<p>NiO/CeO₂/MoS₂–MoO₃ heterostructured photocatalysts were synthesized via a hydrothermal method and evaluated for photocatalytic hydrogen evolution from formic acid under UV and visible light irradiation. The design strategy integrated oxygen vacancies in CeO₂, sulfur vacancies in MoS₂, and the electron-trapping capacity of Ni/NiO to enhance charge separation and light harvesting. Four compositions (NCM-145, NCM-334, NCM-352, NCM-523) with varied Ni, CeO₂, and MoS₂/MoO₃ mass ratios were comprehensively characterized using TEM, SAED, XRD, UV-DRS, PL, Raman, and XPS analyses. Among these, NCM-334 (3 wt% Ni / 3 wt% CeO₂ / 4 wt% MoS₂) achieved the highest hydrogen production rate (386 µmol g⁻¹ h⁻¹) under UV light, sustained notable activity under visible light, and exhibited an optimal band gap (3.17&#xa0;eV), high crystallinity, and efficient electron–hole separation. PL confirmed reduced recombination, and XPS verified the presence of Ni²⁺, Ce⁴⁺/Ce³⁺, and Mo⁴⁺/Mo⁶⁺ species contributing to redox activity. The optimized NCM-334 achieved a conversion of 91.7% and selectivity of 94.4%, underscoring the critical role of compositional tuning in heterostructure catalysts for sustainable hydrogen production from formic acid.</p> Graphical Abstract <p></p>

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Enhanced Photocatalytic Hydrogen Evolution Via Efficient Electron Transfer Mechanism in Ni/NiO/CeO₂/MoS₂-MoO3 Heterostructures Under UV Light Irradiation

  • Ali İmran Vai̇zoğullar,
  • Mehmet Poyraz,
  • Huseyn Osman,
  • Mehmet Uğurlu

摘要

NiO/CeO₂/MoS₂–MoO₃ heterostructured photocatalysts were synthesized via a hydrothermal method and evaluated for photocatalytic hydrogen evolution from formic acid under UV and visible light irradiation. The design strategy integrated oxygen vacancies in CeO₂, sulfur vacancies in MoS₂, and the electron-trapping capacity of Ni/NiO to enhance charge separation and light harvesting. Four compositions (NCM-145, NCM-334, NCM-352, NCM-523) with varied Ni, CeO₂, and MoS₂/MoO₃ mass ratios were comprehensively characterized using TEM, SAED, XRD, UV-DRS, PL, Raman, and XPS analyses. Among these, NCM-334 (3 wt% Ni / 3 wt% CeO₂ / 4 wt% MoS₂) achieved the highest hydrogen production rate (386 µmol g⁻¹ h⁻¹) under UV light, sustained notable activity under visible light, and exhibited an optimal band gap (3.17 eV), high crystallinity, and efficient electron–hole separation. PL confirmed reduced recombination, and XPS verified the presence of Ni²⁺, Ce⁴⁺/Ce³⁺, and Mo⁴⁺/Mo⁶⁺ species contributing to redox activity. The optimized NCM-334 achieved a conversion of 91.7% and selectivity of 94.4%, underscoring the critical role of compositional tuning in heterostructure catalysts for sustainable hydrogen production from formic acid.

Graphical Abstract