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<p>LaFeO₃ perovskite powders were synthesized by a solid-state reaction assisted by low-energy ball milling. Mechanical treatment of precursor oxides La₂O₃ and Fe₂O₃ (0–8&#xa0;h) prior to calcination at 800&#xa0;°C promoted the formation of orthorhombic LaFeO₃ (<i>Pnma</i>) phase. The as-synthesised samples were characterised using powder X-ray diffraction, Field-Emission Scanning Electron Microscopy, Fourier transform infrared spectroscopy, Mössbauer spectroscopy, and vibrating-sample magnetometry. FESEM indicates the occurrence of a distribution of the particles of irregular grains with an agglomeration of nanometer-sized particles and micrometre-sized agglomerates. After a short time post-milling, micro-strain increased from 0.03 to 0.11%, while crystallite size decreased from 100 to ~ 91 nm, whereas the crystal structure remained unchanged. Magnetic measurements revealed weak ferromagnetic contributions associated with strain-mediated uncompensated spins and a minor fraction of α-Fe₂O₃ impurities. Electrochemical characterization showed pseudocapacitive behavior in both acidic and alkaline solutions. The sample without additional post-milling exhibited the highest specific capacitance and a superior methanol oxidation current, whereas additional milling resulted in slightly reduced conductivity. The overall results indicate that low-energy mechanical activation is an effective and scalable strategy for preparing LaFeO<sub>3</sub>, enabling its use as an electrode material and catalytic support for alcohol oxidation.</p>

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Synthesis and characterisation of perovskite-type LaFeO3 using solid-state reaction assisted by low-energy ball milling

  • 期刊论文

  • 发表日期：

    2026年3月28日

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  • Juan A. Jaén,
  • Fernando Higuera,
  • Oscar Gil,
  • Eduardo Chung,
  • Griselda Caballero-Manrique

摘要

LaFeO₃ perovskite powders were synthesized by a solid-state reaction assisted by low-energy ball milling. Mechanical treatment of precursor oxides La₂O₃ and Fe₂O₃ (0–8 h) prior to calcination at 800 °C promoted the formation of orthorhombic LaFeO₃ (Pnma) phase. The as-synthesised samples were characterised using powder X-ray diffraction, Field-Emission Scanning Electron Microscopy, Fourier transform infrared spectroscopy, Mössbauer spectroscopy, and vibrating-sample magnetometry. FESEM indicates the occurrence of a distribution of the particles of irregular grains with an agglomeration of nanometer-sized particles and micrometre-sized agglomerates. After a short time post-milling, micro-strain increased from 0.03 to 0.11%, while crystallite size decreased from 100 to ~ 91 nm, whereas the crystal structure remained unchanged. Magnetic measurements revealed weak ferromagnetic contributions associated with strain-mediated uncompensated spins and a minor fraction of α-Fe₂O₃ impurities. Electrochemical characterization showed pseudocapacitive behavior in both acidic and alkaline solutions. The sample without additional post-milling exhibited the highest specific capacitance and a superior methanol oxidation current, whereas additional milling resulted in slightly reduced conductivity. The overall results indicate that low-energy mechanical activation is an effective and scalable strategy for preparing LaFeO3, enabling its use as an electrode material and catalytic support for alcohol oxidation.