濕法製備氧化鋅摻雜鋁之透明導電膜

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姓名

胡英傑(Ying-Jie Hu) 查詢紙本館藏

畢業系所

化學工程與材料工程學系

論文名稱

濕法製備氧化鋅摻雜鋁之透明導電膜
(Transparent and conductive Al-doped ZnO film prepared by spin coating)

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摘要(中)

本研究之目的為製備氧化鋅摻雜鋁之透明導電薄膜。在製備溶膠的部分，我們使用氯化鋅摻雜硝酸鋁和氫氧化鈉的乙二醇溶液，在pH值9.1下進行中和，得到白色乳狀的中和液，再將中和液以80℃加熱3小時，即可得到泛藍光且透明度高的氧化鋅摻雜鋁EG溶膠。此EG溶膠在合成後的固含量約含3.2 wt% ZnO，在可見光（600 nm）的穿透度大於90 %，而波長小於370 nm之光線會被吸收，由DLS測量結果得溶膠的平均粒徑大小約為25 nm。接著再用油酸將分散在EG中的氧化鋅相轉移到己烷中，即可得到泛藍光且透明度高的氧化鋅摻雜鋁己烷溶膠。此己烷溶膠的固含量為8 wt%時，在可見光（600 nm）的穿透度約為89 %，由DLS測量結果得溶膠的平均粒徑大小約為15 nm。
接著使用旋轉塗佈法來鍍膜。在鍍膜完成後，用2克酒精加2克水的80℃蒸氣蒸薰鍍膜50分鐘以得到表面平整的膜和密質化的氧化鋅層，再用5克的酒精浸洗鍍膜試片以洗去鍍膜表面大部分的有機物。接著在空氣中從室溫加熱到425℃煅燒10分鐘以燒去有機物，然後通入氮氣繼續升溫到500℃煅燒1小時，接著在氮氣中退火到室溫，如此可以防止鍍膜產生細微的龜裂並可以增加氧空缺提升導電度。最後可以得到鍍膜的穿透度約為95%、電阻率約為16 Ωcm。
另外，在實驗的過程中，鋁的摻雜量、蒸氣處理的溫度和時間、煅燒溫度和退火溫度，一值都是我們實驗的重點。必須重複改變多種實驗條件，以獲得最低電阻率和高透明度的薄膜。

摘要(英)

Transparent and conductive Aluminum doped zinc oxide (AZO) thin films have been prepared from hexane dispersed nanocrystal sol using spin-coating technique. The AZO nanocrystal was synthesized via the ethylene route developed in our lab and transferred to hexane phase after capping with oleic acid. The 8 wt% hexane sol has 89 % transmittance in visible range and its particle size is about 15 nm.
The spin-coating was done at 3000 rpm on FEA glass substrate. Then use EtOH and water vapor heating films at 80 oC for 50 min, subsequently soak in EtOH. The effects of sol and aluminum concentration, heat treatment and annealing atmosphere on the microstructure as well as on the electrical and optical properties were studied. Under favorable conditions, good quality films with better than 95% transmittance in visible range and a specific resistivity of 16Ωcm could be obtained. The optimum doping was found to be 5 mole% Al. The heat treatment should be carried out by calcination in air at 425 oC, then annealed at 500 oC under nitrogen.

關鍵字(中)

★ 氧化鋅摻雜鋁
★ 濕法
★ 透明導電膜

關鍵字(英)

★ spin-coating
★ AZO
★ TCO

論文目次

摘要............................................................I
總目錄.........................................................II
第一章緒論.....................................................1
1.1 氧化鋅材料簡介..............................................1
1.2 透明導電薄膜................................................2
1.2.1 透明導電薄膜簡介..........................................2
1.2.2 透明導電薄膜的製備方法....................................3
1.3 氧化鋅薄膜之製備與應用......................................5
1.3.1 氧化鋅薄膜之製備..........................................5
1.3.1.1 摻雜（doping）的作用與原理..............................6
1.3.1.2 柏斯坦-摩斯偏移（Burstein-Moss shift）理論..............7
1.3.2 氧化鋅薄膜之應用..........................................7
1.4 文獻回顧....................................................8
1.5 研究目的與方向.............................................14
第二章濕法製備氧化鋅摻雜鋁之透明導電膜........................15
2.1 溶膠的製備.................................................15
2.1.1 配製藥品.................................................15
2.1.2 溶膠的合成...............................................16
2.2 膜的製備...................................................19
2.2.1 基材的前處理.............................................19
2.2.2 鍍膜.....................................................20
2.3 儀器分析...................................................23
2.3.1 動態雷射散射儀（DLS）分析................................23
2.3.2 紫外光-可見光光譜儀分析（光學性質）......................23
2.3.3 熱重損失分析（TGA）......................................24
2.3.4 溶膠乾燥後粉體的晶相鑑定分析（XRD）......................24
2.3.5 穿透式電子顯微鏡（TEM）分析..............................25
2.3.6 掃描式電子顯微鏡（SEM）分析..............................25
2.3.7 四點探針儀測量薄膜的電阻率...............................25
2.3.7.1 導電度的定義...........................................25
2.3.7.2 四點探針儀的測.........................................27
2.3.7.3 半導體的導電度範圍.....................................28
第三章實驗結果和討論..........................................29
3.1 溶膠的粒徑大小、穿透度、吸收度和TEM照片比較................29
3.2 溶膠乾燥後的TGA分析（熱分析）..............................30
3.3 溶膠乾燥後粉體的XRD分析....................................31
3.4 煅燒溫度和退火溫度對鍍膜穿透度和電阻率的影響...............32
3.5 改變蒸氣加熱時間和溫度對薄膜的影響.........................34
3.6 改變鋁的摻雜量對薄膜電阻率的影響...........................35
3.7 以EDS成分分析確定Al/Zn比例.................................36
第四章結論與未來研究方向......................................37
參考文獻.......................................................40
附錄一實驗使用之藥品..........................................44
附錄二實驗使用之測量儀器......................................45
表目錄.........................................................46
圖目錄.........................................................50

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指導教授

蔣孝澈(Anthony S.T. Chiang)

審核日期

2006-7-13

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