrix nanocomposites (MMNCs) are anticipated to offer significantly better performance than existing superalloys. Nickel/alumina nanocomposite samples were fabricated with a powder metallurgy method, combining high-energy ball milling (HEBM) and spark plasma sintering (SPS). The objective of this research is to determine the effect of alumina nanoparticle fraction and HEBM parameters on the powder preparation and sintering processes, and resultant microstructure and properties. Nickel-based powders containing various fractions (1, 5 and 15 vol.%) alumina nanoparticles were prepared by HEBM. The initial particle sizes were 44 m and 50 nm for nickel and alumina, respectively. The milling process was conducted by starting with mixing at 250 rpm for 5 min, followed by cycling operation at high and low speeds (1200 rpm for 4 min and 150 rpm for 1 min). Samples at different milling times (30, 60, 90 and 120 min) of each composition were obtained. Scanning electron microscopy (SEM) was used to evaluate the dispersion of nanoparticles in the powders at different milling times. SPS technique was used for consolidation of the prepared powders. SEM images showed that alumina nanoparticles are homogeneously dispersed in the metal matrix in the sample containing 15 vol.% alumina. Hardness measurements in cross sections of SPSed samples showed higher values for Ni/Al2O3 MMNC compared to pure Ni.