臺灣博碩士論文加值系統

　　以鉻(Cr)、鈦(Ti)及鋁(Al)元素為基礎之過渡金屬氮化物硬質薄膜，如AlTiN、AlCrN及AlCrSiN等薄膜，由於其高強度、硬度、耐磨性及熱穩定性等優異機械性質已被作為切削和成形工具的保護性薄膜。在本研究中使用陰極電弧蒸鍍技術(CAE)使用鋁鈦(AlTi)、鈦矽(TiSi)、三元鋁鉻矽(AlCrSi)合金靶材及純鉻(Cr)靶材沉積AlTiN、AlCrSiN及改變偏壓之AlTiCrSiN多層薄膜，並優化AlCrSiN和AlTiCrSiN介層設計以改善薄膜殘留應力、提高附著強度及增強韌性。透過控制不同的中介層和基材負偏壓，AlCrSiN和AlTiCrSiN具有不同的微結構和機械性質。
　　藉由場發射掃描電子顯微鏡(FE-SEM)及高解析穿透式掃描電子顯微鏡(HR-TEM)觀察其薄膜微結構並搭配特徵X光能量分散光譜儀(EDS)測量元素成分分析，再利用X光繞射分析儀(XRD)觀察薄膜之晶體結構及結晶相分析。機械性質分析先利用洛氏壓痕試驗機評估薄膜與基材之間的附著性能，接著透過微克氏壓痕試驗機及奈米壓痕試驗機測量薄膜硬度值及彈性係數，並透過球對盤磨耗試驗機(ball-on-disk)觀察薄膜耐磨性能。為了研究沉積薄膜的抗衝擊疲勞能力與硬度/彈性模量比之間的相關性，使用碳化鎢壓頭之循環加載裝置作為衝擊探針進行衝擊疲勞試驗，最後進行油霧濕式之端銑削加工SUS316L不鏽鋼並探討刀具薄膜磨損情形。
根據研究結果顯示AlTiCrSiN多層薄膜屬於fcc B1-NaCl奈米晶結構與非晶結構組成之奈米複合薄膜，具有效抑制晶粒成長導致晶粒細化形成緻密結構，阻礙差排移動，以AlTiCrSiN-100V多層薄膜具有高硬度(40 GPa)、抗塑性變形、優異抗衝擊疲勞性能(承受至七十萬次)及高耐磨性能，在800℃高溫氧化後沒有明顯相變化仍維持優良機械性質，具有熱穩定性，在常溫及高溫氧化後AlTiCrSiN-20V多層薄膜後具有最低的磨耗率8.9 x 10^(-7) (mm^3/Nm)及1.1 x 10^(-6) (mm^3/Nm)。根據切削結果得多層薄膜設計之AlTiCrSiN具有高強度及優異的耐磨性及抗衝擊性能，減少刀具磨耗及進刀過程產生的崩裂，保持刃口平整均勻磨耗，其中以AlTiCrSiN-20V切削不鏽鋼至75m刀尖磨耗量最少，有效提升切削加工性及刀具壽命，故適用於不鏽鋼之油霧濕式切削加工。

　　Transition metal nitride coatings based on Cr, Ti and Al, such as AlTiN, AlCrN and AlCrSiN, have been used as protective coating materials of cutting and forming tools due to their high hardness and thermal stability. In this study, AlTiN and AlCrSiN and AlTiCrSiN coatings were deposited onto tungsten carbide tools using AlTi, TiSi, Cr and ternary AlCrSi alloy targets in a Cathodic-arc evaporation (CAE) system. Optimal design of interlayers of the AlCrSiN and AlTiCrSiN can offer an efficient way of controlling residual stress, improving adhesion strength and enhancing toughness. By controlling the different interlayers and negative bias voltages, the AlCrSiN and AlTiCrSiN possessed different microstructures and mechanical properties.
　　The microstructure of the deposited coatings was investigated by field emission scanning electron microscope (FE-SEM) and field emission gun high-resolution transmission electron microscope (FEG-HRTEM), equipped with an energy-dispersive x-ray analysis spectrometer (EDS). Glancing angle X-ray diffraction was used to characterize the microstructure and phase identification of the coatings. Mechanical properties, such as the hardness and young’s modulus, were measured by means of nanoindention. The adhesion strength of the coatings was evaluated by a standard Rockwell indentation test. In order to evaluate the impact fatigue behavior of the coated samples, an impact test was performed using a cyclic loading device with a tungsten carbide indenter as an impact probe. For the cutting experiment, 316L stainless steel was machined by the coated end mills under oil mist condition using a CNC milling machine.
　　According to the experimental result, it showed that AlTiCrSiN were nanocomposites coatings composed of nanocrystalline B1-NaCl structure and amorphous phase structure. The interaction between the grains hindered the generation of dislocations and prevented cracks propagation due to the suppression of grain boundary sliding. The design of multilayered AlTiCrSiN-100V coatings possessed the higher hardness of 40GPa, plastic deformation resistance, impact resistance (higher than 7× 10^5 impacts) and wear resistance. The crystalline phase does not change after high-temperature oxidation and still maintains excellent mechanical properties with thermal stability. For the ball-on-disk wear tests, the as-deposited AlTiCrSiN-20V and which after 800˚C annealing in air possessed the lowest wear rates of 8.9 x 10^(-7) (mm^3/Nm) and 1.1 x 10^(-6) (mm^3/Nm), respectively. According to the cutting test results, the AlTiCrSiN-20V showed the minimum end cutting edge wear, which can effectively improve the machinability and tool life. Thus, the AlTiCrSiN coatings with a multilayered structure of AlTiN and CrTiSiN showed the best wear resistance and cutting performance of 316L stainless steel.

摘要............i
Abstract............ii
誌謝............iv
目錄............v
表目錄............x
圖目錄............xii
第一章 緒論............1
1.1 前言............1
1.2 研究動機與目的............2
第二章 文獻回顧............3
2.1 陰極電弧蒸鍍系統(cathodic arc evaporation, CAE)............3
2.1.1 陰極電弧蒸鍍原理............3
2.1.2 陰極電弧蒸鍍微粒的形成與改善方法............4
2.2薄膜成長機制............11
2.3 薄膜結構............13
2.4 薄膜強化理論............15
2.4.1 晶粒細化強化（strengthening by grain size reduction）............15
2.4.2 固溶強化(solid-solution strengthening)............16
2.4.3 應變硬化(strain hardening)............17
2.4.4 奈米晶與非晶複合結構強化............17
2.4.5 多層薄膜韌性強化............18
2.5 硬質薄膜介紹............20
2.5.1 氮化鉻(CrN)薄膜............20
2.5.2 氮化鋁鈦(AlTiN)薄膜............22
2.5.3 氮化鈦矽(TiSiN)薄膜............24
2.5.4 氮化鋁鉻矽(AlCrSiN)薄膜............27
2.5.5 氮化鋁鈦鉻矽(AlTiCrSiN)薄膜............30
2.6 刀具磨損機制............34
第三章 實驗方法............36
3.1 實驗流程............36
3.2 薄膜設計與實驗方法............37
3.2.1 前處理及鍍膜步驟............37
3.2.2 單層AlTiN薄膜製程設計............39
3.2.3 漸進層AlCrSiN薄膜製程設計............40
3.2.4 AlTiCrSiN奈米複合多層薄膜製程設計............41
3.3 真空退火系統(Vacuum Annealing System)............42
3.4 新型電漿增強電磁控弧源............44
3.5 薄膜機械性質分析............45
3.5.1 洛氏硬度試驗機(Rockwell Hardness)............45
3.5.2 維氏硬度試驗機(Vickers Hardness)............47
3.5.3 奈米壓痕試驗機(Nano-indentation)............48
3.5.4 磨耗試驗機(Tribometer)............49
3.5.5 動態衝擊疲勞試驗機(Cyclic Impact Fatigue)............50
3.6 薄膜結構與表面分析............51
3.6.1 場發射掃描式電子顯微鏡(Field Emission Scanning Electron Microscope, FE-SEM)............51
3.6.2 穿透式電子顯微鏡(Transmission Electron Microscopy, TEM)............53
3.6.3 X光繞射分析儀(X-Ray Diffractometer, XRD) 54
3.7 切削加工............56
第四章 結果與討論............57
4.1 薄膜常溫微結構分析............57
4.1.1 SEM微結構及EDS元素成分分析............57
4.1.2 X光繞射分析............60
4.1.3 AlTiCrSiN-20V薄膜之TEM微結構分析............63
4.2 薄膜常溫機械性質分析............66
4.2.1 洛氏壓痕分析............66
4.2.2 微小硬度分析............67
4.2.3 奈米壓痕分析............68
4.2.4 薄膜殘留應力分析............70
4.2.5 磨耗試驗分析............71
4.2.6 衝擊疲勞試驗分析............76
4.3 高溫氧化後之薄膜微結構分析............82
4.3.1 SEM微結構及EDS元素成分分析............82
4.3.2 X光繞射分析............92
4.4 薄膜高溫機械性質分析............94
4.4.1 800℃高溫氧化後之洛氏壓痕分析............94
4.4.2 800℃高溫氧化後之磨耗試驗分析............95
4.4.3 500℃高溫衝擊疲勞試驗分析............100
4.5 切削試驗分析............104
第五章 結論............108
5.1 薄膜微結構分析結論............108
5.2 機械性質分析結論............109
5.3 切削性能分析結論............110
5.4 總結............110
參考文獻............111
Extended Abstract............119

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