The invention discloses a core/shell structure Ti3C2 ene/Cu powder and a preparation method thereof. By using the chemical plating technology, Ti3C2 ene is used as a carrier, and the surface of the Ti3C2 ene is wrapped by one layer of shell film composed of copper particles. A plating solution is mainly composed of copper sulfate pentahydrate, ethylenediamine tetraacetic acid disodium and 2,2'-bipyridine, a reducing agent is hydrazine hydrate, the reaction temperature is 45-95 DEG C, and pH is controlled at 9-13. The process is simple, cost is low, the core/shell structure Ti3C2/Cu powder canbe stably acquired within short time, it is not needed to perform roughening, sensitization, activation and other pre-treatment on a substrate, the thickness of a plated film and the particle size canboth be adjustable, and thus, a core/shell nanocomposite in different properties can be prepared. The core/shell powder has broad application prospects in the aspects of catalysis, optics, electromagnetics and the like. The method is also applicable to MXene/metal powder in other core/shell structures, and (MXene comprises M2Xene, M3X2ene, M4X3ene and the like; and shell layer metal comprises Cu,Ni, Sn, Co and the like).