利用非平衡磁控濺鍍系統在工具鋼上鍍著不同厚度的Ti-Si-N覆膜之機械性質與防蝕性質研究

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研究生：	鄭雲楷 Cheng, Yun-Kai
論文名稱：	利用非平衡磁控濺鍍系統在工具鋼上鍍著不同厚度的Ti-Si-N覆膜之機械性質與防蝕性質研究 Influence of thickness on mechanical and corrosion properties of Ti-Si-N coatings on D2 steel by unbalanced magnetron sputtering
指導教授：	黃嘉宏 Huang, Jia-Hong 喩冀平 Yu, Ge-Ping
口試委員:	李志偉 Lee, Jyh-Wei 駱榮富 Louh, Rong-Fuh
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：	2012
畢業學年度：	100
語文別：	英文
論文頁數：	104
中文關鍵詞：	鈦矽氮奈米複合膜、硬度、殘餘應力、附著強度、腐蝕
外文關鍵詞：	Ti-Si-N nanocomposite, hardness, residual stress, adhesion strength, corrosion
相關次數：	點閱：2 下載：0
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本研究利用非平衡磁控濺鍍系統在D2工具鋼上鍍著不同厚度的鈦-矽-氮覆膜。其目的在於研究鍍層厚度對鈦-矽-氮覆膜的成分、結構、機械性質與腐蝕抗性的影響，同時也探討鈦介層對鈦-矽-氮覆膜的結構與特性的影響。結果顯示，隨著鍍膜時間增加，鍍層厚度從696 nm成長至3019 nm，最大厚度可達3 μm以上。不同厚度之鈦-矽-氮覆膜的優選方向都呈現 (111) 優選方向。加入矽與鈦介層都可改變鈦-矽-氮覆膜中氮化鈦相的優選方向從 (200) 轉為 (111) 方向。從XRD與XPS的結果得知，本實驗所鍍著的覆膜為一奈米複合結構，由奈米晶的氮化鈦以及非晶形的氮化矽所組成。硬度分布範圍從23 GPa到36 GPa，硬度的變化與鈦-矽-氮覆膜結構中的氮化鈦晶粒尺寸及優選方向有關。由 cos2αsin2 X光繞射方法量測到的殘餘應力值顯示，在奈米複合覆膜中，氮化鈦的殘餘應力並不隨著厚度增加有明顯變化。動態極化掃描的結果顯示，覆膜後的試片在0.5 M硫酸與5 wt%鹽水環境中具有良好的防蝕能力。從刮痕測試與動態極化掃描的結果來看，增加鈦介層有助於增加覆膜的附著性與抗蝕性。

TiSiN nanocomposite coatings with different thickness were deposited on D2 tool steel substrates using unbalance magnetron sputtering (UBMS). The purpose of this study was to investigate the influence of coating thickness on the compositions, structure, mechanical properties, and corrosion resistance of TiSiN coatings. The effect of Ti interlayer on structure and properties of TiSiN coatings was also studied. The coating thickness increased with increasing deposition duration ranging from 696 to 3019 nm and the maximum thickness could reach over 3 μm. TiN (111) was the preferred orientation in all TiSiN coatings. The incorporation of Si or addition of Ti interlayer could change the preferred orientation of TiN phase from (200) to (111) in TiSiN coatings. The results of X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) revealed that the nanocomposite coatings were composed of nanocrystalline TiN and amorphous SiNx. The hardness, ranging from 23 to 36 GPa, was related to the grain size and texture of TiN in TiSiN coatings. The residual stresses of TiN in nanocomposite coatings measured by XRD cos2αsin2ψ method were all compressive and had no significant variation with increasing coating thickness. The results of the potentiodynamic polarization scan indicated that the TiSiN-coated samples possessed good corrosion resistance in both 0.5 M H2SO4 and 5 wt% NaCl solutions. From the results of scratch test and potentiodynamic polarization scan, the addition of Ti interlayer was beneficial for the adhesion strength and corrosion resistance of the TiSiN coatings.

中文摘要    i
Abstract    ii
誌謝    iii
Content    v
List of Figures    viii
List of Tables    x
Chapter 1  Introduction    1
Chapter 2  Literature Review    3
1 Deposition Method    3
2 Characteristics of TiSiN Nanocomposites    7
2.1 TiN    7
2.2 SiNx    7
2.3 TiSiN Nanocomposites    8
3 The Origin of High Hardness of TiSiN Nanocomposites    10
3.1 The Hardening Mechanism    10
3.2 The Roles of Interfacial SiNx Phase and Si Content    10
3.3 Thermodynamically Driven Phase Separation – The Spinodal Decomposition    11
3.4 Influence of Impurity    12
4 The Corrosion Resistance of TiSiN Nanocomposites    13
5 The Adhesion Strength of TiSiN Coating    14
6 The Applications of TiSiN Nanocomposites    14
Chapter 3  Experimental Details    17
1 Substrate Preparation    17
2 Coating Process    17
3 Characterization Methods for Structure and Composition    22
3.1 X-Ray Photoelectron Spectroscopy (XPS)    22
3.2 Field-Emission Gun Scanning Electron Microscopy (FEG-SEM)    22
3.3 Secondary Ion Mass Spectrometer (SIMS)    22
3.4 Thickness Measurement    22
3.5 X-Ray Diffraction (XRD) and Glancing Incidence XRD (GIXRD)    23
3.6 Atomic Force Microscopy (AFM)    24
4 Characterization Methods for Properties    25
4.1 Hardness    25
4.2 Residual Stress: cos2αsin2ψ Method    25
4.3 Scratch Test    26
4.4 Corrosion Resistance and Wettability    27
4.4.1 Potentiodynamic Polarization Scan    27
4.4.2 Salt Spray Test    28
4.4.3 Wettability    28
4.5 Electrical Resistivity    30
Chapter 4  Results    35
1 Compositions and Structure    35
1.1 SIMS Compositional Depth Profiles    35
1.2 SEM    42
1.3 Thickness    42
1.4 XRD    46
1.5 GIXRD    47
1.6 XPS    51
1.7 Atomic Force Microscopy (AFM)    55
2 Mechanical properties    55
2.1 Hardness    55
2.2 Residual Stress    56
2.3 Scratch Test    56
3 Corrosion Resistance    61
3.1 Contact Angle and Wettability    61
3.2 Potentiodynamic Polarization Scan    62
A. 0.5 M H2SO4 + 0.05 M KSCN    62
B. 5 wt% NaCl    63
3.3 Salt Spray Test    63
4 Electrical Resistivity    64
Chapter 5  Discussion    72
1 The Structure and Mechanical Properties of TiSiN Coatings    72
1.1 Structure    72
1.2 Hardness    73
1.3 Residual Stress    75
1.4 Adhesion Strength    76
1.5 Corrosion Resistance    77
2 Effect of Ti interlayer on Structure and Properties of TiSiN Coatings    78
2.1 Texture    78
2.2 Hardness    78
2.3 Residual Stress    79
2.4 Adhesion Strength    79
2.5 Corrosion Resistance    80
Chapter 6  Conclusions    82
References    83
Appendix A  XPS Deconvolution Spectra    90
Appendix B  Surface Morphology    100

                                

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