極小孔徑陽極氧化鋁模板之製備及在矽基材上生成大面積規則排列氧化鋁模板及奈米點陣列之研究

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研究生：	劉柏廷 Po-ting Liu
論文名稱：	極小孔徑陽極氧化鋁模板之製備及在矽基材上生成大面積規則排列氧化鋁模板及奈米點陣列之研究 Synthesis of Freestanding AAO Template with Ultra-small Pore Size, and Fabrication of Well-ordered Thin AAO Templates and Nanodots Array on Si Substrate
指導教授：	鄭紹良 Shao-liang Cheng
口試委員:
學位類別：	碩士 Master
系所名稱：	工學院 - 化學工程與材料工程學系 Department of Chemical & Materials Engineering
畢業學年度：	98
語文別：	中文
論文頁數：	97
中文關鍵詞：	陽極氧化鋁、奈米點陣列
外文關鍵詞：	nanodots array, AAO
相關次數：	點閱：16 下載：0
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本研究之內容主要分成極小孔徑陽極氧化鋁奈米模板與矽基規則陽極氧化鋁奈米模板之製備兩部分，並針對其孔洞排列、孔徑大小與分佈進行量測分析。在製備出矽基材上大面積規則排列陽極氧化鋁奈米模板後，利用此模板製備兩種零維奈米點陣列，並對各奈米點之形貌與晶體結構進行分析鑑定。
在極小孔徑陽極氧化鋁奈米模板的部分，我們成功地利用高純度鋁片以兩次陽極氧化處理法製備出孔徑可調變 ( 10 - 60 nm ) 之陽極氧化鋁，並經由移除鋁片與氧化鋁孔道底部之阻障層得到極小孔徑陽極氧化鋁模板 ( 平均孔徑大小 < 10 nm ) ，此極小孔徑奈米模板相信將可用於大量製備極細一維奈米線陣列結構。
在矽晶基材上製備低深寬比之規則陽極氧化鋁奈米模板方面，本研究結合奈米球微影術與電漿蝕刻技術，在矽基鋁薄膜上預置遮罩並定義鋁薄膜之反應區域進行一次陽極氧化處理，可成功地製備出大面積規則有序排列之矽基氧化鋁奈米薄膜，並經由磷酸蝕刻底部阻障層後可得到大面積孔洞規則排列且孔徑可由奈米球遮罩調變之矽基氧化鋁奈米模板。應用此製程移除表層之氧化鋁模板，可得到大面積規則有序排列之奈米點陣列，經 AFM、TEM 與 SAED 鑑定後為非晶形之氧化矽奈米點陣，其高度約為 32 - 40 nm 。此外我們也使用上述所製備之低深寬比規則氧化鋁模板結合電子槍蒸鍍鎳金屬，經移除氧化鋁模板後可得到大面積規則有序排列之奈米點陣列，經 TEM 與 SAED 鑑定分析可知其為多晶之鎳金屬奈米點陣列結構。

In this study, we show the successfully fabrication of two types of anodic aluminum oxide (AAO) templates. One is the free standing AAO nanotemplate with ultra-small pore size (<10nm), and the other is the thin AAO template with 2-D periodic nanopore structure on Si substrate.
To fabricate free standing AAO nanotemplates, high purity Al foils were used as the start materials, and a two-step anodizing process was employed. In this works, the pore diameters of AAO nanotemplates can be tuned from 9 to 60 nm by varying the electrolyte composition, applied voltage, and processing temperature. The obtained AAO nanotemplates can be extended to fabricate a large amount of ultra-narrow nanowires.
The present study also demonstrated that the thin AAO templates with well-ordered nanopore arrays were successfully fabricated on (001)Si substrates by employing the nanosphere lithography technique and selective anodic oxidation process. The pore diameter and the interspacing can be readily controlled by adjusting the diameters of the colloidal nanospheres and the anodic etching conditions. After removal of the AAO templates, large-area periodic SiOx nanodots array was found to form on Si substrate. Furthermore, the hexagonally arrayed porous AAO membrane can be used as the template for fabrication of metal nanodot arrays on Si substrate. After the deposition of Ni thin films and subsequent lift-off of the AAO template, the hexagonal periodic Ni nanodot arrays were found to form on the surface of (001)Si substrate. The size of the deposited Ni nanodots were measured to be about 170 nm, corresponding to the pore size of the thin AAO template. Based on TEM and SAED analyses, it is found that the crystal structure of Ni nanodots is polycrystalline.

第1章 簡介..........................................1
1-1 前言..........................................1
1-2 多孔性陽極氧化鋁奈米模板..........................................3
1-2-1 氧化鋁模板的發展背景..........................................3
1-2-2 氧化鋁模板的原理與製備..........................................4
1-2-3 陽極氧化反應的各種變因與影響..........................................6
1-2-4 陽極氧化鋁模板的相關應用..........................................7
1-3 在矽基材上製作陽極氧化鋁奈米模板..........................................8
1-3-1 直接轉置法..........................................8
1-3-2 鍍製鋁膜氧化法..........................................9
1-4 奈米球微影術..........................................10
1-4-1 奈米球自組裝技術..........................................10
1-4-2 奈米球微影術的發展..........................................10
1-4-3利用奈米球微影術製備各式規則排列新穎奈米結構..........................................11
1-5 規則排列之奈米點陣列..........................................11
1-6 研究動機..........................................12
第2章 實驗步驟..........................................14
2-1 以高純度鋁片製備陽極氧化鋁模板..........................................14
2-2 在矽基材上製備陽極氧化鋁模板..........................................16
2-2-1 矽晶片之清洗..........................................16
2-2-2 沉積鋁薄膜..........................................16
2-2-3 氧化鋁模板的製備：兩次陽極處理法..........................................17
2-3 在矽基材上製備規則有序排列之陽極氧化鋁模板..........................................17
2-3-1 矽基材上的鋁薄膜製備..........................................17
2-3-2 自組裝奈米球陣列..........................................18
2-3-3 調變奈米球球徑..........................................18
2-3-4 遮罩蒸鍍與奈米球之舉離..........................................18
2-3-5 一次陽極氧化與移除底部阻障層..........................................19
2-4 於矽基材上製備規則排列之鎳金屬奈米點..........................................19
2-5 矽基材上規則排列氧化矽點陣列的製作..........................................19
2-6 實驗設備..........................................20
2-6-1 氧化鋁模板製備系統..........................................20
2-6-2 直流式真空濺鍍系統..........................................20
2-6-3 電漿蝕刻系統..........................................20
2-6-4 電子槍蒸鍍系統..........................................21
2-7 分析儀器..........................................21
2-7-1 掃描式電子顯微鏡..........................................21
2-7-2 穿透式電子顯微鏡..........................................22
2-7-3 原子力顯微鏡..........................................22
第3章 結果與討論..........................................23
3-1 高純度鋁片製備之陽極氧化鋁模板..........................................23
3-1-1 以草酸為電解液製備陽極氧化鋁模板..........................................24
3-1-2 以硫酸為電解液製備陽極氧化鋁模板..........................................25
3-1-3 藉由電流曲線圖觀察陽極氧化之變因影響..........................................27
3-1-4 極小孔徑奈米模板之製程..........................................28
3-2 兩次陽極處理法製備矽基材上之陽極氧化鋁模板..........................................29
3-2-1 於矽基材表面沉積鋁金屬薄膜..........................................29
3-2-2 矽基氧化鋁奈米模板孔洞排列規則度之探討..........................................30
3-3 結合奈米球微影術進行陽極處理製備規則排列之氧化鋁奈米模板..........................................31
3-3-1 預置反應區域之矽基鋁金屬薄膜..........................................32
3-3-2 大面積規則有序排列矽基陽極氧化鋁模板之製備..........................................33
3-3-3 不同方式製備有序排列矽基氧化鋁模板結果比較..........................................34
3-4 大面積規則有序排列奈米點陣列之製備..........................................35
3-4-1 氧化矽奈米點陣列之製備與分析..........................................36
3-4-2 鎳金屬奈米點陣列之製備與分析..........................................37
第4章 結論與未來展望..........................................39
4-1 結論..........................................39
4-2 未來展望..........................................40
4-2-1 在不同基材上製備規則排列之陽極氧化鋁模板..........................................40
4-2-2 矽晶基材上大面積規則排列之金屬矽化物..........................................40
參考文獻..........................................41
圖目錄..........................................49

                                

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