Alumina-nickel powders have been prepared via electroless-nickel (EN) coating of submicrometer-sized alumina powder. The EN layers contain 5.1 ؎ 0.4 wt% phosphorus and are very unevenly distributed on the surfaces of the alumina particles. These layers consist of amorphous and microcrystalline phases. At temperatures ≥1300°C, the EN layers de-wet from the alumina surfaces to become discrete, round particles in the alumina matrix. The alumina-EN pellets can be sintered to reach ∼95% of the theoretical density at 1500°C for 4 h in graphite crucibles. The phases of the sintered samples consist of alumina, nickel, and nickel phosphides. However, in the exterior region of the sample sintered at 1500°C for 4 h, Ni 3 Al will also form.