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研究生： 李國豪
Lee, Kuo-Hao
論文名稱： 化學氣相沈積法成長氮化鎵奈米線之材料特性與應用分析
Characterizations and Applications of GaN Nanowires Synthesized by Chemical Vapor Deposition
指導教授： 陳引幹
Chen, In-Gann
學位類別： 博士
Doctor
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： 2010
畢業學年度： 98
語文別： 中文
論文頁數： 193
中文關鍵詞： 奈米線 、拉曼 、離子佈植
外文關鍵詞： nanowire, Raman, implant
相關次數： 點閱：86  下載：0 
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    • 本實驗利用金屬鎵與氨氣氣體做為反應物，搭配附著在矽基板上的鉑顆粒做為催化劑，在置於水平式高溫爐內的矽基板上利用化學氣相沈積反應，以固相液相氣相成長機制進行氮化鎵奈米線成長。實驗中，先以改變不同的反應壓力、氨氣氣體流量與成長溫度，做為選擇成長氮化鎵奈米線的實驗參數。實驗參數確定後，再透過搭配不同氣體流量比例的成長參數，觀察氣體流量比例變化對奈米線所產生的應力與電性表現的影響。此外，氮化鎵奈米線的成長製程亦將分別搭配矽基板在奈米金水溶液浸泡處理的實驗以及離子佈植劑量改變的實驗，用來做為奈米線線徑控制方法與觀察材料電子結構變化的分析。氮化鎵奈米線應用的部分，則是將上述不同氣體流量比例所成長的奈米線以及搭配電子束蒸鍍技術處理程序的奈米線，進行應用在場發射與表面增顯拉曼表現的分析。
    第一部份實驗，將以固定總氣體流量，改變不同反應氣氛(H2/NH3)流量比例，進行氮化鎵奈米線成長。並分別用拉曼量測與電流電壓曲線量測系統，分析不同反應氣氛流量比例對氮化鎵奈米線所產生的應力與電性變化的影響。拉曼量測結果顯示，反應過程中H2氣體流量比例變大時，奈米線晶體內會有壓縮應力現象產生; 電流電壓量測曲線結果顯示，反應過程中H2氣體流量比例變大時，奈米線的啟動電壓值也越來越大，原因是因為有大量的氫原子形成電子捕獲中心缺陷，造成啟動電壓值上升。而奈米線電阻值下降的原因，是因為有氮原子形成贈體缺陷與穿遂電流現象的產生。
    在第二部分，本實驗提供一種簡易快速的方式，控制催化劑粒徑大小，並利用催化劑尺寸的改進，進一步控制氮化鎵奈米線的成長線徑尺寸，藉以改善線徑分佈不均的情況。實驗結果顯示，透過電漿處理與浸泡奈米金水溶液的方式，我們可以在矽基板上控制金顆粒大小，其尺寸分佈標準差可以從未改善前的20 nm 縮小至改善後的8 nm; 而所對應成長的氮化鎵奈米線線徑尺寸分佈標準差可以從未改善前的35 nm縮小至改善後的10 nm。這結果顯示，電漿處理與浸泡水溶液的方式，可以分別減少催化劑粒徑與線徑的分佈差異。
    在第三部分，本實驗利用離子佈值技術，將不同銪離子劑量佈植於相同成長條件的氮化鎵奈米線。對於離子轟擊所產的點缺陷，以X光吸收光譜與光激發螢光光譜量測進行分析。X光吸收光譜分析結果顯示，離子轟擊後的氮化鎵奈米線，由於有氮插入型與氮懸鍵缺陷的形成，因此可以觀察到氮化鎵奈米線的電子躍遷軌域會從sp3為主的混成軌域逐漸轉向sp2混成軌域。當電子躍遷以sp2混成軌域為主時，會造成氮化鎵奈米線在光激發螢光光譜近能帶邊緣放射光強度減弱。氮插入型與氮懸鍵缺陷的X光吸收光譜強度隨著佈植劑量增加而上升的趨勢顯示，離子轟擊氮化鎵奈米線時，這些點缺陷特別容易形成。
    最後部分，則是利用氮化鎵奈米線進行應用在場發射與表面增顯拉曼方面的量測與分析。場發射的量測結果顯示，利用氮化鎵奈米線表面具有大量微小突起物的外型特徵，其場發射起始電場可以減少至8.5 V/μm; 場增強因子為315。這些微小奈米級的氮化鎵突起物可以作為巨大數量的場發射源，而這些場發射源整體的場發射表現會比單一尖細的場發射源效果更為優越。表面增顯拉曼的實驗結果顯示，利用電子束蒸鍍技術加熱金屬銀靶材，並搭配適當蒸鍍時間的改變，可以讓氮化鎵奈米線表面有不同的銀薄膜覆蓋率變化。將不同銀薄膜覆蓋率的氮化鎵奈米線浸泡在10-3 M的R6G測試溶液中進行表面增顯拉曼量測，其量測的變化趨勢顯示，隨著銀膜覆蓋率越高，表面增顯拉曼強度會逐漸變弱。電子顯微鏡觀察結果顯示，在表面增顯拉曼強度最強的試片中，其對應奈米線表面所覆蓋的銀膜是以圓球形的奈米顆粒外形呈現。這結果顯示圓球外形的奈米顆粒是有助於表面增顯拉曼的表現。在偵測R6G溶液濃度的量測中，實驗結果顯示R6G的最小偵測濃度可以到達10-12M。並且在10-3到10-12M濃度之間，表面增顯拉曼訊號的強度變化有隨R6G濃度變化呈現近似線性的變化趨勢。這趨勢顯示，有銀奈米顆粒附著的氮化鎵奈米線，具有作為表面增顯拉曼活性基板的應用潛力。

    In this study, we have used metallic Ga and NH3 gas to synthesize GaN nanowires on Pt catalyst coated Si substrate in a high temperature furnace by using the chemical vapor deposition process. The nanowire growth process was followed the vapor-liquid-solid growth mechanism. First of all, we change the reaction pressure, NH3 flow rate and temperature to grow GaN nanowires. When we have the optimum growth parameters, we change the flow ratio of the reaction gas to characterize the generation of stress and current-voltage properties for synthesized nanowires. In order to demonstrate an easy method of controlling the diameter of GaN nanowires and characterize the electronic structure of as-implanted GaN nanowires, the GaN nanowires growth processes were also treated with Si substrate immersed in Au nanoparticle solution and ion implantation experiments, respectively. For the application field, the GaN nanowires which were grown in different flowing ratio and treated with electron beam evaporation method were characterized by the field emission and surface enhanced Raman scattering measurements, respectively.
    For the first experiment, we keep the constant total flow rate of the reaction gas and changed the flow ratio of H2/NH3 to grow GaN nanowires. Raman analysis shows that as the H2/NH3 ratio increased, the H2 atom relaxation phenomenon was generated in the crystal structure and lead to compressive stress. The results of current-voltage measurement reveal that as the H2/NH3 ratio increased, the threshold voltage increased. This result is caused by the formation of H2 related electron defect trap centers. When H2/NH3 ratio increases, the resistances of nanowire is decreasing. The reason should be attributed to the formation of donor like defect for nitrogen defect and tunneling current behavior.
    For the second experiment, we demonstrate an easy and fast method of controlling the average diameter of Au nanoparticles and GaN nanowires. The experimental results reveal that the plasma exposure and immersion treatments can be used to control the diameter of nanoparticle and nanowires. After the above experiments, the Au nanoparticles diameter has the standard deviation (SD) of 8 nm, which is much lower than the previous size (20 nm). The GaN nanowires have the SD of 10 nm, which is much lower than the previous size (35 nm). This result shows that both of the plasma exposure and immersion treatments are effective to reduce the diameter difference between nanoparticle and nanowires
    For the third experiment, Eu ions were implanted on GaN nanowires with fluence from 1013 to 1015 cm-2. The defects which were created by ion bombardment were analyzed by the X-ray absorption spectroscopy and photoluminescence measurement. X-ray absorption spectroscopy analysis show the formations of nitrogen interstitials and dangling bond defects within as-implanted GaN nanowires and the transformation of electron transition from sp3 to sp2 environment. When the electron transition is dominated in sp2 environment, the emission intensity of photoluminescence is decreasing. The increase of the X-ray absorption intensity of nitrogen interstitials and dangling bond defects signals reveal that these nitrogen related defects were easily created by ion bombardment.
    For the field emission property of the GaN nanowires, the measurement results reveal that when nano-size protrusions were formed on the surface of the nanowires, the turn on field could be decreased to 8.5 V/μm and its corresponding enhanced factor was 315. The observations suggest that the nanoscale GaN protrusions can act as multiple field emission sources that provide better overall field emission performance than that of a single sharp tip.
    For the surface enhanced Raman scattering (SERS) performance, our analysis show that the e-beam evaporation method can be used to control the Ag coverage on surface of the GaN nanowires. When GaN nanowires with different Ag deposition thickness were immersed in the R6G (10-3M), the SERS measurements reveal that the SERS intensity is decreasing with the increasing of the Ag deposition thickness. Transmission electron microscopy images reveal that the shape of the Ag deposition can be divided into circle shape and irregular island shape. The circle shape of Ag nanoparticle is suitable for the SERS performance. Moreover, SERS measurement indicates that the R6G concentration of 10-12M can be detected. The relationship between SERS intensity and R6G concentration also suggests that GaN nanowires decorated with Ag nanoparticles can be a potential active substrate in the field of bio-materials.

    中文摘要 I Abstract IV 誌謝 VII 目錄 IX 表目錄 XII 圖目錄 XIII 第一章 序論 1 第二章 文獻回顧與研究背景 3 2.1氮化鎵材料發展過程與應用 3 2.1.1氮化鎵材料的發展過程 3 2.1.1.1 氮化鎵材料的性質 4 2.1.2 氮化鎵材料的應用 6 2.2 奈米材料介紹 8 2.2.1 奈米材料成長機制 8 2.2.2 由上而下(top-down)成長技術 15 2.2.3 由下而上(bottom up)成長技術 18 2.2.4奈米元件的發展 20 2.3 氮化鎵奈米線的研究背景 24 2.4 離子佈植法佈植半導體奈米線的介紹與研究背景 29 2.4.1 離子佈植法介紹 29 2.4.2 研究背景 29 2.5場發射介紹與研究背景 33 2.5.1 場發射介紹 33 2.5.2 場發射研究背景 35 2.6 表面增顯拉曼散射介紹與研究背景 37 2.6.1 拉曼光譜介紹 37 2.6.1.1 拉曼光譜散射之理論 38 2.6.1.2 拉曼光譜散射之量子理論 40 2.6.2 表面增顯拉曼光譜介紹 41 2.6.2.1表面增強拉曼光譜原理簡介 41 2.6.3 表面增顯拉曼散射研究背景 42 第三章 實驗系統與分析儀器 73 3.1 實驗系統 73 3.1.1 化學氣相沈積實驗步驟 75 3.2 實驗分析儀器 76 3.2.1 掃描式電子顯微鏡 76 3.2.2 低掠角X光薄膜繞射儀 76 3.2.3 微拉曼光譜儀 77 3.2.4 光激發螢光譜儀 79 3.2.5 化學分析電子光譜儀 80 3.2.6 場發射量測儀 81 3.2.7 穿透式電子顯微鏡 82 3.2.8 電流-電壓電性量測 82 3.2.9 X光吸收光譜量測 82 3.2.10 核磁共振光譜儀 84 第四章 實驗結果與討論 89 4.1 不同反應壓力、氣體流量與反應溫度對氮化鎵奈米線成長影響 89 4.1.1前言 89 4.1.2 實驗方法：改變成長壓力 90 4.1.2.1 結果與分析 90 4.1.3實驗方法：改變氣體流量 91 4.1.3.1結果與分析 91 4.1.4 實驗方法：改變成長溫度 91 4.1.4.1 結果與分析 92 4.2 以拉曼散射光譜與電流電壓量測技術分析氮化鎵奈米線所產生的應力與氮空缺 94 4.2.1 前言 94 4.2.2 實驗方法 95 4.2.3 結果與討論 96 4.2.3.1 拉曼光譜量測分析 96 4.2.3.2 電流電壓量測分析 99 4.2.4 結論 101 4.3 在電漿活化的矽基板上，利用金奈米顆粒改善成長氮化鎵奈米線線徑 控制效果 101 4.3.1 前言 101 4.3.2 實驗方法 102 4.3.3 結果與討論 105 4.3.3.1 化學位移分析 105 4.3.3.2 金顆粒粒徑大小分析 106 4.3.3.3 金顆粒粒徑與奈米線線徑分析 107 4.3.3.4 奈米線晶體結構分析 108 4.3.4 結論 109 4.4 利用X光吸收光譜與光激發螢光光譜分析氮化鎵奈米線的氮插入與氮懸鍵點缺陷 110 4.4.1 前言 110 4.4.2 實驗方法 111 4.4.3 結果與討論 112 4.4.3.1 材料結構與光學分析 112 4.4.3.2 X光吸收光譜分析 113 4.4.4 結論 116 4.5 奈米級突起物對氮化鎵奈米線場發射特性的影響 116 4.5.1 前言 116 4.5.2 實驗方法 117 4.5.3 結果與討論 118 4.5.3.1 表面形貌分析 118 4.5.3.2. 晶體結構分析 119 4.5.3.3 場發射量測分析 120 4.5.4 結論 122 4.6 氮化鎵奈米線應用在表面增顯拉曼量測的分析 123 4.6.1 前言 123 4.6.2 實驗方法 124 4.6.3 結果與討論 125 4.6.3.1晶體結構分析 126 4.6.3.2 表面形貌分析 126 4.6.3.3 銀膜蒸鍍厚度對氮化鎵奈米線表面銀覆蓋率與表面增顯拉曼強度的變化 127 4.6.3.4 不同R6G濃度對表面增顯拉曼的影響 128 4.6.4 結論 129 第五章 結論 168 參考文獻 171

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