▎ 摘　　要

NOVELTY - Preparing three-dimensional nanoporous graphene-coated metal oxide/hydroxide/sulfide composite in situ comprises e.g. preparing multi-component nanoporous metal NixCu30-xMn70 or NixCo30-xMn70 multi-component alloy foil, then chemically de-alloying to form a bicontinuous three-dimensional nanoporous structure, washing and drying to obtain nanoporous metal having an initial pore structure, growing (nitrogen-doped) graphene on the surface of nanoporous metal, placing the nanoporous metal of the initial pore structure into the quartz boat and placing the quartz boat in the outer region of the reaction quartz tube in the furnace, then introducing hydrogen and argon with the gas flow ratio of hydrogen:argon, adjusting the pressure of the gas mixture system, increasing the furnace temperature, moving the quartz boat into the high temperature zone in the middle of the furnace and calcining at this temperature, then introducing ammonia, acetylene or methane, hydrogen and argon. USE - The method is useful for preparing three-dimensional nanoporous graphene-coated metal oxide/hydroxide/sulfide composite in situ. DETAILED DESCRIPTION - Preparing three-dimensional nanoporous graphene-coated metal oxide/hydroxide/sulfide composite in situ comprises (i) preparing multi-component nanoporous metal NixCu30-xMn70 or NixCo30-xMn70 multi-component alloy foil, where x has a value of 0-30, then chemically de-alloying to form a bicontinuous three-dimensional nanoporous structure, washing and drying to obtain nanoporous metal having an initial pore structure; (ii) growing (nitrogen-doped) graphene on the surface of the nanoporous metal, placing the nanoporous metal of the initial pore structure into the quartz boat and placing the quartz boat in the outer region of the reaction quartz tube in the furnace, then introducing hydrogen and argon with the gas flow ratio of hydrogen (100 -200 sccm):argon (200-500sccm), adjusting the pressure of the gas mixture system to 20 Torr, increasing the furnace temperature to 600-1000 degrees C, quickly moving the quartz boat into the high temperature zone in the middle of the furnace when the furnace is raised to the specified temperature and calcining at this temperature for 1-30 minutes, then introducing ammonia, acetylene or methane, hydrogen and argon, where the gas flow ratio of ammonia (0-50 sccm): acetylene or methane (5-50 sccm):hydrogen (100-200 sccm): argon (200-500 sccm) and reacting at this temperature for 3-10 minutes, then quickly moving the quartz boat from the high temperature zone in the middle of the furnace to the low temperature zone outside the furnace, and is rapidly cooling in a pure argon atmosphere after the temperature of the reaction tube is lowered to room temperature, opening the furnace cover and taking the sample out from the quartz boat to obtain composite structure of three-dimensional nitrogen-doped graphene-coated nanoporous metal; (iii) partially etching of the three-dimensional nitrogen-doped graphene-coated nanoporous metal by configuring with a 0.5-6 M (2-3 M) hydrochloric acid solution and uniformly stirring the mixture with the solution, then pacing the three-dimensional nitrogen-doped graphene-coated nanoporous metal composite structure in the solution at a constant temperature of 20-100 degrees C (preferably 40-60 degrees C) with the treatment time is 1-24 hours (2-8 hours, then repeatedly washing the mixture with deionized water and absolute ethanol for many times, then placing in a vacuum drying oven to be dried to obtain three-dimensional nitrogen-doped graphene-coated partial nanoporous metal composite structure; and (iv) using sulfation solution required for in-situ growth configuration of metal oxide/hydroxide/sulfide:0.1-5 M sodium sulfide or thiourea solution or oxidation/hydrogenation solution of 1-30 wt.% of hydrogen peroxide, then uniformly stirring and uniformly mixing the solution, then pouring the composite structure of the three-dimensional nitrogen-doped graphene-coated partial nanoporous metal into the lining of the hydrothermal reaction kettle together with the prepared sulfurization or oxidation/hydrogenation solution, then installing the hydrothermal reaction reactor, tightening and placing in a blast oven for water heat at the temperature of 50-200 degrees C for 5-35 hours, cooling the hydrothermal kettle to room temperature, opening, taking out the sample, washing and vacuum drying.