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研究生： 劉又嵻
Liu, Yu-Kang
論文名稱： AlCrNbSiTi 多層膜之開發
Development of AlCrNbSiTi Multilayer Films Deposited by DC Magnetron Sputtering
指導教授： 葉均蔚
Yeh, Jein-Wei
口試委員: 洪健龍
楊智超
曹春暉
學位類別： 碩士
Master
系所名稱： 工學院 - 材料科學工程學系
Materials Science and Engineering
論文出版年： 2018
畢業學年度： 106
語文別： 中文
論文頁數： 267
中文關鍵詞： 高熵合金 、硬質薄膜 、多層薄膜 、磁控濺鍍
外文關鍵詞： High entropy alloy, Hard coating, Multilayer coating, Magnetron Sputtering
相關次數： 點閱：2  下載：0 
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    • 本實驗以真空電弧熔煉製備 AlCrNbSiTi 高熵合金靶材，使用本實驗室新進之反應式直流磁控濺鍍機，以氬氣、氮氣流量的調整及擋板的開關與反應氣氛的抽除，在固定溫度與負偏壓下鍍製交替堆疊之多層膜，並藉由改變多層膜成分探討成分變化對多層薄膜的微結構、殘留應力、硬度、附著性及耐磨耗性的影響。並將薄膜進行 900 oC 2 h 大氣退火以瞭解其抗氧化性。
    實驗結果發現 200R2060 擁有最佳的綜合性質，硬度 37.6 GPa，HRC 附著性測試落在最好的 HF1 等級，經過 900 oC 2h大氣退火，也可觀察到薄膜具有良好抗氧化性，氧化膜層厚度僅 95 nm。WC-Co 平面基板上鍍 200R2060 與鉻鋼球進行 3000 圈磨耗測試無磨耗深度。

    In this experiment, AlCrNbSiTi high-entropy alloy target was prepared by vacuum arc melting. Multilayer films were deposited by reactive DC magnetron sputtering, with the switching of the baffle, the adjustment of the reaction atmosphere, deposition temperature and negative bias voltage. Microstructure, residual stress, hardness, adhesion wear resistance and oxidation resistance of the multilayer films were investigated.
    The experimental results reveal that film 200R2060 has the best comprehensive properties. Film 200R2060 has a hardness of 37.6 GPa and the best HF1 grade obtained with the HRC adhesion test. In 900 °C 2h oxidation test, film 200R2060 exhibits remarkable oxidation resistance with an only 95 nm-thick oxide layer. In wear test, film 200R2060 deposited on WC-Co flat substrate shows no wear depth after worn by chrome steel balls for 3000 cycles.

    致 謝 1 摘 要 3 Abstract 4 目 錄 5 圖目錄 12 表目錄 24 壹、前 言 26 貳、文獻回顧 28 2.1 薄膜鍍製技術 28 2.1.1 物理氣相沉積 (PVD) 28 2.1.2 濺鍍技術 30 2.1.3 磁控介紹及優點 33 2.1.4 薄膜沉積與附著 35 2.1.5 薄膜微結構 37 2.2 薄膜種類與發展 43 2.2.1 薄膜發展概況 43 2.2.2 薄膜分類與介紹 47 2.2.3 多層膜強化機制 58 2.3 高熵合金薄膜簡介 63 2.3.1 高熵合金之源起 63 2.3.2 高熵合金定義 64 2.3.3 高熵合金特色 67 2.3.4 歷屆高熵氮化膜發展 72 參、實驗流程 75 3.1 靶材製作 77 3.2 基板準備 80 3.3 反應式直流磁控濺鍍/磁過濾陰極真空電弧鍍膜機 82 3.4 薄膜製程 87 3.5 薄膜基本性質分析 95 3.5.1 成分 95 3.5.2 晶體結構 97 3.5.3 薄膜形貌與微結構 97 3.6 薄膜機械性質分析 98 3.6.1 硬度與楊氏係數 98 3.6.2 附著性 102 3.6.3 薄膜殘留應力分析 104 3.6.4 耐磨耗性 106 3.6.5 切削性 108 3.7 薄膜抗氧化性質分析 110 肆、結果與討論 111 4.1 試片命名 111 4.2 單層鍍膜參數之測試 112 4.2.1 不同試片擺放位置對薄膜之影響 112 4.2.1.1 鍍率分析 114 4.2.1.2 表面形貌與截面形貌觀察 115 4.2.1.3 殘留應力分析 118 4.2.1.4 硬度與楊氏模數分析 121 4.2.2 基板偏壓變量對薄膜之影響 123 4.2.2.1 鍍率分析 123 4.2.2.2 成分分析 126 4.2.2.3 晶體結構分析 127 4.2.2.4 表面形貌與截面形貌觀察 130 4.2.2.5 殘留應力分析 133 4.2.2.6 硬度與楊氏模數分析 135 4.2.3 基板溫度變量對薄膜造成的影響 137 4.2.3.1 鍍率分析 137 4.2.3.2 成分分析 139 4.2.3.3 晶體結構分析 140 4.2.3.4 表面形貌與截面形貌觀察 144 4.2.3.5 殘留應力分析 146 4.2.3.6 硬度與楊氏模數分析 147 4.2.4 與歷屆AlCrNbSiTi單層飽和氮化膜數據比較 148 4.3 氮氣流率對單層薄膜影響及R20、R60下不同偏壓的影響 149 4.3.1 氮氣流率變量對薄膜之影響 149 4.3.1.1 鍍率分析 150 4.3.1.2 成分分析 152 4.3.1.3 晶體結構分析 154 4.3.1.4 表面形貌與截面形貌觀察 155 4.3.1.5 殘留應力分析 160 4.3.1.6 硬度與楊氏模數分析 162 4.3.2 R60 之基板偏壓變量對薄膜的影響 164 4.3.2.1 鍍率分析 164 4.3.2.2 成分分析 166 4.3.2.3 晶體結構分析 167 4.3.2.4 表面形貌與截面形貌觀察 169 4.3.2.5 殘留應力分析 172 4.3.2.6 硬度與楊氏模數分析 174 4.3.3 R20 之基板偏壓變量對薄膜的影響 176 4.3.3.1 鍍率分析 176 4.3.3.2 成分分析 178 4.3.3.3 晶體結構分析 179 4.3.3.4 表面形貌與截面形貌觀察 180 4.3.3.5 殘留應力分析 183 4.3.3.6 硬度與楊氏模數分析 184 4.4 多層製程優化 186 4.4.1 不同換氣時間對多層膜之影響 186 4.4.1.1 截面觀察 187 4.4.1.2 硬度分析 189 4.4.2 不同進氣路線對多層膜之影響 190 4.4.2.1 截面觀察 191 4.4.4.2 硬度分析 193 4.4.3 轉盤轉速對多層膜之影響 194 4.4.3.1 截面觀察 194 4.4.3.2 硬度分析 196 4.4.4 不同層數對多層膜之影響 197 4.4.4.1 截面觀察 197 4.4.4.2 殘留應力分析 199 4.4.4.3 硬度分析 200 4.5 第三號進氣路線對單層膜及多層薄膜之影響 201 4.5.3 第三號進氣路線下單層薄膜性質分析 201 4.5.5.1 成分分析 202 4.5.5.2 晶體結構分析 203 4.5.5.3 表面形貌與截面形貌觀察 204 4.5.5.4 殘留應力分析 206 4.5.5.5 硬度分析 207 4.5.5.6 附著性分析 209 4.5.5.7 耐磨耗性分析 211 4.5.5.8 抗氧化性分析 215 4.5.6 第三號進氣路線下 200R060 及 200R2060 多層薄膜之分析 217 4.5.6.1 表面形貌與截面形貌觀察 217 4.5.6.2 殘留應力分析 219 4.5.6.3 硬度分析 221 4.5.6.4 附著性分析 222 4.5.6.5 耐磨耗性分析 223 4.5.6.6 抗氧化性分析 225 4.5.7 第三號進氣路線下多層薄膜切削性能分析 228 4.5.8 與歷屆多層薄膜數據比較 251 伍、結 論 252 陸、本實驗貢獻 255 柒、未來研究方向 256 參考文獻 257

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