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<p>In this study, NiFe-based layered double hydroxide (LDH) nanocrystals with different Pd content were synthesized via the sol-gel hydrothermal method using polyvinyl alcohol as a surfactant. The resulting material was thoroughly characterized using XRD, ATR-FTIR, HRTEM, FESEM, EDS, and TGA analyses. XRD analysis revealed that Pd<sup>2+</sup> incorporation improves crystal grain ordering and growth, as indicated by narrowing full width at half maximum with increasing Pd<sup>2+</sup> concentrations. FESEM imaging showed that Pd incorporation alters the crystal growth mechanism, resulting in dynamic changes to particle size, shape, and surface texture. Thermal and kinetic studies revealed relationships among activation energy (E<sub>a</sub>), residual organic components, and activation free energy (ΔG<sup>*</sup>), with citrate/PVA moiety. This study highlights the potential of Pd-modified NiFe-LDH composites for advanced electrocatalytic applications. Electrochemical impedance spectroscopy (EIS) and cathodic polarization were used to evaluate the hydrogen evolution reaction (HER) for the various materials in an alkaline solution (1.0 M KOH). According to the results, electrocatalytic performance for alkaline HER is improved by adding trace amounts of Pd<sup>2+</sup> ions to NiFe-based layered double hydroxide. The presence of less amount Pd in the NiFe-LDH matrix decreases the hydrogen overpotential at 10 mA cm<sup>-2</sup> (<i>η</i><sub>10</sub>) from 0.1869 for NiFe-LDH to 0.1739 V for Pd<sub>0.1</sub>Ni<sub>0.9</sub>Fe-LDH, and enhances the catalytic activity of NiFe-LDH to HER more than the Pd<sub>0.2</sub>Ni<sub>0.8</sub>Fe-LDH (<i>η</i><sub>10</sub> = 0.2109 V) and Pd<sub>0.3</sub>Ni<sub>0.7</sub>Fe-LDH (<i>η</i><sub>10</sub> = 2099 V) electrodes. Additionally, as compared to the <i>R</i><sub>ct</sub> measured for the other electrodes under investigation, the Pd<sub>0.1</sub>Ni<sub>0.9</sub>Fe-LDH/NF electrode exhibits the lowest resistance for H<sub>2</sub> evolution. The superior HER activity of the Pd<sub>0.1</sub>Ni<sub>0.9</sub>Fe-LDH catalyst in alkaline environments can be attributed to a synergistic interplay of its structural, electronic, and catalytic characteristics.</p> Graphical Abstract <p></p>

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Understanding the impact of Pd content on the electrocatalytic performance of Pd-NiFe LDH as an efficient cathode materials for alkaline hydrogen evolution reaction

  • 期刊论文

  • 发表日期：

    2026年1月8日

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  • Ibraheem O. Ali,
  • H. H. Mohamed,
  • M. M. El-Rabiei,
  • Ebtsam K. Alenezy,
  • Karam S. El-Nasser,
  • A. Ibrahim,
  • H. Nady

摘要

In this study, NiFe-based layered double hydroxide (LDH) nanocrystals with different Pd content were synthesized via the sol-gel hydrothermal method using polyvinyl alcohol as a surfactant. The resulting material was thoroughly characterized using XRD, ATR-FTIR, HRTEM, FESEM, EDS, and TGA analyses. XRD analysis revealed that Pd2+ incorporation improves crystal grain ordering and growth, as indicated by narrowing full width at half maximum with increasing Pd2+ concentrations. FESEM imaging showed that Pd incorporation alters the crystal growth mechanism, resulting in dynamic changes to particle size, shape, and surface texture. Thermal and kinetic studies revealed relationships among activation energy (Ea), residual organic components, and activation free energy (ΔG*), with citrate/PVA moiety. This study highlights the potential of Pd-modified NiFe-LDH composites for advanced electrocatalytic applications. Electrochemical impedance spectroscopy (EIS) and cathodic polarization were used to evaluate the hydrogen evolution reaction (HER) for the various materials in an alkaline solution (1.0 M KOH). According to the results, electrocatalytic performance for alkaline HER is improved by adding trace amounts of Pd2+ ions to NiFe-based layered double hydroxide. The presence of less amount Pd in the NiFe-LDH matrix decreases the hydrogen overpotential at 10 mA cm-2 (η10) from 0.1869 for NiFe-LDH to 0.1739 V for Pd0.1Ni0.9Fe-LDH, and enhances the catalytic activity of NiFe-LDH to HER more than the Pd0.2Ni0.8Fe-LDH (η10 = 0.2109 V) and Pd0.3Ni0.7Fe-LDH (η10 = 2099 V) electrodes. Additionally, as compared to the Rct measured for the other electrodes under investigation, the Pd0.1Ni0.9Fe-LDH/NF electrode exhibits the lowest resistance for H2 evolution. The superior HER activity of the Pd0.1Ni0.9Fe-LDH catalyst in alkaline environments can be attributed to a synergistic interplay of its structural, electronic, and catalytic characteristics.

Graphical Abstract