Suspensions of cobalt spinel (Co3O4) powders were rf plasma sprayed to form electrocatalytically active anode layers. Stable cobalt oxide suspensions of low viscosity exceeding 50 wt% solid phase have been processed. A spheroidization study revealed the formation of large spherical powder particles (- 30 + 80 µm). Cobalt oxide coatings were produced by rf suspension plasma spraying. The porosity was controlled by optimizing spray distance and reactor pressure. The main disadvantage of the thermal plasma processing of cobalt spinel is that the decomposition of the spinel phase into CoO could not be prevented, not even with the application of an 80% oxygen plasma. However, with a relatively low power oxygen plasma post-treatment, the deposited CoO layers can be oxidized to Co3O4, greatly improving the electrochemical performance of the anode layers.