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系統識別號 U0002-1108201411340200
中文論文名稱 以聚苯胺及三氧化鎢薄膜搭配丁二腈/聚乙二醇固態電解質組裝可撓式互補型電致色變元件及其性質研究與效能最佳化
英文論文名稱 Fabrication, Characterization and Optimization of Flexible Complementary Electrochromic Device Based on Polyaniline and Tungsten Trioxide Thin Films with Succinonitrile/Polyethylene Glycol Solid-state Electrolyte
校院名稱 淡江大學
系所名稱(中) 化學工程與材料工程學系碩士班
系所名稱(英) Department of Chemical and Materials Engineering
學年度 102
學期 2
出版年 103
研究生中文姓名 陳恩
研究生英文姓名 En Chen
學號 601400384
學位類別 碩士
語文別 中文
口試日期 2014-07-16
論文頁數 113頁
口試委員 指導教授-林正嵐
委員-鄭廖平
委員-陳志賢
中文關鍵字 電致色變元件  固態電解質  聚苯胺  三氧化鎢  丁二腈  聚乙二醇 
英文關鍵字 Electrochromic device  Solid-state Electrolyte  Polyaniline  Tungsten Trioxide  Succinonitrile  Polyethylene Glycol 
學科別分類
中文摘要 本研究使用聚苯胺(polyaniline, Pani)及三氧化鎢(tungsten trioxide, WO3)薄膜,搭配丁二腈/聚乙二醇(succinonitrile/polyethylene glycol, SN/PEG)混合物作為固態電解質,組裝可撓式互補型固態電致色變元件(electrochromic device, ECD),探討並最佳化其電致色變效能。
Pani與WO3薄膜以定電位法析鍍在indium tin oxide (ITO)導電玻璃或indium tin oxide-polyethylene naphthalate (ITO-PEN)導電塑膠上,作為ECD的工作電極,面積為2 × 2 cm2。本研究先以含有0.1 M LiClO4與1.0 mM HClO4之碳酸丙烯酯(propylene carbonate, PC)溶液為電解質,使用析鍍於ITO上之Pani與WO3薄膜為電極組裝液態電解質ECD (l-ECD),以循環伏安法與交流阻抗法分析元件之電化學行為,量測其電致色變性質(包含吸收光譜、穿透率調幅(ΔT%)、著色效率(coloration efficiency, CE)與著色/去色應答時間(tc/tb)),取得Pani與WO3薄膜的最適析鍍參數與電量比,決定元件安全操作電位範圍,並評估其循環使用穩定性。本研究提出新的實驗方法決定元件之安全操作電位範圍。取得最適之薄膜製備參數與ECD的操作條件後,接著使用含有0.1 M LiClO4與1.0 mM HClO4以及不同PEG(分子量=400)含量之SN為固態電解質,並分別以ITO或ITO/PEN為電極基材,組裝固態電解質ECD (s-ECD)與可撓式固態電解質ECD (fs-ECD)。SN中PEG的含量分別為2.5、5.0、7.5、10.0、12.5、15.0、25.0與35.0 wt%,量測其穿透率隨PEG含量之改變,並以光學顯微鏡觀察其表面型態。對所得之ECD進行電化學行為、電致色變性質與穩定性量測,並將所得結果與l-ECD比較。l-ECD在波長700 nm處之ΔT% = 56.66 %,tc/tb = 20.3/9.1秒,CE = 111.1 cm2/C,於1300次著色/去色循環操作ΔT%降至初始值之90%,其值為50.77 %。s-ECD在波長700 nm處之ΔT% = 51.25 %,tc/tb = 28.4/14.4秒,CE = 105.0 cm2/C,於4600次著色/去色循環操作ΔT%降至初始值之90%,其值為39.01 %。fs-ECD於700 nm處之ΔT% = 50.76 %,tc/tb = 26.6/16.3秒,CE = 100.4 cm2/C,於4400次著色/去色循環操作ΔT%降至初始值之90%,其值為41.25 %。
英文摘要 In this study, flexible complementary electrochromic devices (ECD) constructed using polyaniline (Pani) and tungsten trioxide (WO3) thin films with succinonitrile/polyethylene glycol (SN/PEG) composite solid-state electrolyte are fabricated and characterized. Pani and WO3 thin films are prepared by potentiostatic electrodeposition on indium tin oxide (ITO) conducting glass (at part 1 and part 2) or indium tin oxide-polyethylene naphthalate (ITO-PEN) conducting plastic (part 3) as the electrochromic layers. At part 1, liquid electrolyte contain 0.1 M LiClO4 and 1 mM HClO4 in propylene carbonate (PC) solution are prepared and are used to fabricate the ECD. The area of the ECD is 2 × 2 cm2. ECD constructed using stationarty deposition time of Pani thin film and different deposition time of WO3 thin film, then find the best deposition time ratio according to transmittance modulation ability (ΔT) and current density. Using the new method to find the best operation potential range of ECD. Composite solid-state electrolytes contain 0.1 M LiClO4 and 1 mM HClO4 with different SN/PEG ratios (from 95/5 to 65/35 (w/w)) are prepared and are used to fabricate the ECDs. The electrochromic performances of the ECDs using a liquid electrolyte (l-ECD) with ITO or solid-state electrolyte with ITO (s-ECD) or solid-state electrolyte with ITO-PEN (fs-ECD) are investigated and compared. Ion diffusion rate of liquid electrolyte and solid-state electrolyte are investigated by electrochemical impedance spectroscopy (EIS).
Experimental results reveal that the deposition time ratio of Pani thin film and WO3 thin film as 100s:1200s have larger ΔT and current density than other ratio. The best operation potential of the ECD is determined to be 1.0 V for coloring and -0.3 V for bleaching process. Solid-state electrolyte of SN/PEG ratio (90/10) can be effectively inhibit crystallization of SN. l-ECD achieved ΔT of 56.66 % at 700 nm. The ΔT% of s-ECD at SN/PEG ratio of 90/10 is 51.25 % at 700 nm. The ΔT of fs-ECD at SN/PEG ratio of 90/10 is 50.76 % at 700 nm. The coloring/bleaching response times are 20.3 s/9.1 s for l-ECD and are 28.4 s/14.4 s for s-ECD (SN/PEG = 90/10), and fs-ECD (SN/PEG = 90/10) are 26.6 s/16.3 s.The coloration efficiency of l-ECD、s-ECD (SN/PEG = 90/10) and fs-ECD (SN/PEG = 90/10) are 97.0、105.0 and 100.4 cm2/C, respectively. The l-ECD after switching for 1300 cycles, ΔT% decline of 10% compared to the initial ΔT%. The s-ECD (SN/PEG = 90/10) after switching for 4600 cycles, ΔT% decline of 10% compared to the initial ΔT%. The fs-ECD (SN/PEG = 90/10) after switching for 4400 cycles, ΔT% decline of 10% compared to the initial ΔT%. The l-ECD less stable than s-ECD and fs-ECD because liquid electrolyte prone to leak.
論文目次 目錄
中文摘要 I
Abstract III
目錄 V
圖目錄 VIII
表目錄 XII
第一章、簡介 1
第二章、實驗設備與方法 11
2-1、儀器設備 11
2-2、實驗藥品 12
2-3、實驗方法 14
2-3-1、系統架構 14
2-3-2、導電基材的前處理 15
2-3-3、聚苯胺(Pani)薄膜製備之程序 16
2-3-4、三氧化鎢(WO3)薄膜製備之程序 17
2-3-4-1、WO3薄膜之製備 17
2-3-4-2、白金黑之製備 18
2-3-5、液態電解質之製備 18
2-3-6、固態電解質之製備 18
2-3-7、互補式電致色變元件之組裝 19
2-4、實驗分析 20
2-4-1、電化學性質分析 20
2-4-2、光學特性分析 22
2-4-3、電解質表面結構之探討 23
第三章、結果與討論 24
3-1、電致色變薄膜之性質探討 24
3-1-1、Pani 薄膜之電致色變性質 24
3-1-1-1、Pani 薄膜之電化學行為 24
3-1-1-2、Pani 薄膜之吸收光譜特性 26
3-1-1-3、Pani 薄膜之應答時間及著色效率 28
3-1-2、WO3薄膜之電致色變性質 31
3-1-2-1、WO3薄膜之電化學行為 31
3-1-2-2、WO3薄膜之吸收光譜特性 33
3-1-2-3、WO3薄膜之應答時間及著色效率 34
3-2、使用液態電解質組裝ECD及其效能最佳化 36
3-2-1、Pani及WO3析鍍時間比之最佳化 36
3-2-2、決定ECD之最佳操作電位範圍 43
3-3、液態電解質ECD (l-ECD)之電致色變性質探討 52
3-3-1、l-ECD之電化學行為 52
3-3-2、l-ECD之吸收光譜特性 55
3-3-3、l-ECD之應答時間及著色效率 56
3-3-4、l-ECD之交流阻抗分析 58
3-3-5、l-ECD之穩定性 63
3-4、固態電解質ECD (s-ECD)之組裝與其性質探討 69
3-4-1、固態電解質之製備及其性質探討 69
3-4-2、不同PEG比例之s-ECD 之電化學與光學特性分析 75
3-4-3、10 wt% PEG之s-ECD之電致色變性質分析 81
3-4-3-1、10 wt% PEG 之s-ECD之電化學行為 83
3-4-3-2、10 wt% PEG 之s-ECD之吸收光譜特性 85
3-4-3-3、10 wt% PEG 之s-ECD之應答時間及著色效率 87
3-4-3-4、10 wt% PEG之s-ECD之交流阻抗分析 88
3-4-3-5、10 wt% PEG 之s-ECD之穩定性 93
3-5、可撓式固態電解質ECD (fs-ECD)之性質探討與比較 95
第四章、結論 104
第五章、參考文獻 106

圖目錄
圖1-1、典型ECD示意圖。 2
圖1-2、聚苯胺結構圖。 4
圖1-3、丁二腈結構示意圖 8
圖2-1、導電玻璃前處理完成示意圖。 15
圖2-2、Pani實驗流程圖。 16
圖2-3、WO3實驗流程圖。 17
圖2-4、固態電解質製備流程圖。 19
圖2-5、組裝ECD示意圖。 20
圖2-6、三電極式電化學系統示意圖。 22
圖2-7、UV-Vis搭配電化學儀器示意圖。 23
圖3-1、Pani薄膜之循環伏安圖(掃描速率 = 50 mV/s)。 25
圖3-2、Pani薄膜之連續循環伏安圖(掃描速率 = 50 mV/s)。 25
圖3-3、Pani薄膜在不同施加電位下之可見光區吸收光譜圖。 27
圖3-4、在波長700 nm處,Pani薄膜之應答時間圖。 29
圖3-5、於波長700 nm處,Pani薄膜的著色反應電量與光學密度差之關係圖。 30
圖3-6、WO3薄膜之循環伏安圖(掃描速率 = 50 mV/s)。 32
圖3-7、WO3薄膜之連續循環伏安圖(掃描速率 = 50 mV/s)。 32
圖3-8、WO3薄膜在不同施加電位下之可見光區吸收光譜圖。 33
圖3-9、在波長700 nm處,WO3薄膜之吸收度變化圖。 35
圖3-10、於波長700 nm處,WO3薄膜的著色反應電量與光學密度差之關係圖。 35
圖3-11、不同析鍍時間比之ECD的吸收度變化圖,(a) 100s : 100s;(b) 100s : 200s;(c) 100s : 300s;(d) 100s : 600s;(e) 100s : 800s;(f) 100s : 1000s;(g) 100s : 1200s;(h) 100s : 1400s;(i) 100s : 1600s。 41
圖3-12、不同析鍍時間比之ECD之循環伏安圖(第10圈疊圖)。 42
圖3-13、決定操作電位測量方式示意圖。 45
圖3-14、ECD在不同電位下之吸收光譜圖。 45
圖3-15、Pani薄膜對應於ECD不同電位下之吸收光譜圖。 46
圖3-16、WO3薄膜對應於ECD不同電位下之吸收光譜圖。 46
圖3-17、Pani薄膜各電位對應之吸收度圖 (at 700 nm)。 48
圖3-18、WO3薄膜各電位對應之析收度圖 (at 700 nm)。 49
圖3-19、Pani薄膜及WO3薄膜換算之電位對應於ECD之電位比較圖。 51
圖3-20、Pani薄膜在不同著色電位下之可見光區吸收光譜圖。 51
圖3-21、l-ECD之循環伏安圖 (掃描速率 = 20 mV/s)。 54
圖3-22、l-ECD之吸收度隨循環伏安法變化圖。 54
圖3-23、l-ECD在不同施加電位下之可見光區吸收度光譜圖。 55
圖3-24、在波長 550、700及800 nm下,l-ECD之吸收度變化圖。 57
圖3-25、在波長550、700及800 nm 下,l-ECD的著色反應電量與光學密度差之關係圖。 57
圖3-26、ECD之等效電路圖。 59
圖3-27、l-ECD在不同施加電位下之交流阻抗分析圖。 59
圖3-28、l-ECD在不同施加電位下之交流阻抗分析圖(高頻區放大)。 60
圖3-29、l-ECD在電位-0.3 V下之交流阻抗擬合圖。 60
圖3-30、l-ECD在電位+0.65 V下之交流阻抗擬合圖。 61
圖3-31、l-ECD在電位+1.0 V下之交流阻抗擬合圖。 61
圖3-32、l-ECD在電位+1.3 V下之交流阻抗擬合圖。 62
圖3-33、l-ECD之穩定性圖(-0.3 V 至+1.3 V)。 65
圖3-34、l-ECD之穩定性圖(-0.3 V 至+1.0 V)。 65
圖3-35、不同比例(wt % PEG)之固態電解質圖。 71
圖3-36、固態電解質之穿透度量測示意圖。 72
圖3-37、不同PEG比例之固態電解質之OM圖(放大倍率50倍)。 73
圖3-38、不同 PEG 比例之固態電解質之OM圖(放大倍率100倍)。 74
圖3-39、不同PEG比例之s-ECD之循環伏安圖 (掃描速率 = 20 mV/s,-0.3 V至+1.0 V)。 78
圖3-40、在波長700 nm下,不同PEG比例之s-ECD之應答時間圖(-0.3 V至+1.0 V)。 79
圖3-41、在波長700 nm下,不同PEG比例之s-ECD 之穿透度調幅圖。 80
圖3-42、在波長700 nm下,不同PEG比例之s-ECD之應答時間比較圖。 80
圖3-43、10 wt% PEG之固態電解質在不同固化時間下之影像圖。 82
圖3-44、10 wt% PEG 之s-ECD之循環伏安圖 (掃描速率20 mV/s)。 84
圖3-45、10 wt% PEG 之s-ECD之吸收度隨循環伏安法變化圖。 84
圖3-46、10 wt% PEG 之s-ECD在不同施加電位下之可見光區吸收度光譜圖。 86
圖3-47、波長 550、700及800 nm下,10 wt% PEG之s-ECD之吸收變化圖。 87
圖3-48、在波長550、700及800 nm 下,10 wt% PEG 之s-ECD之著色效率圖。 88
圖3-49、10 wt% PEG 之s-ECD在不同施加電位下之交流阻抗分析圖。 89
圖3-50、10 wt% PEG 之s-ECD在不同施加電位下之交流阻抗分析圖(高頻區)。 90
圖3-51、10 wt% PEG 之s-ECD在電位-0.3 V下之交流阻抗擬合圖。 90
圖3-52、10 wt% PEG 之s-ECD在電位+0.65 V下之交流阻抗擬合圖。 91
圖3-53、10 wt% PEG 之s-ECD在電位+1.0 V下之交流阻抗擬合圖。 91
圖3-54、10 wt% PEG 之s-ECD之穩定性圖(-0.3 V至+1.0 V)。 93
圖3-55、三種ECD(液態電解質、固態電解質、可撓式)之循環伏安圖(掃描速率 = 20 mV/s)。 97
圖3-56、三種ECD(液態電解質、固態電解質、可撓式)之吸收度變化圖(-0.3至+1.0 V)。 97
圖3-57、fs-ECD之穩定性圖(-0.3 V至+1.0 V)。 98

表目錄
表1-1、SN+PEG之電解質。 8
表1-2、Pani-WO3互補式ECD文獻回顧。 9
表3-1、Pani薄膜、WO3薄膜及ECD對應於ECD各電位之吸收度比較表。 47
表3-2、Pani薄膜及WO3薄膜換算之電位加總與ECD各電位比較表。 50
表3-3、l-ECD在不同施加電位下之各電阻及電容表。 62
表3-4、l-ECD之穩定性表(-0.3 V至+1.3 V)。 66
表3-5、l-ECD之穩定性表(-0.3 V至+1.0 V)。 67
表3-6、不同PEG比例之固態電解質之穿透度。 72
表3-7、不同 PEG 比例之s-ECD之穿透度調幅與應答時間數據表。 79
表3-8、s-ECD在不同施加電位下之各電阻及電容表。 92
表3-9、l-ECD及s-ECD離子擴散速率之結果比較表。 92
表3-10、10 wt% PEG之s-ECD之穩定性表(- 0.3 V 至 + 1.0 V)。 94
表3-11、可撓式膠態ECD 之穩定性表 (- 0.3 V 至 + 1.0 V)。 99
表3-12、三種 ECD (liquid、gel、flexible) 之電致色變性質表。 101
表3-13、過去三年內之各種互補式電致色變元件參考文獻。 102

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