This paper presents a novel process that uses RF plasma spraying and premixed elemental powders to produce intermetallic matrix composites in situ without having to add reinforcement fibers or particles. Splats were collected on a stainless steel substrate and were analyzed to determine if nitrides had formed in metal droplets during flight and how it affected splat morphology. The typical splat morphology of impinged Ti droplets is disk-type with an outer peripheral fringe. Aluminum splats, on the other hand, are classified into two categories: a disk-type with an irregular outer periphery and a semi-massive-type. Other composites produced and examined include TiAl, AlN, and Ti2AlN.