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Co-doping two metal elements into diamond-like carbon (DLC) films can reach the desirable combined properties, but the preparation and commercialized application of metal co-doped DLC films with well-defined structural properties are currently hindered by the non-comprehensive understanding of structural evolutions under different process parameters. Here, we fabricated the Ti/Al-DLC films using a unique hybrid ion beam system which enabled the independent control of metal content and carbon structure. The evolutions of microstructure, residual compressive stress and mechanical properties induced by the different process parameters including sputtering currents, C 2 H 2 or CH 4 source gases and bias voltages were investigated systematically in order to perform in-depth analysis on the relation between the structure and properties in Ti/Al-DLC films. Results revealed that the variations of process parameters seriously affected the concentration and chemical bond state of co-doped Ti/Al atoms in amorphous carbon matrix or incident energies of C ions, which brought the complicated effect on amorphous carbon structures, accounting for the change of residual compressive stress, hardness and toughness. The present results provide the guidance for suitable, effective parameters selection to tailor the Ti/Al-DLC films with high performance for further applications. [ABSTRACT FROM AUTHOR]