CuCo2S4 is an important mixed-metal spineltype sulfide that is typically synthesized using high-temperature solid-state reactions, which produce agglomerated particles with low surface areas that are not optimal for applications such as heterogeneous catalysis. Here, we show that highly crystalline and nonagglomerated colloidal CuCo2S4 nanoparticles can be synthesized in solution at 200 degrees C, which is significantly lower than previously reported methods. The CuCo2S4 nanoparticles were found to be highly active electrocatalysts for the oxygen evolution reaction (OER) under strongly alkaline conditions (1.0 M KOH, pH 14), requiring an OER overpotential of 395 mV to produce a current density of 10 mA cm(-2). X-ray photoelectron spectroscopy (XPS) studies showed evidence of oxide formation, suggesting, in conjunction with the observed electrocatalytic properties, that the mixed-metal sulfides may serve as precursors to oxides and/or hydroxides, which are likely to be the catalytically active species.