The oxygen evolution reaction (OER) is an important reaction in water splitting. Nickel-iron layered double hydroxide (NiFe LDH) has been considered a potential catalyst for OER. Herein, we report a simple/green approach to improve the oxygen evolution activity of NiFe LDH supported on carbon black (CB). Specifically, ultrasonic exfoliation (UIP500hd, 20 kHz, 500 W) in pure water has been applied to boost the activity of NiFe LDH/CB towards OER. The exfoliated NiFe LDH/CB nanosheets display significantly higher OER activity than their corresponding bulk NiFe LDH/CB in an alkaline solution, with an overpotential of 220 mV at a current density of 10 mA cm-2, which is 60 mV lower than the 280 mV of the bulk NiFe LDH/CB. Notably, it is comparable with the current record overpotential (~200 mV) and superior than other non-precious catalysts. Additionally, after exfoliation, it possesses outstanding kinetics (Tafel slope of 35 mV dec-1) for OER. Besides the improved activity, the exfoliated NiFe LDH/CB has shown a high stability with nearly a constant potential through 12 h electrolysis at a current density of 10 mA cm-2. The characterization analysis reveal that the improved electrochemical performance is closely related to the synergistic effects of the Ni2+ and Fe2+ enriched surface of the exfoliated NiFe LDH/CB, as well as single/few layers structure after exfoliation.

• The influence of parameters on ultrasonic exfoliation of the NiFe LDH in pure water was studied. • Various Concentration, amplitude, sonication times were investigated for exfoliation. • The optimum condition of ultrasonic exfoliation of 60%, 10 mg mL⁻¹ and 15 min. • The best OER activity shows 250 mV overpotential at a current density of 10 mA cm^−1. • Enriched Fe³⁺ were found on the surface of the exfoliated NiFe LDH.