以過濾式陰極電弧電漿系統合成非晶質碳膜與摻雜元素對結構與物理特性影響之研究

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研究生：	謝維仁 Wei-Jen Hsieh
論文名稱：	以過濾式陰極電弧電漿系統合成非晶質碳膜與摻雜元素對結構與物理特性影響之研究 Extrinsic atom doping effects on the structures and physical properties of amorphous carbon film synthesized by filtered cathodic 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：	2005
畢業學年度：	94
語文別：	英文
論文頁數：	118
中文關鍵詞：	非晶質碳膜、非晶質碳氮膜、非晶質碳氮硼膜、非晶質碳氟膜、對苯二甲酸乙二酯、陰極發光
外文關鍵詞：	a-C, a-C:N, a-C:N:B, a-C:F, polyethylene terephthalate, cathodoluminescence
相關次數：	點閱：3 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合成非晶質碳材薄膜，並在碳材中摻雜不同的元素，如:氮、硼及氟等原子。主要合成出四種材料：非晶質碳膜(a-C)、非晶質碳氮膜(a-C:N)、非晶質碳氮硼膜(a-C:N:B)、非晶質碳氟膜(a-C:F)，並探討其微結構變化、機械性質、電性及光學性質。
在非晶質碳氮膜裡，發現存在有奈米尺寸的鑽石顆粒，其存在可提升非晶質碳氮薄膜的機械強度，亦會影響材料本身的光學特性。在非晶質碳氮膜中摻雜硼元素形成非晶質碳氮硼膜，對電子場發射特性有一定的影響，影響原因有三項：分別為石墨化程度、表面粗糙度和摻雜原子效應。
在本研究中，基板的選擇不只有矽晶片亦選用對苯二甲酸乙二酯 (polyethylene terephthalate, PET) 材料，為一可繞曲的高分子基板，成功地在PET上成長a-C:F薄膜，藉調變實驗參數，可控制非晶質碳氟薄膜的表現型態，可形成奈米尺寸的非晶質碳氟顆粒球，其為蝕刻速率與沉積速率兩者競爭達平衡的結果。
本論文的另一重點是利用陰極發光技術分析非晶質碳材的光學性質，發現在非晶質碳氮膜可發出藍光(~2.67 eV)和紅光(~1.91 eV)，但非晶質碳膜只發出紅光(~2.04 eV)，而在非晶質碳氮膜裡摻雜硼原子形成a-C:N:B膜只發出藍光(~2.67 eV)。非晶質碳氟膜發出不同頻率的光(2.03和1.97 eV)，而非晶質碳氟奈米顆粒(a-C:F nano-particles)膜可發出2.10、2.03和1.97 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。

Carbon based materials were synthesized by using the filter cathodic arc plasma system, and extrinsic atoms, e.g. nitrogen, boron and fluorine elements were doped into the thin films in this study. Four types of carbon-related films were studied, they are: amorphous carbon (a-C), amorphous carbon nitride (a-C:N), boron doped amorphous carbon nitride (a-C:N:B) and fluorine doped amorphous carbon (a-C:F); their mechanical, electronic, optical properties and micro-structures are thoroughly discussed.
Nano-crystalline diamond clusters were found to be embedded in the a-C:N film, which enhance the mechanical strength and affect the optical properties. Boron doped a-C:N (a-C:N:B) films affect the electrical field emission due to the degree of graphitization, surface morphology and acceptor effects.
Not only Si wafer but also polyethylene terephthalate (PET), which is flexible, were applied as the substrates upon which a-C:F films were successfully deposited. The transform of the surface morphology of the a-C:F film to the a-C:F nano-particles film by optimizing the parameters and by discussing the growth mechanism and optical properties.
The result of cathodoluminescence measurements indicated that the a-C:N films produce the blue (~2.67 eV) and red light (~1.91 eV) while the boron doped a-C:N (a-C:N:B) films and the a-C films only generate the respective blue (~2.67 eV) and red light (~2.04 eV). The most prominent cathodoluminescence of the a-C:F films is the orange light (~2.03 eV) and red light (~1.97 eV), but the a-C:F nano-particles film exhibits several luminescences at 2.10, 2.03 and 1.97 eV. These luminescences are main due to the π-π* transition, extrinsic atom doping and the defect energy level.

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 Motivation………………………………….……..……..………1
1.2 Overview……………………………………..….….…….……..2
1.3 Form of carbon………………………..….………….….……….3
1.3.1 Diamond………………..……………………….………..3
1.3.2 Graphite…………………………………..………………3
1.3.3 Amorphous carbon………………..………….……...…...5
1.4 Cathodic arc plasma……………………………………....….….7
1.4.1 Principle………………………….……….………….…..7
1.4.2 Vacuum Arc………………………..…….……………...10
1.4.3 Arc Sources……………………………….……..……...10
1.4.4 Additional magnet behind targets……………………....11
1.4.5 Macro-particles…………………………………...….…12
1.4.6 Macro-particle filter…………………..………….…..…12
Chapter 2 Instrumentation and characterization….……………………..15

2.1 Deposition system- Filtered cathodic arc plasma deposition (FCAP)………………………………………………………..15
2.2 Overview of the experiment procedures…..…………...……....17
2.3 Characterization…………………………….……….….……...19
2.3.1 Atomic Force Microscope (AFM)………..….……...…..19
2.3.2 Field emission scanning electron microscopy (FESEM)………………………………………………...19
2.3.3 High-resolution transmission electron microscopy (TEM).…………………………………………………...19
2.3.4 X-ray diffraction…..………………………….………....19
2.3.5 Raman spectroscopy……………………..……….……..20
2.3.6 Fourier transform infrared spectroscopy (FTIR)……......20
2.3.7 X-ray photoelectron spectroscopy (XPS)……..…….…..21
2.3.8 Optical emission spectroscopy (OES)………..………....21
2.3.9 Electron field emission measurement………….……….22
2.3.10 Nano-indentation…………….………………………...22
2.3.11 Cathodoluminescence (CL)…………………………....23

Chapter 3 Characterization and formation of nano diamonds in a-C:N films………………….……………………………...………24
3.1 Synthesis of nano diamonds embedded in a-C:N films………..24
3.2 Microstructures………………………………………………...25
3.3 Mechanical property……………………….…………………..38

Chapter 4 Cathodoluminescence of a-C:N films………………….....….40
4.1 Introduction……………………………..……………………...40
4.2 Synthesis of a-C:N films……...……….……………………….41
4.3 Cathodoluminescence measurement……...……………………43
4.4 Microstructures…………………………….…………………..46

Chapter 5 The relation between structure and optical property of a-C:N films…………………………………………..……………..53

Chapter 6 Cathodoluminescence and electron field emission of boron-doped a-C:N films……………………..……….……60
6.1 Synthesis of boron-doped a-C:N films…….………..…………60
6.2 Microstructures……………………………………….………..61
6.3 Cathodoluminescence measurement………….…….………….70
6.4 Field emission measurement……………………..…………….72

Chapter 7 Cathodoluminescence of fluorine doped amorphous carbon nanoparticles.………………...…………………..……..…79
7.1 Introduction………………………........……………….………79
7.2 Synthesis of fluorine doped amorphous carbon nanoparticles...80
7.3 Microstructures…………………………………….…………..80
7.4 Cathodoluminescence measurement…………..……………….90

Chapter 8 Summary………………………………………....…………..93

References…………………………………………………...……….…96
Publications……………………………………………………….……111
Vita (in Chinese)…………...…………………………………………..117

Table lists
Table I Values of D-band and G-band’s the position, FWHM, the ratio (ID/IG) and N/C atomic ratio for various nitrogen flows…………50

Table II Values of the Eto, Eth, resistivity (ρ), ID/IG and Rrms of the a-C:N and a-C:N:B films………………………………………………..78

Figure Captions
Fig. 1.1 (a) Diamond structure (b) Graphite structure……………………4
Fig. 1.2 The scheme of the radicals excited by the vacuum arc.…………9
Fig. 1.3 Different types of filters (a) 90□-bend filter (b) S-bend filter….14
Fig. 2.1 The scheme of the cathodic arc filter…………………………..16
Fig. 2.2 The FCAP system in our laboratory…………………………....16
Fig. 2.3 The experiment procedures……………………………….……18
Fig. 3.1 (a) SEM fracture cross-section image of the a-C:N film on silicon (b) SEM surface morphology of the a-C:N film on silicon…...…26
Fig. 3.2 XPS survey scan spectra of the a-C:N film on silicon with (a) as-deposited  specimens  and (b) 15 sec sputter cleaned by Ar+………………………………………………………………..28
Fig. 3.3 Deconvolution of (a) N (1s) core-level peak of a-C:N films on silicon, and (b) C (1s) core-level peak of a-C:N films on silicon.……………………………………………………………29
Fig. 3.4 XPS survey scan spectra for the film at various negative dc pulsed bias (a) -150, (b) -350 and (c) -650 V………………..…...30
Fig. 3.5 The Raman spectrum of the a-C:N film at (a) 0, (b) -150, (c) -250, (d) -350, (e) -450 and (f) -650 V pulsed substrate bias voltages....32
Fig. 3.6 Variation of the ID/IG as a function of substrate bias voltage…...33
Fig. 3.7 FTIR spectra of the a-C:N films synthesized at (a) -100, (b) -350 and (c) -650 V pulsed substrate bias voltages……………….…...35
Fig. 3.8 MAC glancing incident X-ray pattern of the a-C:N film on silicon………………………………………………………....37
Fig. 3.9 Selected area diffraction (SAD) pattern showing nanocrystalline diamond structures in the a-C:N film and bright-field image of nanocrystalline diamond in the a-C:N film…………………...37
Fig. 3.10 Nanohardness measurements of the a-C:N film  at (a) 0, (b) -250, (c) -350, (d) -450 and (e) -650 V of negative pulsed substrate bias voltages…………………………………..…….39
Fig. 3.11 Variation of the hardness as a function of substrate bias voltage…………………………………………………….…..39
Fig. 4.1 OES for the various N2 flows in the FCAP system…………….42
Fig. 4.2 CL spectra of a-C:N films synthesized at various nitrogen flows of 0, 10, 20, 30, 40 and 50 sccm at 300K……………..………….45
Fig. 4.3 The relation of the blue light intensity (IB) and red light intensity (IR) emitted by a-C:N, and the ratio (IB/IR) with various nitrogen flows…………………………………………………………..….45
Fig. 4.4 The variety of the Raman spectroscopy from 0-50 sccm nitrogen flows……………………………………………………………...47
Fig. 4.5 The deconvolution of the Raman spectroscopy of a-C:N films synthesized at 50 sccm nitrogen flows………………………...…47
Fig. 4.6 XPS survey scan spectra for the film at various nitrogen flows of 0, 10, 20, 30, 40 and 50 sccm…………….....……………………49
Fig. 4.7 The FTIR spectra of the a-C:N films synthesized at (a) 0, (b) 10 and (c) 50 sccm nitrogen flows……………………….………….52
Fig. 5.1 A simplified model of possible electronic transitions of the a-C:N film…………………………………………………………….…54
Fig. 5.2 Plot of (αhυ)1/2 vs. hυ of the a-C:N film…………………...56
Fig. 5.3 Plot of Tauc gap vs. N/C ratio of the a-C:N film………………57
Fig. 5.4 Raman spectroscopy of the a-C:N films in different N/C ratio of 0.05, 0.12, 0.34 and 0.56…………………………………………59
Fig. 6.1 Typical SIMS depth profile for the a-C:N:B film……….……..62
Fig. 6.2 Typical (a) C1s, (b) N1s and (c) B1s core level XPS spectra of the a-C:N:B film……………..………………………………..64,65
Fig. 6.3 Differences in the Raman spectroscopy of the a-C:N and a-C:N:B film……………………………………………………..67
Fig. 6.4 FTIR spectra of the (a) a-C:N and (b) a-C:N:B films………….69
Fig. 6.5 CL spectra of the a-C:N and a-C:N:B films…………………....71
Fig. 6.6 (a) J-E curves of the a-C:N and a-C:N:B films (b) Fowler-Nordheim (F-N) plots of the a-C:N and a-C:N:B films....74
Fig. 6.7 AFM 3D image of the (a) a-C:N film and (b) a-C:N:B film…..77
Fig. 7.1 The chemical formulas of Polyethylene terephthalate…………79
Fig. 7.2 Typical top-view SEM image for the (a) a-C:F films and (b) a-C:F NPs films…………………………………………………..82
Fig. 7.3 The growth mechanism of a-C:F films and a-C:F nanoparticles films………………………………………………………………83
Fig. 7.4 AFM 3D image of the (a) PET and (b) a-C:F NPs films coated on PET…………………………………..………….………………..84
Fig. 7.5 XPS survey scan spectra for the film at various CF4 flows of 20, 30, 40, 50 and 60 sccm……………………….…………………..86
Fig. 7.6 Typical core level XPS spectra of the a-C:F films formed at various CF4 flows of 20, 30, 40, 50 and 60 sccm (a) C(1s) and (b) F(1s)……………………………………………………………...87
Fig. 7.7 MAC glancing incident X-ray pattern of (a) the PET substrates and (b) the a-C:F NPs films coated on PET……………………...89
Fig. 7.8 Differences in the Raman spectroscopy of the PET and a-C:F NPs films coated on PET……………….………………………..89
Fig. 7.9 (a) CL spectra of a-C:F films synthesized at various CF4 flows of 20, 30, 40, 50 and 60 sccm at 300K (b) The relation of the orange light intensity (Iorange) and red light intensity (Ired) emitted by a-C:F films, and the ratio (Iorange/Ired) with various CF4 flows…………….92

                                

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