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Through direct nanoparticle nucleation and growth on nitrogen doped, reducedgraphene oxide sheets and cation substitution of spinel Co3O4 nanoparticles, amanganese-cobalt spinel MnCo2O4/graphene hybrid was developed as a highlyefficient electrocatalyst for oxygen reduction reaction (ORR) in alkalineconditions. Electrochemical and X-ray near edge structure (XANES)investigations revealed that the nucleation and growth method for forminginorganic-nanocarbon hybrid results in covalent coupling between spinel oxidenanoparticles and N-doped reduced graphene oxide (N-rmGO) sheets. Carbon K-edgeand nitrogen K-edge XANES showed strongly perturbed C-O and C-N bonding in theN-rmGO sheet, suggesting the formation of C-O-metal and C-N-metal bonds betweenN-doped graphene oxide and spinel oxide nanoparticles. Co L-edge and Mn L-edgeXANES suggested substitu-tion of Co3+ sites by Mn3+, which increased theactivity of the catalytic sites in the hybrid materials, further boosting theORR activity compared to the pure cobalt oxide hybrid. The covalently bondedhybrid afforded much greater activity and durability than the physi-cal mixtureof nanoparticles and carbon materials including N-rmGO. At the same massloading, the MnCo2O4/N-graphene hybrid can outperform Pt/C in ORR currentdensity at medium overpotentials with superior stability to Pt/C in alkalinesolutions.

Covalent Hybrid of Spinel Manganese-Cobalt Oxide and Gra-phene as Advanced Oxygen Reduction Electrocatalysts