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研究生： 魏良儒
Wei, Liang-Ju
論文名稱： 優選方向對氮化釩硬膜破裂韌性之影響
Effect of Preferred Orientation on the Fracture Toughness of VN Hard Coatings
指導教授： 黃嘉宏
Huang, Jia-Hong
喻冀平
Yu, Ge-Ping
口試委員: 張銀祐
張奇龍
學位類別： 碩士
Master
系所名稱： 原子科學院 - 工程與系統科學系
Department of Engineering and System Science
論文出版年： 2017
畢業學年度： 105
語文別： 英文
論文頁數： 117
中文關鍵詞： 破裂韌性 、殘留應力 、氮化釩覆膜 、累積內能誘發破裂法 、織構
外文關鍵詞： Fracture toughness, Residual stress, VN coating, Internal energy induced cracking (IEIC) method, texture
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    • 本研究之主要目的為利用累積內能引發鍍層破裂之原理(IEIC法)量測氮化釩硬膜的破裂韌性，並調查織構對破裂韌性的影響。利用非平衡磁控濺鍍系統在兩種不同的氮氣流量下，鍍覆不同織構的氮化釩薄膜於矽(100)基材上。本研究把統計方法運用在IEIC法之量測過程中，以提升量測數值的正確性與可靠性。實驗結果顯示破裂韌性與織構相關，具有random織構之氮化釩薄膜的破裂韌性為26.5±2.2 J/m^2，而具有(200)織構之氮化釩薄膜則是46.6±3.7 J/m^2。兩種織構在破裂韌性之差異可能歸因於殘留應力的影響。因為氮化釩薄膜在<200>方向的彈性常數為三大主要平面中之最大，在基材的固定邊界情況下<200>方向的殘留應力也就相對較高，因而造成破裂韌性的提升。不論是random織構或(200)織構，薄膜的破裂形貌是相似的，裂縫傳遞路徑皆由木紋狀的R1區域和鋸齒狀的R2區域所組成。由於相對較平緩的應力梯度，邊緣的拉伸應力作用於薄膜中局部的缺陷處促使裂縫生成。其與氮化鋯薄膜的破裂行為相似，同樣是自由邊界效應造成之應力分布隨著裂縫前端移動，因而推動主要裂縫的階梯式成長。與敝實驗室之氮化鈦和氮化鋯之文獻結果相比，氮化釩硬膜具有相對較高的破裂韌性，特別是(200)織構。氮化鋯的破裂形貌中只有R2區域被觀察到，R1區域是氮化釩與氮化鋯在裂縫傳播路徑上的主要差異。

    The main objectives in this study were to measure the fracture toughness (Gc) of VN hard coatings using internal energy induced cracking (IEIC) method, and investigate the effect of preferred orientation on the fracture toughness. VN coatings were deposited on Si (100) substrates by unbalanced magnetron sputtering (UBMS) with two different nitrogen flow rates to prepare coatings with different textures. In the present research, statistical procedures were introduced in the IEIC method to increase the accuracy and reliability of the measured data. The results showed that Gc was texture-dependent, and the Gc values for specimens with random texture and (200) texture were 26.5±2.2 and 46.6±3.7 J/m^2, respectively. The difference in Gc may be attributed to the residual stress. Since the elastic constant of VN in <200> direction is the largest among the three major directions, the residual stress in <200> direction will be higher for the VN coatings under substrate constraint, and thereby increasing Gc. The fracture morphology of the coatings is similar regardless of random or (200) texture, where the crack path consisted of wood-grain R1 and zigzag R2 regions. The VN coatings have a relatively smooth compressive stress gradient, and thus crack initiation may occur due to the edge stress acting at local defects ahead of the edge inside the film. Similar to the fracture behavior in ZrN coatings, the stress distribution due to free edge effect can move with the crack front and consequently drive the main crack propagating stepwise. Compared with TiN and ZrN, VN hard coatings have relatively higher fracture toughness, especially for (200) texture. The existence of R1 region is the major difference in crack path compared with ZrN, where only R2 region was observed.

    Content 摘要....i Abstract....ii Content....iii List of Figures....vi List of Tables....x Chapter 1 Introduction....1 Chapter 2 Literature Review....3 2.1 Characteristics and Applications of VN....3 2.2 Texture Transitions of VN....6 2.2.1 Thermodynamic Theories....6 2.2.2 Kinetic Theories....6 2.2.3 Effect of Texture on Hardness....7 2.2.4 Effect of Deposition Parameters on the Texture of VN Thin Films....8 2.3 Measurement of Fracture Toughness on Thin Films....10 2.3.1 Indentation....10 2.3.2 Buckling....12 2.3.3 Bending....13 2.3.4 Tension....14 2.3.5 IEIC method....16 Chapter 3 Theoretical Basis....18 3.1 Assumptions of the Fracture Model....18 3.2 Energy Release Rate Approach....19 3.3 Griffith’s Criterion Approach [75]....23 3.4 Comparison of the Two Approaches....24 Chapter 4 Experimental Details....25 4.1 Specimen Preparation and Deposition Process....25 4.2 Characterization of Composition and Structure....28 4.2.1 Composition: XPS....28 4.2.2 Crystal Structure and Preferred Orientation: XRD and GIXRD....30 4.2.3 Cross-sectional image and Thickness: FEG-SEM....31 4.2.4 Topography and Cross-sectional Morphology of Fracture Surface: FIB/SEM....31 4.2.5 Surface Roughness: AFM....32 4.3 Characterization of Properties....32 4.3.1 Hardness and Young’s Modulus: NIP....32 4.3.2 Residual Stress....33 4.3.2.1 Overall Residual Stress: LCM....33 4.3.2.2 Local Residual Stress: XRD cos^2αsin^2ψ Method and Layer-by-layer Method....36 4.3.3 Fracture Toughness Measurement....38 4.3.4 Electrical Resistivity: Four Point Probe....39 Chapter 5 Results....41 5.1 Chemical Compositions....44 5.2 Crystal Structure and Texture....44 5.3 Microstructure....49 5.4 Surface Morphology and Roughness....51 5.5 Fracture Morphology....54 5.6 Mechanical Properties....62 5.6.1 Hardness....62 5.6.2 Residual Stress....62 5.6.3 Stored Energy and Fracture Toughness....67 5.7 Electrical Resistivity....69 Chapter 6 Discussion....71 6.1 Uncertainty of Measurement....71 6.1.1 Statistical Criterion for Determining Film Fracture....71 6.1.2 Thermal Stress....72 6.1.3 Estimation of Fracture Toughness....73 6.2 Effect of Texture on VN Coatings....73 6.2.1 Relations between Nitrogen Flow Rates, Textures, and Properties....73 6.2.2 Effect of Texture on Fracture Toughness and Residual Stress....75 6.3 Crack Propagation and Fracture Mechanism....77 6.4 Comparison of Fracture Toughness among Different Hard Coatings....80 Chapter 7 Conclusions....83 References....84 Appendix A Deconvoluted Results of XPS Spectra....91 Appendix B XRD & GIXRD Patterns....93 Appendix C SEM Images....97 Appendix D AFM images....105 Appendix E XRD cos2αsin2ψ....109 Appendix F Statistics of Hand-Cut Si....117

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