The invention relates to the field of the synthesis of composite materials, and provides an in-situ preparation method of a three-dimensional conductive MOF@MXene
composite electrode in order to solvethe problem of poor
conductivity of MOFs, which comprises the following steps: adding MAX phase
powder into an HF solution,
etching for 5-24 hours, centrifugally washing with deionized water until the pH value of the upper solution is 6-7, and carrying out
vacuum drying to obtain multilayer MXene
powder; uniformly dispersing the
powder in the deionized water, adding
chloroacetic acid, stirring atroom temperature, adding a NaOH solution, carrying out stirring reaction for 1-12 hours, carrying out centrifugal washing, and carrying out
vacuum drying to obtain MXene-COOH powder; dispersing the powder into the deionized water, adding a
metal salt, a ligand and
ammonia water in order, carrying out air-blowing stirring reaction at 50-70 DEG C, and finally, carrying out centrifugal washing and
drying to obtain the three-dimensional conductive MOF@MXene composite powder. The method is efficient and stable in process and simple in process, the prepared composite powder can serve as a super-
capacitor electrode material, and the stable and efficient
energy storage is achieved.