fuels. [1][2][3][4][5] However, as a half reaction, oxygen evolution reaction (OER) involves multiple electron and proton transfer and is considered to be the bottleneck of the overall water splitting. [6] It is of vital importance to develop efficient OER catalysts to accelerate the sluggish reaction and reduce the energy consumption. [7][8][9] Unfortunately, although the noble metalbased catalysts (e.g., IrO 2 , RuO 2 ) have been recognized to be the state-of-the-art OER catalysts, their dearth and high cost greatly impede their scalable application and commercialization. Therefore, developing OER catalysts with low cost as well as high performance is still a great challenge.Earth-abundant transition metal (especially Fe, Co, Ni) oxides or hydroxides, which possess multiple oxidation states, are often regarded as alternatives to precious metal-based catalysts towards OER. [10,11] Among them, NiFe (oxy) hydroxide has been proven to be one of the most effective materials under alkaline conditions. It is worth noting that transition metal oxides or hydroxides are semiconductors with poor intrinsic conductivity, which greatly obstruct their catalytic performance. [12] Thus, different strategies are developed to enhance electron transfer. One common approach is to fabricate metallic precursors (metals, [13] alloys, [14,15] phosphides, [16][17][18] nitrides, [19][20][21] borides [22] ) as precatalysts. The surface would be oxidized to oxide or hydroxide as the real active sites, which is evidenced by the experimental observations after the process of OER. The heterojunction between the metallic core and the (oxy)hydroxide shell is of great benefit to charge transport and OER activity. [23,24] For example, the improved electron transfer could be attributed to the in situformed interface metal/metal hydroxide heterojunction. [23] Coupling with electrically conductive materials (carbon nanotube, [25] graphene [26] ) seems to be another promising method. There are also some studies that investigate how the vacancies increase the conductivity of the electrocatalysts. [27,28] According to density functional theory calculations, introducing oxygen vacancies led to easy excitation of delocalized electron to conduction band, and hence the conductivity was enhanced. [28] On the other hand, the electrocatalytic OER process occurs at the electrode/electrolyte interface, which means that higher value of electrochemical active surface area (ECSA) Efficient electrocatalysts for the oxygen evolution reaction (OER) are highly desirable because of the intrinsically sluggish kinetics of OER. Herein, coreshell structured nanospheres of NiFe x Sn@NiFe (oxy)hydroxide (denoted as NiFe x Sn-A) are prepared as active OER catalysts by a facile electrochemical strategy, which includes electrodeposition of NiFe x Sn alloy nanospheres on carbon cloth (CC) and following anodization. The alloy core of NiFe x Sn could promote charge transfer, and the amorphous shell of NiFe (oxy)hydroxide is defect-rich and nanoporous due to the selective electroch...