在過去的幾十年中，光電化學（photoelectrochemical）太陽能水分解已經成為一個核心的研究主題，許多研究學者投入了相當大的努力來開發高效能的催化劑。研究方向包含理論計算和實驗的結合來設計與開發新的半導體材料以及發展有效解決現有常見半導體材料限制的方法。然而，讓高效率的讓電荷從電極轉移到電解質介面的方法仍未開發完全，因此本論文專注於利用表面工程的方法來改善BiVO4光電化學水分解的效率。
第一個實驗章節為利用溶劑調整的方法來製造高機械強度及結晶良好的單斜晶系BiVO4。以硼酸鹽溶液為電解質，BiVO4光電極於水分解反應上表現出相對低的起始電位(0.4 V vs. RHE)以及高光電流密度為1.04 mA/cm2 (在1.23 V vs. RHE)，此優異的表現在單純的BiVO4水分解相關文獻名列前1%，此樣品經過1小時後的水分解實驗，仍能保持約70%的光電流。於第二個實驗章節中，將太陽能電池中的電洞傳輸材料的概念引進至光電化學電池。與單純BiVO4的1.22 mA/cm2相比，隨著BiVO4 / CuSCN奈米柱異質光陽極結構的產生，光電流密度增加至1.78 mA/cm2。更重要的是，析氧反應(oxygen evolution reaction)的起始電位顯著的往陰極偏移（~230 mV）。異質結構在350-450 nm範圍還具有約50％的量子效率，太陽能轉換效率（0.5％）和不錯的氧化效率（~90％）。獨特的電極結構設計，可提供更多的活性位點，便於光激發之電洞的運輸和參與水氧化反應。第三個實驗章節則是合成層狀雙氫氧化物（layered double hydroxides, LDH）作為一種新的助催化劑，以用於增強BiVO4光陽極的光電化學水氧化效率。改良的光陽極展現出1.7倍的光電流密度，同時起始電位也向陰極偏移300 mV。複合光陽極PEC的效能提升，可歸咎於LDH的多功能作用，包含降低動力學屏障，促進光激發電荷分離，從而延遲光激發電荷的重組。在最後的實驗章節中，我們開發了一種簡便製備新型低成本磷酸鐵(ferrite phosphate)助催化劑的方法，此助催化劑可抑制電荷重組並穩定BiVO4光電極。複合光陽極可提供2.28 mA/cm2的光電流密度，與原始BiVO4相比增加250%。在溫和的鹼性環境中，助催化劑可讓起始電位產生陰極偏移~500 mV並且此複合光陽極具有高達90%的電洞氧化效率和超過120分鐘的良好穩定性，此外利用光電化學分析結果可發現，磷酸鐵可快速移轉”光激發半導體 - 電解質界面”上的電洞，增強了光轉換效率並防止光陽極的光氧化，確保了長期穩定性，因此提高底層BiVO4的光電化學性質。

In the past decades, photoelectrochemical (PEC) solar water splitting has become a central research theme and considerable efforts have been devoted for the development of efficient catalyst materials for chemical fuel generation. One direction is to design and search new semiconductor materials through a combination of computational and experimental efforts. The other one is to develop efficient strategies to address the existing limitations in the commonly used semiconductor materials. However, the efficient methodologies for charge transfer at electrode/electrolyte interface remain underdeveloped. Motivated by these challenges, this dissertation focuses on improving PEC materials, namely BiVO4, by surface engineering.
The first experimental chapter presents solvent-engineering approach for fabricating well-crystalized monoclinic BiVO4 with robust mechanistic properties as electrode material for solar water splitting. When applied as electrode material for water splitting in borate electrolyte solution, the BiVO4 electrode exhibited a relatively low onset potential of 0.4 V vs. RHE and a high photocurrent density of 1.04 mA/cm2 at 1.23 V vs. RHE which is among top 1% the highest results reported in the literature for bare BiVO4. Long-term stability witnessed a fairly stable behavior in which around 70% photo-induced current was maintained after one hour. In the second experimental chapter of this thesis, a new concept that integrates an appropriate hole transport material into the conventional photoelectrochemical cell is introduced by inspiring the devotion of hole transport material in the solar cell. With the creation of BiVO4/CuSCN heterojunction photoanodes, the photocurrent density increased to 1.78 mA cm-2 compared to 1.22 mA cm-2 of bare BiVO4. More importantly, the onset potential for oxygen evolution reaction exhibits a dramatic cathodic shift (~230 mV). The heterojunction also possesses internal quantum efficiency of approximately 50% in the range from 350-450 nm with relatively high solar energy conversion efficiency (0.5%) and much higher water oxidation efficiency (~90%). The unique electrode architecture design favoring the simple water splitting process over conventionally fabricated electrode by providing more active sites and facilitates transportation and consumption of photoinduced holes. The next section demonstrates a proof-of-concept electrochemical approach to synthesize hierarchical layered double hydroxides (LDH) for as a new co-catalyst for enhancing photoelectrochemical water oxidation of bismuth vanadate photoanode. The modified photoanodes exhibited 1.7 times increase in photocurrent density and a 300 mV cathodic shift in onset potential. The improved PEC performance of the composite photoanode could be attributed to the multifunctional roles of LDH that reduce kinetic barrier, facilitate photogenerated charges separation, thus retarded the recombination of photogenerated charges. In the last experimental chapter, a facile process is developed for preparing a new type of low-cost ferrite phosphate as an efficient co-catalyst to suppress charge recombination and stabilize bismuth vanadate (BiVO4) photoelectrodes. The composite photoanode exhibit a high photocurrent density of 2.28 mAcm-2, which corresponds to a 250% increase compared to that of pristine BiVO4. Deposition of cocatalyst has yielded a large cathodic shift (∼500 mV) in the onset potential, high oxidation efficiency of about 90% and a good stability of over 120 minutes in a mild basic medium. Comprehensive photoelectrochemical studies suggest that ferrite phosphate could boost the photoelectrochemical properties of the BiVO4 underlayer by mediating hole extraction across the photoexcited semiconductor-electrolyte interface. This in turn enhances photoconversion efficiency and prevents the photooxidation of the photoanode, ensuring prolonged stability.

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