在本研究中，我們詳細探討以氧化銅鉍為主之修飾電極的製備方法以及其應用於電催化葡萄糖氧化(第三章)與光電化學產氫之應用(第四章)。所製備氧化銅鉍修飾電極的表面形貌及結構、晶相、化學組成、光學性質以及電化學催化性質係利用掃描式及穿透式電子顯微鏡、X光繞射儀、紫外光至可見光吸收光譜、循環伏安法、線性掃描伏安法、計時電流分析法以及電化學阻抗等技術來進行分析。
在第三章中，我們透過電鍍方法先將奈米片狀之氧化鉍碘電鍍在透明導電電極上，再利用滴鍍法將含有銅離子的醇類溶液滴鍍在碘氧化鉍上，最後經由熱處理將其轉換成氧化銅奈米粒子修飾之具奈米樹枝狀氧化銅鉍。藉由調整滴鍍液體積，我們可以控制不同轉換程度與對葡萄糖氧化催化能力。本研究顯示氧化銅以及氧化銅鉍分別對葡萄糖氧化都有催化活性，然而，當兩者形成樹枝狀孔洞型複合材料時，由於協同作用我們發現其催化活性比純質氧化銅或氧化鉍還優越，在詳細探討其催化機制後，結果顯示此複合材料能夠作為良好的葡萄糖感測材料。
在第四章中，我們先利用旋轉塗布法，將含有銅鉍離子之醇類溶液塗布在透明導電電極上，並經過熱處理製備氧化銅鉍晶種層，接著利用化學沉積法將氧化銅鉍微米柱成長於晶種層上，形成陣列式柱狀氧化銅鉍修飾電極。我們詳細探討晶種層製備條件，包括鍍液組成和鍛燒溫度效應，與化學沉積溶液的組成與成長時間等，並經過參數最佳化後，我們合成出長1.2微米、寬0.25微米、高寬比4.8的氧化銅鉍微柱。在光電化學產氫之應用方面，在光照下、除氧電解液中，氧化銅鉍微柱出現了光腐蝕現象，然而，在富氧電解液中，氧化銅鉍展現了良好的光電流以及穩定性。這個結果顯示表面反應之反應動力對氧化銅鉍微柱的光電催化行為有著極大的關聯。因此我們利用電鍍方法將鎳硼化合物修飾在氧化銅鉍表面，作為產氫之共觸媒，發現鎳硼化合物對氧化銅鉍的光腐蝕有些微抑制的效果，然而，更多表面修飾相關研究仍須被詳細探討以達到更高的光電極穩定性。

In this study, copper bismuth oxide (CuBi2O4) based modified electrodes were fabricated and their applications in electrocatalytic oxidation of glucose (Chapter 3) and photoelectrochemical (PEC) hydrogen generation (Chapter 4) were thoroughly investigated. Surface morphology, structure, crystal phase, chemical composition, optical properties, and electrocatalytic properties of the fabricated CuBi2O4 based modified electrodes were characterized using scanning electron microscopy, transmission electron microscopy, X-ray diffraction, UV-vis spectroscopy, cyclic voltammetry, linear sweep voltammetry, chronoamperometry, and electrochemical impedance spectroscopy.
In chapter 3, a chemically modified electrode, consisting of CuO nanoparticles decorated nano-dendrite-structured CuBi2O4 (nanoCuBi2O4|CuO), was fabricated by firstly electrodepositing BiOI nanosheet array (nanoBiOI) on the flourine-doped tin oxide coated glass substrate, followed by its conversion into nanoCuBi2O4|CuO via drop-casting a ethanolic Cu2+ solution and follow-up thermal treatment. The degree of conversion of nanoBiOI into nanoCuBi2O4|CuO and electrocatalytic activites of resultant nanoCuBi2O4|CuO were controlled by adjusting the dosage of the ethanolic Cu2+ precursor solution. It was found that both CuO and CuBi2O4 are active in electrocatalyzing the oxidation of glucose, but the porous structure of nanoCuBi2O4|CuO along with the synergistic catalytic enhancement, exerted by CuBi2O4 and CuO, renders nanoCuBi2O4|CuO superior electrocatalytic activity than CuO or CuBi2O4 alone. The mechanism of electrocatalytic oxidation of glucose on nanoCuBi2O4|CuO is proposed. Finally, the sensing characteristics of nanoCuBi2O4|CuO was evaluated, and the results indicate nanoCuBi2O4|CuO is a promising sensing material for the electrochemical detection of glucose.
In Chpater 4, CuBi2O4 microrods (microCuBi2O4) modified electrodes were prepared by firstly depositing a seed layer via spin-coating and follow-up thermal annealing, followed by growth of microCuBi2O4 using chemical bath deposition (CBD) process. Important parameters in tuning of microstructure of microCuBi2O4 modified electrode, including concentration of Cu2+/Bi3+ and chelating reagent of precursor solution and annealing temperature for seed layer preparation, thickness of seed layer, and the concentration of Cu2+/Bi3+, solvent and the growing time for the growth of microCuBi2O4 in CBD process were investigated. Under optimal conditions, microCuBi2O4 with length and diameter of ~1.2 and ~0.25 m, respectively, corresponding to an aspect ratio of 4.8 was obtained. Regarding the applicability of microCuBi2O4 in PEC hydrogen generation, microCuBi2O4 suffered photoinstability under N2 atmosphere, but exhibited high photocurrent response and photostability under O2 atmosphere, suggesting the PEC performance of microCuBi2O4 is highly dependent on the kinetics of PEC reactions on its surface. The photostability of microCuBi2O4 under N2 atmosphere was slightly improved by deposition a layer of nickel based hydrogen evolution catalyst onto its surface. Further optimization on the parameters in surface modification process on microCuBi2O4 is still required to improve its photostability and photo-activity.

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