The invention discloses a Cu-Fe bimetallic nanosheet and a preparation method thereof. The preparation method comprises the following steps of 1, preparing a NaOH solution, specifically, dissolving NaOH in a beaker with deionized water, after the solution is cooled, transferring the solution to a volumetric flask, and conducting washing, volume fixing and uniform shaking for laer use; 2) preparinga Cu salt solution and a Fe salt solution, specifically, respectively dissolving a Cu salt and a Fe salt in different beakers by using deionized water, respectively transferring the two solutions todifferent volumetric flasks after the Cu salt and the Fe salt are completely dissolved, and conducting washing, volume fixing and uniform shaking for later use; 3) putting the NaOH solution prepared in the step 1) into a flask, adding the Cu salt solution and the Fe salt solution prepared in the step 2) into the single-neck flask, then adding a complexing agent and a reducing agent, conducting uniform mixing, and conducting heating in a water bath; and (4) after water bath heating in the step (3) is finished, subjecting a reaction product to centrifugal separation, and conducting drying to obtain a product, namely, the CuFe bimetallic nanosheet. The prepared CuFe bimetallic nanosheet has excellent catalytic performance in the aspect of catalyzing degradation of Congo red, and the degradation rate of the prepared Cu0.6Fe0.4 nanosheet for catalyzing the Congo red reaches 97%.