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<p>Developing efficient catalysts for the electrochemical nitrogen reduction reaction (NRR) under mild conditions remains a key challenge toward sustainable ammonia production. In this work, the microwave-assisted hydrothermal synthesis of Ce-doped Fe<sub>2</sub>(MoO<sub>4</sub>)<sub>3</sub> is reported as an effective and robust electrocatalyst for N<sub>2</sub> reduction. Structural (X-Ray Diffraction and Raman) and compositional characterization (Energy Dispersive Spectroscopy) confirmed the successful incorporation of nominally 2% cerium into the structure with a homogeneous distribution across the bulk catalyst without significantly altering the crystal structure. Electrochemical tests conducted in phosphate buffer (PBS, 0.1&#xa0;mol L⁻¹, pH 7.0) saturated with N<sub>2</sub> demonstrated that the 2% Ce–Fe–Mo sample achieved the highest ammonia production: 12.8 µmol/L and 42% Faradaic efficiency for 2&#xa0;h electrolysis at + 0.022&#xa0;V vs. RHE. Normalization by mass and electrolysis time revealed that this low overpotential electrolysis effectively suppressing hydrogen evolution, provides a twofold increase in NH<sub>3</sub> production compared to similar processes reported at more negative overpotentials. Chronoamperometry (7&#xa0;h) followed by post-electrolysis Raman spectroscopy confirmed electrochemical and structural stability under these conditions. The improved performance is attributed to the synergistic interaction between Mo and Ce facilitating N<sub>2</sub> adsorption and conversion. Ce-doped Fe–Mo oxides are promising candidates for ambient N<sub>2</sub>-to-NH<sub>3</sub> conversion via electrochemical pathways, combining high efficiency, stability, affordability and significant cost-benefit advantage compared to noble-metal-based systems.</p> Graphical Abstract <p></p>

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Microwave-Assisted Hydrothermal Synthesis of Ce-doped Fe2(MoO4)3 for Low Overpotential Electrocatalytic N2-to-NH3 Reduction

  • 期刊论文

  • 出版模式：

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  • 发表日期：

    2026年1月9日

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  • Lara Kelly Ribeiro,
  • Laura Libero,
  • Lucia Helena Mascaro,
  • Frank Marken

摘要

Developing efficient catalysts for the electrochemical nitrogen reduction reaction (NRR) under mild conditions remains a key challenge toward sustainable ammonia production. In this work, the microwave-assisted hydrothermal synthesis of Ce-doped Fe2(MoO4)3 is reported as an effective and robust electrocatalyst for N2 reduction. Structural (X-Ray Diffraction and Raman) and compositional characterization (Energy Dispersive Spectroscopy) confirmed the successful incorporation of nominally 2% cerium into the structure with a homogeneous distribution across the bulk catalyst without significantly altering the crystal structure. Electrochemical tests conducted in phosphate buffer (PBS, 0.1 mol L⁻¹, pH 7.0) saturated with N2 demonstrated that the 2% Ce–Fe–Mo sample achieved the highest ammonia production: 12.8 µmol/L and 42% Faradaic efficiency for 2 h electrolysis at + 0.022 V vs. RHE. Normalization by mass and electrolysis time revealed that this low overpotential electrolysis effectively suppressing hydrogen evolution, provides a twofold increase in NH3 production compared to similar processes reported at more negative overpotentials. Chronoamperometry (7 h) followed by post-electrolysis Raman spectroscopy confirmed electrochemical and structural stability under these conditions. The improved performance is attributed to the synergistic interaction between Mo and Ce facilitating N2 adsorption and conversion. Ce-doped Fe–Mo oxides are promising candidates for ambient N2-to-NH3 conversion via electrochemical pathways, combining high efficiency, stability, affordability and significant cost-benefit advantage compared to noble-metal-based systems.

Graphical Abstract