電催化甘油氧化反應是一個結合陰極電解水產氫與陽極電解甘油產出高價值產物的熱門領域。在此，本研究使用光化學金屬有機沉積法(PMOD method)，合成出非晶相鎳氧化物(NiOx)作為電陽極使用，並於甘油-四硼酸鈉電解液中施加電位1.75 V vs. RHE，得到了 2.9 mA/cm-2 的電流密度，以及高價值產物包含 41%的甘油醛(GLAD)與 37%的二羥基丙酮(DHA)。
此外，筆者探討晶相/非晶相材料對於電化學表現、產物分佈的差異，顯示非晶相材料的確展現出更好的表現與發展前景。並透過一系列 pH 值調整、輔助電解質選擇與濃度調整、甘油濃度調整等測詴，表明產出高選擇性之高價值產物，其關鍵包含適切的酸鹼值(以利 DHA、GLAD 穩定留存)，以及良好的輔助電解質-四硼酸鈉，解離出豐富的陰離子型態以提供電催化活性與反應動力學。並在後續章節最佳化四硼酸鈉-甘油電解液之組合，發現兩者之濃度適當提升，分別有益於 DHA、GLAD 的產率增加，這可能揭露了硼酸根離子與甘油的交互作用現象。
最後，透過結合電化學系統與拉曼光譜儀的原位拉曼光譜(in-situ Raman spectra)，探討於四硼酸鈉-甘油電解液組合下的材料型態變化，闡明 NiOOH 為 NiOx的電催化甘油氧化的活性位點。

Electrocatalytic glycerol oxidation is a prominent field that combines cathodic electrolysis for hydrogen production with anodic electrolysis of glycerol to yield high-value products. In this study, we employed photochemical metal-organic deposition (PMOD) method to synthesize amorphous nickel oxide (NiOx) as an anode for electrochemical reaction. Applying a potential of 1.75 V vs. RHE in a glycerol-sodium tetrahydroborate electrolyte, a current density of 2.9 mA/cm-2 was achieved. This process led to the formation of valuable products, including 41% glyceraldehyde (GLAD) and 37% dihydroxyacetone (DHA).
Furthermore, the investigation into the disparities in electrochemical performance and product distribution between crystalline and amorphous materials indicated the superior performance and potential of amorphous materials. Through a series of tests involving pH value adjustment, supporting electrolyte selection, concentration tuning, and glycerol concentration modification, it was demonstrated that achieving highly selective and valuable products is contingent upon appropriate pH value (to stabilize DHA and GLAD), as well as effective supporting electrolyte – sodium tetrahydroborate (Borax), which releases abundant anionic species to facilitate electrocatalytic activity and reaction kinetics. Subsequently, the optimization of the sodium tetrahydroborate-glycerol electrolyte combination revealed that moderate increases in their concentrations individually enhance the yields of DHA and GLAD, potentially elucidating interaction phenomena between borate ions and glycerol.
Finally, through the integration of electrochemical systems and in-situ Raman spectroscopy, the material change in the sodium tetrahydroborate-glycerol electrolyte were examined, elucidating NiOOH as the active site for the electrocatalytic glycerol oxidation of NiOx.

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