以非平衡磁控濺鍍法鍍製氮化鈦鋯薄膜往往會產生高殘留應力。先前研究指出利用高功率脈衝與直流磁控共濺鍍法製備薄膜能夠增加鍍膜速率並降低殘留應力。本研究之目的為探討佔空比及工作氣壓對氮化鈦鋯薄膜之結構和性質的影響。氮化鈦鋯薄膜是利用高功率脈衝與非平衡磁控共濺鍍法鍍製於矽 (100) 基板上。鈦靶放置於高功率脈衝磁控濺鍍槍上並調控佔空比從5到100% (D系列)與調控工作氣壓從3到10 mTorr (P系列)。調控佔空比及工作氣壓可以控制氮化鈦鋯薄膜的壓應力。從光譜分析儀量測結果發現，在5%佔空比的情況下，僅產生少量Ti+離子而沒有多價Ti離子產生；因此施加基板偏壓，離子轟擊效應仍然不顯著。佔空比降低會增加入射粒子能量，此能量轉移到吸附與基材之金屬原子並增加其移動性。此外，工作氣壓增加會減少電漿粒子的平均自由徑。結果顯示D和P系列試片最大的殘留應力分別為-2.63和-2.48 GPa。在佔空比 50%的試片中，鍍膜速率和高功率脈衝磁控濺鍍槍的工作時間有關。當佔空比< 10% (高功率脈衝區)，鍍膜速率僅降低21%。增加離子轟擊和離子穿隧效應是兩個可能造成(200)織構的原因。在高工作氣壓下鍍製的試片(P10)則由於電漿粒子平均自由徑縮短，使得吸附金屬原子能量降低，因而在低能量鍍膜條件下會生成(111)織構。鈦鋯比會隨佔空比和工作氣壓的降低而減少，而調控佔空比對於鈦鋯比之影響比調控工作氣壓更顯著。

TiZrN coatings deposited by unbalanced magnetron sputtering (UBMS) usually have high residual stress. Previous studies indicated that thin films deposited by hybrid high power impulse magnetron sputtering and DC magnetron sputtering (HiPIMS/DCMS) could increase the deposition rate and lower the residual stress. The purpose of this study was to investigate the effect of duty cycle and working pressure on structure and properties of TiZrN coatings. TiZrN coatings were deposited by co-sputtering of HiPIMS/DCMS on Si (100) substrate. The duty cycle of the HiPIMS sputtering gun with Ti target varied from 5 to 100 % (D-series) and working pressure ranged from 3 to 10 mTorr (P-series). Compressive residual stress of the TiZrN coatings can be controlled by adjusting duty cycle and working pressure. Even at 5% duty cycle, the HiPIMS gun generated small amount of Ti+ species, and no multivalent Ti ions was found in OES spectra. Therefore, ion peening effect on the film surface was not very intense even with applied substrate bias. The mobility of adatoms were enhanced by the energy delivering from the incoming energetic species due to decreasing duty cycle. Furthermore, the mean free path of the plasma species decreased with increasing working pressure. The results showed that the maximum residual stresses for D and P-series specimens were -2.63 and -2.48 GPa, respectively. For specimens deposited at duty cycle  50%, the deposition rate was related to the pulse-on time of HiPIMS sputtering gun. The deposition rate only lowered 21% in HiPIMS regime with duty cycle < 10%. The increase of ion bombardment and ion channeling effect may be the two reasons for the emergence of (200) texture. For specimen deposited at high working pressure (P10), (111) texture was attributed to the low-energy deposition condition, where the mean free path of the plasma species was reduced by the high working pressure. The Ti/(Ti+Zr) ratio of the TiZrN thin film decreased with decreasing duty cycle or decreasing working pressure. Tuning the duty cycle was more effective on changing Ti/(Ti+Zr) ratio than adjusting working pressure.

摘要 i
Abstract ii
致謝 iii
Contents v
List of Figures vii
List of Tables ix
Chapter 1 Introduction 1
Chapter 2 Literature Review 3
2.1 Characteristics of Transition Metal Nitride Coatings 3
2.2 Characteristics of TiZrN Coatings 5
2.2.1 Structure 5
2.2.2 Texture Evolution 7
2.2.2.1 Overall Energy Minimization 7
2.2.2.2 Competitive Growth Theory 8
2.2.2.3 Ion Channeling Effect 8
2.2.3 Properties 9
2.3 Residual Stress 9
2.4 High Power Impulse Magnetron Sputtering (HiPIMS) 11
2.4.1 High adhesion thin film 12
2.4.2 Film conformability 12
2.4.3 Dense Film 13
2.5 Hybrid Technologies 13
Chapter 3 Experimental Procedures 15
3.1 Substrate Preparation 15
3.2 Deposition Procedures 15
3.3 Characterization Methods for Compositions and structure 20
3.3.1 X-Ray Diffraction (XRD) and Glancing Incidence X-Ray Diffraction (GIXRD) 20
3.3.2 Field Emission Gun Scanning Electron Microscope (FEG-SEM) 21
3.3.3 Atomic Force Microscope (AFM) 21
3.3.4 Field Emission Electron Probe Microanalyzer (FE-EPMA) 21
3.3.5 X-Ray Photoelectron Spectroscopy (XPS) 22
3.4 Characterization of Properties 23
3.4.1 Residual Stress - Laser Curvature Method (LCM) 23
3.4.2 Hardness - Nanoindentation 25
3.4.3 Electrical Resistivity – Four-Point Probe 25
3.5 High Power Impulse Magnetron Sputtering (HiPIMS) 26
3.5.1 HiPIMS Power Monitoring - Oscilloscope 26
3.5.2 Plasma Diagnosis - Optical Emission Spectroscope (OES) 27
Chapter 4 Results 28
Part I Effect of Duty Cycle 31
4.1 Oscilloscope and Optical Emission Spectroscope 31
4.1.1 Oscilloscope 31
4.1.2 Optical Emission Spectroscope (OES) 31
4.2 Chemical Composition and Structure 36
4.2.1 Chemical Compositions 36
4.2.2 Crystal Structure and Preferred Orientation 38
4.2.3 Cross-sectional Microstructure 42
4.2.4 Surface Roughness 42
4.3 Properties 46
4.3.1 Hardness, Young’s Modulus and Electrical Resistivity 46
4.3.2 Residual Stress 46
Part II Effect of Working Pressure of HiPIMS Process 49
4.4 Oscilloscope and Optical Emission Spectroscope 49
4.4.1 Oscilloscope 49
4.4.2 Optical Emission Spectroscope 49
4.5 Chemical Composition and Structure 50
4.5.1 Chemical Compositions, Crystal Structure and Preferred Orientation 50
4.5.2 Cross-sectional Microstructure and Surface Roughness 54
4.6 Properties 58
4.6.1 Hardness and Young’s Modulus 58
4.6.2 Residual Stress 58
4.6.3 Electrical Resistivity 58
Chapter 5 Discussion 62
5.1 Effect of Duty Cycle 62
5.1.1 Texture Evolution and Chemical Composition 62
5.1.2 Deposition Rate 67
5.1.3 Residual Stress 67
5.2 Effect of Working Pressure 68
5.2.1 Texture Evolution and Chemical Composition 68
5.2.2 Residual Stress 69
5.3 Adjusting parameters to control low residual stress 71
Chapter 6 Conclusions 74
References 75
Appendix A SEM Images 86
Appendix B 2D AFM Images 87
Appendix C 3D Plots of effects of duty cycle and working pressure on the structure and properties of TiZrN thin films 89

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