In this work, we studied new materials free of noble metals that are active in photocatalytic H2 generation from ethanol aqueous solutions (EtOHaq), which can be obtained from biomass. MoxC/g-C3N4 photocatalysts containing hexagonal (hcp) Mo2C and/or cubic (fcc) MoC nanoparticles on g-C3N4 nanosheets were prepared, characterized, and evaluated for photocatalytic hydrogen production from EtOHaq (25% v/v). Tailored MoxC/g-C3N4 nanocomposites with MoxC crystallite sizes in the 4-37 nm range were prepared by treatment with ultrasound of dispersions containing MoxC and g-C3N4 nanosheets, formerly synthesized. The characterization of the resulting nanocomposites, MoxC/g-C3N4, by different techniques, including photoelectrochemical measurements, allowed us to relate the photocatalytic performance of materials with the characteristics of the MoxC phase integrated onto g-C3N4. The samples containing smaller hcp Mo2C crystallites showed better photocatalytic performance. The most performant nanocomposite contained nanoparticles of both hcp Mo2C and fcc MoC and produced 27.9 mmol H2 g-1 Mo; this sample showed the lowest recombination of photogenerated charges, the highest photocurrent response, and the lowest electron transfer resistance, which can be related to the presence of MoC-Mo2C heterojunctions. Moreover, this material allows for easy reusability. This work provides new insights for future research on noble-metal-free g-C3N4-based photocatalysts.
© 2024 The Authors. Published by American Chemical Society.