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<p>The development of pseudocapacitive electrodes with enhanced charge-storage capability is crucial for advancing high-performance electrochemical energy storage devices. In this work, NiO and NiOₓS<sub>γ</sub> thin-film electrodes were directly fabricated via a facile electroless deposition route using ammonium thiosulfate as an in-situ sulfur source to investigate the influence of sulfur incorporation on the microstructure and electrochemical performance. Structural characterization revealed that sulfur incorporation transformed the sparsely distributed NiO nanocrystals into a dense, interconnected mesoporous architecture with increased electrochemically active surface area and improved ion-transport pathways. X-ray diffraction and Raman analyses confirmed the formation of a mixed NiOₓS<sub>γ</sub> phase with sulfur-induced structural defects. Electrochemical measurements demonstrated that sulfur incorporation significantly enhanced the pseudocapacitive behavior, yielding a specific capacitance of 305&#xa0;F g⁻¹ at 10 mV s⁻¹ and 164&#xa0;F g⁻¹ at 0.2&#xa0;mA cm⁻², together with improved charge-transfer kinetics and reduced interfacial resistance compared with pristine NiO. Mott–Schottky analysis further revealed an increased donor density and a more negative flat-band potential, indicating enhanced charge transport characteristics. These results demonstrate that sulfur-induced microstructural and electronic modulation of electroless-deposited NiOₓS<sub>γ</sub> thin films provides an effective strategy for developing scalable, high-performance pseudocapacitive electrodes for next-generation electrochemical energy storage devices.</p>

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Sulfurization-induced microstructural tuning of electroless-deposited NiO thin films for enhanced pseudocapacitive performance

  • 期刊论文

  • 发表日期：

    2026年7月27日

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  • Ghadah M. Al-Senani,
  • Stephen O. Oyetoro,
  • Maruf M. Popoola,
  • Salhah D. Al-Qahtani,
  • Nada S. AlKadhi,
  • Lukman O. Animasahun,
  • Saheed A. Adewinbi

摘要

The development of pseudocapacitive electrodes with enhanced charge-storage capability is crucial for advancing high-performance electrochemical energy storage devices. In this work, NiO and NiOₓSγ thin-film electrodes were directly fabricated via a facile electroless deposition route using ammonium thiosulfate as an in-situ sulfur source to investigate the influence of sulfur incorporation on the microstructure and electrochemical performance. Structural characterization revealed that sulfur incorporation transformed the sparsely distributed NiO nanocrystals into a dense, interconnected mesoporous architecture with increased electrochemically active surface area and improved ion-transport pathways. X-ray diffraction and Raman analyses confirmed the formation of a mixed NiOₓSγ phase with sulfur-induced structural defects. Electrochemical measurements demonstrated that sulfur incorporation significantly enhanced the pseudocapacitive behavior, yielding a specific capacitance of 305 F g⁻¹ at 10 mV s⁻¹ and 164 F g⁻¹ at 0.2 mA cm⁻², together with improved charge-transfer kinetics and reduced interfacial resistance compared with pristine NiO. Mott–Schottky analysis further revealed an increased donor density and a more negative flat-band potential, indicating enhanced charge transport characteristics. These results demonstrate that sulfur-induced microstructural and electronic modulation of electroless-deposited NiOₓSγ thin films provides an effective strategy for developing scalable, high-performance pseudocapacitive electrodes for next-generation electrochemical energy storage devices.