▎ 摘　　要

NOVELTY - Preparing black phosphorus-activated graphene heterojunction loaded nickel nitride particles involves: (a) carrying out mechanical ball milling on the black phosphorus nanosheet layer material and activating the graphene nanosheet layer material by alkali liquor under the protection of argon for 40-50 hours; respectively washing the obtained 1st precursor with isopropanol, absolute ethyl alcohol and deionized water for 3-5 times, and carrying out vacuum drying on the obtained product; (b) nickel nitrate hexahydrate, ammonium fluoride and urea at molar ratio of 0.5-1:1.5-2.5:3-5, and then placing the mixture into a polytetrafluoroethylene reaction kettle, carrying out hydrothermal reaction, calcining the 2nd precursor in an ammonia atmosphere, and heating; and (c) carrying out mechanical ball milling on the black phosphorus-activated graphene heterojunction material and the nickel nitride particles under the protection of argon for 50-70 hours; washing, and carrying out vacuum drying. USE - The method is useful for preparing black phosphorus-activated graphene heterojunction loaded nickel nitride particles (claimed). ADVANTAGE - The electrocatalytic oxygen evolution activity and the stability of the catalyst are effectively improved, the hydrogen production efficiency is improved, the preparation method is simple, the raw materials are easy to obtain, and the method is suitable for large-scale production. DETAILED DESCRIPTION - Preparing black phosphorus-activated graphene heterojunction loaded nickel nitride particles involves: (a) carrying out mechanical ball milling on the black phosphorus nanosheet layer material and activating the graphene nanosheet layer material by alkali liquor under the protection of argon for 40-50 hours, the mass ratio of the black phosphorus nanosheet layer material to the graphene nanosheet layer material is 1:0.5-1.5, and the set speed of the ball mill is 400-700 revolutions per minute (r/min) to obtain a 1st precursor; respectively washing the obtained 1st precursor with isopropanol, absolute ethyl alcohol and deionized water for 3-5 times, and carrying out vacuum drying on the obtained product at 50-60 degrees C to obtain the black phosphorus-activated graphene heterojunction material; (b) mixing nickel nitrate hexahydrate, ammonium fluoride and urea at molar ratio of 0.5-1:1.5-2.5:3-5, dissolving in deionized water, and then placing the mixture into a polytetrafluoroethylene reaction kettle, carrying out hydrothermal reaction at 140-180 degrees C for 3-5 hours to obtain a 2nd precursor, calcining the 2nd precursor in an ammonia atmosphere, heating at 140-160 degrees C at a rate of 3-5 degrees C/minute, maintaining for 20-30 minutes, heating at 350-380 degrees C at a rate of 1-4 degrees C/minute, maintaining for 40-60 minutes, and naturally cooling to room temperature to obtain nickel nitride particles; and (c) carrying out mechanical ball milling on the black phosphorus-activated graphene heterojunction material and the nickel nitride particles under the protection of argon for 50-70 hours, the mass ratio of the black phosphorus-activated graphene heterojunction material to the nickel nitride particles is 1:0.25-1, and the set speed of the ball mill is 600-800 r/min to obtain a 3rd precursor; respectively washing the obtained 3rd precursor with isopropanol, absolute ethyl alcohol and deionized water for 3-5 times, and carrying out vacuum drying on the obtained product at 40-50 degrees C to obtain the black phosphorus-activated graphene heterojunction loaded nickel nitride particles.