Abstract: Nickel-phosphorus-titanium silicalite zeolite (Ni-P-HTS-1/NF-T) composite was prepared by electroless composite plating and in-situ treatment process with hierarchical titanium silicalite (HTS-1) zeolite as composite phase and nickel foam (NF) as matrix materials, and its electrocatalytic oxygen evolution reaction (OER) performance was studied. The results show that Ni-P-HTS-1/NF-T composite has faster OER kinetics and electron transfer rate, excellent OER performance and long-term stability in 1.0 mol/L KOH electrolyte. The doping of HTS-1 zeolite and in-situ treatment process reduce the electron transfer resistance of Ni-P-HTS-1/NF-T composite, increase its electrocatalytic active surface area, and change the chemical composition of the composite to form nickel phosphide and hydroxide which can provide catalytic active centers for electrocatalytic oxygen evolution reaction, thus effectively improving the OER performance of Ni-P-HTS-1/NF-T composite.