Expanded mesocarbon microbeads (eMCMBs) are prepared by chemical oxidation. Ni foam with reduced eMCMBs (reMCMB) acts as a highly conductive scaffold. NiCo2O4 nanoflakes grow around the Ni foam with attached reMCMBs for capacitors. NiCo2O4/Ni foam/reMCMBs electrode exhibits a high specific capacitance of 1025 F g−1.