臺灣博碩士論文加值系統

本篇論文我們研究以硫酸鋅(ZnSO4.Zinc sulfate)去製作生長氧化鋅奈米柱，並且成功生長在銅網的基板上，使用電鍍(electroplating)的方式製作一層晶種層，再以水熱法(hydrothermal method)的方式使硫酸鋅溶液成功生長氧化鋅奈米柱。進一步地，使用硫化納（Na2S•Sodium sulfide）在氧化鋅奈米柱的表面生長一層硫化鋅殼層。為了研究在硫酸鋅生長氧化鋅奈米柱與硫酸鋅生長氧化鋅奈米柱表面硫化鋅殼層之生長時間對於其表面形態樣貌以及其特性，用多種分析例如: 場發射掃描式電子顯微鏡(FESEM)、、光致發光光譜分析儀(PL)、穿透式電子顯微鏡(TEM)測試等等，來進行分析。

This thesis, ZnO/ZnS core/shell structures were fabricated on copper grids and on silicon substrate. With solutions containing ZnO(NO3)2 and ZnSO4. Zinc sulfate was incorporated in the solution to grow ZnO nanorods on copper grids. Firstly, the seed layer was electroplated on the grids or substrates and followed by hydrothermal growth to form ZnO nanorods. Afterwards, ZnS shell was grown on ZnO nanorods’surface in solutions containing Sodium sulfide to form the core shell structure. In order to investigate the characteristics of the structure with various growth time, multiple analyses, such as field-emission scanning electron microscope (FESEM), photoluminescence (PL), transmission electron microscope (TEM) and surface contact angle measurement were performed.

目次

謝誌 i
摘要 ii
Abstract iii
目次 iv
表目次 vii
圖目次 viii
第一章 緒論 1
1-1前言 1
1-2 研究動機 1
第二章 研究材料介紹及文獻 4
2-1奈米材料 4
2-2表面效應 5
2-3奈米材料之量子穿隧效應 5
2-4奈米材料之量子尺寸效應 7
2-5二氧化矽（SiO2）的介紹 8
2-6氧化鋅(ZnO)介紹 8
2-7硫化鋅（ZnS）介紹 9
2-8材料文獻參考 10
2-9化學反應式 13
第三章 實驗儀器與步驟 14
3-1分析用儀器 14
3-1-1場發射掃描式電子顯微鏡 14
3-1-2 X射線繞射分析儀 15
3-1-3光致發光光譜分析儀 16
3-1-4接觸角分析 17
3-1-5穿透式電子顯微鏡 18
3-1-6化學分析電子能譜儀 19
3-2 實驗藥品 20
3-3 實驗儀器 26
3-4 實驗方法 30
3-4-1溶膠凝膠法 30
3-4-2 水熱法 30
3-5 實驗步驟 31
3-5-1 清洗基板 31
3-5-2 氧化鋅奈米柱電鍍晶種層溶液配製 32
3-5-3 電鍍晶種層 32
3-5-4 水熱法生長溶液配製 33
第四章 以旋塗法生長氧化鋅奈米柱在二氧化矽基板上 34
4-1使用二氧化矽(SiO2)基板生長氧化鋅奈米柱 34
4-2 硫酸鋅溶液生長氧化鋅奈米柱FE-SEM與EDS之分析 35
4-3硝酸鋅溶液生長氧化鋅奈米柱FE-SEM與EDS之分析 37
4-4 硫酸鋅XRD之分析 39
4-5硫酸鋅溶液有無加入環六亞甲基四胺生長氧化鋅奈米柱 41
4-6改變硫酸鋅溶液濃度加入環六亞甲基四胺生長氧化鋅奈米柱 43
4-7硫酸鋅生長奈米柱在硫化殼層結構 45
4-8硫酸鋅生長奈米柱之硫化殼層結構XRD之分析 48
4-9 硫酸鋅生長奈米柱之硫化殼層結構PL分析 49
4-10硫酸鋅生長奈米柱之硫化殼層結構接觸角分析 50
4-11 硫酸鋅生長奈米柱之5分鐘硫化殼層結構穿透式電子顯微鏡 52
第五章 結果與討論 56
5-1 掃描電子顯微鏡(Scanning Electron Microscope) 56
5-2 能量分散分析儀(Energy-dispersive X-ray spectroscopy) 60
5-3 穿透式電子顯微鏡(Transmission electron microscope, TEM) 62
第六章 結論 65
參考文獻 66

表目次

表3- 1晶種層藥品 20
表3- 2電鍍晶種層藥品 21
表3- 3水熱法生長硫酸鋅溶液 22
表3- 4水熱法生長溶液 23
表3- 5水熱法生長硫化鋅溶液 24
表3- 6基材介紹 25

圖目次
圖2- 1表面原子數與粒徑大小關係 4
圖2- 2表面效應 5
圖2- 3量子穿隧效應[23] 6
圖2- 4硫化鋅 9
圖2- 5硫酸鋅溶液 10
圖2- 6生長硫化鋅殼層示意圖 13

圖3- 1場發射掃描式電子顯微鏡 14
圖3- 2布拉格繞射圖 15
圖3- 3 XRD 工作原理圖 15
圖3- 4 PL分析儀示意圖 16
圖3- 5接觸角分析示意圖 17
圖3- 6穿透式電子顯微鏡示意圖 18
圖3- 7化學分析電子能譜儀示意圖 19
圖3- 8旋轉塗佈機 26
圖3- 9水熱槽 26
圖3- 10加熱攪拌器 27
圖3- 11 PID控制加熱板 27
圖3- 12超音波震洗機 28
圖3- 13電子分析天秤 28
圖3- 14電源供應器 29
圖3- 15水熱法 30
圖3- 17電源供應器 32

圖4- 1硫酸鋅隨時間變化 35
圖4- 2硫酸鋅EDS隨時間變化 36
圖4- 3硝酸鋅隨時間變化 37
圖4- 4硝酸鋅EDS隨時間變化 38
圖4- 5氧化鋅隨時間增加XRD繞射圖 39
圖4- 6 SIO2基板生長氧化鋅奈米柱之加入環六亞甲基四胺分析(X10,000) 41
圖4- 7 SIO2基板生長氧化鋅奈米柱之加入環六亞甲基四胺分析(X50,000) 41
圖4- 8 SIO2基板生長氧化鋅奈米柱之加入環六亞甲基四胺分析(X100,000) 41
圖4- 9 SIO2基板生長氧化鋅奈米柱之未加入環六亞甲基四胺分析(X10,000) 42
圖4- 10 SIO2基板生長氧化鋅奈米柱之未加入環六亞甲基四胺分析(X50,000) 42
圖4- 11 SIO2基板生長氧化鋅奈米柱之未加入環六亞甲基四胺分析(X100,000) 42
圖4- 12 SIO2基板改變硫酸鋅溶液位未加入六亞甲基四胺 43
圖4- 13 SIO2基板改變硫酸鋅溶液位加入六亞甲基四胺 44
圖4- 14 SIO2基板生長氧化鋅硫化5分鐘殼層結構分析(X10,000) 45
圖4- 15 SIO2基板生長氧化鋅硫化5分鐘殼層結構分析(X50,000) 45
圖4- 16 SIO2基板生長氧化鋅硫化5分鐘殼層結構分析(X100,000) 45
圖4- 17 SIO2基板生長氧化鋅硫化10分鐘殼層結構分析(X10,000) 46
圖4- 18 SIO2基板生長氧化鋅硫化10分鐘殼層結構分析(X50,000) 46
圖4- 19 SIO2基板生長氧化鋅硫化10分鐘殼層結構分析(X100,000) 46
圖4- 20 SIO2基板生長氧化鋅硫化20分鐘殼層結構分析(X10,000) 47
圖4- 21 SIO2基板生長氧化鋅硫化20分鐘殼層結構分析(X50,000) 47
圖4- 22 SIO2基板生長氧化鋅硫化20分鐘殼層結構分析(X100,000) 47
圖4- 23 化鋅隨時間增加XRD繞射圖 48
圖4- 24 酸鋅PL分析 49
圖4- 25氧化鋅奈米柱接觸角分析 50
圖4- 26氧化鋅生長硫化殼層結構5分鐘接觸角分析 50
圖4- 27氧化鋅生長硫化殼層結構10分鐘接觸角分析 51
圖4- 28氧化鋅生長硫化殼層結構20分鐘接觸角分析 51
圖4- 29硫酸鋅硫化殼層奈米柱 50NM 52
圖4- 30硫酸鋅硫化EDS圖 53
圖4- 31硫酸鋅硫化殼層奈米柱比例圖50NM 53
圖4- 32氧化鋅晶格 54
圖4- 33硫酸鋅晶格 54
圖4- 34硫化鋅晶格 54
圖4- 35硫酸鋅SAED 55

圖5- 1硫酸鋅(左) 硝酸鋅(右) 1萬倍率 56
圖5- 2硫酸鋅(左) 硝酸鋅(右) 5萬倍率 57
圖5- 3硫酸鋅(左) 硝酸鋅(右) 10萬倍率 57
圖5- 4硫酸鋅(左) 硝酸鋅(右) 1萬倍率 58
圖5- 5硫酸鋅(左) 硝酸鋅(右) 5萬倍率 58
圖5- 6硫酸鋅(左) 硝酸鋅(右) 10萬倍率 59
圖5- 7硫酸鋅EDX圖 60
圖5- 8硝酸鋅EDX圖 60
圖5- 9硫酸鋅硫化EDX圖 61
圖5- 10硝酸鋅硫化EDX圖 61
圖5- 11硫酸鋅硫化殼層奈米柱100NM 62
圖5- 12硫酸鋅硫化殼層奈米柱20NM 63
圖5- 13硫酸鋅硫化殼層奈米柱5NM 63
圖5- 14硫酸鋅晶格 64
圖5- 15硫酸鋅SAED 64

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