Development of low‐cost, high‐performance, and bifunctional electrocatalysts for water splitting is essential for renewable and clean energy technologies. Although binary phosphides are inexpensive, their performance is not as good as noble metals. Adding a third metal element to binary phosphides (Ni‐P, Co‐P) provides the opportunity to tune their crystalline and electronic structures and thus their electrocatalytic properties. Here, ternary phosphide (NiCoP) films with different nickel to cobalt ratios via an electrodeposition technique are synthesized. The films have a triple‐layered and hierarchical morphology, consisting of nanosheets in the bottom layer, ≈90–120 nm nanospheres in the middle layer, and larger spherical particles on the top layer. The ternary phosphides exhibit versatile activities that are strongly dependent on the Ni/Co ratios and Ni0.51Co0.49P film is found to have the best electrocatalytic activities for both hydrogen evolution reactions and oxygen evolution reactions. The high performance of the ternary phosphide film is attributed to enhanced electric conductivity so that reaction kinetics is accelerated, enlarged surface area due to the hierarchical and three‐layered morphology, and increased local electric dipole so that the energy barrier for the water splitting reaction is lowered.

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The coordination of valeric acid (VA), glutaric acid (GA), and tricarballylic acid (TA) with Fe−OH on the Fe 3 O 4 nanoparticle surface has been systematically studied to elucidate the effects of COOH, molecular configuration, and ligand concentration on the coordination by the combined use of attenuated total reflectance Fourier transform infrared (ATR-FTIR) and thermogravimetric analysis (TGA). The results show that the binding ability of the acids increases with the increase in the COOH number. Multiple conformations coexist for the dicarboxylic and tricarboxylic acid coordinated on the iron oxide NPs. Saturated coordination formed with only a one-, two-, or three-COOH conformation for VA, GA, and TA, respectively, occurs under ligand-scarce conditions, while unsaturated coordination formed with the mixture of uncoordinated, one-, and/or two-COOH conformations for VA, GA, and TA, respectively, exists under ligand-abundant conditions. The maximum coordination numbers for monolayer adsorption for VA, GA, and TA on Fe 3 O 4 NPs are 9, 2.4, and 2.7 nm −2 , respectively. This study helps us to understand the fine coordination mechanism caused by the acid molecules with different configurations and elucidates, for the first time, the fine conformational variance incurred by the surrounding ligand with different concentrations and the way in which the ligand is added.