傳統均相芬頓反應可透過 Fe2+ 活化 H2O2 生成具有高氧化能力之氫氧自由基 (•OH)，並有效降解水中有機污染物，然而其仍受限於酸性操作條件、金屬離子不易回收及鐵泥生成等問題。為改善上述限制，開發具可回收性、較寬操作 pH 範圍與表面活性位點可調控之非均相類芬頓試劑，為高級氧化程序應用中的重要研究方向。本研究以釩鉍氧化物作為非均相類芬頓試劑，探討前驅物 V/Bi 比、製程方法對材料晶相、形貌、實際 V/Bi 比、V–O 配位形式對類芬頓染料降解活性之影響，並評估其作為固態類芬頓試劑之可行性。本研究分別以微波水熱法、傳統水熱法與化學沉澱法製備釩鉍氧化物，並利用 XRD、SEM、UV–Vis、ICP-OES、EDS、XPS、Raman 與 EPR 等技術，分析材料之晶體結構、表面形貌、元素組成、局部鍵結、表面化學態與活性氧物種生成行為。結果顯示，釩鉍氧化物在類芬頓反應中降解有機染料能力大於光催化反應，其中含釩 δ-Bi2O3 於甲酸輔助下展現出最佳之類芬頓染料降解能力與使用循環壽命。本研究透過調控類芬頓反應條件，深入探討含釩 δ-Bi2O3 之類芬頓反應與反應活性物種關聯性，解析含釩 δ-Bi2O3 之類芬頓反應機制。

The conventional homogeneous Fenton reaction activates hydrogen peroxide (H2O2) through ferrous ions (Fe2+) to generate highly oxidative hydroxyl radicals (•OH) for the degradation of organic pollutants. However, its application is limited by acidic operating conditions, difficult metal-ion recovery, and iron-sludge generation. Therefore, developing recoverable heterogeneous Fenton-like reagents with broader pH applicability and tunable surface-active sites is important for advanced oxidation processes.In this study, vanadium–bismuth oxides were investigated as heterogeneous Fenton-like reagents. The effects of precursor V/Bi ratio and synthesis method on crystalline phase, morphology, actual V/Bi ratio, V–O coordination, and dye degradation activity were examined. The materials were synthesized by microwave-assisted hydrothermal, conventional hydrothermal, and chemical precipitation methods. Their structural, compositional, surface chemical, and reactive oxygen species characteristics were analyzed using XRD, SEM, UV–Vis spectroscopy, ICP-OES, EDS, XPS, Raman spectroscopy, and EPR spectroscopy.The results showed that vanadium–bismuth oxides exhibited higher dye degradation activity in Fenton-like reactions than in photocatalytic reactions. Vanadium-containing δ-Bi2O3 displayed the best degradation performance and operational lifetime under formic-acid-assisted conditions. By regulating the reaction conditions and identifying the generated reactive species, the relationship between material structure and Fenton-like activity was clarified, and the reaction mechanism of vanadium-containing δ-Bi2O3 was proposed.

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