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研究生： 梁加宏
Liang, Chia-Hung
論文名稱： 溶膠凝膠法製備TiO2/ITO光電極及其在產氫程序上之應用
Preparation of Sol-gel Derived TiO2/ITO Photoelectrode and Application in Hydrogen Evolution Process
指導教授： 陳慧英
Chen, Huey-Ing
學位類別： 碩士
Master
系所名稱： 工學院 - 化學工程學系
Department of Chemical Engineering
論文出版年： 2007
畢業學年度： 95
語文別： 英文
論文頁數： 120
中文關鍵詞： 光電化學 、二氧化鈦 、溶膠凝膠法 、光電極 、產氫程序
外文關鍵詞： titanium dioxide, hydrogen evolution process, photoelectrode, sol-gel method, photo-electrochemical
相關次數： 點閱：76  下載：1 
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    • 本研究旨在製備具光敏性之二氧化鈦/ITO (TiO2/ITO)電極，以進行光電分解水產製氫之反應，研究中，首先以醇氧化鈦(Ti(OBun)4)為前驅鹽與雙氧水溶液反應，產生TiO2溶膠，再以旋轉塗佈法在ITO玻璃基板上塗覆TiO2薄膜經鍛燒而製成電極。其次，針對電極之製作，並藉XRD、SEM、BET及UV/VIS吸收光譜等儀器來進行薄膜特性分析。並針對薄膜製備條件包含旋轉塗佈次數及鍛燒溫度，來加以探討。另外，以TiO2/ITO作為光陽極組裝光電化學反應(PEC)系統以測試光電極之活性，並探討PEC之反應溫度、電解液種類與濃度對光電流轉換效率及產氫速率之影響。
    實驗結果顯示，以溶凝膠法所製備之TiO2膜，經300-600oC鍛燒1h後，主要具有銳鈦礦(anatase)結構。在照光下(低壓汞燈，極板照度1.05mW/cm2)，塗覆一層(TiO2膜厚約0.2μm) TiO2溶膠，經600oC鍛燒所得TiO2/ITO電極之飽和光電流(0.326 mA/cm2)為最大，其光電流轉換效率為2.4%，最大產氫速率約為0.075 mL/cm2-h。
    另外，本研究中合成之電極與商用P25-TiO2/ITO比較，結果發現實驗，合成之TiO2/ITO電極具較高之光電化學轉換特性。研究中並嘗試含浸鎳於TiO2/ITO上以製備Ni-TiO2/ITO電極，初步實驗結果發現，鎳微粒會抑制光電子由TiO2至ITO之傳遞，而導致其光電活性下降。

    In this work, photosensitive TiO2/ITO electrodes were prepared for the production of hydrogen via PEC reaction. Experimentally, TiO2 sol was firstly prepared by sol-gel method starting from tetrabutyl orthotitanate (Ti(OBun)4) reacted with hydrogen peroxide. Subsequently, TiO2/ITO electrodes were obtained by spin-coating the TiO2 sol following by calcination. The preparation conditions including number of coating and calcination temperature were investigated. The XRD, SEM, BET and UV/VIS absorption spectroscopic techniques were used for the characterization of TiO2/ITO electrodes. Furthermore, PEC cells were constructed for measuring the activities of prepared TiO2/ITO electrodes. The effects of reaction temperature as well as the nature and concentration of electrolytes on both hydrogen production rate and photoefficiency conversion of PEC system were also investigated.
    The experimental results showed that the sol-gel derived TiO2 layers calcined at 300-600 oC were mainly anatase structure. From the result of PEC reactions under UV illumination (λmax＝253.7 nm), it found that the TiO2/ITO photoelectrode (calcined at 600oC, thickness of TiO2 layer of about 0.2 μm) demonstrated a maximum saturation current (0.326 mA/cm2) with a high PEC conversion efficiency of 2.39%. In this case, the hydrogen evolution rate is about 0.075 mL/cm2h.
    As compared with the P25-TiO2/ITO electrode prepared starting from the commercial Degussa P25-TiO2, the sol-gel synthesized TiO2/ITO electrode demonstrated much higher PEC conversion efficiency. In addition, nickel-loaded TiO2/ITO (Ni-TiO2/ITO) electrode was prepared by impregnation technique for trying to enhance the light absorption in visible region. However, the rudimentary results showed the photoactivity of this electrode was reduced because the loaded nickel particles on TiO2 could trap electrons and thus led to the depression of photo-induced electrons transferred from TiO2 to ITO.

    Page 摘要……………………………………………………………………Ⅰ ABSTRACT………………………………………………………………Ⅲ LIST OF CONTENTS……………………………………………………Ⅹ LIST OF TABLES……………………………………………………ⅩⅢ LIST OF FIGURES……………………………………………………ⅩⅣ CHAPTER 1 INTRODUCTION………………………………………………1 　　1.1　Hydrogen……………………………………………………1 　　1.2　Hydrogen generation methods……………………………2 　　　1.2.1　Direct thermal decomposition of water…………3 　　　1.2.2　Thermo-chemical hydrogen production……………3 　　　1.2.3　Biological and photo-biological processes……4 　　　1.2.4　Electrolysis of water………………………………4 　　　1.2.5　Photo-electrochemical hydrogen generation……5 　　1.3　Titanium oxide……………………………………………6 　　　1.3.1　Preparation……………………………………………7 　　　1.3.2　Photocatalytic property……………………………8 　　　1.3.3　Applications…………………………………………8 　　1.4　Objectives…………………………………………………9 CHAPTER　2　THEORETICAL……………………………………………25 　　2.1　Sol-gel method……………………………………………25 　　　　2.1.1Mechanism…………………………………26 　　2.2　Principles of photo-electrochemical hydrogen 　　　　　　　generation………………………………………………28 　　　　2.2.1　Band model representation of PEC……………29 　　　　2.2.2　Properties of photoelectrodes………………30 　　　　2.2.3　Principles for catalysis of photoelectrode32 　　　　2.2.4　Conversion efficiency of PEC…………………33 CHAPTER 3 　EXPERIMENTAL……………………………………………38 　　3.1　Chemicals and Materials………………………………38 　　 3.1.1　Chemicals……………………………………………38 　3.1.2　Materials……………………………………………39 　　3.2　Apparatus and Analyses…………………………………39 　　　3.2.1　Instruments…………………………………………39 　　　3.2.2　Analyses………………………………………………40 　　3.3　Preparation of TiO2/ITO electrodes…………………42 　　　3.3.1　Pretreatment of ITO substrate…………………43 　　　3.3.2　TiO2/ITO preparation………………………………43 　　3.4　Photoelectrochemical systems…………………………44 　　　3.4.1　Design and fabrication of reactor……………44 　　　3.4.2　Procedures……………………………………………45 　　　3.4.3　Collection of hydrogen……………………………45 　　　3.4.4　Calculation of conversion efficiency…………46 CHAPTER 4　RESULTS AND DISCUSSION………………………56 　　4.1 Characterization of TiO2 and TiO2/ITO……………56 　　　4.1.1　Stability of PPT sol………………………………56 　　　4.1.2　Fourier transform infrared spectroscopy 　　　　　　　　　analysis………………………………………………57 　　　4.1.3　XRD analysis…………………………………………57 　　　4.1.4　UV/VIS absorption analysis………………………58 　　　4.1.5　SEM analysis…………………………………………59 　　　4.1.6　BET surface area analysis………………………60 　　4.2　PEC activity of TiO2/ITO electrodes………………60 　　　　4.2.1　PEC activity of sol-gel derived TiO2/ITO 　　　　　　　electrodes……………………………………………61 　　　　　4.2.1.1 Effect of TiO2 layer thickness…………61 　　　　　4.2.1.2 Effect of calcination temperature………62　　　　　4.2.1.3 Effect of applied bias……………………63 　　　　　4.2.1.4 Effect of electrolyte………………………64 　　　　4.2.2　PEC activity of P25-TiO2/ITO electrodes…65 　　　　4.2.3　PEC activity of Ni-loaded TiO2/ITO 　　　　　　　　　　　electrodes…………………………………………66 　　　　　4.2.3.1　A. Photocurrent in the ultraviolet 　　　　　　　　　　　region…………………………………………66 　　　　　4.3.3.2　B. Photocurrent in the visible 　　　　　　　　　　　　　region…………………………………………67 　　4.3　Photoefficiency and hydrogen evolution……………67 　　　　4.3.1　Effect of calcination temperature…………68 　　　　4.3.2　Effect of applied bias…………………………68 　　　　4.3.3　Effect of electrolyte temperature…………69 CHAPTER 5　CONCLUSIONS AND SUGGESTION………………………111 　　5.1　Conclusions………………………………………………111 　　5.2　Suggestions………………………………………………112 REFERENCE……………………………………………………………114

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