臺灣博碩士論文加值系統

本研究中採用陰極電弧蒸鍍技術(CAE)，搭配鋁鈦矽(AlTiSi)、鋁鉻矽(AlCrSi)、純鉻靶(Cr)，沉積氮化鋁鈦矽(AlTiSiN)、氮化鋁鉻矽(AlCrSiN)。同時利用兩個靶材共鍍AlTiSiN / AlCrSiN元多層氮化物薄膜，再針對AlTiSiN及AlCrSiN靶電流進行優化，調整薄膜元素原子比例以提升薄膜高溫性質。接著進行雷射熱疲勞試驗，針對薄膜多層薄膜的微結構、機械性質進行探討。
本研究使用多種儀器來分析薄膜的特性，其中使用場發射掃描式電子顯微鏡(FESEM)和場發射穿透式電子顯微鏡(FETEM)來觀察薄膜橫截面微結構，利用場發射電子微探儀(EPMA)進行薄膜元素成分分析，並使用低掠角薄膜X光繞射儀(GIXRD)分析薄膜晶體結構和結晶相。此外機械性質的部分，還使用洛式壓痕試驗機及刮痕試驗機來評估薄膜與基材之間的附著力，並使用奈米壓痕試驗機和球對盤磨耗試驗機來量測薄膜的硬度、彈性係數和抗磨耗性能。最後，對於薄膜的雷射熱疲勞試驗實驗，利用二次離子質譜儀(TOF-SIMS)與化學分析電子光譜儀(ESCA)針對薄膜氧化層進行分析，及探討觀察雷射氧化薄膜化學鍵結態。
根據研究結果顯示，XRD分析得知AlTiSiN/AlCrSiN薄膜及AlTiSiN、AlCrSiN薄膜皆屬於FCC晶體結構，因添加Si元素能有效抑制晶粒成長，使晶粒細化形成緻密的奈米結構，同時受到奈米多層膜的強化機制使AlTiSiN/AlCrSiN薄膜硬度得到提升(25.7 GPa)與低磨耗率(1.88x10-6 mm3/Nm)。透過毫秒光纖脈衝雷射經由100次循環雷射後薄膜，因表面生成氧化物如Al2O3、Cr2O3使得各薄膜的摩擦係數明顯降低。由SEM觀察薄膜單次雷射後表面形貌， AlTiSiN/AlCrSiN薄膜相較於AlTiSiN及AlCrSiN薄膜，並未出現因雷射表面熱應力所產生的熱裂紋，說明了多層薄膜耐熱衝擊性優於單層薄膜。根據FIB-SEM截面觀察經100次循環雷射後薄膜，得知適當成分配比之AlTiSiN/AlCrSiN薄膜因熱應力所產生的熱裂紋得到減緩，證實奈米多層結構薄膜能提升熱穩定性。

In this study, cathodic arc evaporation (CAE) technique was used in combination with aluminum titanium silicon (AlTiSi), aluminum chromium silicon (AlCrSi), and pure chromium (Cr) targets to deposit aluminum titanium silicon nitride (AlTiSiN) and aluminum chromium silicon nitride (AlCrSiN) films. Additionally, a multilayered nitride film of AlTiSiN/AlCrSiN was deposited using two targets, and the target currents for AlTiSiN and AlCrSiN were optimized to adjust the atomic ratio of film elements and enhance the high-temperature properties of the films. Laser thermal fatigue tests were conducted to investigate the microstructure and mechanical properties of the multilayered films.
Various instruments were employed to analyze the characteristics of the films. Field Emission Scanning Electron Microscope (FE-SEM) and Field Emission Transmission Electron Microscope (FETEM) were used to observe the cross-sectional microstructure of the films. Energy dispersive X-ray spectroscopy (EDX) was used for elemental composition analysis, and grazing incidence X-ray diffraction (GIXRD) was used to analyze the crystal structure and phases of the films. In terms of mechanical properties, nanoindentation and scratch tests were conducted to evaluate the adhesion between the films and substrates, and nanohardness, elastic modulus, and wear resistance of the films were measured using a nanoindentation instrument and a ball-on-disk wear tester. Finally, for the laser thermal fatigue tests of the films, time-of-flight secondary ion mass spectrometry (TOF-SIMS) and electron spectroscopy for chemical analysis (ESCA) were utilized to analyze the oxide layers on the films and investigate the chemical bonding states of laser-oxidized films.
 

According to the research results, XRD analysis revealed that the AlTiSiN/AlCrSiN films and the AlTiSiN and AlCrSiN films all had the FCC crystal structure. The addition of Si elements effectively inhibited grain growth, resulting in refined grains and a dense nanostructure. At the same time, the AlTiSiN/AlCrSiN films benefit from the strengthening mechanism of the nanolayered structure, leading to increased hardness (25.7 GPa) and low wear rate (1.88x10-6 mm3/Nm). After subjecting the films to 100 cycles of laser irradiation with millisecond fiber laser pulses, the formation of surface oxides such as Al2O3 and Cr2O3 significantly reduced the friction coefficients of the Unlike the monolayered AlTiSiN and AlCrSiN films, observation of the surface morphology of the films after a single laser irradiation using SEM showed that the AlTiSiN/AlCrSiN films exhibited no thermal cracking caused by surface thermal. This indicates that the thermal stability of the multilayer films is superior to that of the monolayer films. Furthermore, FIB-SEM cross-section observation of the films after 100 cycles of laser irradiation, it was found that the AlTiSiN/AlCrSiN films exhibited reduced thermal cracking caused by thermal stress, confirming that the nanolayered structure in the thin films enhances thermal stability.

摘要....i
Abstract....ii
誌謝....iv
目錄....v
表目錄....vii
圖目錄....viii
第一章 緒論....1
1.1 前言....1
1.2 研究動機....2
第二章 文獻回顧 ....3
2.1 薄膜強化理論....3
2.1.1 奈米多層薄膜強化機制....3
2.1.2 固溶強化機制....4
2.1.3 晶粒細化強化機制....5
2.2 多元氮化物薄膜介紹....6
2.2.1 氮化鋁鉻....6
2.2.2 氮化鋁鈦....9
2.2.3 氮化鋁鉻矽....12
2.2.4 氮化鋁鈦矽 ....15
2.2.5 氮化鋁鈦鉻矽....18
2.3 雷射熱穩定性....20
2.3.1 不同雷射系統作用下之比較....20
2.3.2 毫秒脈衝雷射模擬熱疲勞....21
2.3.3 連續波雷射奈米多層薄膜之熱穩定性....25
第二章 實驗方法....28
3.1 實驗流程....28
3.2 薄膜設計與實驗方法....29
3.2.1 前處理及鍍膜步驟....29
3.2.2 單層AlTiSiN及AlCrSiN薄膜製程設計....31
3.2.3 多層AlTiCrSiN薄膜製程設計....33
3.3 雷射熱疲勞試驗....34
3.4 薄膜機械性質分析....37
3.4.1 洛氏硬度試驗機(Rockwell Hardness)....37
3.4.1 奈米壓痕試驗機(Nano-indentation)....38
3.4.2 刮痕試驗機(Scratch Test)....40
3.4.3 磨耗試驗機(Tribometer)....42
3.5 薄膜微結構與成分分析....43
3.5.1 超高解析熱電子型場發射掃描式電子顯微鏡(Ultra High Resolution Thermal Field Emission Scanning Electron Microscope, FESEM)....43
3.5.2 高階三束型聚焦離子束顯微鏡(Focused Ion and Electron Beam System)....45
3.5.3 場發射穿透式電子顯微鏡(Field Emission Transmission Electron Microscope, FETEM)....46
3.5.4 二次離子質譜儀(Secondary Ion Mass Spectrometer, SIMS)....48
3.5.5 化學分析電子能譜儀(Electron Spectroscope for Chemical Analysis, ESCA) ....49
3.5.6 X光繞射分析儀(X-Ray Diffractometer, XRD)....50
3.5.7 高解析電子微探儀 (Field Emission Electron Probe Microanalyzer, EPMA) ....52
第四章 結果與討論....53
4.1 薄膜常溫微結構分析....53
4.1.1 SEM微結構分析....53
4.1.2 EPMA表面元素成分定量分析....54
4.1.3 X光繞射分析....55
4.1.4 TEM微結構分析....58
4.2 薄膜機械性質分析....60
4.2.1 洛式壓痕分析....60
4.2.2 刮痕試驗分析....61
4.2.3 奈米壓痕分析....62
4.2.4 磨耗試驗分析....63
4.3 表面雷射後之薄膜微結構分析....65
4.3.1 SEM表面微結構分析....65
4.3.2 FIB-SEM截面微結構分析....67
4.3.3 EPMA表面元素成分定量分析....69
4.3.4 二次離子質譜儀縱深成分分析(SIMS)....70
4.3.5 XPS化學鍵結態與成分分析....74
4.3.6 TEM微結構分析....78
4.4 表面雷射後之薄膜機械性質分析....80
4.4.1 磨耗試驗分析....80
第五章 結論....85
5.1 薄膜微結構分析及表面性質....85
5.2 薄膜機械性質分析....86
未來展望....87
參考文獻....88
Extended Abstract....94

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