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研究生：	楊朝竣 Yang, Chao-Chun
論文名稱：	以氧化鋅奈米柱改善氧化鎳電致變色元件性能之研究 Improving performances of nickel oxide electrochromic device by ZnO nanowire arrays
指導教授：	洪敏雄 Hon, Min-Hsiung
學位類別：	碩士 Master
系所名稱：	工學院 - 材料科學及工程學系 Department of Materials Science and Engineering
論文出版年：	2009
畢業學年度：	98
語文別：	中文
論文頁數：	112
中文關鍵詞：	氧化鋅奈米柱、電致變色、氧化鎳
外文關鍵詞：	ZnO nanowire arrays, electrochromic, nickel oxide
相關次數：	點閱：127 下載：1
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本實驗所用之電致變色材料為氧化鎳，因其具有良好光學調節性，穩定性，價格低廉等優點。在本實驗所選擇之製程為化學水浴法，以1M的硫酸鎳，0.25M過硫酸鉀與氨水作為前驅溶液使其在基板表面沈積氫氧化鎳薄膜，並經由熱處理使其形成氧化鎳薄膜。本實驗分別以ITO基板與氧化鋅奈米柱基板沈積氧化鎳薄膜，探討成長參數對薄膜形態與電致變色性質的影響，並比較兩種基板上電致變色元件性能之差異。
本實驗使用溶膠凝膠法搭配低溫水溶液法成長氧化鋅奈米棒。先在ITO基板上旋轉塗佈氧化鋅的種晶層，再由硝酸鋅及氫氧化鉀所配置成的溶液進行氧化鋅奈米柱之成長，藉由各項參數的控制製作不同形態之ZnO奈米柱陣列。在本實驗中選擇以1M醋酸鋅的sol-gel溶液進行200℃熱處理後並以0.5M硝酸鋅與4M KOH成長2hr所得之氧化鋅奈米柱陣列，作為電致變色元件的氧化鎳變色層之基材，使其發揮高表面積之優點，提高電致變色元件之反應性能。
結果顯示，以CBD之方式製備氧化鎳薄膜時，前驅液中之氨水量提高使得氧化鎳薄膜之微結構尺寸增大，表面緻密度下降；而沈積時間與薄膜厚度呈線性關係成長，藉由適當成長參數控制在ITO與氧化鋅奈米柱基板上成功製備出氧化鎳薄膜。
以ITO為基板所做出元件之著色效率為42；但以氧化鋅奈米柱為基材之著色效率可達47，且以氧化鋅作為電極可提升顏色轉換速度，可知氧化鋅奈米柱作為反應電極可提升電致變色之效能。

This research describes a combined process of sol-gel method and room-temperature aqueous solution method for growing nanorods. First, the ITO substrate was spin-coated with ZnO seed layer. And then ZnO nanowire arrays were grown on the substrate in a solution of zinc nitrate hexahydrate and potassium hydroxide. The process of growing the ZnO nanowire arrays with different experimental parameters was performed to prepare ZnO nanowire arrays of different morphologies.
In this study, electrochromic nickel oxide films were deposited by chemical bath deposition. Precursors of nickel sulfate, potassium and ammonia were prepared and then nickel oxide thin films were deposited on the two substrates respectively. The transmittance and electrochromic properties of NiO films are influenced by the thickness and surface area. Compared with the performance of NiO on different substrates, the coloration efficiency on ZnO substrate is 47, higher than that on ITO substrate of 42. An improved electrochromic property of ZnO substrate comparing to ITO substrate is attributed to the increased electrode area.

總目錄 

摘要	I
Abstract 	II
誌謝	III
總目錄.	IV
圖目錄	VII
表目錄	XI

第一章 緒論	1

第二章 理論基礎 	4

2.1變色材料比較	4
2.2電致變色元件	7
2.2.1電致變色的發展歷史	7
2.2.2 電致色變元件系統	8
2.3氧化鋅材料	14
2.3.1氧化鋅之結構與應用	14
2.3.2 氧化鋅奈米結構合成方法	16
2.4 水溶液法合成一維氧化鋅奈米結構	18
2.4.1 一維氧化鋅奈米結構之演進	18
2.4.2 水溶液法合成氧化鋅奈米柱陣列	21
2.5氧化鎳材料	24
2.5.1氧化鎳基本性質與結構	24
2.5.2氧化鎳電致變色之機制	26
2.5.3製備氧化鎳之方法	28
第三章 實驗方法與步驟	30

3.1實驗藥品	30
3.2實驗流程圖	31
3.3實驗流程	33
3.3.1試片清洗	33
3.3.2種晶溶液配置	33
3.3.3水溶液法成長	33
3.3.4氧化鎳成長	33
3.3.5電致變色元件封裝	34
3.4分析與鑑定	35
3.4.1掃瞄式電子顯微鏡（SEM）	35
3.4.2光學性質分析	35
3.4.3電致變色性質量測	35

第四章 結果與討論	37

4.1水溶液法成長氧化鋅奈米柱陣列	37
4.1.1硝酸鋅濃度對氧化鋅奈米棒的影響	37
4.1.2氫氧化鉀的濃度對氧化鋅奈米棒成長的影響	42
4.1.3 氧化鋅成長時間的影響	46
4.2在ITO基板上沈積氧化鎳薄膜	50
4.2.1 退火溫度對薄膜之影響	50
4.2.2 氨水含量對薄膜之影響	54
4.2.3 成長時間對薄膜之影響	57
4.2.4 電致變色性質分析	60
4.3在ZnO基板上沈積氧化鎳薄膜	76
4.3.1氨水含量對薄膜之影響	76
4.3.2成長時間對薄膜之影響	78
4.3.3電致變色性質分析	80
4.4電解質濃度對電致變色的影響	92
4.4.1光學性質分析	92
4.4.2 電致變色性質影響	94
4.5基板對電致變色之性質比較	97
4.5.1 不同基板之電致變色壽命與效率比較	97
4.5.2 組成元件之電致變色性質	101

第五章 結論	104
參考文獻 	106
圖目錄

Fig.1-1 The periodic table of elements, excluding the lanthanides and actinides. The shaded boxes refer to the transition metals whose oxides have well-documented cathodic and anodic electrochromism	3
Fig.2-1 Electrochromic device design, illustrating the movement of ions under an applied voltage	8
Fig.2-2 ZnO wurtzite structure	14
Fig.2-3 Aggregation and Ostwald ripening in growth of the ZnO crystals	19
Fig.2-4 Idealized growth habit of the ZnO crystal.	22
Fig.2-5 Schematic diagram of zinc oxide crystal structure.	23
Fig.2-6 Schematic diagram of nickel oxide crystal structure.	24
Fig.3-1 Flow chart for preparing ZnO nanowires. 	31
Fig.3-2 Flow chart for preparing NiO film. 	32
Fig.4-1 SEM images of ZnO nanowires grown in (a)(b)0.3M (c)(d)0.35M (e)(f)0.4M (g)(h)0.45M and (i)(j)0.5M Zn(NO3)2•6H2O and 4M KOH for 2hr.	40
Fig.4-2 Length of ZnO nanowire arrays prepared in solutions of various concentrations of Zn(NO3)2•6H2O.	41
Fig.4-3 SEM images of ZnO nanowires grown in 0.5M Zn(NO3)2•6H2O and (a)(b)2M (c)(d)2.5M (e)(f)3M (g)(h)3.5M and (i)(j)4M KOH for 2hr.	44
Fig.4-4 Length of ZnO nanowire arrays prepared in various concentrations of KOH.	45
Fig.4-5 SEM images of ZnO nanowires grown in 0.5M Zn(NO3)2•6H2O and 4M KOH for (a)(b)10min(c)(d)30min(e)(f)1hr(g)(h)1.5hr and (i)(j)2hr.	48
Fig.4-6 Length of ZnO nanowire arrays prepared for various growth time.	49
Fig.4-7 SEM images of NiO thin film deposited and annealed at (a)(b)300℃ (c)(d)350℃ and (e)(f)400℃.	51
Fig.4-8 XRD diffraction patterns of NiO thin film annealed at (a)300℃ (b)350℃ and (c)400℃.	53
Fig.4-9 SEM images of NiO thin film deposited on ITO substrate with 10.6M NH3 of (a)(b)10ml(c)(d)12.5ml (e)(f)15ml (g)(h)17.5ml and (i)(j)20ml.	56
Fig.4-10 Thickness of NiO thin film prepared with various volume of NH3.	56
Fig.4-11 SEM images of NiO thin film deposited on ITO substrate for (a)(b)10min (c)(d)20min (e)(f)30min (g)(h)1hr.	59
Fig.4-12 Thickness of NiO thin film prepared for various growth time.	59
Fig.4-13 Transmittance spectra of NiO films after annealing at various temperatures. (a)bleached state (b)colored state.	61
Fig.4-14 Transmittance spectra of NiO films from soluitions with various volume of NH3. (a)bleached state (b)colored state.	63
Fig.4-15 Transmittance spectra of NiO films for various growth times. (a)bleached state (b)colored state.	65
Fig.4-16 Cyclic voltammograms of NiO thin film on ITO substrate with 10.6M NH3 of (a)10ml (b)12.5ml (c)15ml (d)17.5ml (e)20ml.	71
Fig.4-17 The coloration efficiency of NiO films prepared with various concentration of NH3.	71
Fig.4-18 Cyclic voltammograms of NiO thin film on ITO substrate for (a)10min (b)20min (c)30min (d)1hr 	74
Fig.4-19 The coloration efficiency of NiO films prepared for various growth times.	75
Fig.4-20 SEM images of NiO thin film deposited on ZnO nanowire arrays substrate with NH3 of (a)6ml (b)7ml (c)8ml (d)9ml (e)10ml..	77
Fig.4-21 SEM images of NiO thin film deposited on ZnO nanowire arrays substrate for (a)1min(b)2min(c)3min(d)4min (e)10min.	79
Fig.4-22 Transmittance spectra of NiO films on ZnO nanowire arrays substrate with various volume of NH3 (a)bleached state (b)colored state.	81
Fig.4-23 Cyclic voltammograms of NiO thin film on ZnO nanowire arrays substrate with NH3 of (a)6ml(b)7ml(c)8ml(d)9ml (e)10ml NH3.	85
Fig.4-24 The coloration efficiency of NiO films on ZnO nanowire arrays substrate prepared with various volume of NH3.	85
Fig.4-25 Transmittance spectra of NiO films on ZnO substrate for various growth time (a)bleached state (b)colored state.	87
Fig.4-26 Cyclic voltammograms of NiO thin film on ZnO substrate for (a)1min(b)2min(c)3min(d)4min (e)10min.	91
Fig.4-27 The coloration efficiency of NiO films on ZnO substrate prepared for various growth time..	91
Fig.4-28 Transmittance spectra of NiO films on ITO substrate with various concentrations of electrolyte (a)bleached state (b)colored state.	93
Fig.4-29 Cyclic voltammograms of NiO thin film on ZnO substrate with KOH electrolyte of (a)0.1M (b)0.5M (c)1M	96
Fig.4-30 The coloration efficiency of NiO films on ZnO substrate with various concentration of electrolyte.	96
Fig.4-31 SEM images of NiO thin film deposited on (a)(b) ITO substrate and (c)(d) ZnO nanowire arrays substrate.	98
Fig.4-32 Cyclic voltammograms of NiO thin films on (a) ITO substrate and (b) ZnO nanowire arrays substrate.	99
Fig.4-33 Electrochromic performance photographs of NiO thin film on (a)(b)ITO substrate and (c)(d)ZnO nanowire arrays substrate..	100
Fig.4-34 Absorbance spectra of NiO films deposited on (a) ITO substrate (b) and ZnO nanowire arrays substrate..	102
Fig.4-35 Transmittance spectra of NiO films deposited on (a) ITO substrate (b) and ZnO nanowire arrays substrate.	103
 
表目錄

Table.2-1 Comparison of the electrochromic material. 	6
Table.2-2 Various chromic materials of transition metal oxides	13
Table.2-3 The properties of zinc oxide	15
Table.2-4 The electrochromic mechanism of NiO films prepared by various methods.	27
Table.4-1 Decline of the cyclic voltammograms of NiO thin film on ITO substrate with 10.6M NH3 of various volume	71
Table.4-2 Charge intercalated during electrochromic cycling at different deposition time.	75


                                    

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