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Graphene: Properties, Preparation, Characterisation and Devices
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Graphene: Properties, Preparation, Characterisation and Devices reviews the preparation and properties of this exciting material. Graphene is a single-atom-thick sheet of carbon with properties, such as the ability to conduct light and electrons, which could make it potentially suitable for a variety of devices and applications, including electronics, sensors, and photonics.
Chapters in part one explore the preparation of , including epitaxial growth of graphene on silicon carbide, chemical vapor deposition (CVD) growth of graphene films, chemically derived graphene, and graphene produced by electrochemical exfoliation. Part two focuses on the characterization of graphene using techniques including transmission electron microscopy (TEM), scanning tunneling microscopy (STM), and Raman spectroscopy. These chapters also discuss photoemission of low dimensional carbon systems. Finally, chapters in part three discuss electronic transport properties of graphene and graphene devices. This part highlights electronic transport in bilayer graphene, single charge transport, and the effect of adsorbents on electronic transport in graphene. It also explores graphene spintronics and nano-electro-mechanics (NEMS).
Graphene is a comprehensive resource for academics, materials scientists, and electrical engineers working in the microelectronics and optoelectronics industries.
Explores the graphene preparation techniques, including epitaxial growth on silicon carbide, chemical vapor deposition (CVD), chemical derivation, and electrochemical exfoliation Focuses on the characterization of graphene using transmission electron microscopy (TEM), scanning tunneling microscopy (STM), and Raman spectroscopy A comprehensive resource for academics, materials scientists, and electrical engineersAcțiuni carte
Începeți să citițiInformații despre carte
Graphene: Properties, Preparation, Characterisation and Devices
Până la Elsevier Science
Descriere
Graphene: Properties, Preparation, Characterisation and Devices reviews the preparation and properties of this exciting material. Graphene is a single-atom-thick sheet of carbon with properties, such as the ability to conduct light and electrons, which could make it potentially suitable for a variety of devices and applications, including electronics, sensors, and photonics.
Chapters in part one explore the preparation of , including epitaxial growth of graphene on silicon carbide, chemical vapor deposition (CVD) growth of graphene films, chemically derived graphene, and graphene produced by electrochemical exfoliation. Part two focuses on the characterization of graphene using techniques including transmission electron microscopy (TEM), scanning tunneling microscopy (STM), and Raman spectroscopy. These chapters also discuss photoemission of low dimensional carbon systems. Finally, chapters in part three discuss electronic transport properties of graphene and graphene devices. This part highlights electronic transport in bilayer graphene, single charge transport, and the effect of adsorbents on electronic transport in graphene. It also explores graphene spintronics and nano-electro-mechanics (NEMS).
Graphene is a comprehensive resource for academics, materials scientists, and electrical engineers working in the microelectronics and optoelectronics industries.
Explores the graphene preparation techniques, including epitaxial growth on silicon carbide, chemical vapor deposition (CVD), chemical derivation, and electrochemical exfoliation Focuses on the characterization of graphene using transmission electron microscopy (TEM), scanning tunneling microscopy (STM), and Raman spectroscopy A comprehensive resource for academics, materials scientists, and electrical engineersMostră carte
Graphene
Graphene
Properties, preparation, characterisation and devices
Edited by
Viera Skákalová
Alan B. Kaiser
Table of Contents
Cover image
Title page
Copyright
Contributor contact details
Woodhead Publishing Series in Electronic and Optical Materials
Preface
Part I: Preparation of graphene
1. Epitaxial growth of graphene on silicon carbide (SiC)
Abstract:
1.1 Introduction
1.2 Ultrahigh vacuum (UHV) thermal decomposition of single-crystal SiC
1.3 Thermal decomposition of single-crystal SiC under ambient pressure conditions
1.4 Thermal decomposition of single-crystal SiC thin films and polycrystalline SiC substrates
1.5 Epitaxial graphene formed by intercalation
1.6 Conclusion
1.7 Acknowledgements
1.8 References
2. Chemical vapor deposition (CVD) growth of graphene films
Abstract:
2.1 Introduction
2.2 Chemical vapor deposition (CVD) on nickel
2.3 Graphene with large domain sizes on copper
2.4 Growth on copper single crystals
2.5 Periodically stacked multilayers
2.6 Isotope labeling of CVD graphene
2.7 Conclusion
2.8 Acknowledgment
2.9 References
3. Chemically derived graphene
Abstract:
3.1 Introduction
3.2 Synthesis of graphene oxide (GO)
3.3 Reduction of graphene oxide (GO)
3.4 Physicochemical structure of graphene oxide (GO)
3.5 Electrical transport in graphene oxide (GO)
3.6 Applications of graphene oxide/reduced graphene oxide (GO/RGO)
3.7 Conclusion
3.8 Acknowledgements
3.9 References
4. Graphene produced by electrochemical exfoliation
Abstract:
4.1 Introduction
4.2 Synthesis of graphene by electrochemical exfoliation: a basic concept
4.3 Applications of graphene and graphene-based materials
4.4 Conclusion
4.5 Acknowledgments
4.6 References
Part II: Characterisation of graphene
5. Transmission electron microscopy (TEM) of graphene
Abstract:
5.1 Introduction
5.2 Graphene structure basics
5.3 Electron diffraction analysis of graphene
5.4 Graphene and defects in graphene observed by aberration-corrected transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM)
5.5 Insights from electron microscopic studies of graphene
5.6 Conclusion
5.7 References
6. Scanning tunneling microscopy (STM) of graphene
Abstract:
6.1 Introduction
6.2 Morphology, perfection and electronic structure of graphene flakes deposited on inert substrates
6.3 Morphology, perfection and electronic structure of graphene epitaxially grown on semiconductor and metallic substrates
6.4 Scanning tunneling microscopy (STM)/scanning tunneling spectroscopy (STS) of point defects
6.5 STM/STS on graphene nanoribbons (GNR)
6.6 Conclusion
6.7 References
7. Raman spectroscopy of graphene
Abstract:
7.1 Introduction
7.2 Principles of Raman scattering
7.3 Phonons in graphene
7.4 Electronic structure of graphene
7.5 Raman spectrum of graphene
7.6 Conclusion
7.7 Acknowledgement
7.8 References
8. Photoemission of low-dimensional carbon systems
Abstract:
8.1 Introduction
8.2 Photoemission spectroscopy
8.3 Accessing the electronic properties of carbon sp² hybridized systems: the C1s core level
8.4 Chemical state identification: inspection of bonding environments
8.5 Valence-band electronic structure
8.6 Conclusion
8.7 Acknowledgements
8.8 References
Part III: Electronic transport properties of graphene and graphene devices
9. Electronic transport in graphene: towards high mobility
Abstract:
9.1 Introduction
9.2 Metrics for scattering strength
9.3 Methods of graphene synthesis
9.4 Sources of scattering in graphene
9.5 Approaches to increase carrier mobility
9.6 Physical phenomena in high-mobility graphene
9.7 Conclusion
9.8 Acknowledgments
9.9 References
10. Electronic transport in bilayer graphene
Abstract:
10.1 Introduction
10.2 Historical development of bilayer graphene
10.3 Transport properties in bilayer graphene systems
10.4 Many-body effects of transport properties in bilayer graphene
10.5 Conclusion
10.6 References
11. Effect of adsorbents on electronic transport in graphene
Abstract:
11.1 Introduction
11.2 Interaction of adsorbates with graphene
11.3 Transfer-induced metal and molecule adsorptions
11.4 Influence of adsorbates on graphene field-effect transistors
11.5 Removal of polymer residues on graphene
11.6 Conclusion
11.7 References
12. Single-charge transport in graphene
Abstract:
12.1 Introduction
12.2 Single-charge tunneling
12.3 Electrical properties of graphene
12.4 Single-charge tunneling in graphene
12.5 Charge localization in graphene
12.6 Conclusion
12.7 References
13. Graphene spintronics
Abstract:
13.1 Introduction
13.2 Theories and important concepts
13.3 Experiments for generating pure spin current and the physical properties of pure spin current
13.4 Conclusion and future trends
13.5 References
14. Graphene nanoelectromechanics (NEMS)
Abstract:
14.1 Introduction
14.2 Graphene versus silicon
14.3 Graphene mechanical attributes
14.4 Fabrication technology for graphene microelectromechanical systems (MEMS)
14.5 Graphene nanoresonators
14.6 Graphene nanomechanical sensors
14.7 Conclusion and future trends
14.8 References
Index
Copyright
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Contributor contact details
(* = main contact)
Editors
Viera Skákalová*
University of Vienna, Faculty of Physics, Physics of Nanostructured Materials, Boltzmanngasse 5, 1090 Vienna, Austria
E-mail: viera.skakalova@univie.ac.at
Alan B. Kaiser
MacDiarmid Institute for Advanced Materials and Nanotechnology, School of Chemical and Physical Sciences, Victoria University of Wellington, Kelburn Parade, Wellington, New Zealand
E-mail: Alan.Kaiser@vuw.ac.nz
Chapter 1
Han Huang, Andrew Thye Shen Wee
Department of Physics, National University of Singapore, 2 Science Drive 3, Singapore, 117542
Shi Chen
Division of Physics and Applied Physics, Nanyang Technological University, 21 Nanyang Link, Singapore 637371
Wei Chen*
Department of Physics and Department of Chemistry, National University of Singapore, 2 Science Drive 3, Singapore, 117542
E-mail: phycw@nus.edu.sg
Chapter 2
Otakar Frank
Department of Electrochemical Materials, J. Heyrovsky Institute of Physical Chemistry of the AS CR, v. v. i., Dolejskova 2155/3, Prague 8, CZ-182 23, Czech Republic
E-mail: otakar.frank@jh-inst.cas.cz
Martin Kalbac*
Department of Low-Dimensional Systems, J. Heyrovsky Institute of Physical Chemistry of the AS CR, v. v. i., Dolejskova 2155/3, Prague 8, CZ-182 23, Czech Republic
E-mail: martin.kalbac@jh-inst.cas.cz
Chapter 3
Ravi S. Sundaram
University of Cambridge, Center for Advanced Photonics and Electronics, 9 JJ Thomson Avenue, CB3 0FA, Cambridge, UK
E-mail: rss55@cam.ac.uk
Chapter 4
Saswata Bose, Tapas Kuila, Nam Hoon Kim, Joong Hee Lee*
Department of BIN Fusion Technology and Department of Polymer Nano Science and Technology, Chonbuk National University, Jeonju, Jeonbuk, 561-756, Republic of Korea
E-mail: jhl@chonbuk.ac.kr; jhl@jbnu.ac.kr
Chapter 5
Jannik C. Meyer
University of Vienna, Faculty of Physics, Physics of Nanostructured materials, Boltzmanngasse 5, 1090 Vienna, Austria
E-mail: Jannik.meyer@univie.ac.at
Chapter 6
Amadeo L. Vázquez de Parga*, Rodolfo Miranda
Condensed Matter Physics Department, Autonomous University of Madrid, Cantoblanco 28049, Madrid, Spain
Madrid Institute for Advanced Studies in Nanoscience (IMDEA-Nanociencia), Cantoblanco 28049, Madrid, Spain
E-mail: al.vazquezdeparga@uam.es; rodolfo.miranda@imdea.org
Chapter 7
Martin Hulman
International Laser Center and Danubia NanoTech, Ilkovičova 3, 841 04 Bratislava, Slovak Republic
E-mail: hulman@ilc.sk
Chapter 8
Paola Ayala
University of Vienna, Faculty of Physics, Strudlhofgasse 4, A-1090 Vienna, Austria
E-mail: paola.ayala@univie.ac.at
Chapter 9
Kirill Bolotin
Physics & Astronomy Department, Vanderbilt University, 2401 Vanderbilt Place, Nashville, TN 37240-1807, USA
E-mail: kirill.bolotin@vanderbilt.edu
Chapter 10
Reza Asgari
Institute for Research in Fundamental Sciences (IPM), School of Physics, Tehran, 19395-5531, Iran
E-mail: asgari@ipm.ir
Chapter 11
Yung Chang Lin*, Po Wen Chiu
Department of Electrical Engineering, National Tsing Hua University, 101 Kuang-Fu Rd., Sec. 2, 30013 Hsinchu, Taiwan, Republic of China
E-mail: yclin0827@gmail.com; pwchiu@ee.nthu.edu.tw
Chapter 12
Dong Su Lee
Soft Innovative Materials Research Center, Korea Institute of Science and Technology (KIST), Eunha-ri San 101, Bongdong-eup, Wanju-gun, Jeonbuk 565–905, South Korea
E-mail: d.s.lee@kist.re.kr
Chapter 13
Masashi Shiraishi
Department of Electronic Science and Engineering, Kyoto University, Kyoto-Daigaku-Katsura, Nishigyo-ku, Kyoto 615-8510, Japan
E-mail: shiraishi@ee.es.osaka-u.ac.jp
Chapter 14
Zakaria Moktadir
Southampton University, Highfield SO17 1BJ, Southampton, UK
E-mail: zm@ecs.soton.ac.uk
Woodhead Publishing Series in Electronic and Optical Materials
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2 Signal processing in electronic communications: For engineers and mathematicians
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6 Designing a structured cabling system to ISO 11801: Cross-referenced to European CENELEC and American Standards Second edition
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7 Microscopy techniques for materials science
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8 Materials for energy conversion devices
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9 Digital image processing: Mathematical and computational methods Second edition
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10 Nanolithography and patterning techniques in microelectronics
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11 Digital signal processing: Mathematical and computational methods, software development and applications Second edition
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13 Materials for fuel cells
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14 Solid-state hydrogen storage: Materials and chemistry
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15 Laser cooling of solids
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Edited by C. A. C. Sequeira and D. A. F. Santos
17 Advanced piezoelectric materials: Science and technology
Edited by K. Uchino
18 Optical switches: Materials and design
Edited by S. J. Chua and B. Li
19 Advanced adhesives in electronics: Materials, properties and applications
Edited by M. O. Alam and C. Bailey
20 Thin film growth: Physics, materials science and applications
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21 Electromigration in thin films and electronic devices: Materials and reliability
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22 In situ characterization of thin film growth
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23 Silicon–germanium (SiGe) nanostructures: Production, properties and applications in electronics
Edited by Y. Shiraki and N. Usami
24 High-temperature superconductors
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25 Introduction to the physics of nanoelectronics
S. G. Tan and M. B. A. Jalil
26 Printed films: Materials science and applications in sensors, electronics and photonics
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27 Laser growth and processing of photonic devices
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28 Quantum optics with semiconductor nanostructures
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29 Ultrasonic transducers: Materials and design for sensors, actuators and medical applications
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30 Waste electrical and electronic equipment (WEEE) handbook
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32 MEMS for automotive and aerospace applications
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33 Semiconductor lasers: Fundamentals and applications
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34 Handbook of terahertz technology for imaging, sensing and communications
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35 Handbook of solid-state lasers: Materials, systems and applications
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36 Organic light-emitting diodes (OLEDs): Materials, devices and applications
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37 Lasers for medical applications: Diagnostics, therapy and surgery
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38 Semiconductor gas sensors
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39 Handbook of organic materials for optical and (opto)electronic devices: Properties and applications
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40 Metallic films for electronic, optical and magnetic applications: Structure, processing and properties
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41 Handbook of laser welding technologies
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42 Nanolithography: The art of fabricating nanoelectronic and nanophotonic devices and systems
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43 Laser spectroscopy for sensing: Fundamentals, techniques and applications
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44 Chalcogenide glasses: Preparation, properties and applications
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45 Handbook of MEMS for wireless and mobile applications
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46 Subsea optics and imaging
Edited by J. Watson and O. Zielinski
47 Carbon nanotubes and graphene for photonic applications
Edited by S. Yamashita, Y. Saito and J. H. Choi
48 Optical biomimetics: Materials and applications
Edited by M. Large
49 Optical thin films and coatings
Edited by A. Piegari and F. Flory
50 Computer design of diffractive optics
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51 Smart sensors and MEMS: Intelligent devices and microsystems for industrial applications
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52 Fundamentals of femtosecond optics
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53 Nanostructured semiconductor oxides for the next generation of electronics and functional devices: Properties and applications
S. Zhuiykov
54 Nitride semiconductor light-emitting diodes (LEDs): Materials, technologies and applications
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56 Sensor technologies for civil infrastructures Volume 2: Applications in structural health monitoring
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57 Graphene: Properties, preparation, characterisation and devices
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58 Silicon-on-insulator (SOI) technology
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59 Biological identification: DNA amplification and sequencing, optical sensing, lab-on-chip and portable systems
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60 High-performance silicon imaging: Fundamentals and applications of CMOS and CCD sensors
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61 Nanosensors for chemical and biological applications: Sensing with nanotubes, nanowires and nanoparticles
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62 Composite magnetoelectrics: Materials, structures, and applications
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64 Advances in non-volatile memory and storage technology
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65 Laser surface engineering: Processes and applications
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Preface
Graphene burst onto the world science scene as the new miracle material in 2004. It caught the imagination of the general public as well as materials scientists. Who would have thought 50 years ago that it would possible to image a single layer of atoms?
The excitement of the discovery was reminiscent of the discovery of high-temperature superconductors in 1986, with hundreds of scientists trying to push the superconducting onset temperature Tc up to room temperature. Alex Müller and Georg Bednorz took the record for the fastest Nobel Prize when they were awarded the Nobel Prize for Physics the following year (1987). Unfortunately, Tc never got to room temperature (at least so far), although high-Tc superconductors are in service in many practical applications.
The Nobel Prize for graphene to Andrei Geim and Kostya Novoselov was not so immediate, but at 6 years after their discovery it was still unusually rapid. As is usually the case, other groups were working at the same time to achieve the same goal. Here the goal was separating from a graphite crystal just a single plane, the now familiar hexagonal pattern of a single layer of carbon atoms. One of the promising ideas considered at Columbia University by Philip Kim’s group was using an Atomic Force Microscopy (AFM) instrument tip made of graphite and pressing it against a substrate in the hope that some trace of graphite might be a single graphitic plane.
Finally, the method successfully used by Geim and Novoselov to separate graphene layers was hardly at the cutting edge of technology, in fact just the opposite – a piece of sticky tape took with it layers of graphene when it was pulled off a piece of graphite. Some of the carbon layers were one atom thick (monolayers), others bilayers or multilayers. In fact, it turns out that we have all made graphene monolayers just by writing on paper with a graphite pencil – but we didn’t know it! The problem is not so much forming graphene sheets but identifying their existence.
Was it good luck that the silicon substrate that was used for depositing graphene was covered with 300 nm oxide layer? It became clear later that this was the best substrate which, under an optical microscope, yielded very strong contrast owing to favourable interference of light reflected from the bottom and top interfaces of the silicon oxide layer. Geim and Novoselov and their team were able in this way to identify the number of layers of graphene on a silicon substrate.
But why was this discovery worthy of the Nobel Prize? Most importantly, Geim and Novoselov with contributions from others went on to perform many experiments that demonstrated what an amazingly novel material graphene is. It was these ‘groundbreaking experiments’ revealing the behaviour of electrons in a two-dimensional (2D) material that had not been observed previously that amply justified the Nobel Prize. In addition, the large variety of possibilities for applications of graphene owing to its great strength as well as its unusual electronic properties over a wide range of temperatures mean that graphene is or will be incorporated in many devices for use in our everyday life.
Regarding graphene, the theorists were far ahead of experiments. The now-famous paper of the Canadian physicist Philip Wallace in 1947 calculated the electronic band structure of electrons in a 2D graphene layer (i.e. the energy of the different available states of the electrons in the layer). This calculation is much easier for the 2D graphene sheet than for 3D graphite. Wallace showed that the band structure of graphene is quite different from that in ordinary metals or semiconductors. Graphene could be called a metal with zero density of states at Fermi level or, equally well, it could be called a semiconductor with a zero band gap.
This band structure of graphene means that its properties can be dramatically altered and controlled by doping that can be provided either through a field effect transistor (FET) device or by chemical or electrochemical approaches. Thus, the graphene layer can be used for various applications in electronics.
We should mention that other novel forms of carbon closely related to graphene have been discovered, in fact before graphene. A structural modification leads to a change in the electronic properties of the material. This is why each member of the ‘graphene family’ has its own character and a different perspective for industrial application. The important modified structures based on graphene are fullerenes (miniature carbon ‘soccer balls’ formed by changing specific hexagons to pentagons), nanohorns of conical shapes, nanowalls grown perpendicular to the substrate, and nanofoam with the topology extended to 3D space.
Carbon nanotubes deserve special attention: if a sheet of graphene is rolled up with the carbon atoms on opposite edges matched up, a carbon nanotube is formed. These hollow carbon tubes can be single-wall with diameters down to less than one nanometre, or could consist of multiple shells (multiwall carbon nanotubes). Carbon nanotubes, like graphene, have a range of very attractive properties, such as, for example, strength, flexibility, and electrical and thermal conduction, that are finding applications in nanoscale electronics and composite materials. In this respect, carbon nanotubes represent the most serious competitor to graphene.
In this book, the articles take an in-depth look at the key aspects of graphene, both a single layer of graphene (monolayer) as well as bilayers and few-layer graphene. We start with chapters that introduce the most developed methods of preparation of graphene in Part I. The methods discussed are epitaxial growth of graphene through thermal decomposition of a SiC crystal, chemical vapour deposition growth of large-area graphene on catalytic substrates, and layer-exfoliation from graphite using chemical and electrochemical routes. Each of the methods produces graphene of different quality, size, and amount. In order to evaluate these factors we need to characterize synthesized graphene.
Part II contains chapters describing the most powerful techniques for characterization of graphene atomic and electronic structures. The principles and applications of particular characterization techniques are discussed. Transmission electron microscopy visualises the structure of suspended graphene down to the atomic level, giving information on crystalline grain size and structural defects as well as chemical modifications. Scanning tunnelling microscopy can give an atomic resolution image of graphene either grown in situ or transferred onto a conductive surface. In the spectroscopy mode, the electronic structure of graphene under various environmental conditions can be obtained through recording differential conductivity while sweeping the bias voltage between the conductive tip and substrate. Raman and photoemission spectroscopies provide us with a detailed picture of electronic structure that is affected by structural disorder, bending and thickness. Important insight into these spectroscopic methods is offered by the two last chapters in Part II.
The focus of Part III is on electronic transport in monolayer and in bilayer graphene and on electronic devices towards applications. In addition to presenting the unusual and fascinating electronic transport properties, the effect of absorbents on electronic transport is analysed. Quantum (single-electron) transport through a constricted area of graphene and a very strong effect of electronic disorder on the transport properties are discussed in a separate chapter. The final chapters cover graphene spintronics and graphene nanoelectromechanical systems (NEMS) where graphene is shown to be a promising material for these technological applications.
Part I
Preparation of graphene
Outline
1 Epitaxial growth of graphene on silicon carbide (SiC)
2 Chemical vapor deposition (CVD) growth of graphene films
3 Chemically derived graphene
4 Graphene produced by electrochemical exfoliation
1
Epitaxial growth of graphene on silicon carbide (SiC)
H. Huang, National University of Singapore, Singapore
S. Chen, Nanyang Technological University, Singapore
A.T.S. Wee and W. Chen, National University of Singapore, Singapore
Abstract:
This chapter provides an overview of the epitaxial growth of graphene films on various silicon carbide (SiC) substrates, their growth mechanism, and atomic scale characterization. The chapter focuses on the growth of epitaxial graphene (EG) via the thermal decomposition of single-crystal SiC in ultrahigh vacuum (UHV) and under ambient pressure. There is also a discussion of the thermal decomposition of polycrystalline SiC thin films and the intercalation methods used to produce EG.
Key words
thermal decomposition; epitaxial graphene; silicon carbide
1.1 Introduction
The realization of technologically feasible graphene-based electronic, optoelectronic, chemical- and bio-sensing devices greatly relies on the development of large-scale production of high-quality graphene thin films. In the last few years, intensive research efforts have been devoted to methods for production of single-layer or few-layer graphene films, including the micromechanical exfoliation from bulk graphite using sticky tape,¹,² chemical exfoliation from bulk graphite powders,³ chemical or physical reduction from graphene oxides,⁴–⁷ chemical vapour deposition of hydrocarbons on transition metal substrates⁸–¹⁷ such as Cu, Ni, Ru, Ir and Pt, thermal decomposition of solid carbon sources on metals, semiconductors or insulators substrates, and thermal decomposition of commercial silicon carbide (SiC) substrates in vacuum or under atmospheric pressure conditions.¹⁸,¹⁹ Epitaxial graphene (EG) films thermally grown on SiC can be patterned using CMOS-compatible nanolithography methods, making it compatible with current semiconductor technology and hence a promising growth process for future graphene-based devices.²⁰,²¹ In particular, high-performance devices, such as field-effect transistors,²² photodetectors,²³ and chemical sensors²⁴ have been demonstrated using EG on SiC. The aim of this chapter is to provide an overview of the epitaxial growth of graphene films on various SiC substrates, their growth mechanism, and atomic-scale characterization. The chapter focuses on the growth of EG via the thermal decomposition of single-crystal SiC in ultrahigh vacuum (UHV) and under ambient pressure, followed by a discussion of the thermal decomposition of polycrystalline SiC thin films and intercalation methods to produce EG.
1.2 Ultrahigh vacuum (UHV) thermal decomposition of single-crystal SiC
The formation of crystalline graphite layers on SiC via thermal heating at high temperature in UHV was first observed by van Bommel et al. in 1975.²⁵ However, the crystalline graphite layers later known as EG received little attention initially. About the time when the first isolation of free-standing graphene by mechanical exfoliation was reported, Berger and coworkers demonstrated that EG on SiC has nearly identical properties to those of free-standing graphene and is compatible with the CMOS-compatible lithography process for device fabrication.¹⁸ Single-crystal graphene with a controlled number of atomic layers can be epitaxially grown on SiC, depending only on the annealing temperature and time. The growth of EG depends on SiC surface polarity (i.e. silicon or carbon face) but shows little variation for different SiC polytypes (such as 3C, 4H and 6H). To understand this growth behaviour, we provide a brief description of the SiC structure.
SiC contains carbon and silicon in 1:1 stoichiometry. Each Si (or C) atom is covalently bonded to four nearest-neighboring C (or Si) atoms in a tetrahedral coordination (sp³ configuration). These tetrahedral Si–C bonds are arranged in a hexagonal bilayer with carbon and silicon in alternating positions. The Si–C bilayers can be stacked in various stacking and orientation sequences along the direction perpendicular to the bilayer plane, leading to more than 200 polytypes in the SiC bulk structure. There are two main configurations for these polytypes: one has cubic symmetry, i.e. face-centred cubic (fcc); the other has hexagonal symmetry, i.e. hexagonal close-packed (hcp). Among those polytypes, 3C-SiC, 4H-SiC and 6H-SiC are the most important, where the number 3 (4 or 6) indicates the number of bilayers per unit cell and C (H
plane in 4H-SiC and 6H-SiC. The unique physical and electrical properties of each polytype are attributed to the different stacking sequences. The termination of Si–C bilayer (i.e. Si on top or C on top) influences the silicon sublimation and carbon segregation processes, and thus results in distinct differences in graphene formation. We first focus on the Si-terminated or Si-face 6H-SiC(0001) to elucidate the properties of graphene on SiC and then discuss graphene formation on C-terminated or C-face SiC.
1.1 Stacking sequence for three typical polytypes of SiC: (a) 3C-SiC(111), (b) 4H- and (c) 6H-SiC(0001).
The growth of EG can be achieved via thermal decomposition of bulk SiC. At high temperatures, Si atoms start to evaporate from the surface. C atoms segregate on the surface to form C-rich surface layers, ranging from the interfacial graphene (IG) layer, to single-layer EG, bilayer EG and few-layer EG. Because this growth process involves a series of surface reconstructions, we use the growth of EG on 6H-SiC(0001) as an example to describe the evolution of these surface reconstructions as a function of substrate annealing temperature, as characterized by in situ low-energy electron diffraction (LEED, upper panel in Fig. 1.2) and scanning tunneling microscopy (STM, lower panel in Fig. 1.2).²⁶ After annealing the bare 6H-SiC(0001) at around 850 °C under a Si flux in UHV, a Si-rich 3 × 3 superstructure appears, comprising a twisted Si adlayer and Si tetramers on bulk SiC substrate (Fig. 1.2(a) and (e)).
1.2 
and (d) and (h) single-layer EG. (Reprinted from reference 26, with permission from IOP Publishing Limited, copyright 2007.)
ML, where ML is monolayer.
reconstruction, which has been also referred to as the ‘graphene buffer layer’ or IG.³¹,³² For consistency, we refer to this phase as ‘IG’ henceforth. Annealing the 6H-SiC sample at 1200 to 1400 °C leads to the formation of single-crystal EG layers with thickness ranging from a single layer to a few layers atop IG. The LEED and STM images of a single layer EG on SiC are shown in Fig. 1.2(d) and (h), respectively.
The formation of EG on SiC can be clearly evidenced by C 1s x-ray photoemission spectroscopy (XPS). The synchrotron-based high-resolution C 1s XPS spectra of SiC as a function of annealing temperature are shown in 
reconstructed surface, only the bulk SiC related peak at 282.9 eV below Fermi energy (EF) appears in the C 1s spectrum. On a surface with partial IG coverage, an IG-related component appears at 285.1 eV. The C 1s spectrum from the full-coverage IG surface is dominated by the peak at 285.1 eV, accompanied by a shoulder at 283.9 eV. The graphene-related C 1s peak at 284.4 eV in the spectrum is recorded from the sample annealed at higher than 1100 °C, indicating graphitization of the surface. The C 1s spectrum of full coverage EG surface is dominated by this peak.
1.3 The evolution of synchrotron-based high-resolution C 1s spectra of various annealing-induced SiC surface reconstructions. (Reprinted from reference 31, with permission from Elsevier B.V., copyright 2005.)
The EG formed on SiC can be characterized by Raman spectroscopy. In Fig. 1.4, typical Raman spectra of single-layer and bilayer EG on 6H-SiC(0001), single-layer mechanically cleaved graphene (MCG), bulk graphite, and bare 6H-SiC(0001) substrate are shown.³³ On the single-layer or bilayer EG, the bulk SiC related peaks appear at ~ 1520 and ~ 1713 cm−1, as on the bare SiC substrate. Three other peaks related to EG are observed: the defect-induced D band at − 1368 cm−1, in-plane vibrational G band at ~ 1597 cm−1 and the two-phonon 2D band at ~ 2725 cm−1. The insertion clearly shows that the 2D band of bilayer EG is wider than that of single-layer EG (95 compared with 60 cm−1) and occurs at higher frequency (2736 compared with 2715 cm−1), in line with the trend observed on MCG. The interfacial stress caused by the large lattice mismatch between SiC (a = 3.07 Å) and graphene (a = 2.46 Å) leads to a significant blue shift of the G (1597 cm−1) and 2D (2715 cm−1) bands of single-layer EG relative to that of the single-layer MCG (G band at 1580 cm−1 and 2D band at 2673 cm−1).
1.4 Typical Raman spectra of single-layer and bilayer EG on SiC, compared with bulk graphite and single-layer MCG. (Reprinted from reference 33, with permission from American Physical Society, copyright 2008.)
The IG layer is carbon rich and is believed to have a similar atomic structure to graphene. However, the IG layer does not have the same electronic properties as graphene. For comparison, the entire valence band structures of IG and single-layer EG are shown in the angular-resolved photoemission spectroscopy (ARPES) images in Fig. 1.5(a) and (b), respectively.³⁴ Both show a strongly dispersing σ-band between ~ 23 and ~ 8 eV below EF, indicating that IG has a similar carbon–carbon distance to that of graphene. The features in the region from about 12.5 to 2.5 eV are dominated by the emission from the bulk valence bands of SiC. Figure 1.5(b) clearly shows graphene’s linearly dispersed π-band at K point around EF. Instead, broad structures are observed on IG as shown in Fig. 1.5(a). Moreover, except for surface-related hardly dispersing features at 1.8 and 0.6 eV below EF, there are no occupied states near EF, suggesting partial coupling between the carbon pz orbitals in IG and the dangling bonds of SiC(0001).
1.5 ARPES images of (a) IG and (b) single-layer EG on 6H-SiC(0001) (hv = 50 eV). (Reprinted from reference 34, with permission from American Physical Society, copyright 2008.)
The dispersion of π-band at the K point around EF of single-layer, bilayer and multilayer EG on SiC varies considerably, giving rise to differing transport properties. Figure 1.6(a) to (d) displays the ARPES results and the corresponding tight-binding simulation of the π-band in the vicinity of the Dirac point (ED) of single-layer to quadlayer EG on SiC, respectively.³⁵ The position of ED below EF is attributed to charge transfer from the SiC substrate to graphene via IG. The EF position relative to ED point of EG can be adjusted by intercalation, as discussed in 1.5. The bands of single-layer EG shown in Fig. 1.6(a) are strongly renormalized, i.e. they deviate from the expected linear dispersion, owing to many-body interactions. The band of bilayer EG in Fig. 1.6(b) shows a band gap of 0.15 eV, owing to charge transfer from the substrate. This leads to a graded charge carrier concentration and thus the two layers have different onsite Coulomb potential.³⁶ A complex band structure is observed in Fig. 1.6(c) and (d) for trilayer and quadlayer EG, respectively.
1.6 (a)–(d) The π- and π*-bands near EF for 1–4 EG layers on 6H-SiC(0001), respectively (hv = 94 eV, T = ~ 30 K), where k|| = 1.703 Å−1 corresponds to the K point, the corner of the hexagonal Brillouin zone. The dashed lines are from a calculated tight binding band structure. The number of π-bands increases with the number of layers owing to interlayer splitting. (Reprinted from reference 35, with permission from American Physical Society, copyright 2007.)
EG on SiC grown in UHV is usually inhomogeneous. Various graphene layers coexist on the same sample. This is because the growth temperature is sufficient for silicon desorption but is not sufficient for homogeneous growth of graphene films. As shown in the low-energy electron microscopy (LEEM) image in Fig. 1.7(a), EG grown on SiC(0001) in UHV is a mixture of single-layer to quadlayer. The regions with different contrast correspond to a different number of EG layers, marked (1)–(4). The electron reflectivity versus kinetic energy of the incident electron beam allows a direct determination of the number of graphene layers, as shown in Fig. 1.7(b).³⁷,³⁸ The number of local minima (dips) in the reflectivity curve represents the number of graphene layers and it is clear that the areas correspond to 1–4 layers of graphene, respectively.
1.7 The nonuniformity of EG on SiC(0001). (a) LEEM image from an area with various numbers of graphene layers. The field of view (FOV) is 20 μm and the electron energy is 4.2 eV. Insets are μ-LEED patterns collected at E = 53.3 eV from the four labelled areas. (b) Electron reflectivity spectra extracted from the four representative areas labelled (1)–(4) and corresponding to graphene of 1–4 ML thick, respectively. (c) Raman spectral map of 2D peak position and (d) the corresponding AFM image from an area without macro-defects. ((a) and (b) are reprinted from reference 37, with permission from IOP Publishing Limited, copyright 2010; (c) and (d) are reprinted from reference 38, with permission from American Chemical Society, copyright 2009.)
Alternatively, the number of graphene layers can also be determined by μ-LEED as shown in Fig. 1.7(a). Owing to the short penetration depth of low-energy electrons, when the number of graphene layers increases, the six buffer-layer diffraction spots around the graphene spot (the centre/middle spot) gradually fade away. These six spots are barely visible from areas with three layers and are not possible to detect when the number of layers is larger than three.
The inhomogeneity of the prepared graphene samples is also manifested in inhomogeneous strain with the film. For single-layer EG on SiC, whose thickness is independently verified by photoemission spectroscopy, the strain can vary over a distance shorter than 300 nm; such strain may also be uniform over roughly 1 μm. The Raman spectral map of the
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