SummaryThe structure of electrodeposited composite coatings of Ni-Al-Al 2 O 3 , with Ni as the matrix and Al and Al 2 O 3 as second-phase particles, was investigated using light microscopy and scanning electron microscopy. Ni coatings with no particles, which were used as reference samples, had progressively coarser structures with increasing current density. Co-deposition with Al resulted in refinement of the Ni matrix structure at high (>10 A dm ¹2 ) current densities. For single-particle baths, the co-deposition of Al 2 O 3 was more strongly affected by current density and bath particle content than was the co-deposition of Al. However, for baths containing both Al and Al 2 O 3 the amount of incorporated Al 2 O 3 no longer depended on current density. With the choice of appropriate conditions, coatings of Ni with up to 39 vol.% Al 2 O 3 were made. Similar experiments with Al yielded a maximum of 17 . 5 vol.% only. Uniform and graded mixed-particle coatings were also produced. When coatings containing Al were annealed, the reaction of the two elements resulted in the formation of either single-phase g or two-phase g-g 0 alloys, in agreement with the equilibrium phase diagram.