請用此 Handle URI 來引用此文件：
http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/58537完整後設資料紀錄
| DC 欄位 | 值 | 語言 |
|---|---|---|
| dc.contributor.advisor | 黃慶怡 | |
| dc.contributor.author | Cheng-kai Chang | en |
| dc.contributor.author | 張政凱 | zh_TW |
| dc.date.accessioned | 2021-06-16T08:18:59Z | - |
| dc.date.available | 2019-03-08 | |
| dc.date.copyright | 2014-03-08 | |
| dc.date.issued | 2014 | |
| dc.date.submitted | 2014-02-10 | |
| dc.identifier.citation | Chapter 1
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H.; Ni, J.; Kvashnin, A. G.; Kvashnin, D. G.; Lou, J.; Yakobson, B. I.; Ajayan, P. M., Large Scale Growth and Characterization of Atomic Hexagonal Boron Nitride Layers. Nano Lett 2010, 10 (8), 3209-3215. 8. Shi, Y. M.; Hamsen, C.; Jia, X. T.; Kim, K. K.; Reina, A.; Hofmann, M.; Hsu, A. L.; Zhang, K.; Li, H. N.; Juang, Z. Y.; Dresselhaus, M. S.; Li, L. J.; Kong, J., Synthesis of Few-Layer Hexagonal Boron Nitride Thin Film by Chemical Vapor Deposition. Nano Lett 2010, 10 (10), 4134-4139. 9. Ci, L.; Song, L.; Jin, C. H.; Jariwala, D.; Wu, D. X.; Li, Y. J.; Srivastava, A.; Wang, Z. F.; Storr, K.; Balicas, L.; Liu, F.; Ajayan, P. M., Atomic layers of hybridized boron nitride and graphene domains. Nat Mater 2010, 9 (5), 430-435. 10. Chen, L. C.; Hwang, J. Y.; Kuo, C. C.; Chen, K. H., Correlating defect density with carrier mobility in large-scaled graphene films: Raman spectral signatures for the estimation of defect density. Nanotechnology 2010, 21 (46). 11. Lei, W.; Portehault, D.; Dimova, R.; Antoniettit, M., Boron Carbon Nitride Nanostructures from Salt Melts: Tunable Water-Soluble Phosphors. J Am Chem Soc 2011, 133 (18), 7121-7127. 12. Kawaguchi, M., B/C/N materials based on the graphite network. Advanced Materials 1997, 9 (8), 615-625. 13. Ozaki, J.; Kimura, N.; Anahara, T.; Oya, A., Preparation and oxygen reduction activity of BN-doped carbons. Carbon 2007, 45 (9), 1847-1853. 14. Ismach, A.; Chou, H.; Ferrer, D. A.; Wu, Y. P.; McDonnell, S.; Floresca, H. C.; Covacevich, A.; Pope, C.; Piner, R.; Kim, M. J.; Wallace, R. M.; Colombo, L.; Ruoff, R. S., Toward the Controlled Synthesis of Hexagonal Boron Nitride Films. Acs Nano 2012, 6 (7), 6378-6385. 15. Moulder, J.; Stickle, W.; Sobol, P.; Bomben, K., Handbook of X-ray Photoelectron Spectroscopy. Physical Electronics, Inc.: Eden Prairie, Minnesota, USA, 1995. 16. Ferrari, A. C., Raman spectroscopy of graphene and graphite: Disorder, electron-phonon coupling, doping and nonadiabatic effects. Solid State Commun 2007, 143 (1-2), 47-57. 17. Cancado, L. G.; Jorio, A.; Ferreira, E. H. M.; Stavale, F.; Achete, C. A.; Capaz, R. B.; Moutinho, M. V. O.; Lombardo, A.; Kulmala, T. S.; Ferrari, A. C., Quantifying Defects in Graphene via Raman Spectroscopy at Different Excitation Energies. Nano Lett 2011, 11 (8), 3190-3196. 18. Ni, Z. H.; Ponomarenko, L. A.; Nair, R. R.; Yang, R.; Anissimova, S.; Grigorieva, I. V.; Schedin, F.; Blake, P.; Shen, Z. X.; Hill, E. H.; Novoselov, K. S.; Geim, A. K., On Resonant Scatterers As a Factor Limiting Carrier Mobility in Graphene. Nano Lett 2010, 10 (10), 3868-3872. 19. Frueh, S.; Kellett, R.; Mallery, C.; Molter, T.; Willis, W. S.; King'ondu, C.; Suib, S. L., Pyrolytic Decomposition of Ammonia Borane to Boron Nitride. Inorganic chemistry 2011, 50 (3), 783-792. 20. Kim, K. K.; Hsu, A.; Jia, X. T.; Kim, S. M.; Shi, Y. S.; Hofmann, M.; Nezich, D.; Rodriguez-Nieva, J. F.; Dresselhaus, M.; Palacios, T.; Kong, J., Synthesis of Monolayer Hexagonal Boron Nitride on Cu Foil Using Chemical Vapor Deposition. Nano Lett 2012, 12 (1), 161-166. 21. Brito, W. H.; Kagimura, R.; Miwa, R. H., B and N doping in graphene ruled by grain boundary defects. Phys Rev B 2012, 85 (3). 22. Sutter, P.; Cortes, R.; Lahiri, J.; Sutter, E., Interface Formation in Monolayer Graphene-Boron Nitride Heterostructures. Nano Lett 2012, 12 (9), 4869-4874. | |
| dc.identifier.uri | http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/58537 | - |
| dc.description.abstract | Defects in the CVD-derived graphene have been demonstrated to have great impacts on its optical and electrical properties. In this study, we engineered the defects in graphene by the process control in the thermal chemical vapor deposition (CVD) and by doping in both substitutional and chemical approaches.
First of all, a series of graphene with different degrees of structure disorder were produced by changing the growth conditions in the CVD process. Two stages, nanocrystallization and amorphization, of amorphization trajectory for CVD-graphene were introduced and the corresponding evolution of Raman line position, line width and intensity were monitored. At the stage of nanocrystallization, grain boundaries increase and both G and 2D peaks show blue-shift. 2D peak has much larger variation than G peak, which implies the change in the paths of phonon scattering due to the variation of the electronic structure. The high I2D/IG ratio indicates the hexagonal structure of graphene is still maintained. At the stage of amorphization, the broadened D and G peaks, dramatic drop of 2D intensity, and the great upshift in G peak position indicate the localized collapse of graphitized structure due to the incorporation of amorphous phases. Secondly, the conducting polymer, PANI, was physically doped on the graphene by a self-assemble method. The PANI-modified graphene shows a dramatic decrease in its sheet resistance from ~2500 Ω/sq to ~550 Ω/sq, while maintaining its transmittance at 96%. The work function of PANI-modified graphene is comparable to that of graphite. The recovery of the sheet resistance was also observed in defected graphene. The PANI-modified process is simple, green, and scalable. It is highly appropriate for the transparent conductivity film (TCF) application. Thirdly, band gap opening and engineering is one of the high priority goal in the development of graphene electronics. To create a band gap, we co-doped B and N in large-scaled graphene films (BNG) by low-pressure chemical vapor deposition. TEM images and EELS results indicate that the segregated BN domains appeared when the concentration was over 8%. Below this concentration, BN will disperse uniformly in the graphene lattice. Based on the synchrotron-radiation XAS-XES measurements, a significant band gap (600 meV) was observed in low-BN-doped graphene which is attributed to the opening of band gap of graphene. The results of field effect transistor measurements also confirmed that the semiconductor behavior in BN-doped graphene. | en |
| dc.description.provenance | Made available in DSpace on 2021-06-16T08:18:59Z (GMT). No. of bitstreams: 1 ntu-103-D98549001-1.pdf: 4567961 bytes, checksum: 30421c6001598e5b08e736d38e6e7c5f (MD5) Previous issue date: 2014 | en |
| dc.description.tableofcontents | Table of Contents
誌謝 I 摘要 II Abstract IV Chapter 1 History of graphene 1 1.1 Preface 1 1.2 Roadmap of graphene 4 1.3 Scope of the thesis 5 1.4 Reference 6 Chapter 2 Graphene related synthesis, theories and mechanisms 8 2.1 Synthesis of graphene 9 2.1.1 Mechanically cleaved graphene 9 2.1.2 CVD-graphene 9 2.1.3 Reduced graphene oxide 10 2.2 Properties of graphene 11 2.2.1 Electrical property 11 2.2.2 Optical property 13 2.3 Raman characterization 15 2.3.1 D band of graphene 15 2.3.2 G band of graphene 16 2.3.2.1 Peak position and FWHM as a function of doping level 17 2.3.2.2 Temperature dependence 20 2.3.3 2D band of graphene 22 2.4 Doping effect 24 2.4.1 Chemical doping 24 2.4.2 Substitutional doping 26 2.5 Reference 29 Chapter 3 Experimental 37 3.1 Material sources 37 3.2 Preparation procedure for graphene 38 3.2.1 Furnace 38 3.2.2 Transfer process 39 3.3 Characterization of composites 40 3.3.1 Absorption spectroscopy 40 3.3.2 Raman spectroscopy 40 3.3.3 X-ray photoelectron spectroscopy (XPS) 41 3.3.4 Ultraviolet photoelectron spectroscopy (UPS) 41 3.3.5 X-ray absorption (XAS) and emission (XES) spectra 41 3.3.6 Fouier transform infrared (FTIR) 42 3.3.7 Auger electron spectroscopy (AES) 42 3.3.8 Hall measurement 42 3.3.9 Field effect transistor (FET) 43 3.4 Morphology 44 3.4.1Transmission electron microscopy (TEM) 44 3.4.2 Atomic force microscopy (AFM) 44 3.5 Computer simulations 45 Chapter 4 Correlating defect density in CVD-graphene by Raman study 46 4.1 Characterization of CVD graphene with different defect density 46 4.2 Copper analysis by Auger electron spectroscopy (AES) 50 4.3 Morphology of CVD-graphene on copper 53 4.4 Different defect density of graphene 55 4.5 Temperature-dependent Raman spectra 67 4.6 Remark 72 4.7 Reference 73 Chapter 5 Chemical doping: self-assembly of polyaniline on CVD-graphene: a scalable production of transparent conducting films with enhanced electrical property 79 5.1 Introduction of chemical doping 79 5.2 PANI-modified graphene preparation 81 5.3 Identification PANI-modified graphene by optical analysis 83 5.4 Charge distribution calculation 87 5.5 Raman characterization of PANI-modified with difference modification time 90 5.6 Electronic property measurement 93 5.7 Transmittance and sheet resistance measurement on PANI/grapheme with different defect density 94 5.8 Remark 96 5.9 Reference 97 Chapter 6 Substituent doping: B and N co-doped graphene for band gap engineering 100 6.1 Introduction 100 6.2 Experimental process 102 6.2.1 Temperature control of precursor 103 6.2.1 Flow rate control of methane at the same temperature of the precursor 104 6.3 Results and Discussion 105 6.3.1 Identification of BN quantity 105 6.3.2 Raman characterization of graphene & BNG 109 6.3.3 Optical band gap analysis 113 6.3.4 Transmission electron microscopy analysis 115 6.3.5 Map the band gap by XES & XAS 121 6.3.5 Electrical characterization by the field effect device 123 6.4 Remark 127 6.5 Reference 128 Chapter 7 Conclusion 132 Figures Figure 1.1 Related material of graphene 2 Figure 1.2 Number of publication on graphene as a function of years 3 Figure 1.3 Graphene applications as a function of year 4 Figure 2.1 Electrical properties of graphene (a-d) and conventional two dimensional systems (e–i) 13 Figure 2.2 Plot of the transmittance with monolayer and bilayer graphene 14 Figure 2.3 Plot of the transmittance as a function of wavelength with number of layers 14 Figure 2.4 D band inelastic scattering process 16 Figure 2.5 Phonon dispersion curves of simulation (lines) and experimental (points) 17 Figure 2.6 (a) The diagram of the experiment. The black dotted on graphene (blue stripe), which is the polymer electrolyte (PEO t LiClO4). The left image shows the optical image of a single-layer graphene and drain gold electrodes. Scale bar: 5 mm. The right cartoon is the illustration of the top gating, with Li+ (magenta) and ClO4 - (cyan) ions and the Debye layers. (b) Position of the G band, (c) FWHM of G band, (d) 2D/G ratio as a function of the electron concentration 19 Figure 2.7 (a) Optical image of th exfoliated graphene on the SiO2. (b) Raman spectra of the monolayer graphene sample of (a), the suspended graphene (red solid line) and supported graphene (blue dashed line). (c) Defect reign of graphene on Raman spectra. (d) Detailed comparison of the G mode, both for suspend and support graphene. The red open circles and blue open squares, for suspended and supported graphene, are the experiment data, respectively. On the side, the solid lines are fit with Voigt profiles. 20 Figure 2.8 Temperature dependence as a function of the G band for the single- (a) and bilayer (b) graphene. The insets show G band 21 Figure 2.9 Double resonance process of 2D band 23 Figure 2.10 Gases sensitivity of graphene 26 Figure 3.1 Schematic diagram of the experimental setup 38 Figure 3.2 Methodology used for the deposition of graphene 39 Figure 3.3 Transfer process of graphene 39 Figure 4.1 AES spectra of Cu foil obtained at different temperatures 51 Figure 4.2 AES spectra of Cu foil depicting the evolution of (a) S, (b) C, (c) N and (d) O regions with temperature 51 Figure 4.3 AES spectra of Cu foil after annealing at 1000 C for two days 52 Figure 4.4 The (a,b) SEM and (c) AFM images of CVD-graphene showing wrinkled structure. The scale bar for SEM images is 300 nm and the AFM image is 5 × 5m 54 Figure 4.5 (a,b) AFM images of CVD-graphene on Cu foil (before transfer). (c) Schematic showing the possible mechanism how wrinkled structure formed after transfer process. (d) Cross-sessional analysis of the graphene/Cu along the white line in (b). The AFM images are (a) 10 × 10 um and (b) 3 × 3 um, respectively. 54 Figure 4.6 A series of Raman spectra proving the amorphization trajectory, ranging from single crystal graphene (MCG) to amorphous graphene. 55 Figure 4.7 Illustration of amorphization trajectory for CVD-graphene. The nanocrystallization stage describes the single-crystal graphene (MCG) evolves into multi-crystal graphene (LDG and HDG); the amorphization stage depicts the process of incorporation of large amount of amorphous phase 59 Figure 4.8 Optical images along with Raman contour plots of MCG (upper row), LDG (middle row), and HDG (bottom row), respectively. The Raman images were plotted using fitted parameters of ID/IG ratio, I2D/IG ratio, and width(2D), as noted at the corner of each plots. The red arrows in MCG image indicate multilayer areas and the black arrows in CVD-graphene suggest the wrinkled structures formed during transfer process 62 Figure 4.9 Plots of (a,d), position(2D) (b,e), width(G), and (c,f) I2D/IG ratio as a function of position(G). The left-hand parts used fitted parameters from spatial mapping of four samples, and the right-hand parts compared the data of different produced samples 66 Figure 4.10 Temperature dependence of the G peak position for (■) MCG, (○) LDG, and (◇) LAG. The lines are the linear fitting of data of each group and the fitted slopes were extracted as the temperature coefficient 69 Figure 5.1 Schematic diagram of the PANI synthesizing process 81 Figure 5.2 Schematic illustration of the graphene transferring process and the subsequent modification of PANI 82 Figure 5.3 The FTIR spectra of pristine PANI and PANI-graphene. The pristine PANI was powder prepared by chemical polymerization 84 Figure 5.4 XPS spectra of (a) C1s and (b) N1s core levels for PANI-graphene. The black lines are raw data and red lines are fitting spectra 85 Figure 5.5 UPS spectra of graphene and PANI-graphene 86 Figure 5.6 The electronic structure and the charge redistribution diagram of pristine PANI/graphene system 88 Figure 5.7 The amount of the charge transfer from graphene against PANI doping level represented by the number of chlorine ions (Cl-) per unit cell 89 Figure 5.8 (a) Raman spectra of pristine graphene, pristine PANI and PANI-graphene with different modification time. The evolution of Raman parameters of (b) G peak position, (c) 2D peak position, and (d) 2D/G intensity ration 92 Figure 5.9 The sheet resistance as a function of PANI modification time 93 Figure 5.10 Transmittance measurement of graphene films in visible region. Inset figure shows Raman spectrum of graphene with different defect density (a) lower quality (b) high quality 95 Figure 6.1 (a) Schematic diagram of the experimental set up used in the present study. (b) Methodology used for the deposition of BNG films 102 Figure 6.2 BN concentration versus precursor temperature 103 Figure 6.3 BN concentration versus methane flow rate 104 Figure 6.4 Typical XPS spectra of (a) C 1s, (b) N 1s and (c) B 1s core levels for 8BNG film. The empty circles are raw data and solid lines are the fitted spectra. (d) N 1s spectra for different BNG films as a function of increasing BN concentration. Dashed lines are guide to eyes 108 Figure 6.5 Typical AES spectra for 2BNG sample 109 Figure 6.6 (a) Raman spectra of BNG films acquired using 633 nm wavelength laser. Raman area mapping of ID/IG ratio for (b) 2BNG and (c) 6BNG films 112 Figure 6.7 UV-Raman spectra of 27BNG films 113 Figure 6.8 UV-vis spectra for different BNG films depicting the evolution of h-BN phase 114 Figure 6.9 Tauc's plot for pristine graphene and BNG films 115 Figure 6.10 EELS analysis of (a) 2BNG and (b) 8 BNG film 117 Figure 6.11 (a) High-resolution TEM image of a BNG film showing the layer number, and the inset represents the electron diffraction pattern taken at the corresponding region. (b) High resolution TEM image of 2BNG sample with Fast-Fourier Transform (FFT) in the inset showing only graphene crystalline structure (c) High resolution TEM image of 8BNG sample depicting the distribution of h-BN domains (encircled regions) in graphene. The inset is FFT of the image indicating the presence of crystalline domains of both graphene and h-BN. (Scale Bar is 5 nm). (d) Schematic diagram depicting the structural evolution in BNG films with increase in BN concentration. Carbon, nitrogen and boron atoms are represented by black, red and blue circles, respectively 118 Figure 6.12 EELS mapping for C, B and N in 8BNG sample 119 Figure 6.13 (a) XPS spectra of N1s peak and (b) Raman spectra of BNG smaples grown at different flow rates of CH4 120 Figure 6.14 XES and XAS spectra of HOPG, pristine graphene and BNG films. A band gap of around 600 meV is observed for 6BNG sample 123 Figure 6.15 (a) Resistance versus temperature curve for pristine graphene and 2BNG film. Plot of Ids as a function of Vg at Vds = 1 V for back gated FET device for (b) pristine graphene and (c) 2BNG sample at different temperatures. All measurements were carried out in a vacuum of the order of 10-4 mbar 125 Tables Table 4-1 The fitted Raman parameters of MCG and CVD-graphene with different degree of disorder showing the structural evolution stages. The average and standard deviation were given from fitted parameters of Raman spectra obtained from different regions and different produced samples 70 Table 4-2 Temperature coefficient for CVD-graphene and other carbon materials 71 Table 5-1 The sheet resistance and transmittance of pristine graphene and PANI-graphene with both defect density 95 Table 6- 1 Defect density and crystallite size in BNG films calculated using ID/IG ratio obtained from Raman spectra 126 | |
| dc.language.iso | en | |
| dc.title | 化學氣相沉積石墨烯之缺陷調控：製程控制與摻雜效應 | zh_TW |
| dc.title | Defect Engineering of CVD-graphene: Process Control and Doping Effects | en |
| dc.type | Thesis | |
| dc.date.schoolyear | 102-1 | |
| dc.description.degree | 博士 | |
| dc.contributor.coadvisor | 陳貴賢,林麗瓊(chenlc@ntu.edu.tw) | |
| dc.contributor.oralexamcommittee | 陳俊維(chunwei@ntu.edu.tw),陳瑞山,黃智賢 | |
| dc.subject.keyword | 石墨烯,拉曼,摻雜效應,導電薄膜,半導體, | zh_TW |
| dc.subject.keyword | graphene,Raman,doping effect,transparent conductivity film,semiconductor, | en |
| dc.relation.page | 133 | |
| dc.rights.note | 有償授權 | |
| dc.date.accepted | 2014-02-10 | |
| dc.contributor.author-college | 工學院 | zh_TW |
| dc.contributor.author-dept | 高分子科學與工程學研究所 | zh_TW |
| 顯示於系所單位： | 高分子科學與工程學研究所 | |
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