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[Display omitted] • Hierarchically devised NiFeO x H y catalyst showed high OER activity under alkaline condition. • NiFeO x H y /Ni heterostructure was in-situ formed via a surface reconstruction process. • Charge transfer at the catalyst-electrolyte interface was improved with Fe incorporation into Ni (oxy)hydroxide. • Fe species located at the outer surface of NiOOH structure served as the OER active site. Nickel iron (oxy)hydroxide (NiFeO x H y) is among the most active electrocatalysts for oxygen evolution reaction (OER) in the alkaline media. Development of new design strategy for NiFeO x H y electrode with respect to intrinsic activity and number of active species is highly attractive. Here we report a hierarchical fabrication for NiFeO x H y electrode towards efficient oxygen evolution. Three-dimensional mesoporous NiO was initially prepared and reduced to a polycrystalline Ni metal framework. Despite the poor OER activity for Ni-based catalyst, the incorporation of surface Fe species induced a notably high current density for the oxygen evolution. The results indicated that the Fe species, located at outer surface region, played a key role as the OER active sites. It is also found that the surface of metallic Ni was reconstructed to (oxy)hydroxide phase with ease compared to NiO. As a result, a heterostructure composed of an OER-active NiFe (oxy)hydroxide shell and an electron-conductive Ni core was formed. In this fabricated NiFeO x H y /Ni catalyst, the promoted intrinsic activity, number of active sites and charge-transfer ability all taken into account contribute to an efficient OER process. [ABSTRACT FROM AUTHOR]

• MNi/CNTs with controlled metal distribution was successfully synthesized. • The secondary metal M had profound effects on reducibility and surface property. • CoNi/CNTs showed the best abilities in anti-sintering and coke resistance. • Hydrogen was more selective over CoNi/CNTs by promoting water gas shift reaction. The bimetallic MNi/CNTs (M Co, Cu and Fe) catalysts with controlled metal distribution were prepared by a two-step impregnation method. The catalysts were characterized by N 2 adsorption/desorption, XRD, XPS, TPR, HAADF-STEM, TEM and TG to study the porous structure, changes in crystalline phases during the reaction, surface chemical state, reducibility, the element distribution, sintering of metal particles and the deposited coke for the calcined and/or spent catalysts. The results showed that the Ni oxide was successfully introduced into the cave and the other one was dispersed on the external wall of CNTs. The addition of the secondary metals had significant influences on the reducibility, resulting in the quite different surface properties which was directly linked to the products distribution in glycerol reforming reaction. The sample CoNi/CNTs performed better in both anti-sintering and coke resistance, and over which the product was more selective to hydrogen by enhancing the water gas shift reaction. [ABSTRACT FROM AUTHOR]