Design and fabrication of 2D multi-metal oxalate materials with desired electrochemical activities are highly needed in electrocatalysis and supercapacitors. Herein, assisted by the deep eutectic solvothermal (DES) method, multi-metal oxalate consisting of Fe, Co, Ni, Cu, and Zn with different morphology was the controlled synthesis. It was found that the structure and composition of DES can control the nucleation and growth of multi-metal oxalate. High molecular PEG and gradually slow-release oxalic acid are in favor of the formation of 2D structure, while the low molecular EG and abundant oxalic acid are positive for the formation of 3D nanoparticles. The properties of the obtained multi-metal oxalates are confirmed by multi-analysis, which involves the single Ni-oxalate phase, morphological evolution ranging from particles to nanosheets, and complex composition up to five metal elements including Fe, Co, Ni, Cu as well as Zn. Notably, the well-designed 2D (FeCoNiCuZn)(C2O4)·2H2O nanosheets exhibit an ultralow overpotential of 334 mV at 100 mA cm−2 for OER as electrocatalyst with prolonged durability over 30 h at 10 mA cm−2 and a high specific capacity of 1337 C g−1 for aqueous supercapacitor.
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