本研究目的是藉由高功率脈衝磁控濺鍍 (HPPMS) 在D2鋼上製備氮化鉬鍍層並探討調整佔空比與工作氣壓對鍍層結構與機械性質的影響。實驗結果顯示，(200)織構係數隨著佔空比與工作氣壓的下降而上升。佔空比下降能提升靶瞬時功率密度，而工作壓力的下降能增加氣體粒子的平均自由徑。這兩項參數的下降都會使電漿粒子有更大的能量，進而增加離子穿隧效應，有利於(200)織構的生長。實驗亦發現，藉由調控佔空比能使鍍層的殘留應力從很小的張應力至壓應力。鍍層的殘留壓應力與硬度會隨著佔空比與工作氣壓下降而增加，歸因於高能量的電漿粒子會增強離子轟擊效應，在鍍層中產生較多的缺陷。鍍層經過磨耗測試後發現，在沒有發生附著問題時，磨耗率都很低從0.12 至 0.98  10-6 mm3N-1m-1，這可能是因為氮化鉬鍍層所形成氧化相，如拉曼光譜觀察到的MoO3 或 Mo4O11，這些氧化相有很強的自潤滑特性因而超越其他因素主導了磨耗率。刮痕測試顯示所有鍍層都具有較低的Lc1與相當高的Lc2，因此磨耗測試中偶爾會發生鍍層破裂剝離問題。我們建議未來使用鉬金屬介層加強附著強度以確保耐磨性來解決此問題。實驗結果發現，鍍層在矽基板上的殘留應力使用LCM(LCM)與AXS(AXS)量測時，二者的結果有顯著的差異。我們提出了功率週期誘發疲勞(PCIF)的機制來解釋這個差異，在HPPMS製備過程中，高頻的功率可能在矽基板造成往復彎曲應力，進而引發高週疲勞導致矽基板的上部裂縫成長，使得矽基板的曲率釋放而降低LCM。

The purposes of this work were to produce single phase γ-Mo2N coatings by high power pulsed magnetron sputtering (HPPMS) and to investigate the effects of duty cycle and working pressure on structure and mechanical properties of the coatings on D2 steel. The results showed that the (200) texture coefficient of γ-Mo2N coatings increased with decreasing duty cycle and working pressure. The decrease of duty cycle was associated with increasing target peak power density, and the decrease of working pressure led to increasing mean free path of plasma species. The decrease of both parameters can increase the energy of plasma species, which enhances the ion channeling effect, thereby promoting the (200) texture in the coatings. It was found that the residual stress of the coatings could be controlled from slightly tensile to compressive stress by adjusting duty cycle. The compressive residual stress and hardness of the coatings increased with decreasing duty cycle or working pressure because high-energy plasma species enhanced the ion-peening effect and generated more defects in the coatings. The wear rates of all samples were very low ranging from 0.12 to 0.98  10-6mm3N-1m-1 when no adhesion issue occurred, and the wear mechanism was mostly abrasive wear. The major factor that affected wear resistance could be the formation of self-lubricating oxide phases such as MoO3 or Mo4O11 which was confirmed by the Raman spectra. The critical loads of the coatings showed low Lc1 and fairly high Lc2, and delamination occasionally occurred. Adding a Mo interlayer is suggested to be a solution to improve the adhesion strength and ensure the wear resistance. The results showed large deviation between the residual stresses of the coatings on Si measured by LCM(LCM) and AXS(AXS). A power cycle-induced fatigue (PCIF) mechanism was proposed to account for the deviation. The high frequency power cycle during HPPMS deposition process may give rise to alternating bending stress on the Si substrate, which could induce high-cycle fatigue crack growth and caused the relaxation of bending curvature in Si substrate, and thus lowering LCM.

摘要 i
Abstract ii
Content iv
List of Figures vi
List of Tables viii
Chapter 1 Introduction 1
Chapter 2 Literature Review 3
2.1 Characteristics of Molybdenum Nitride 3
2.1.1 Crystal Structure of Molybdenum Nitride 4
2.1.2 Mechanical Properties of Molybdenum Nitride 6
2.2 Tribological Behavior 7
2.2.1 Adhesion Strength 7
2.2.2 Wear Resistance 7
2.2.3 Self-lubrication of Molybdenum Nitride 8
2.3 High Power Pulsed Magnetron Sputtering (HPPMS) 10
2.3.1 Advantages of HPPMS 10
2.3.2 Effect of Duty Cycle 10
2.3.3 Effect of Working Pressure 11
2.4 Effect of Process Parameters 12
2.4.1 Nitrogen Flow Rate and Substrate Bias 12
2.4.2 Substrate Temperature 13
2.4.3 Gas Ion Current Density 13
Chapter 3 Experimental Detail 14
3.1 Substrate Preparation and Deposition Procedures 14
3.2 Characterization of Compositions and Structure 18
3.2.1 Chemical Compositions 18
3.2.2 Crystal Structure and Preferred Orientation 18
3.2.3 Cross-sectional Observation and Surface Morphology 19
3.2.4 Surface Roughness 20
3.3 Characterization of Properties 20
3.3.1 Hardness and Young’s Modulus 20
3.3.2 Residual Stress 21
3.3.3 Electrical Resistivity 22
3.3.4 Scratch test 22
3.3.5 Pin-on-disk Wear Test 24
3.3.6 Wettability 25
Chapter 4 Results 27
Part I: Effect of Duty Cycle (D-series Specimens) 30
4.1 Plasma Compositions 30
4.2 Target Voltage and Current 32
4.3 Chemical Compositions and Structure 34
4.3.1 Chemical compositions 34
4.3.2 Crystal structure 34
4.3.3 Microstructure and surface roughness 36
4.3.4 Deposition rate 38
4.4 Properties 38
4.4.1 Hardness and Young’s modulus 38
4.4.2 Residual stress 39
4.4.3 Electrical resistivity 40
4.4.4 Adhesion strength 41
4.4.5 Wear resistance 44
Part II: Effect of Working Pressure 48
4.5 Target Voltage and Current 48
4.6 Chemical Compositions and Structure 50
4.6.1 Chemical compositions 50
4.6.2 Crystal structure 50
4.6.3 Microstructure and surface roughness 52
4.6.4 Deposition rate 54
4.7 Properties 54
4.7.1 Hardness and Young’s modulus 54
4.7.2 Residual stress 55
4.7.3 Electrical resistivity 56
4.7.4 Adhesion strength 56
4.8 Wear Resistance 58
4.9 Raman spectra 62
4.10 Residual Stress from LCM 62
Chapter 5 Discussion 64
5.1 Effect of Duty Cycle 64
5.1.1 Preferred orientation 64
5.1.2 Residual stress and hardness 65
5.2 Effect of Working Pressure 67
5.2.1 Preferred orientation 67
5.2.2 Residual stress and hardness 68
5.3 Differences of effect between duty cycle and working pressure 69
5.4 Differences of residual stress between LCM and AXS on Si substrate 70
5.5 Tribological Behavior 74
5.5.1 Wear resistance of γ-Mo2N coatings 74
5.5.3 Adhesion issue of γ-Mo2N coatings 75
Chapter 6 Conclusions 79
Reference 81
Appendix A AFM Images 90
Appendix B Optical spectra 91

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