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<p>In this study, we successfully synthesized chlorine self-doped SnO₂ nanomaterials enriched with oxygen vacancies via an in situ carbothermal reduction strategy under a strongly reducing closed atmosphere. Using a tin hydroxy chloride precursor and varying the crucible configuration (open vs. sealed) and carbon black placement, we constructed a localized reducing microenvironment during heat treatment in an air atmosphere. This approach enabled the progressive evolution of chlorine from surface residues to bulk doping. X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) confirmed that chloride ions successfully substituted lattice oxygen sites, inducing high-concentration oxygen vacancies and lattice distortion. Ultraviolet-visible diffuse reflectance spectroscopy (UV-Vis DRS) revealed that the bandgap narrowed from 3.50&#xa0;eV to 3.30&#xa0;eV, extending light absorption into the visible region. Photocurrent and electrochemical impedance spectroscopy (EIS) measurements demonstrated that the synergistic effect of chlorine doping and oxygen vacancies effectively promoted the separation and migration of photogenerated charge carriers. Under visible light irradiation, the optimized sample (S2) exhibited excellent photocatalytic performance for methyl orange (MO) degradation, achieving complete degradation of a 20&#xa0;mg/L MO solution within 45&#xa0;min. Active species trapping experiments indicated that superoxide radicals (•O₂⁻) were the dominant reactive species, followed by holes (h⁺), while hydroxyl radicals (•OH) made the weakest contribution. Combined with band structure calculations and quenching experiments, we elucidated the thermodynamic mechanism underlying reactive species generation. This study provides a new approach for defect engineering in metal oxide photocatalysts. The proposed preparation method is simple and environmentally friendly, showing promising potential for organic pollutant degradation.</p>

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Preparation of chlorine self-doped SnO₂ and its visible-light photocatalytic degradation of methyl orange

  • 期刊论文

  • 发表日期：

    2026年6月27日

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  • Baoyan Liang,
  • YuZhe Wei,
  • Jingtao Wu,
  • JiZhou Zhang,
  • YanLi Zhang

摘要

In this study, we successfully synthesized chlorine self-doped SnO₂ nanomaterials enriched with oxygen vacancies via an in situ carbothermal reduction strategy under a strongly reducing closed atmosphere. Using a tin hydroxy chloride precursor and varying the crucible configuration (open vs. sealed) and carbon black placement, we constructed a localized reducing microenvironment during heat treatment in an air atmosphere. This approach enabled the progressive evolution of chlorine from surface residues to bulk doping. X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) confirmed that chloride ions successfully substituted lattice oxygen sites, inducing high-concentration oxygen vacancies and lattice distortion. Ultraviolet-visible diffuse reflectance spectroscopy (UV-Vis DRS) revealed that the bandgap narrowed from 3.50 eV to 3.30 eV, extending light absorption into the visible region. Photocurrent and electrochemical impedance spectroscopy (EIS) measurements demonstrated that the synergistic effect of chlorine doping and oxygen vacancies effectively promoted the separation and migration of photogenerated charge carriers. Under visible light irradiation, the optimized sample (S2) exhibited excellent photocatalytic performance for methyl orange (MO) degradation, achieving complete degradation of a 20 mg/L MO solution within 45 min. Active species trapping experiments indicated that superoxide radicals (•O₂⁻) were the dominant reactive species, followed by holes (h⁺), while hydroxyl radicals (•OH) made the weakest contribution. Combined with band structure calculations and quenching experiments, we elucidated the thermodynamic mechanism underlying reactive species generation. This study provides a new approach for defect engineering in metal oxide photocatalysts. The proposed preparation method is simple and environmentally friendly, showing promising potential for organic pollutant degradation.