Nanostructured titanium dioxide (TiO2) was synthesized using hy drothermal (HT) and sol-gel (SG) methods with two titanium metal pre cursors: titanium butoxide (TBOT) and titanium isopropoxide (TTIP). The samples were calcinated at different temperatures for two hours under argon (Ar) and oxidative atmospheres. The calcination temperature was chosen for a rutile content of 20 to 25 percent, consistent with the commercial P25 Degussa ma terial. For hydrothermal samples, the optimal calcination temperature under argon was 680 degrees C for TBOT-HT and 710 degrees C for TTIP-HT, while for sol-gel samples, the ideal temperatures were 590 degrees C for TBOT-SG and 570 degrees C for TTIP-SG. These temperatures were also applied for calcination under an oxy gen atmosphere. The titanium oxide was combined with pyrolyzed biomass (B1000) via mechanochemical synthesis, and the nanohybrid was used to pro duce hydrogen by light water splitting. Calcination under argon resulted in the formation of a black material con sisting of titanium dioxide and carbon, as confirmed by Raman spectroscopy. Although XPS did not detect Ti3+ in the black samples, EPR measurements confirmed the presence of oxygen vacancies, along with shifts observed in the Raman spectra. The synthesized materials were characterized using X-ray dif fraction (XRD), diffuse reflectance spectroscopy (DRS), FTIR, scanning elec tron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and electron paramagnetic resonance (EPR). The optimal concentration of pyrolyzed bamboo for forming the hybrid was 8 percent for all the samples. A 15 Hz frequency was used during ball milling for hydrothermal samples, while for sol-gel samples, 50 Hz. Comparing the two metal precursors, TBOT-synthesized samples produced higher H2 (in (micro)mol gcat−1 h−1) than TTIP-synthesized ones. Furthermore, hydrothermal samples demonstrated superior photocatalytic performance. The TBOT-HT sample calcined under argon produced 100.1 (micro)mol gcat−1 h−1, which is 3.6 times the hydrogen production of P25, while the same sample calcined in an oxidative atmosphere generated 328.7 (micro)mol gcat−1 h−1, 11.9 times higher than P25, both using 8 percent B1000 and 15 Hz.