Nickel diamond-like (Ni-DLC) composite electrodes with different Ni contents were prepared on pure Ti substrate by high power pulsed magnetron sputtering technology, which was used to construct enzyme-free glucose sensor. The surface morphology, microstructure and electrochemical performance of Ni-DLC composite electrode were characterized by X-ray diffractometer, atomic force microscope, Raman spectrometer and electrochemical workstation. The results show that: (1) with the increase of Ni content, the particle protrusion on the surface of Ni-DLC film increases gradually, and the diameter of agglomeration particles also increases, which significantly increases the active sites on the surface of Ni-DLC film. The content of sp2 bond in Ni-DLC film increases, the order degree of the film increases, and the conductivity of the film is improved. No obvious Ni-C bond is formed in the film, and Ni mainly exists in elemental form. (2) Glucose sensor made of Ni-DLC composite electrode was placed in glucose solution for testing, and the results showed that: Ni-DLC composite electrode has a good catalytic effect on glucose, electrode reaction is mainly controlled by diffusion, oxidation peak current density and glucose concentration has a good linear relationship, Ni-DLC composite electrode for glucose detection sensitivity of 796 μAmM-1cm-2, the lower limit of detection LOD = 0.5 μM, The response time is 5 s, and the electrode has good anti-interference performance for uric acid and ascorbic acid. The electrode has a broad application prospect in the construction of enzyme-free glucose sensor.