A facile and new anion exchange process is presented, which involves the conversion of NiCo-CO layered double hydroxide (LDH) nanosheet arrays in an alkaline solution. The anion exchange between CO and OH results in the construction of a reservoir for OH anions, and the decoration of thin nanoflakes on the surface of nanosheets effectively enlarges the surface area of NiCo LDH nanoarrays. The capacitance of the as-soaked NiCo LDH nanoarrays electrode increases from 1.78 F cm (684 F g ) to 6.22 F cm (2391 F g ) at 2 mA cm after soaking for 12 h. Moreover, the soaked NiCo-OH LDH electrode exhibits an enhanced rate capacity, high coulombic efficiency, and good cycling stability compared with the Ni-Co-S nanosheet electrode synthesized through a hydrothermal sulfuration process. The as-assembled all-solid-state NiCo LDH//active carbon asymmetric supercapacitor shows a maximum energy density of 83.4 W h kg at a power density of 1066 W kg .
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