Three carbon materials (CMs) were prepared for the first time by the mechanochemical reaction of calcium carbide (CaC2) and a transition metal chloride (MCln: FeCl3, ZnCl2, or CuCl). Their composition and structure were characterized, and their electrochemical performance was evaluated by cyclic voltammetry, constant current charge and discharge, cycle life, and ac impedance, respectively. The reactions may occur through a series reaction, i.e., metathesis reaction between CaC(2 )and MCln and self-redox of the resulting metal carbides, forming mesoporous CMs with layered structure and specific area of (160-360 m(2).g(-1)). The CM made from ZnCl2 shows good electrochemical performance and higher specific capacity of 84 F.g(-1) . Further, CMs with better electrochemical performance may be prepared by using other metal halides. This study validates the effectiveness of mechanochemistry for the activation of CaC2 , provides a novel method for CMs synthesis at ambient temperature and mild conditions, and might inspire the development of CaC(2 )chemistry.