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<p>Amorphous MoS<sub>2</sub> has recently attracted attention as an electronically active interlayer in multi-component electrocatalysts, but its role in finely engineered NiFe-LDH/sulfide architectures remains insufficiently understood. In this work, we design and fabricate a hierarchical NiFe-LDH/MoS<sub>2</sub>/Ni<sub>3</sub>S<sub>2</sub>@Ni-foam anode in which each layer is introduced in a stepwise and function-oriented manner: crystalline Ni<sub>3</sub>S<sub>2</sub> is first grown on Ni foam via thiourea-assisted hydrothermal sulfidation, an ultrathin MoS₂ film is then conformally deposited by DC sputtering, and finally NiFe-LDH nanosheets are hydrothermally assembled on top of the MoS<sub>2</sub>/Ni<sub>3</sub>S<sub>2</sub> scaffold. X-ray diffraction and field-emission scanning electron microscopy confirm the formation of a crystalline Ni<sub>3</sub>S<sub>2</sub> backbone decorated with sheet-like NiFe-LDH, while the sputtered MoS<sub>2</sub> remains XRD-silent but is confirmed as an amorphous MoS<sub>2</sub> phase by XPS and Raman spectroscopy, supporting its role as an electronically active interlayer. Electrochemical measurements in 1.0&#xa0;M KOH reveal that the tri-layered NiFe-LDH/MoS<sub>2</sub>/Ni<sub>3</sub>S<sub>2</sub>@NF electrode outperforms control electrodes (Ni<sub>3</sub>S<sub>2</sub>@NF, MoS<sub>2</sub>/Ni<sub>3</sub>S<sub>2</sub>@NF, NiFe-LDH@NF, NiFe-LDH/Ni<sub>3</sub>S<sub>2</sub>@NF, and NiFe-LDH/MoS<sub>2</sub>@NF), delivering the lowest overpotentials at 50 and 100&#xa0;mA·cm<sup>−2</sup>, the smallest Tafel slope, and the lowest charge-transfer resistance. The optimized electrode also exhibits the largest double-layer capacitance (2.87 mF) and electrochemically active surface area (71.8 cm<sup>2</sup>), indicating a greatly increased density of accessible active sites. A 100&#xa0;h chronopotentiometric test at 50&#xa0;mA·cm<sup>−2</sup> yields a potential retention of 98.49% and an exceptionally low degradation rate of 0.246&#xa0;mV·h<sup>−1</sup>, demonstrating excellent durability. These results show that the amorphous MoS<sub>2</sub> interlayer functions as an effective electronic bridge between the Ni<sub>3</sub>S<sub>2</sub> backbone and the NiFe-LDH shell, simultaneously enhancing charge transport, promoting the formation of high-valent NiFe (oxy)hydroxides, and stabilizing the multi-layered architecture for efficient alkaline oxygen evolution. </p>

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Amorphous MoS2 as an electronic bridge in NiFe-LDH/MoS2/Ni3S2@Ni-foam hierarchical electrodes for enhanced alkaline oxygen evolution

  • 期刊论文

  • 发表日期：

    2026年3月13日

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  • Tae Kwang An,
  • Yun Seok Jang,
  • Donghyeon Lee,
  • Yong Jin Jeong,
  • Jeong Ho Ryu

摘要

Amorphous MoS2 has recently attracted attention as an electronically active interlayer in multi-component electrocatalysts, but its role in finely engineered NiFe-LDH/sulfide architectures remains insufficiently understood. In this work, we design and fabricate a hierarchical NiFe-LDH/MoS2/Ni3S2@Ni-foam anode in which each layer is introduced in a stepwise and function-oriented manner: crystalline Ni3S2 is first grown on Ni foam via thiourea-assisted hydrothermal sulfidation, an ultrathin MoS₂ film is then conformally deposited by DC sputtering, and finally NiFe-LDH nanosheets are hydrothermally assembled on top of the MoS2/Ni3S2 scaffold. X-ray diffraction and field-emission scanning electron microscopy confirm the formation of a crystalline Ni3S2 backbone decorated with sheet-like NiFe-LDH, while the sputtered MoS2 remains XRD-silent but is confirmed as an amorphous MoS2 phase by XPS and Raman spectroscopy, supporting its role as an electronically active interlayer. Electrochemical measurements in 1.0 M KOH reveal that the tri-layered NiFe-LDH/MoS2/Ni3S2@NF electrode outperforms control electrodes (Ni3S2@NF, MoS2/Ni3S2@NF, NiFe-LDH@NF, NiFe-LDH/Ni3S2@NF, and NiFe-LDH/MoS2@NF), delivering the lowest overpotentials at 50 and 100 mA·cm−2, the smallest Tafel slope, and the lowest charge-transfer resistance. The optimized electrode also exhibits the largest double-layer capacitance (2.87 mF) and electrochemically active surface area (71.8 cm2), indicating a greatly increased density of accessible active sites. A 100 h chronopotentiometric test at 50 mA·cm−2 yields a potential retention of 98.49% and an exceptionally low degradation rate of 0.246 mV·h−1, demonstrating excellent durability. These results show that the amorphous MoS2 interlayer functions as an effective electronic bridge between the Ni3S2 backbone and the NiFe-LDH shell, simultaneously enhancing charge transport, promoting the formation of high-valent NiFe (oxy)hydroxides, and stabilizing the multi-layered architecture for efficient alkaline oxygen evolution.