A class of 2D layered materials exhibits substantial potential for high‐performance electrocatalysts due to high specific surface area, tunable electronic properties, and open 2D channels for fast ion transport. However, liquid‐phase exfoliation always utilizes organic solvents that are harmful to the environment, and the active sites are limited to edge sites. Here, an environmentally friendly exfoliator in aqueous solution is presented without utilizing any toxic or hazardous substance and active site self‐assembly on the inert base of 2D materials. Benefiting from thin 2D/2D heterostructure and strong interfacial coupling, the resultant highly disordered amorphous NiFe/2D materials (Ti3C2 MXene, graphene and MoS2) thin nanosheets exhibit extraordinary electrocatalytic performance toward oxygen evolution reaction (OER) in alkaline media. DFT results further verify the experimental results. The study emphasizes a viable idea to probe efficient electrocatalysts by means of the synergistic effect of environmentally friendly exfoliator in aqueous solution and active site self‐assembly on the inert base of 2D materials which forms the unique thin 2D/2D heterostructure in‐suit. This new type of heterostructure opens up a novel avenue for the rational design of highly efficient 2D materials for electrocatalysis.

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In this work, Ti3SiC2, layered ternary transition metal carbide called MAX phase, was invoked as the anode material for lithium‐ion batteries. Oxygen‐doped Ti3SiC2, named O‐Ti3SiC2, was produced by calcination in air. The initial reversible capacity was ∼70 mAh g−1 at 10 C, which increased to ∼180 mAh g−1 after 3000 cycles. The capacity was four times higher than original Ti3SiC2, showing a suitable electrochemical performance.

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