臺灣博碩士論文加值系統

微波輔助化學浴沉積法(microwave-assisted chemical bath deposition, MWCBD)是一種新的快速合成 ZnO 單晶奈米柱的方法，本研究使用MWCBD，以硝酸鋅六結晶水(Zn(NO3)2∙6H2O)當作鋅離子源，六亞甲基四胺(HMT, C6H12N4)作為酸鹼緩衝劑，在低於 100 °C 溫度條件下沉積，基板為晶格常數匹配程度與 ZnO 相近的 GaN， 探討成長高品質之 ZnO 磊晶薄膜所需之條件，特別是用檸檬酸鈉(Na3C6H5O7)改質劑在微波環境中對成長氧化鋅晶柱的影響，並且探討溫度、濃度、時間對在使用微波加熱的水溶液 ZnO 析出以及 pH值的影響。
從溶液外觀的顏色特徵觀察結果發現，當溫度越高時水溶液的顏色就越純白並且產生更多的 ZnO 粉末，pH 值的變化則是約降低為5.5；而濃度越高時，製程結束之後的 ZnO 粉末就越多，水溶液的 pH值也更低。
在 ZnO 磊晶方面，從掃描式電子顯微鏡之觀察，可以確定 MWCBD 在加入檸檬酸鈉後，有助於成長出連續膜磊晶； ZnO 膜厚約為 1 m，X 光繞射 –scan 量測得到(0004)面的半高寬為 860 arcsec，約為 GaN 半高寬的兩倍，而 ZnO (303 ̅2)面的半高寬則為 1288 arcsec，略高於 GaN 之 1078 arcsec，因此 ZnO 成核過程中所形成的螺旋差排是影響 ZnO 結晶品質的因子。檸檬酸鈉濃度為 0.04 mM 時，對晶柱側向成長即有明顯之效果，ZnO 晶柱的高寬比約 0.83 左右，平均成膜速率 ~ 1 m/h。

Microwave-assisted chemical bath deposition (MWCBD) is a newly developed method for rapid synthesis of single-crystalline ZnO nanorods. In this study, MWCBD was used to synthesize ZnO with high-quality epitaxial ZnO film, using hexahydrate zinc nitrate (Zn(NO3)2∙6H2O) as the Zn2+ source, hexamethylenetetramine (HMT, C6H12N4) as pH buffer, GaN/sapphire as the substrate with small lattice mismatch with ZnO, at temperature less than 100°C. Also, the effect of sodium citrate (Na3C6H5O7) as the capping agent on lateral growth of ZnO rod for continuous film formation has been explored based on the evolution of the measured aspect ratio of height-to-width in the microwave environment. Additionally, the effects of temperature, concentration, and time on pH change of aqueous solutions with precipitation of ZnO powders and during microwave heating were evaluated.
When the heating temperature is increased, the color of the aqueous solution as seen from the visual appearance becomes more pure white as more precipitated ZnO powders were produced and the pH value decreases from 6.8 to about 5.5. Increasing the concentration of zinc nitrate precursor results in the higher quantity of ZnO powders and reduction of the pH value of the aqueous solution.
In the study of ZnO epitaxy on GaN, scanning electron microscopy observations in top view and cross-section show that thin film of epitaxial ZnO in thickness of about 1 μm can be effectively grown on GaN/sapphire with MWCBD by adding sodium citrate to the solution to enhance the lateral growth of ZnO rods with coalescence. It is found that to reach an aspect ratio of height to width of 0.83, the concentration of sodium citrate is required to increase to 0.04 mM which can still have an average growth rate of ~ 1 m/h. The film quality as characterized by x-ray diffraction in –scan shows a full width at half maximum of the (0004) rocking curve in 860 arcsec, which is twice as high as substrate of GaN, whereas it is 1288 arcsec for (303 ̅2) FWHM slightly increased from 1078 arcsec for GaN, suggesting that ZnO film quality is mainly affected by screw dislocations formed in rod nucleation.

目錄
摘要………………………………..…………………..…………i
ABSTRACT…………………….……………………………….iii
目錄………………………..……………………………..………v
圖目錄…………………………….…………………………..……..ix
表目錄…………………..………………………..……………….xiii
第一章、前言...................................................................1
1.1緒論.......................................................................................1
1.2微波加熱…………..........................................................2
第二章、文獻回顧................................................................................6
2.1氧化鋅之晶體結構..........................................................6
2.2氧化鋅之常見製程…………………………………………….9
2.2.1濺鍍(sputtering) ………………………………….9
2.2.2脈衝雷射沉積((pulsed laser depositon , PLD) ……..9
2.2.3分子束磊晶(molecular beam epitaxy , MBE)……….10
2.2.4金屬有機化學氣相沉積(Metal-organic Chemical Vapor Deposition , MOCVD)……………………………………….. 11
2.2.5化學浴沉積法(Chemical bath deposition) ……………14
2.2.5.1加入改質劑控制形貌…………………………….16
2.2.5.2 pH值於化學浴…………………………………16
2.3微波輔助加熱化學浴(簡稱MWCBD)………….……17
2.3.1微波輔助加熱…………………………..………………17
2.3.2以MWCBD成長ZnO…………………………….….19
2.3.2.1 微波功率............................................................19
2.3.2.2 前驅物與形貌.................................................20
2.3.2.3 成長速率與磊晶情況............................................21
2.4研究動機.................................................................22
第三章、氧化鋅之實驗流程與設備.....................................................31
3.1微波輔助化學浴系統實驗....................................................31
3.1.1實驗之機台............................................................31
3.1.2微波機台之特色....................................................32
3.1.2.1 PID控制系統.................................................32
3.1.2.2穩定的微波源...............................................33
3.1.3 實驗之流程.......................................................33
3.1.4 實驗之參數.........................................................35
3.2材料分析設備與技術.................................................................44
3.2.1掃描式電子顯微鏡(Scanning Electron Microscope)........44
3.2.2 X光繞射分析儀(X-ray Diffraction)..............................45
3.2.3穿透式電子顯微鏡(Transmission Electron Microscope)..48
3.2.4聚焦離子束(Focus ion beam, FIB) ...............................49
3.2.5光激發光光譜(Photoluminescence , PL)……….……..51
3.2.6 二次離子質譜儀(Secondary ion mass spectroscope)…...51
第四章、微波輔助加熱水溶液之現象與問題......................................53
4.1高濃度前驅物溶液的配置.......................................53
4.1.1去除去離子水的氣體溶解量…………..….………..53
4.1.2溶液配置的順序…………………………….……..…53
4.2水溶液pH值的變化...........................................54
4.3 ZnO白色粉末....................................................55
4.3.1粉末情況..............................................................55
4.3.2試片正反面之影響……………………………….…….56
4.3.3攪拌子的使用.............................................................56
4.4濃度對水溶液外觀以及 pH 值的影響....................................63
4.4.1濃度對水溶液外觀的影響...................................63
4.4.2濃度對水溶液pH值的影響...................................64
4.5溫度對水溶液外觀以及 pH 值的影響...................................70
4.5.1溫度對水溶液外觀的影響...................................70
4.5.2溫度對水溶液pH值的影響...................................72
第五章、ZnO磊晶結果與討論............................................................77
5.1 磊晶的ZnO................................................................79
5.1.1 XRD分析.................................................................80
5.1.2 SEM分析................................................................93
5.1.3 PL分析…………………….………………………..98
5.1.4 TEM分析……………...………………………….…102
5.2 檸檬酸鈉濃度對ZnO的影響.............................................103
5.2.1 ZnO的高寬比………………………………….…....103
5.2.2 檸檬酸鈉濃度對發光特性的影響...……….…………109
5.2.3 檸檬酸鈉濃度的SIMS分析...……….………………111
第六章、結論.......................................................................112
參考文獻.............................................................................114


 
圖目錄
圖1- 1 ZnO的wurtzite結構。 - 4 -
圖1- 2 微波在電磁波譜中的位置。 - 4 -

圖2- 1 六方纖鋅礦ZnO的晶體結構與晶格常數。 - 7 -
圖2- 2 (a)纖鋅礦ZnO之單位晶胞(b)和(c)表不同的Zn-O鍵長，導致自發極化場。 - 7 -
圖2- 3 六方堆積結構c、a與m面幾何關係圖。 - 8 -
圖2- 4 一般sputter機台示意圖。 - 12 -
圖2- 5 PLD機台示意圖。 - 12 -
圖2- 6 MBE機台示意圖。 - 13 -
圖2- 7 MOCVD機台示意圖。 - 13 -
圖2- 8 HMT分子外觀。 - 23 -
圖2- 9 25°C的溶液中 (a) ZnO(s)-H2O和 (b) Zn(OH)2-H2O相穩定圖。 - 23 -
圖2- 10不同pH值造成的氧化鋅結晶形貌。 - 24 -
圖2- 11 微波加熱與傳統加熱方式的差異(左為微波右為傳統)。 - 24 -
圖2- 12 微波影響極性分子轉動示意圖。 - 25 -
圖2- 13 元素週期表中常見原子的電負度值。 - 25 -
圖2- 14 C原子與Si原子的sp3鍵結和sp2鍵結。 - 26 -

圖3- 1 機台外觀。 - 38 -
圖3- 2 腔體內部外觀。 - 38 -
圖3- 3 內部構造示意圖。 - 39 -
圖3- 4 控制台實際面板情況(a)溫度瓦數時間圖，(b)內部監測影像，(c)實驗參數圖。 - 40 -
圖3- 5 控制台外觀。 - 41 -
圖3- 6 PID控制系統所觀測到的溫度功率時間圖。 - 41 -
圖3- 7 微波曲線對時間積分之後所計算出的平均功率(a)升溫時為336W，(b)整體平均為303W。 - 42 -
圖3- 8 載具於溶液中的情況。 - 43 -
圖3- 9 水溶液配置順序示意圖。 - 43 -

圖4- 1 溶液配置順序示意圖。 - 60 -
圖4- 2 左與右分別為持溫 1h 與 5h 的 SEM 橫截面圖。 - 60 -
圖4- 3 以70°C成長30 min在SEM底下看到有Zn(OH)2 的晶型。….. - 60 -
圖4- 4 在90C下30 min後溶液中白色粉末的 XRD 訊號。 - 61 -
圖4- 5 在80C下成長10min 之SEM影像。(a)正面朝上，白色粉末污染嚴重，(b)正面朝下，白色粉末汙染不嚴重。 - 61 -
圖4- 6 在80C下成長30min 之SEM影像。使用攪拌子參與製程，導致ZnO產生不平整堆疊之SEM圖像。 - 62 -
圖4- 7 不同濃度的白色粉末沉澱量(a) 0.1 M，(b) 0.05 M，(c) 0.025 M。 - 69 -
圖4- 8 不同前驅物濃度的pH值與對應溫度及時間之關係圖。 - 69 -
圖4- 9 相同濃度不同持溫的pH值與對應溫度及時間之關係圖。…… - 76 -
圖4- 10 (a)升溫中的平均微波功率，(b)持溫時的平均為微波功率。… - 76 -

圖5- 1 利用(0002)、、(2023)、(3032)三個面的FWHM外插得到刃差排之FWHM示意圖。 - 85 -
圖5- 2 D製程與S製程成長ZnO的XRD-2θ結果。 - 87 -
圖5- 3 D製程(黑)與S製程(紅)成長ZnO的XRD-2θ結果 (72°至73°)。 - 87 -
圖5- 4 GaN與D製程成長ZnO的φscan以及半高寬。 - 88 -
圖5- 5 GaN與S製程成長ZnO的φscan以及半高寬。 - 88 -
圖5- 6 D製程成長之GaN的(0004) ωscan以及半高寬。 - 89 -
圖5- 7 D製程成長之ZnO的(0004) ωscan以及半高寬。 - 89 -
圖5- 8 D製程成長之GaN (3032)的ωscan以及半高寬。 - 90 -
圖5- 9 D製程成長之ZnO (3032)的ωscan以及半高寬。 - 90 -
圖5- 10 S製程成長之GaN的(0004) ωscan以及半高寬。 - 91 -
圖5- 11 S製程成長之ZnO的(0004) ωscan以及半高寬。 - 91 -
圖5- 12 S製程成長之GaN (3032)的ωscan以及半高寬。 - 92 -
圖5- 13 S製程成長之ZnO (3032)的ωscan以及半高寬。 - 92 -
圖5- 14 D製程成長ZnO的SEM俯視圖與橫截面。 - 95 -
圖5- 15 S製程成長ZnO的SEM俯視圖與橫截面。 - 96 -
圖5- 16 S製程中第一階段成長所形成的ZnO粉末物堆積在表面。 ……- 97 -
圖5- 17 D製程與S製程成長之ZnO以及GaN/sapphire基板的PL光譜。 - 101 -
圖5- 18 S製程ZnO與GaN的TEM與FFT圖。 - 102 -
圖5- 19 檸檬酸鈉0 M與0.01 mM的SEM俯視圖與橫截面圖。 …….- 106 -
圖5- 20檸檬酸鈉0.02 M與0.04 mM的SEM俯視圖與橫截面圖。…. - 107 -
圖5- 21 ZnO高度、寬度、高寬比與檸檬酸納濃度的關係。 - 108 -
圖5- 22 檸檬酸鈉0 M與0.04 mM 的PL光譜。 - 110 -
圖5- 23 加入0.02 mM 檸檬酸鈉的ZnO試片之SIMS結果分析。….. - 111 -

表目錄
表1- 1 ZnO的基本性質。 - 5 -

表2- 1部份常見溶劑的極性、介電常數和密度(依分子極性及其類別的差異分類)。 - 26 -

表3- 1 實驗所使用的化學物。 - 37 -
表3- 2 實驗所使用的參數表。 - 37 -
表3- 3 實驗中使用之材料的2θ繞射峰位置、強度與平面間距。 - 47 -

表4- 1 1atm，氣體溶解度與溫度的關係(ml/1ml H2O)。 - 58 -
表4- 2 溶液濃度之外觀差異。 - 59 -
表4- 3 不同濃度下的水溶液情況。 - 67 -
表4- 4 不同溫度下的水溶液外觀。 - 74 -

表5- 1 (a)前驅物濃度為0.025 M，檸檬酸鈉濃度為0.02 mM，在80C下成長10 min之 ZnO 的SEM圖，(b) 前驅物濃度為0.1 M，檸檬酸鈉濃度為0.02 mM，在85C下成長1 h 之 ZnO 的SEM圖。 - 78 -
表5- 2 實驗相關參數。 - 79 -
表5- 3 φscan peak的半高寬值。 - 81 -
表5- 4 (0004)晶面以及(3032)晶面的rocking curve 半高寬值。 - 86 -
表5- 5 實驗參數表。 - 105 -
表5- 6 不同檸檬酸鈉濃度對於ZnO晶柱的高寬比影響。 - 105 -

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