The highly active and stable oxygen evolution reaction (OER) performance of Ni-Fe phosphide/metaphosphate (Ni1-xFex-P/PO3) can originate from in situ generated Fe doped γ-NiOOH. The optimized Ni0.75Fe0.25-P/PO3@fCNT catalyst exhibits excellent activity and stability with an overpotential of 239 mV at 10 mA cm-2 and a negligible decrease after 200 h continuous electrolysis in an alkaline solution.