A gas/liquid interface will be formed when the free volatilized methyl aldehyde gas begins to dissolve in to solution. On the basis of the traditional silver mirror reaction, silver nanoparticle-manganese oxyhydroxide-graphene oxide (Ag-MnOOH-GO) nanocomposite was synthesized at the gas/liquid interface without any protection of inert gas at room temprature. The morphology of the nanocomposites could be controlled by adjusting the reaction temperature and time. The morphology and composition of the nanocomposites were characterized by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, and Fourier transform infrared spectroscopy. The composites were then applied for electrochemical sensing. The electrochemical investigation for the sensor indicates that it has excellent property to catalyze H2O2, and could detect H2O2 with a low detection limit of 0.2μM and wide linear range of 0.5 μM to 17.8 mM. The present study provides a general platform for the controlled synthesis of nanomaterials and can be extended to other optical, electronic, and magnetic nanocompounds.

Tetrahedral NiS2/NiSe2 heterocages with rich‐phase boundaries are synthesized through a simultaneous sulfuration/selenylation process using Ni‐based acetate hydroxide prisms as precursor. Such a nanocage‐like NiS2/NiSe2 heterostructure can expose more active sites, accelerate the mass transport of the ions/gas, and optimize the interfacial electronic structure, which shows a significantly lower overpotential of 290 mV at 20 mA cm−2 than those of NiS/NiS2 and NiSe2 as counterparts. The experimental characterizations and theoretical density functional theory (DFT) calculations unveil that the interfacial electron transfer from NiSe2 to NiS2 at the heterointerface can modulate the electronic structure of NiS2/NiSe2, which further cooperates synergistically to change the Gibbs free energy of oxygen‐containing intermediates as the rate‐determining step (RDS) from 2.16 eV (NiSe2) and 2.10 eV (NiS2) to 1.86 eV (NiS2/NiSe2 heterostructures) during the oxygen evolution reaction (OER) process. And as a result, tetrahedral NiS2/NiSe2 heterocages with dual‐phase synergy efficiently trigger the OER process, and accelerate the OER kinetics. This work provides insights into the roles of the interfacial electron transfer in electrocatalysis, and can be an admirable strategy to modulate the electronic structure for developing highly active electrocatalysts.

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