本研究的目的在於討論佔空比及工作氣壓對氮化鈦鋯薄膜結構和機械性質的影響。氮化鈦鋯薄膜是由高功率脈衝與非平衡磁濺共鍍法鍍製於D2鋼上。藉由調整高功率脈衝與非平衡磁濺共鍍法製程參數以降低氮化鈦鋯薄膜的殘留應力也是本研究的目的之一。鈦和鋯分別藉由高功率脈衝和非平衡磁濺法沉積。控制的參數為佔空比(D系列)和工作氣壓(P系列)。降低佔空比會使靶材的電流密度峰值上升，並提高離化率以及電漿粒子的能量，因此對於成長中薄膜的離子轟擊效應隨之增強，導致殘留應力無法被有效降低以及產生(200)織構的氮化鈦鋯薄膜。在P系列中，工作氣壓增加的同時會導致電漿中粒子的平均自由徑縮短，意味著粒子間的碰撞次數增加，導致電漿粒子能量降低，入射粒子所造成的離子轟擊效應減弱，而薄膜中的殘留應力也隨之下降。氮化鈦鋯薄膜的磨耗率變化幅度相當小，從20.0到28.7x10^(-6) mm^3xN^(-1)xm^(-1)。薄膜與基板間附著力達到30牛頓時即可防止薄膜脫落。結果顯示，多數用來估算抗磨耗性的本質因子與氮化鈦鋯薄膜的磨耗率並無太大關聯性。在磨耗測試過後的磨道裡及磨道兩側都能發現細小的碎屑，可推論磨耗機制可能為三物體間磨料磨損，是由磨球和碎屑同時對薄膜進行磨耗行為，因此不同參數所鍍製出的薄膜其磨耗率差異並不大。從結果可以推論在對(200)織構的薄膜進行磨耗測試時，可能比在(111)織構和隨機織構中更容易產生細小碎屑。

The objective of this study was to investigate the effect of duty cycle and working pressure on structure and mechanical properties of TiZrN coatings deposited on D2 steel by a hybrid high power pulsed magnetron sputtering (HPPMS) and unbalanced magnetron sputtering (UBMS) system. This study also aimed to reduce the residual stress of TiZrN coatings by adjusting the deposition parameters in the hybrid HPPMS/UBMS process. In depositing TiZrN coatings, Ti was deposited by HPPMS and Zr was by UBMS. The controlling parameters were duty cycle (D-series) and working pressure (P-series). The decrease of duty cycle will increase the peak target current density that increases the ionization rate and energy of plasma species, by which the ion-peening effect on the growing film is enhanced, and thus the residual stress cannot be effectively decreased and the resultant TiZrN coatings are with (200) texture. In P-series specimens, the mean free path of plasma species decreases with increasing working pressure, and hence collisions between plasma species increase, thereby decreasing the energy of plasma species. Consequently, the residual stress decreases in the coatings due to less ion-peening effect by the incident particles. The wear rate of the TiZrN coatings varies in a narrow range from 20.0 to 28.7x10^(-6) mm^3xN^(-1)xm^(-1). The adhesion strength (Lc3) of the coatings is above 30 N that is sufficient for resisting delamination. The results showed that most of the internal factors for assessing the wear resistance are not significantly correlated to the wear rate of the TiZrN coatings. Fine coating debris are observed in the wear track and pile-up on both sides, suggesting that the wear mechanism may be three-body abrasive wear, where the coating is worn out by both coating debris and wear ball. Accordingly, the wear rates of the coatings deposited by different parameters do not show distinct difference. It is speculated that (200)-textured coatings may be easier in producing the fine debris during wear test than (111) or random textured coatings.

Content
摘要 ii
Abstract iii
致謝 iv
Content vi
List of Figures ix
List of Tables xi
Chapter 1 Introduction 1
Chapter 2 Literature Review 3
2.1 Characteristics of Transition Metal Nitride Coatings 3
2.2 Characteristics of TiZrN Coatings 3
2.2.1 Structure of TiZrN coatings 5
2.2.2 Texture Evolution 5
2.2.3 Mechanical Properties of TiZrN Coatings 7
2.2.4 Residual Stress 8
2.3 Tribological Behavior 8
2.3.1 Adhesion Strength 8
2.3.2 Wear Resistance 9
2.3.3 Evaluation of Wear Resistance 10
2.4 High Power Pulsed Magnetron Sputtering (HPPMS) 11
2.5 Hybrid Technologies 12
Chapter 3 Experimental Procedures 14
3.1 Substrate Preparation 14
3.2 Deposition Procedures 14
3.3 Characterization Methods for Structure and Compositions 19
3.3.1 Crystal Structure - X-Ray Diffraction (XRD) and Glancing Incidence X-Ray Diffraction (GIXRD) 19
3.3.2 Microstructure - Field Emission Gun Scanning Electron Microscope (FEG-SEM) 20
3.3.3 Chemical Compositions - Field Emission Electron Probe Microanalyzer (FE-EPMA) 20
3.3.4 Surface Roughness - Atomic Force Microscope (AFM) 20
3.4 Characterization of Properties 21
3.4.1 Residual Stress by Laser Curvature Method 21
3.4.2 Residual Stress by Average X-ray Strain (AXS) Method 22
3.4.3 Hardness and Young’s Modulus 23
3.4.4 Adhesion Strength - Scratch Test 23
3.4.5 Wear Rate - Pin-on-disk Wear Test 24
3.4.6 Electrical Resistivity – Four-Point Probe 26
3.5 High Power Pulsed Magnetron Sputtering (HPPMS) 27
3.5.1 HPPMS Power Monitoring – Oscilloscope 27
3.5.2 Plasma Diagnosis – Optical Emission Spectroscope (OES) 28
Chapter 4 Results 29
Part I Effect of Duty Cycle 33
4.1 Oscilloscope and optical Emission Spectrometer 33
4.1.1 Oscilloscope 33
4.1.2 Optical Emission Spectroscopy 33
4.2 Chemical Compositions and Structure 36
4.2.1 Chemical Compositions 36
4.2.2 Crystal Structure and Preferred Orientation 37
4.2.3 Cross-sectional Microstructure 40
4.2.4 Surface Roughness 40
4.3 Properties 41
4.3.1 Hardness and Young’s modulus 41
4.3.2 Residual Stress 41
4.3.3 Adhesion Strength 42
4.3.4 Wear Resistance 44
Part II Effect of Working Pressure of HPPMS Process 48
4.4 Waveform and optical emission spectra 48
4.5 Chemical composition and structure 48
4.5.1 Chemical compositions 48
4.5.2 Crystal Structure and Preferred Orientation 48
4.5.3 Cross-sectional Microstructure and Surface Roughness 51
4.6 Properties 53
4.6.1 Hardness and Young’s Modulus 53
4.6.2 Residual Stress 53
4.6.3 Adhesion Strength and Wear Resistance 53
Chapter 5 Discussion 59
5.1 Effect of Duty Cycle 59
5.1.1 Texture and Chemical Compositions 59
5.1.2 Residual Stress 61
5.2 Effect of Working Pressure 62
5.2.1 Texture 62
5.2.2 Residual Stress and Electrical Resistivity 62
5.3 Tribological Behavior 64
5.3.1 Adhesion Strength 64
5.3.2 Wear Resistance 64
Chapter 6 Conclusions 68
Reference 69
Appendix A Power Cycle Induced Fatigue 80
Appendix B AFM images of the film 82

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