系統識別號 | U0002-0408201001032600 |
---|---|
DOI | 10.6846/TKU.2010.00092 |
論文名稱(中文) | 光放射光譜對化學汽相沉積法合成鑽石薄膜之研究 |
論文名稱(英文) | Optical emission spectrum study in grow diamond films by CVD |
第三語言論文名稱 | |
校院名稱 | 淡江大學 |
系所名稱(中文) | 物理學系碩士班 |
系所名稱(英文) | Department of Physics |
外國學位學校名稱 | |
外國學位學院名稱 | |
外國學位研究所名稱 | |
學年度 | 98 |
學期 | 2 |
出版年 | 99 |
研究生(中文) | 呂理暐 |
研究生(英文) | Lie-Wei Lu |
學號 | 695210574 |
學位類別 | 碩士 |
語言別 | 繁體中文 |
第二語言別 | |
口試日期 | 2010-07-12 |
論文頁數 | 130頁 |
口試委員 |
指導教授
-
林諭男(inanlin@mail.tku.edu.tw)
委員 - 葉炳宏(phyeh331@mail.tku.edu.tw) 委員 - 柳克強(kcleou@ess.nthu.edu.tw) |
關鍵字(中) |
鑽石 化學汽相沈積法 奈米線 氮氣 超耐米晶鑽石膜 |
關鍵字(英) |
MPCVD MCD UNCD Nanorods Diamonds Nitrogen |
第三語言關鍵字 | |
學科別分類 | |
中文摘要 |
本研究主要是利用微波電漿化學汽相沉積系統中用純氫氣、氬氣與氮氣的三種氣氛下沉積鑽石薄膜並在製成過程中,用光發射光譜(opical emission spectropy) 觀察電漿成分及變化,藉此討論電漿與成長鑽石薄膜的關聯性。(i)在甲烷/氫氣電漿中主要是成長出0.5-1um柱狀的鑽石結構也發現隨著壓力變化,大晶粒比例開始變多,而且非鑽石之碳物種以外其他物種比例也開始變多。(ii)在甲烷/氬氣電漿中可成長出2-10 nm的超奈米球鑽石結構。壓力變化下雖然表面形貌與內部結構都相似,但是以150 torr的表面形貌看起來較密集。(iii)在甲烷/氮氣電漿中成功的長出鑽石薄膜,其結構為50-100 nm針狀鑽石結構。另外,也發現2-10 nm的超奈米球結構,在80 torr以後有發現參雜效果增加,在氮氣電漿會產生參雜的效果,導致在氮氣電漿成長之鑽石薄膜有較好的場發射特性。 |
英文摘要 |
This research discussed to growth behaviar of diamond films in methane /argon, methane/hydrogen or methane/nitrogen plasma by MPCVD (microwave plasma chemical vapor depositon)。We examined the optical emission spectrum as to investigate the correlation between plasma and characteristics of diamond films。(i)With methane/hydrogen plasma, we obtianed columnar like diamond films which grain size about 0.5~1 um, besides We found that the relative proportion of larger grains and non-diamond carbonspecies is increasing with pressure。(ii)With methane/argon plasma, we obtained ultrananocrystalline diamond film count grain size about 2~10 nm. With methane/nitrogen plasma, we obrained acicular diamond films crystalline grain size about 50-100 nm, coexisting with the ultrananocrystalline diamond grains with size about 2~10 nm。In addition, we found acicular diamond grains in 80 torr, where the doping effect operating。The diamond films have better field emission value due to doping effect in the methane and nitrogen plasma。 |
第三語言摘要 | |
論文目次 |
誌謝.......................................................I 中文摘要..................................................II 英文摘要.................................................III 目錄......................................................IV 表目錄...................................................VII 圖目錄................................................. VIII 第一章 緒論................................................1 1.1 前言...................................................1 1.2 鑽石的特性.............................................1 1.2.1 鑽石晶體結構.........................................2 1.2.2 石墨晶體結構.........................................2 1.2.3 鑽石的特性與應用.....................................3 1.2.4 鑽石薄膜在場發射特性上之應用.........................7 1.2.5 鑽石的負電子親和力特性...............................9 1.3 論文概要..............................................11 第二章 文獻回顧...........................................21 2.1 化學汽相沉積法的鑽石合成理論..........................21 2.1.1 化學汽相沉積法(CVD method)..........................21 2.1.2 電漿輔助化學汽相沉積法..............................22 2.1.3 微波電漿輔助化學汽相沈積技術........................23 2.1.4 電漿基本原理........................................24 2.2 鑽石薄膜的分類........................................27 2.2.1 微米晶鑽石膜與超奈米晶鑽石膜的比較..................27 2.2.2 鑽石薄膜的孕核的方法................................30 2.2.3 超音波振盪法-鑽石/鈦懸浮液(UM)......................32 第三章 研究方法與實驗步驟.................................35 3.1 實驗設備與方法........................................36 3.1.1 實驗流程 ...........................................36 3.1.2 實驗方法............................................36 3.2 實驗設備..............................................39 3.2.1 製程設備............................................39 3.3 分析設備..............................................40 3.3.1 掃描式電子顯微鏡(Scanning Electron Microscope,SEM)..40 3.3.2 穿透式電子顯微鏡( Transmission Electron Microscope,TEM)...........................................42 3.3.3 拉曼光譜分析(Raman Spectrum)........................43 3.3.4 電子場發射特性之量測(Field Emission,F-E)........... 45 3.3.5 光放射光譜之量測(Optical Emission Spectrum,OES).....46 第四章 光發射光譜觀察氫氣/氬氣/氮氣電漿不同壓力成長鑽石薄膜之研究 4.1 甲烷/氫氣電漿中用不同壓力成長鑽石薄膜.................57 4.1.1 光放射光譜 (Optical Emission Spectrum) 電漿成份分析........................................................58 4.1.2 掃描式電子顯微鏡(Scanning Electron Microscopy)表面形態探........................................................59 4.1.3 可見光拉曼光譜分析(Visible Raman spectrum)..........59 4.1.4 場發射特性量測 (Field Emission)....................59 4.1.5 結果與討論..........................................60 4.2 甲烷/氬氣電漿中用不同壓力成長鑽石薄膜.................60 4.2.1 光放射光譜 (Optical Emission Spectrum) 電漿成份分析........................................................61 4.2.2 掃描式電子顯微鏡(Scanning Electron Microscopy)表面形態探........................................................62 4.2.3 可見光拉曼光譜分析(Visible Raman spectrum)..........62 4.2.4 場發射特性量測 (Field Emission)....................63 4.2.5 結果與討論..........................................63 4.3 甲烷/氬氣電漿中用不同壓力成長鑽石薄膜.................64 4.3.1 光放射光譜 (Optical Emission Spectrum) 電漿成份分析........................................................64 4.3.2 掃描式電子顯微鏡(Scanning Electron Microscopy)表面形態探........................................................65 4.3.3 穿透式電子顯微鏡(Transmission ElectronMicroscopy)結構探討......................................................66 4.3.4 可見光拉曼光譜分析(Visible Raman spectrum)..........67 4.3.5 場發射特性量測 (Field Emission)....................68 4.3.6 成長機制的研究......................................68 4.3.7結果與討論...........................................69 4.4 加總流量後甲烷/氬氣電漿中用不同壓力成長鑽石薄膜.......70 4.4.1 光放射光譜 (Optical Emission Spectrum) 電漿成份分析........................................................70 4.4.2 掃描式電子顯微鏡(Scanning Electron Microscopy)表面形態探........................................................71 4.4.3可見光拉曼光譜分析(Visible Raman spectrum)...........71 4.4.4 場發射特性量測 (Field Emission)....................71 4.4.5結果與討論...........................................72 第五章 總結..............................................105 附錄一 ..................................................121 附錄二 ..................................................129 表目錄 表1-1 鑽石基本特性.........................................................................................14 表1-2 鑽石跟其他材料硬度質比較.................................................................16 表1-3 鑽石跟其他材料摩擦係數.....................................................................17 表1-4 鑽石跟其他材料的熱傳導係數的比較.................................................18表 2-1微米晶鑽石與超奈米微晶鑽石的特性比較………………………….34 表4-1 甲烷/氫氣 的實驗參數……………………………………………….73 表4-2 甲烷/氬氣 的實驗參數……………………………………………….78 表4-3 甲烷/氮氣 總流量100 sccm 實驗參數……………………………83 表4-4 60 toor到90 torr 內部結構與晶粒大小的比較圖………………96 表4-5 甲烷/氮氣 總流量141.4 sccm 實驗參數…………………………97 表4-6 氮氣電漿 總流量100 sccm 與 141.4 sccm 之比較……………104 表5-1 氫氣、氬氣與氮氣 電漿之比較……………………………………106 圖目錄 圖1-1面心立方晶體鑽石結構。………………………………………………12 圖1-2 (a) 立方晶鑽石原子結構。(b) 六方晶鑽石的原子結構。…………13 圖1-3石墨的原子結構。…………………………………………………….....13 圖1-4 金屬-真空能帶示意圖:(a).未加電場 (b)外加高電場………………..19 圖1-5 鉬尖端的薄膜場發射陰極…………………………………………….32 圖1-6 典型的半導體能帶圖:(a).正電子親合力……………………………...20 圖2-1低壓化學汽相沉積系統反應示意圖。………………………………….33 圖2-2 壓力與電子(Te)、離子(Ti)及中性粒子(Tn)溫度關係………………...33 圖2-3 超音波振盪法………………………………………………………….35 圖3-1 合成鑽石薄膜實驗流程圖…………………………………………….48 圖3-2 IPLAS 微波電漿化學汽相沉積系統示意圖………………………….49 圖3-3 本論文所採用IPLAS 微波電漿化學汽相沉積系統…………………50 圖3-4 掃描式電子顯微鏡(SEM)……………………………………………..51 圖3-5 穿透是電子顯微鏡(TEM)……………………………………………..52 圖3-6 穿透式電子顯微鏡的基本構造……………………………………….53 圖3-7 圖 3-7 拉曼(Raman)系統……………………………………………..54 圖3-8 拉曼系統示意圖……………………………………………………….54 圖3-9 電子場發射特性量測示意圖………………………………………….55 圖3-10 光放射光譜量測原理示意圖………………………………………...56 圖3-11 光放射光譜量測與腔體相對位置示意圖…………………………...56 圖4-1 甲烷/氫氣電漿的OES光譜 ………………………………………….73 圖4-2 物種變化與壓力關係圖……………………………………………….74 IX 圖4-3 為甲烷/氫氣CH光強度隨著壓力變化與氣體反應室的剖面相對位置圖……………………………………………………………………………….74 圖4-4 45 torr時CH光強度與氣體反應室的俯視相對位置圖………………75 圖4-5 55 torr時CH光強度與氣體反應室的俯視相對位置圖………………75 圖4-6 65 torr時CH光強度與氣體反應室的俯視相對位置圖………………75 圖4-7 75 torr時CH光強度與氣體反應室的俯視相對位置圖………………75 圖4-8 85 torr時CH光強度與氣體反應室的俯視相對位置圖………………75 圖4-9 95 torr時CH光強度與氣體反應室的俯視相對位置圖………………75 圖4-10 甲烷/氫氣 電漿45 torr到95 torr 的SEM圖……………………..…76 圖4-11 甲烷/氫氣 電漿可見光拉曼…………………………………………77 圖4-12 甲烷/氫氣 場發射特性圖……………………………………………77 圖4-13 甲烷/氫氣電漿的OES光譜…………………………………………78 圖4-14 物種變化與壓力關係圖……………………………………………...79 圖4-15 甲烷/氬氣CH光強度隨著壓力變化與氣體反應室的剖面相對位置圖…………………………………………………………………………….....79 圖4-16 120 torr時CH光強度與氣體反應室的俯視相對位置圖……………80 圖4-17 130 torr時CH光強度與氣體反應室的俯視相對位置圖……………80 圖4-18 140 torr時CH光強度與氣體反應室的俯視相對位置圖……………80 圖4-19 150 torr時CH光強度與氣體反應室的俯視相對位置圖……………80 圖4-20 160 torr時CH光強度與氣體反應室的俯視相對位置圖……………80 圖4-21 170 torr時CH光強度與氣體反應室的俯視相對位置圖……………80 圖4-22 甲烷/氫氣 電漿120 torr到170 torr 的SEM圖……………………81 圖4-23 甲烷/氬氣 電漿可見光拉曼…………………………………………81 X 圖4-24 甲烷/氫氣 場發射特性圖……………………………………………82 圖4-25 甲烷/氮氣電漿的OES光譜 …………………………………………83 圖4-26 物種變化與壓力關係圖……………………………………………...84 圖4-27 CN光強度隨著壓力變化與氣體反應室的剖面相對位置圖………..84 圖4-28 30 torr時CN光強度與氣體反應室的俯視相對位置圖……………..85 圖4-29 40 torr時CN光強度與氣體反應室的俯視相對位置圖…………….85 圖4-30 50 torr時CN光強度與氣體反應室的俯視相對位置圖……………..85 圖4-31 60 torr時CN光強度與氣體反應室的俯視相對位置圖……………..85 圖4-32 70 torr時CN光強度與氣體反應室的俯視相對位置圖……………..85 圖4-33 80 torr時CN光強度與氣體反應室的俯視相對位置圖……………..85 圖4-34 90 torr時CN光強度與氣體反應室的俯視相對位置圖…………….86 圖4-35 100 torr時CN光強度與氣體反應室的俯視相對位置圖……………86 圖4-36 110 torr時CN光強度與氣體反應室的俯視相對位置圖…………….86 圖4-37 甲烷/氮氣 總流量100 sccm電漿50 torr到100 torr 的SEM圖……87 圖4-38 甲烷/氮氣 總流量100 sccm電漿50 torr到100 torr 的SEM圖與TEM 明場相比較圖…………………………………………………………...88 圖4-39 60 torr時選區繞射圖的線性分析…………………………………....89 圖4-40 70 torr時選區繞射圖的線性分析…………………………………....89 圖4-41 80 torr時選區繞射圖的線性分析………………………………….....89 圖4-42 90-1 torr時選區繞射圖的線性分析……………………………….....89 圖4-43 90-2 torr時選區繞射圖的線性分析………………………………….89 圖4-44 甲烷氮氣電漿100 sccm 60 torr針狀鑽石的HRTEM的影像………90 圖4-45 甲烷氮氣電漿100 sccm 60 torr針狀鑽石邊緣HRTEM影像….......90 XI 圖4-46 甲烷氮氣電漿100 sccm 70 torr針狀鑽石的HRTEM的影像………91 圖4-47 甲烷氮氣電漿100 sccm 70 torr針狀鑽石邊緣HRTEM影像………91 圖4-48 甲烷氮氣電漿100 sccm 80 torr針狀鑽石的HRTEM的影像………92 圖4-49 甲烷氮氣電漿100 sccm 80 torr針狀鑽石邊緣HRTEM影像….......92 圖4-50 甲烷氮氣電漿100 sccm 90-1 torr針狀鑽石的HRTEM的影像…….93 圖4-51 甲烷氮氣電漿100 sccm 90-2 torr針狀鑽石邊緣HRTEM影像……93 圖4-52 甲烷/氮氣電漿60 torr到90 torr對針狀鑽石邊緣作整張FFT圖….94 圖4-53 甲烷/氮氣 總流量100 sccm的紫外光拉曼光譜……………………95 圖4-54 甲烷/氮氣 總流量100 sccm的場發射特性圖………………………95 圖4-55 甲烷/氮氣 100 sccm 電漿中CN自由基的光強度與場發射的起始電場作比對圖………………………………………………………………….....96 圖4-56 甲烷/氮氣總流量141.4 sccm電漿OES光譜 ………………………97 圖4-57 物種變化與壓力關係圖……………………………………………...98 圖4-58 為甲烷/氮氣總流量141.4 sccm CN光強度隨著壓力變化與氣體反應室的剖面相對位置圖……………………………………………………….....98 圖4-59 30 torr時CN光強度與氣體反應室的俯視相對位置圖…………….99 圖4-60 40 torr時CN光強度與氣體反應室的俯視相對位置圖…………….99 圖4-61 50 torr時CN光強度與氣體反應室的俯視相對位置圖…………….99 圖4-62 60 torr時CN光強度與氣體反應室的俯視相對位置圖…………….99 圖4-63 70 torr時CN光強度與氣體反應室的俯視相對位置圖…………….99 圖4-64 80 torr時CN光強度與氣體反應室的俯視相對位置圖…………….99 圖4-65 90 torr時CN光強度與氣體反應室的俯視相對位置圖……………100 圖4-66 100 torr時CN光強度與氣體反應室的俯視相對位置圖…………100 XII 圖4-67 110 torr時CN光強度與氣體反應室的俯視相對位置圖…………100 圖4-68 甲烷/氮氣總流量141.4 sccm電漿50 torr到100 torr的SEM圖…..101 圖4-69 甲烷/氮氣 總流量141.4 sccm的紫外光拉曼光譜………………...102 圖4-70 甲烷/氮氣 總流量141.4 sccm的場發射特性圖…………………...102 圖4-71 甲烷/氮氣 總流量100與141.4 sccm的場發射特性圖……………103 圖4-72 甲烷/氮氣 141.4 sccm 電漿中CN自由基的光強度與場發射的起始電場作比對圖………………………………………………………………...103 圖5-1 氫氣、氬氣與氮氣電漿之光發射光譜比較………………………….105 圖5-2 氫氣、氬氣與氮氣電漿之拉曼光譜比較…………………………….107 圖5-3 氫氣、氬氣與氮氣電漿之場發射特性比較………………………….107 |
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