The focus of this study is the formation of a solid solution and metallic nickel in the cobalt-nickel mixed oxide coatings during suspension plasma spray (SPS) deposition. The (Co,Ni)O solid solution is a potential material for inert anode applications in aluminum production. SPS coatings and in-flight collected particles are studied to gain further insight into the melting and mixing phenomena of the NiO and CoO powders as well as phase formation in the deposited coatings. Moreover, the role of suspension feedstock particle sizes on the microstructure of coatings is discussed. SEM, EDS and X-ray diffraction studies helped better understanding the formation of different crystalline phases within the as-sprayed coatings. It was found that the formation of metallic nickel is possible in the coatings. The results support the importance of substrate temperature on the formation of metallic Ni, so that keeping the substrate at low temperature results in an increase of the Ni content in the coatings. In this study, possible causes for the formation of metallic Ni during spraying are discussed.