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研究生:張?淇
研究生(外文):Shiou-ChiChang
論文名稱:反應式共濺鍍硬質披覆鈦-矽-氮?米複合薄膜之微結構與機械性質研究
論文名稱(外文):A study on the microstructure and mechanical properties of hard Ti-Si-N nanocomposite coatings by reactive co-sputtering
指導教授:鍾震桂
指導教授(外文):Cheng-Kui Chung
學位類別:碩士
校院名稱:國立成功大學
系所名稱:機械工程學系碩博士班
學門:工程學門
學類:機械工程學類
論文種類:學術論文
論文出版年:2010
畢業學年度:98
語文別:中文
論文頁數:122
中文關鍵詞:Ti-N/Si-NTi-N/Ti-Si-N/Si-NTi-Si-N/Ti-N熱穩定性
外文關鍵詞:Ti-N/Si-NTi-N/Ti-Si-N/Si-NTi-Si-N/Ti-Nthermal stability
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本研究採磁控共濺鍍系統沈積不同的Ti-N、Ti-Si-N單層奈米複合薄膜與不同堆疊方式的多層薄膜,其中包含了Ti-N/Si-N,Ti-N/Ti-Si-N/Si-N與Ti-Si-N/Ti-N。探討氮氣流量、鈦功率與遮板(Shutter)切換時間等製程參數,對薄膜微結構、形貌、成分與機械性質,及其熱穩定性的影響。
本實驗控制鈦靶功率與遮板切換時間,並通入不同的氮氣流量比進行薄膜沈積。完成後將其以表面粗度儀與四點探針量測薄膜厚度與電阻;以低掠角X光繞射儀分析其微結構與結晶相;以掃描式電子顯微鏡觀察表面形貌;以能量散佈光譜儀檢測薄膜化學成份;並以奈米壓痕器檢測薄膜機械性質。最後藉快速退火爐進行1分鐘500與700 °C的退火並探討薄膜的熱穩定性。
實驗結果顯示多層薄膜的結晶性優於單層薄膜,雖機械性質不會大幅提升,但卻具極佳的熱穩定性。經退火後的試片分析顯示,微結構中氧化物訊號的產生,即TiO與TiO?2相的形成是影響機械性質下降的主因,單層Ti-Si-N薄膜退火溫度500 °C後機械性質就會發生變化,而多層薄膜因層與層之間的介面影響,當退火高達700 °C,微結構與機械性質並無明顯變化,因而得知多層薄膜較單層薄膜具較佳的熱穩定性。
關鍵字:Ti-N/Si-N、Ti-N/Ti-Si-N/Si-N、Ti-Si-N/Ti-N、熱穩定性

In this study, the nanocomposites of Ti-N, Ti-Si-N single layer coatings and multilayer coatings including Ti-N/Si-N, Ti-N/Ti-Si-N/Si-N and Ti-Si-N/Ti-N with different ways were prepared by reactive magnetron co-sputtering system. We’ll discuss the effects of the operating parameters of FN2%, Ti power, and alternating time to the microstructure, morphology, elements, mechanical properties, and thermal stability of those thin films.
The thickness and resistivity were investigated by α-Step and four-point probe, respectively. The microstructure and crystallinity of films were identified by Grazing Incidence X-ray Diffractometer. The morphology was examined by Scanning Electron Microscopy and the chemical composition of the coatings was determined by Energy Dispersive Spectroscopy. The hardness was investigated using a Nano Indenter. Finally, we discussed the thermal stability by using thermal treatments of Rapid Thermal Annealing at 500 °C and 700 °C.
The results revealed the crystallinity of multilayer coatings better than single layer ones resulted in better thermal stability without improving mechanical properties. In analysis of samples after annealing, the diffraction peaks of the main reason of impaired mechanical properties were formation of TiO and TiO2 phases. After annealing at 500 °C, mechanical properties of Ti-Si-N coatings changed. In terms of nano-multilayer coatings annealed at 700 °C, the variation of microstructures and mechanical properties were not apparent due to interface barrier effects. Therefore, the thermal stability of multilayer coatings was better than single layer ones.
Key words:Ti-N/Si-N, Ti-N/Ti-Si-N/Si-N, Ti-Si-N/Ti-N, thermal stability

摘要 I
Abstract II
致謝 III
目錄 V
表目錄 VII
圖目錄 IX
第一章 緒論 1
1-1 前言 1
1-2 研究動機與目的 3
第二章 文獻回顧與理論基礎 5
2-1 濺鍍原理與薄膜之結構區模型 5
2-1-1 濺鍍原理 5
2-1-2 物理氣相沈積薄膜之結構區模型 6
2-2 奈米薄膜強化機制 8
2-3 Ti-Si-N奈米複合薄膜文獻回顧 12
2-3-1 不同N2/Ar流量比的Ti-Si-N薄膜 12
2-3-2 不同矽成份比的Ti-Si-N薄膜 13
2-3-3 不同偏壓的Ti-Si-N薄膜 13
2-4 Ti-N/Si-N奈米多層薄膜文獻回顧 15
2-5 優選方向 20
第三章 實驗步驟與方法 23
3-1 實驗流程 23
3-2 實驗參數與材料 26
3-2-1 實驗參數 26
3-2-2 實驗材料 29
3-3 實驗儀器 30
3-3-1 反應式磁控共濺鍍系統 (Reactive co-sputtering system) 30
3-3-2 快速退火爐 (Rapid thermal annealing system, RTA) 32
3-3-3 微細表面測定儀 (Microfigure measuring instrument,α-Step) 34
3-3-4 四點探針 (Four-point method) 34
3-3-5 低掠角X光繞射 (Glancing incident angle x-ray diffraction) 36
3-3-6 場發射掃描式電子顯微鏡 (Field emission scanning electron microscopy) 38
3-3-7 能量散光譜議 (Energy dispersive spectroscopy, EDS) 40
3-3-8 奈米壓痕試驗機 (MTS nano indenter G200 ) 41
第四章 實驗結果與討論 46
4-1 Ti-N與Ti-Si-N單層奈米複合薄膜 46
4-1-1 濺鍍速率與電阻率 46
4-1-2 微結構與優選方向 49
4-1-3 表面形貌與化學成分 54
4-1-4 機械性質 56
4-1-5 熱穩定性 59
4-2 Ti-N/Si-N多層奈米複合薄膜 64
4-2-1 濺鍍速率與電阻率 64
4-2-2 微結構與優選方向 67
4-2-3 表面形貌與化學成分 71
4-2-4 機械性質 73
4-2-5 熱穩定性 75
4-3 Ti-N/Ti-Si-N/Si-N多層奈米複合薄膜 80
4-3-1 濺鍍速率與電阻率 80
4-3-2 微結構與優選方向 82
4-3-3 表面形貌與化學成分 85
4-3-4 機械性質 87
4-3-5 熱穩定性 89
4-4 Ti-Si-N/Ti-N雙層奈米複合薄膜 97
4-4-1 濺鍍速率與電阻率 97
4-4-2 微結構與優選方向 99
4-4-3 表面形貌與化學成分 102
4-4-4 機械性質 104
4-4-5 熱穩定性 106
第五章 結論與未來展望 114
5-1 結論 114
5-2未來展望 117
5-3本文貢獻 118
參考文獻 119


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