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研究生：	游博盛 You, Bo-Shing
論文名稱：	電沉積CdS/TiO2光陽極以應用於光電化學產氫之研究 A Study on Electrodeposition of CdS/TiO2 Photoanode Applied in Photoelectrochemical Hydrogen Generation
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：	2011
畢業學年度：	99
語文別：	中文
論文頁數：	135
中文關鍵詞：	硫化鎘、二氧化鈦、電沉積、光電化學、產氫
外文關鍵詞：	cadmium sulfide, titanium dioxide, electrodeposition, photoelectrochemical, hydrogen generation
相關次數：	點閱：101 下載：4
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本研究係以氯化鎘及硫代硫酸鈉為前驅物採用脈衝電沉積方式來製備CdS/TiO2光陽極，旨在探討電沉積條件及TiO2模板對所得光陽極組成及微結構之影響，並進一步探討其對光電化學活性及產氫速率之影響。
在電沉積CdS實驗中，在TiO2模板之影響中，吾人針對陽極氧化之電壓及時間來加以探討；吾人改變施加電壓、電解液組成、沉積電量、浸泡時間、溫度、以及煅燒溫度來探討，並利用XRD、SEM、TEM、XPS、及UV等儀器來進行特性分析。進行光陽極之活性分析時，係利用Xe燈源（100 mW/cm2）照射光陽極，以含有0.25 M Na2S及0.35 M Na2SO3之水溶液作為電解液，進行光電化學反應，以評估各光陽極之光活性。最後並利用離子交換膜串連雙槽PEC反應器，測量各光陽極之產氫速率。
由TiO2模板之探討結果顯示，奈米管管徑、壁厚及管長受陽極氧化電壓影響甚鉅，但改變時間僅影響管長。而電沉積變因對CdS之析出量、粒徑大小、表面缺陷(或電荷數)影響甚鉅，進而影響光陽極之光活性。最適之還原電壓為-0.7V（vs AgCl/Ag），而鎘離子與硫代硫酸根之最適濃度分別為0.02、0.2M。因電沉積速率極快，每回通入0.2庫倫電量僅約3分鐘即完成，為避免因擴散不及造成極化現象，在通電間隙靜置浸泡之。實驗結果發現，最適之浸泡時間為10分鐘。當增加沉積電量時，所得CdS量隨之增加，但以通入1.0庫倫電量所得CdS/TiO2光陽極具有最佳之光活性；雖然CdS沉積量增加可產生較多之電子電洞對，但當CdS量過多時，再結合機率大幅增加，光活性反而下降。至於煅燒溫度則以300OC為最適條件，所得光陽極之光學活性及耐光腐蝕最佳。
在本實驗中以40 V、6 hr 陽極氧化之TiO2奈米管作模板(3.0μm)時，所得CdS/TiO2光陽極之光活性最大，其光電流為7.61 mA/cm2、光轉換效率為5.51%，產氫速率為1.88 ml/cm2-h。
綜上所述，本研究所得CdS/TiO2光陽極之光電流及光轉換效率均較化學浴沉積法大，且製程簡單、省時，具有未來開發潛力。

In this work, CdS/TiO2 photoanodes were prepared starting from cadmium chloride and sodium thiosulfate by pulse electrodeposition. The influences of preparation conditions and TiO2 template on the composition and microstructure of resulting photoanodes were investigated. Furthermore, the photoactivity of photoanode and the hydrogen generation rate were studied as well.
From the study of TiO2 template effect, it revealed that the diameter, wall thickness, and length of nanotubes were strongly governed by anodizing voltage, whereas the anodizing time could only manipulate the final tube length. For the study of CdS electrodeposition, preparation conditions including applied voltage, electrolyte composition, input electricity, soaking time, deposition temperature, and calcination temperature were investigated. For the study of TiO2 template effect, both of anodizing voltage and time were investigated by means of XRD, SEM, TEM, XPS, and UV techniques. The activity measurements were carried out in a photoelectrochemical (PEC) cell with an electrolyte of 0.25 M Na2S and 0.35 M Na2SO3 under illumination by Xe lamp (100 mW/cm2). Furthermore, the hydrogen generation rate was measured in a PEC reactor comprised of two compartments separated by an ion exchange membrane.
The experimental results showed that deposition amount, particle size, defect, and surface state of CdS and the corresponding photo-activities can be correlated with deposition conditions. An optimal applied voltage was -0.7 V (vs. Ag/AgCl), and the cadmium and thiosulfate concentrations were 0.02 and 0.2 M, respectively. The rate of electrodeposition was so fast that merely 3 minutes were required for accomplishing each run of input electricity of 0.2 C. For avoiding the polarization due to diffusion limitation, the pulse deposition with proper soaking was adopted in this work. The result also showed that the optimal soaking time was 10 minutes. As increasing the input electricity, the deposited amount of CdS increased and therefore the photoactivity was consistently increased attributing from the generation of more hole-electron pairs. However, the maximum photoactivity of CdS/TiO2 photoanode was obtained at a total input electricity of 1 C. In fact, overloading CdS would contrarily lead to reducing the photoactivity due to considerable increases of hole-electron recombination. Eventually, the optimal calcination temperature was found to be 300 oC.
In this study, with the TiO2 template anodized at 40 V for 6 hr(3.0μm), the resulting CdS/TiO2 photoanode exhibited the maximum photoactivity, e.g., a photocurrent of 7.61 mA/cm2, a photoconversion efficiency of 5.51%, and a hydrogen generation rate of 1.88 ml/cm2-h.
In conclusion, the CdS/TiO2 photoanodes prepared in this work demonstrated larger photocurrent and photoconversion efficiency than those prepared by the sequence-chemical bath deposition (s-CBD), which showed a promising potential of future development.

總目錄

中文摘要......................................I
英文摘要............................................III
誌謝....................................................V
總目錄................................................VI
表目錄...............................................IX
圖目錄..............................................X
符號表..........................................XVII

第一章	緒論
1.1	  氫能之介紹..............................1
1.2	  氫氣之製備方法........................1
1.3	  CdS/TiO2光陽極結構及性質........................3
    1.3.1  二氧化鈦..........................4
    1.3.2  硫化鎘............................5
1.4	  研究目的及概要........................5

第二章	理論
2.1	  製備二氧化鈦薄膜方法.....................19
二氧化鈦奈米管陣列之生成...........................19
2.2	  電沉積.........................................21
      2.2.1   脈衝電鍍.....................22
      2.2.2   線性掃描伏安法..........................22
2.3	  光電化學法原理..........................22
      2.3.1  太陽光譜及AM1.5G...............22
      2.3.2  PEC產氫原理................23
      2.3.3  PEC之能帶模型.................24
      2.3.4  光轉換效率...................24
2.3.5  電子電洞再結合...............26

第三章	實驗部分
3.1	  藥品及材料..............................33
3.2	  儀器及分析設備.......................34
3.2.1	設備及裝置.......................34
3.2.2	分析儀器........................34
3.3	  實驗方法與步驟......................35
3.3.1	奈米管之製備..................35
3.3.2	電沉積製備CdS/TiO2光陽極............................36
3.3.3	光陽極之活性測試............................37
3.3.4	光陽極之特性分析...........................37
3.3.5	產氫實驗.......................39

第四章	光陽極之特性分析與活性探討
4.1	  光陽極之特性分析...........................43
4.1.1	陽極氧化條件對奈米結構之影響..................43
              4.1.1.1  陽極氧化時間之影響.............43
              4.1.1.2  陽極氧化電壓之影響...............44
4.1.2	電沉積條件對奈米結構及組成之影響...............44
              4.1.2.1  電位之影響..................44
              4.1.2.2  電解液濃度之影響................46
              4.1.2.3  浸泡時間之影響...............46
              4.1.2.4  沉積溫度之影響..............47
              4.1.2.5  沉積時間之影響................48
              4.1.2.6  煅燒溫度之影響................48
4.1.3	陽極氧化條件沉積CdS對奈米結構之影響...........49
              4.1.3.1  陽極氧化時間之影響..............49
              4.1.3.2  陽極氧化電壓之影響...............49
4.2	  光陽極之活性探討...........................50
4.2.1	陽極氧化條件對光活性之影響.................50
     4.2.1.1  陽極氧化時間之影響................50
     4.2.1.2  陽極氧化電壓之影響.................50
4.2.2	電沉積條件對光活性之影響..................51
              4.2.2.1  電位之影響................51
              4.2.2.2  電解液濃度之影響................51
              4.2.2.3  浸泡時間之影響.................52
              4.2.2.4  沉積溫度之影響..................52
              4.2.2.5  沉積時間之影響..................53
              4.2.2.6  煅燒溫度之影響....................54
4.2.3	陽極氧化條件沉積CdS對光活性之影響.........55
              4.2.3.1  陽極氧化時間之影響................55
              4.2.3.2  陽極氧化電壓之影響............56
4.3	  產氫實驗與綜合比較...........................56

第五章	結論與建議
5.1	  結論.....................................120
5.2	  建議..................................122

參考文獻......................................124

                                    

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