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In this contribution, 2D Ni/Fe MOF nanosheets were synthesized by a simple two-step ultrasound strategy at room temperature, i.e. the 2D Ni-MOF with a lamellar structure was first synthesized by the top-down ultrasonic assisted stripping route, followed by introducing Fe3+ ions as a metal node and terephthalic acid as an organic ligand to form 2D Ni/Fe MOF nanosheets that exhibited weak oxidase-like and strong peroxidase-like properties. Relative to that of the single metal Ni-MOF and Fe-MOF, the peroxidase-mimicking capability of the