| Photocatalytic/electrocatalytic hydrogen production is considered to be an effective way to develop clean new energy.In this paper,3D hierarchical NiO/CdS hollow microspheres and C@NiO/CdS hollow microspheres were constructed by green microwave-assisted chemical synthesis technology based on 3D hierarchical NiO hollow microspheres.The performance of visible light photocatalytic hydrogen evolution with enhanced structure was evaluated.In addition,the 3D NiO/Ni hollow microspheres were prepared by hydrogenation heat treatment and their electrocatalytic hydrogen evolution performance was evaluated.The specific research content is as follows:(1)0D/3D CdS/NiO hollow microspheres were successfully prepared by using green microwave-assisted technology by Cd(CH3COO)2·2H2O as cadmium source,H2NCSNH2 as sulfur source,and C2H8N2 as surfactant.0D CdS nanoparticles were successfully anchored on 3D NiO hollow microspheres.The diameter of the composite nanomaterial is 800nm-1.2μm,and the CdS particles of 20-40nm are evenly distributed on the surface of NiO.By visible light photocatalytic hydrogen evolution test,the rate of the composite nano-material with the optimal composition ratio is 1.77 mmol/g/h,which is 16.2 times higher than that of the pure CdS nanoparticles.The composite material exhibitied good photocatalytic activity and stability.(2)C@NiO/CdS hollow microspheres were prepared by green microwave-assisted chemical synthesis using glucose as carbon source.The composite retains the 3D hierarchical hollow microspheres structure,and amorphous carbon is evenly distributed on the surface by a series of characterization methods.The performance test of visible light photocatalytic hydrogen evolution shows that the rate of the composite nanomaterials with the optimal component ratio is 17.99 mmol/g/h,which is 10 times higher than that of NiO/CdS hollow microspheres.The surface electric field formed between amorphous carbon and NiO/CdS promoted the photocatalytic hydrogen evolution.(3)3D NiO/Ni hollow microspheres were prepared by hydrogenation heat treatment technology.The composite has a unique 3D hierarchical hollow structure and Ni metal elements are uniformly distributed on the surface of NiO porous nanosheets.The electrocatalytic hydrogen evolution performance was evaluated in alkaline electrolyte,and it was found that the composite nanomaterials with hydrogenation time of 60 minutes had the best performance,with overpotential of-376 mV and Tafel of 145 mV/Dec at the current density of 10 mA/cm2.Meanwhile,NiO/Ni hollow microspheres have good electrochemical cycling stability. |