The invention discloses a CuCo-BDC ultrathin nanosheet, a preparation method and application thereof. The preparation method comprises the following steps: dissolving copper chloride dihydrate, cobalt chloride hexahydrate and terephthalic acid in a mixed solution of N, N-dimethylformamide, ethanol and deionized water in an ultrasonic manner; and stirring the solution obtained in the previous step, adding triethylamine in a stirring state, then putting the solution into an ultrasonic machine for ultrasonic treatment, then centrifuging, cleaning the product obtained after centrifuging with ethanol multiple times, and drying to obtain Cu / Co-BDC powder, namely the CuCo-BDC ultrathin nanosheet. According to the invention, the Cu / Co-BDC ultrathin nanosheet with the optimal performance is obtained by regulating and controlling the proportion of metal elements, and then the Cu / Co-BDC ultrathin nanosheet is directly used as a lithium ion battery negative electrode material, wherein the average discharge potential of the material is improved by doping Cu<2+> ions, the Cu<2+> ions and Co<2+> form a bimetal organic framework, and the electrochemical lithium storage performance of the material is further improved through the coordination effect of bimetal ions.