A new high efficient and non-destructive mental activation process of electroless composite plating was proposed. The process utilized electromagnetic induction equipment to heat the titanium alloy substrate and used its energy to complete the activation process, which could successfully attach the nickel nanoparticles firmly to the surface of the titanium alloy; at the same time, the process pre-activated Al 2O 3 nanoparticles and added the activated nanoparticles to the plating solution. In the process of plating, the activated titanium substrate was used as the catalytic center of electroless nickel plating (ENP) for electroless composite plating. The new activation process avoided complicated traditional processes such as acid etching and zinc dipping. Such traditional processes require huge doses of chemicals, including various strong acids, so improper waste liquid treatment will cause harm to the environment. The important parameters of the process were optimized by orthogonal experiments. A scanning electron microscope (SEM), an X-ray photoelectron spectroscopy (XPS), an energy dispersive spectrometer (EDS), thermal shock experiments and friction and wear experiments were used to characterize and analyze the surface morphology, composition, binding force and friction coefficient of the coating, and analyze the coating quality by measuring the plating rate and the thickness of the coating. The results showed that the rate of electroless composite plating increased with the increase in Al 2O 3 nanoparticle concentration. When the concentration of Al 2O 3 nanoparticles reached 1.5 g/L, the ENP rate decreased with the increase in Al 2O 3 nanoparticle concentration. The adhesion of the sample was evaluated by the scratch test, which showed that the binding grade of the sample was 0, and the Vickers hardness was 688.5 HV. Results showed that the coating produced by this new process has excellent performance. Therefore, the process is an environmentally friendly and fast activation composite plating process.