Thermally Assisted Photocatalytic Hydrogen Production Using TiO₂/Cu: Evaluation of Performance and Stability

Abstract Photocatalytic hydrogen production offers a sustainable alternative to fossil fuels, especially when combined with solar energy and biomass. Noble metals like platinum (Pt) are efficient but costly and scarce, limiting large‐scale use. Copper (Cu), with its interfacial interaction and plasmonic effects in visible light, presents a viable alternative, despite lower efficiency than Pt. This study investigates TiO₂‐based catalysts doped with low Cu concentrations (0.3%, 0.7%, and 1.1%) for hydrogen production using a photo‐thermal approach. Catalysts were synthesized via photodeposition and characterized using SEM, XRD, BET, XPS, and impedance spectroscopy. A fractional factorial design optimized reaction conditions, including Cu concentration, glycerol concentration, pH, and catalyst dosage. Results showed that 0.7% Cu provided the best balance between hydrogen evolution rate (3,847 µmol g −1 h −1 ) and stability. Thermal effects further enhanced production, reaching 10,421 µmol g −1 h −1 at 70 °C. The XPS analysis revealed a decrease in surface Cu concentration and the predominance of Cu⁰/Cu⁺ species, with no detection of Cu 2 ⁺. The study concludes that photo‐thermal reactions can overcome limitations of non‐noble metal catalysts, positioning Cu as a competitive, sustainable option for hydrogen production.