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In this study, a Nb layer was deposited on Ti-6.5Al–2Zr–1Mo–1V alloys by the double glow plasma alloying technique and the effect of pre-diffusion of Nb in the Nb–N films on microstructure and mechanical properties was analyzed. The structure of pre-diffusion samples is characteristic of a thick inter-diffusion layer and a nitride gradient layer. This novel structure is beneficial for relieving the residual stress at the preparation process and the stress field were redistributed during loading because the properties were changed gradually along with the depth. In addition, the pre-processing of diffusion is believed to effectively increase the nitrogen permeation rate and further alter the Ti diffusion path, subsequently achieving the changed structure and phase composition of the Nb–N co-diffusion layer. Ball-on-disc wear tests were carried out at different loads for pre-diffusion and co-diffusion samples. The pre-diffusion sample and counter-ball all showed slighter damage than that of the co-diffusion sample. Image 1 • The pre-processing of Nb diffusion was performed, and the effect of pre-diffusion Nb for Nb-N co-diffusion was discussed in detail. • The Rietveld refinement method was used to further analyze the phase information. • The ratio of elastic work to plastic work was used to evaluate the load capacity of modified layer. • The wear track morphologies of modified sample and ball were observed to investigate the wear behavior. [ABSTRACT FROM AUTHOR]