以過濾式陰極真空電弧電漿系統合成碳化鉻薄膜製程與特性之研究

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研究生：	林君純 Chun-Chun Lin
論文名稱：	以過濾式陰極真空電弧電漿系統合成碳化鉻薄膜製程與特性之研究 Processing and properties of chromium carbide thin films synthesized by a filtered cathodic vacuum arc plasma system
指導教授：	施漢章 Han C. Shih
口試委員:
學位類別：	博士 Doctor
系所名稱：	工學院 - 材料科學工程學系 Materials Science and Engineering
論文出版年：	2007
畢業學年度：	95
語文別：	英文
論文頁數：	147
中文關鍵詞：	filtered cathodic vacuum arc plasma system 、chromium carbide
相關次數：	點閱：2 下載：0
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本研究主要是使用過濾式陰極電弧電漿沉積法在鋼材上合成碳化鉻薄膜，藉由控制製程參數，如沉積溫度、基板偏壓及反應氣體流量 (C2H2/Ar)沉積出結晶與非晶質之碳化鉻薄膜，並探討其微結構變化、機械性質、腐蝕行為及光學性質。
研究結果顯示，使用過濾式陰極電弧電漿系統在沉積溫度500℃下能成功合成出均勻且緻密的碳化鉻薄膜，且在此溫度下，施加不同基材偏壓(-50—-550V)能有效使碳化鉻薄膜由非晶質相轉變成結晶相(cryst-CrC)，為Cr3C2且含有似纖維結構之Cr23C6相。結晶化碳化鉻薄膜相較於非晶質化碳化鉻薄膜具有較佳之機械強度及附著性，也因本身結構緊密且無微粒(micro-particles)存在，故在氯鹽環境下具有極佳抗腐蝕能力。
針對披覆結晶(cryst-Cr3C2)與非晶質(a-CrC)之碳化鉻的鋼材之腐蝕行為做更進一步探討，使用等效電路模擬EIS量測之結果互相比較，以了解cryst-Cr3C2/steel 與a-CrC/steel腐蝕機制的影響。結果顯示cryst-Cr3C2/steel的腐蝕阻抗較a-CrC/steel佳。
本論文的另一重點是利用陰極發光技術分析非晶質碳膜摻雜鉻原子與碳化鉻薄膜的光學性質，結果指出兩者之光學性質相似，發出2.10、2.03和1.99 eV的光譜，主要是由π鍵基態至π鍵激發態能階的跳躍、外來元素的摻雜與缺陷能階所造成。

In this thesis, the 90o-bend filtered cathodic vacuum arc (FCVA) technology was employed to deposit the chromium carbide films on the steel (AISI D2). This investigation was to compare various conditions which including the deposition temperature, the substrate bias voltage and the C2H2/Ar flow. The micro-structures, mechanical properties, corrosion behavior and optical properties of the chromium carbide film are thoroughly discussed.
The uniform and dense of the chromium carbide films have been successfully synthesized using our FCVA system. The chromium carbide is transformed from amorphous to crystallized phase, as the negative substrate bias voltage increases from -50 to -550 V at 500 ℃.Moreover, the crystallized Cr23C6 phase appears as the negative substrate bias voltage further increases. A compact and dense Cr3C2 film with the fibrous structure of Cr23C6 was successfully prepared.
The Cr3C2 coated steel has a relatively high nanohardness and excellent adhesion compare with the amorphous chromium carbide. The corrosion resistance of the Cr3C2 coated steel is owing to the establishment of a defects-free microstructure. No pitting corrosion was observed on the Cr3C2 coated steel.
The corrosion behaviors of cryst-Cr3C2/steel and a-CrC/steel were investigated further. All samples was measured and the results obtained from electrochemical impedance spectroscopy (EIS) simulated by the equivalent circuit to interpret the corrosion mechanism of the cryst-Cr3C2/steel and a-CrC/steel were compared. The results indicated that the cryst-Cr3C2/steel more effectively isolates the defects than dose a-C:Cr/steel in saline environment.
The cathodoluminescence spectra of the DLC:Cr films are evident in the visible region, thereby shifting the red emission to 1.99 eV. The orange emission at 2.03 eV also appears due to transitions between chromium-related electron levels and σ* states. Additionally, the peak at 2.10 eV likely results from the defective structures in the DLC:Cr films. The effect of Cr doping changed DLC band structure and its consequent cathodoluminescence property.

Contents
Abstract (in Chinese) ..……………...………………………………….....I
Abstract (in English)…………………………………….………………III
Acknowledgements (in Chinese) ……………………….……………….V
Contents      …………………………………………………………...…...VII
Table lists………………………………………………………………..XI
Figure captions  …………………………………………………………XII

Chapter 1 Introduction……………………………………….…...…....…1
1.1 Background and Motivation…………………….……..……..…     1
1.2 Overview……………………………………..….….…….……. 4
Chapter 2 Theoretical basis ….……………….……………………....…...….…. 7
2.1 Cathodic arc plasma……………………………………....….….7
2.1.1 Principle………………………….……….………….………..8
2.1.2 Vacuum Arc………………………..…….……………...........10
2.1.3 Arc Sources ……………………………….……..……...........10
2.1.4 Additional magnet behind targets……………………............   11
2.1.5 Macro-particles…………………………………...….………  11
2.1.6 Macro-particle filter…………………..………….…..………13
2.2 Properties and characterization………………………………....15
2.2.1 Nanoindentation method……………………………………...15
2.2.2 Scratch tests…………………………………………………..16
2.2.3 Corrosion resistance evaluation………………………………19
2.2.3.1 Linear polarization…………………….………….………...19
2.2.3.2 Electrochemical impedance spectroscopy (EIS)…………...      20
2.3 Chromium carbides……………………………………………..35
2.3.1 Background…………………………………………………... 35
2.3.2 The chromium-carbon system………………………………..    36
2.3.3 Production of chromium carbides…………………………….37
2.3.4 Applications…………………………………………………..38
2.3.4.1 Wear resistant coatings……………………………………..38
2.3.4.2 Welding electrodes…………………………………………  38
2.3.4.3 Thermal spray applications…………………………………40
2.3.4.4 Chrome plating alternative…………………………………    40
2.3.4.5 Cutting tools…………………………………………...........41
Chapter 3 Instrumentation and experimental procedure.………………..43
3.1 Instrumentation—filtered cathodic vacuum arc system (FCVA)………………………………………………………..43
3.2 Overview of the experiment procedures…..…………...……....45
3.2.1 Materials selection…………………………………………...45
3.2.2 Filtered cathidic vacuum arc deposition process…………….45
3.3 Characterization…………………………….……….….……...48
3.3.1 Microstructure analysis………………………………………48
3.3.2 Phase identification…………………………………………..48
3.3.3 Composition analysis………………………………………...48
3.3.4 Nanomechanical properties…………………………………..50
3.3.5 Cathodoluminescence (CL)………………………………….      51
3.3.6 Corrosion tests……………………………………………….      51
Chapter 4 Results and discussion……………………………………….     54
4.1 Formation and characterization of chromium carbide films…... 54
4.1.1 Effect of deposition temperature……………………………..55
4.1.2 Effect of substrate bias voltage………………………………63
4.2 The effect of the substrate bias voltage on the mechanical and corrosion properties of chromium carbide thin films………………69
4.2.1 Crystallographic orientation and surface morphology    ……...70
4.2.2 Mechanical properties………………………………………...75
4.2.3 Corrosion characteristics……………………………………...........82
4.3 Corrosive behavior of chromium carbide based films formed on steel…………………………………………………………………86
4.3.1 Crystallographic orientation………………………………….    87
4.3.2 Open-circuit potential (OCP)……………………………........90
4.3.3 EIS behavior………………………………………………….93
4.4 Cathodoluminescence of Cr doped DLC film………………...106
4.4.1 Raman analysis……………………………………………...107
4.4.2 XPS and TEM analysis……………………………………...111
4.4.3 Cathodoluminescence spectra……………………………….117

Chapter 5 Conclusion…………………………………....…………….120
References…………………………………………………...…….......123
Publications………………………………………………...…….……143

Table lists
Table 2.1. Standard grades of chromium carbide………………………37
Table 3.1. Deposition parameters of chromium carbide films using 90o–bend magnetic filtered cathodic vacuum arc……………46
Table 4.1. Mechanical properties of Cr3C2 coating as a function of the substrate bias voltages……………………….……………..76
Table 4.2. Corrosion potential Ecorr and corrosion current density icorr for Cr3C2 on AISI D2 steel with varying substrate bias voltages and uncoated steel evaluated in aerated 3.5% NaCl aqueous solutions…………………….................................................83
Table 4.3 Optimum fit parameters of the a-C:Cr/steel and cryst-Cr3C2/steel derived from the equivalent circuit……...............103
Table 4.4. Values of T peak, D band and G band’s position, FWHM, the ratio (ID/IG), and Cr/C atomic ratio for various C2H2/Ar flow………………………………………………………..114

Figure captions
Fig. 2.1 The scheme of the radicals excited by the vacuum arc…………9
Fig. 2.2 Different types of filters (a) 90□-bend filter and (b) S-bend filter…………………………………………………………..15
Fig. 2.3 Schematic representation of failure modes in the scratch test in profile and plan view: (a) spalling failure, (b) buckling failure, (c) chipping failure, (d) conformal cracking and (e) tensile cracking………………………………………………………..18
Fig. 2.4 Cyclic nature of AC voltage……………………………………22
Fig. 2.5 Electrical behavior of an electric double layer…………………22
Fig 2.6 AC voltage-current phase angle………………………………...24
Fig. 2.7 Vector nature of voltage and current…………………………...24
Fig. 2.8 Electrical double layer for an uncoated, oxide-free corroding metal……………………………………………………...…..27
Fig 2.9 Electrified interface structure for a corroding, coated metal…....29
Fig. 2.10 Single time constant complex plane plot……………...…..…..32
Fig. 2.11 Single time constant Bode magnitude plot……………………32
Fig. 2.12 Part of the phase diagram for chromium and carbon…………36
Fig. 3.1 Setup of the 90o–bend magnetic FCVA system………………...44
Fig. 3.2 The FCAP system in our laboratory……………………………44
Fig. 3.3 The experiment procedures…………………………………….47

Figure 4.1 Cross-section SEM images of the amorphous chromium carbide film deposited at the substrate bias of -150V at (a) ambient temperature, (b) 300 ℃, and (c) 500 ℃……….. 56
Figure 4.2 AES depth profile of chromium carbide film deposited at two different deposition temperature: (a)T=300 ℃, (b) T=500 ℃ on the Si wafer. The thickness of the film is 500 nm……………………………………………………….…..61
Figure. 4.3 XPS C 1S(a) and Cr 2p(b) spectra of the chromium carbide
deposited at ambient temperature, 300 ℃ and 500 ℃…….62
Figure 4.4 X-ray diffraction patterns of the Cr3C2 deposited at 500℃ with varying substrate bias voltages………………………..64
Figure 4.5 (a) Cross-section TEM micrograph and (b) SAD pattern of the crystallized chromium carbide/Cr deposited on the Si wafer.......................................................................................67
Figure 4.6 Cross-section TEM micrograph and SAD pattern from an area that covers the top of the chromium carbide film deposited at (a)-250, and (b) -550 V………………………………..…….68
Figure 4.7 Cross-section SEM images of Cr3C2 films deposited at (a)-50V and (b) -550V substrate bias voltage………………………..73
Figure 4.8 Surface morphologies of Cr3C2 films deposited at (a)-50V and (b) -550V substrate bias voltage……………………..……...74
Figure 4.9 The nanoindentation Load-displacement curves of Cr3C2 film
formed at various substrate bias voltages……….…….…….76
Figure 4.10 Friction coefficients of Cr3C2 coated steel against a diamond tip as function of scratch time with various substrate bias voltages…………………………………………………....78
Figure 4.11 Surface morphologies of (a)initial conformal cracking, (b)initial buckling failure and (c)near the end of the scratch track as indicated with white arrows on the scratch track………………………………….………………..…...81
Figure 4.12 Potentiodynamic polarization curves of uncoated steel and Cr3C2 coated steel with various substrate bias voltages, in aerated 3.5% NaCl aqueous solutions……………………..84
Figure 4.13 Ecorr and icorr for Cr3C2 coated AISI D2 steel with varying substrate bias voltages evaluated in aerated 3.5% NaCl aqueous solutions………………………...………………...85
Figure 4.14 XRD patterns of chromium carbide based films with various C2H2/Ar pressures deposited at 500℃ under the substrate bias voltage of -50 V………………………………...…….89
Figure 4.15 Variation of the OCPs with the immersion time of the steel and the coating assemblies in an aerated 3.5 wt% NaCl solution…………………………………………………….92
Figure 4.16. Nyquist plots as a function of immersion time in an aerated
3.5 wt% NaCl solution: (a) steel (AISI D2), (b) a-C:Cr/steel and (c) cryst-Cr3C2/steel……………………………..…….96
Figure 4.17 The SEM images after the 216 h immersion test:(a) a-C:Cr/steel and (b)cryst-Cr3C2/steel…………………………………...98
Figure 4.18 Interface impedance model of the a-C:Cr/steel and the Cr3C2/steel (a) cross-section schematic, and (b) its equivalent circuit………………………………………..104
Figure 4.19 Comparison of the simulated and measured EIS data as a function of immersion time in aerated 3.5 wt% NaCl solution of (a) a-C:Cr/steel and (b) cryst-Cr3C2/steel……………..……………………….…105
Figure 4.20 Raman spectroscopy of the DLC:Cr film deposited at various C2H2 /Ar flows: (a) 5/5, (b) 10/10, (c) 10/30, and (d) 20/20 sccm………………………………………………………110
Figure 4.21 XPS spectra of the C1s core level for DLC:Cr film deposited at various C2H2 /Ar flows: (a) 5/5, (b) 10/10, (c) 10/30, and (d) 20/20 sccm…………………………………………...…….115
Figure 4.22 XPS spectra of the Cr2p core level for DLC:Cr film deposited at various C2H2 /Ar flows: (a) 5/5, (b) 10/10, (c) 10/30, and (d) 20/20 sccm………………...…………….115

Figure 4.23 TEM cross-sectional micrograph and its corresponding SAD pattern of the DLC:Cr film formed at the C2H2 /Ar flow of 20/20 sccm……………………………….………………116
Figure 4.24 CL spectra of the DLC:Cr films synthesized at various C2H2/Ar flows: (a) 5/5, (b) 10/10, (c) 10/30, and (d) 20/20 sccm………………………………………………

                                

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