Photocatalytic water splitting using solar radiation has drawn considerable attention for production of hydrogenbecause of minimal carbon emissions, however huge limitations that still exist are low light harnessing catalysts and high recombination rate of the photo-generated charge carriers. This study focuses on the fabrication of nanomaterials for advanced photocatalytic water splittingas a result, structures of TiO2/CNFs, Cu/TiO2/CNFs, and Zn/TiO2/CNFs nanocomposites of mesoporous nature were synthesized using CNFs and surfactant wrapping sol–gel/hydrothermal method. Impregnation technique was used in copper and zinc loading while characterization of the synthesized catalysts was achieved by XRD, Raman, FESEM, TEM, UV/DRS, BET, FTIR, XPS, and PL techniques. Water splitting was performed byUV light irradiation and the effect of compositing TiO2/CNFs-Cu/Znevaluated. 10 %_TiO2/CNFs/5%Zn composite was the most efficient photocatalyst for hydrogen production when compared with the rest of the samples. 10 %_TiO2/CNFs/5%Zn, 0.53 mol (h g cat.)-1, was 90–100 folds the amount generated over commercial TiO2 – P25, and pure TiO2photocatalysts. The improved photo-activity of the TiO2/CNFs, Cu/TiO2/CNFs, and Zn/ TiO2/CNFs composites were due to the synergistic effect between Cu, Zn and CNFs.This work gives promising route for fabricating TiO2/CNFs/metal (Cu, Zn) composites for advanced H2production using UV-radiation.