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Nanocrystalline diamond/amorphous composite carbon films were deposited by plasma enhanced chemical vapour deposition method. The concentrations of species in the films were determined by RBS (Rutherford backscattering spectrometry) and ERD (elastic recoil detection) methods. The RBS results showed the main concentrations of C in the films. The concentration of hydrogen was approximately 20 at.%. Chemical compositions were analyzed by FTIR spectroscopy. IR results showed the presence of C-H specific bonds. Film was used for photocathode application. The original quantum efficiency of prepared photocathode at energy of FH 15,6 mJ was 1,43 × 10-6 %.