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Plasma enhanced chemical vapor deposition of graphene
: synthesis and energy storage applications

  • Chundong WANG

    Student thesis: Doctoral Thesis

    Abstract

    Graphene is a planar monolayer sheet of sp2-hybridized carbons arranged on a two-dimensional hexagonal lattice. It is considered as the basic building unit of other carbon allotropes, i.e. 0D fullerenes, 1D carbon nanotubes, and 3D graphite. Following the definition, graphene can be divided into three different types: singlelayer graphene (SG), bilayer graphene (BG), and few-layer graphene (FG, number of layers ≤10). Since Geim and his co-workers at Manchester University first obtained single-layer graphene by the micro-mechanical cleavage approach, there has been an explosion of interest both in theoretical studies and experimental investigations. Long-range π-conjugation in graphene yields exotic physical properties of graphene, such as ultrahigh carrier mobility (~200 000 cm 2V-1 S-1 at electron densities of 2 ×1011 cm-2), superior high Young's moduli (0.5-1 TPa), large spring constants (1-5 Nm-1), the ambipolar field effect, and the room-temperature quantum confinement effect. These properties give graphene great potential in applications such as: field effect transistors (FET), high-speed and radio frequency logic devices, transparent electrodes, solar cells, supercapacitors, and rechargeable lithium ion batteries. Though graphene has been extensively studied for 8 to 9 years, achieving facile, environmental benignity and large-area growth of graphene is still the main task for researchers. Furthermore, some preliminary results have shown that graphene can greatly improve both the capacity and cycling stability of lithium ion batteries. In this thesis, we developed two different methods to synthesize graphene from solid carbon sources (polymethylmetacrylate and polydimethylsiloxane) with plasma enhanced chemical vapor deposition (CVD). Two facile N-doping approaches (ex-situ and in-situ) were demonstrated to efficiently incorporate nitrogen atoms into graphene lattices. Meanwhile, a facile one pot hydrothermal method has been proposed to synthesize laminate-structured graphene sheets-Fe3O4 nanocomposites (GNS-Fe3O4), which reveals high capacity LIB performance. Furthermore, a unique three-dimensional graphene scaffold has been fabricated to support Si and Sn nanostructures, which shows outstanding integrative electrochemical properties, excellent cyclability and rate performance. In the first section, microwave plasmas were employed to synthesize singleor double-layer graphene sheets on copper foils using a solid carbon source, polymethylmetacrylate (PMMA). The utilization of reactive plasmas enables graphene growth at reduced temperatures when compared with conventional thermal chemical vapor deposition processes. The effects of substrate temperature on graphene quality were revealed based on Raman analysis. Moreover, a facile approach to incorporate nitrogen into graphene by plasma treatment in a nitrogen/hydrogen gas mixture was demonstrated, and most of the nitrogen atoms were verified to be pyridine-like in carbon networks. The second section reports a novel method to achieve in situ nitrogen-doped graphene by microwave plasma assisted chemical vapor deposition (CVD) using PDMS (polydimethylsiloxane) as a solid carbon source. The percentage of nitrogen in the graphene lattice was observed to be controllable by adjusting the flow rate of nitrogen during the CVD process. The nitrogen atoms doped into graphene lattice were mainly in the forms of pyridinic and pyrrolic structures as confirmed by X-ray photoelectron spectroscopy. Moreover, first-principles calculations show that the incorporated nitrogen atoms can lead to p-type doping of graphene. This in situ approach provides a promising strategy to prepare graphene with controlled electronic properties. In the third section, we developed a facile one pot hydrothermal method to synthesize laminate-structured graphene sheets-Fe3O4 nanocomposites (GNS-Fe3O4). Fe3O4 nanoparticles were distributed densely and homogeneously in the graphene matrix. Galvanostatic charge/discharge cycling of the GNS-Fe3O4 nanocomposites exhibited a reversible specific capacity of over 1200 mAh/g at 100 mA/g without palpable fading for 50 cycles in the voltage range of 0.01-3.0 V. A cell for the rate capacity test reveals a high current density of 946 mAh/g at a cycling rate of 1000 mA/g, which could be recovered in full to 1359 mAh/g at 100mA/g after 50 cycles. The laminated structure of nanocomposites could prevent the agglomeration of Fe3O4 nanoparticles and the restacking of graphene sheets, effectively releasing the strain caused by volume expansion of Fe3O4 nanoparticles and facilitating ion/electron transportation within the electrode and at the electrode/electrolyte interface. In the fourth section, we proposed three-dimensional (3D) silicon (Si) thin films supported on a graphene scaffold to act as an anode electrode for lithium-ion batteries. The as-prepared Si anode exhibited a gravimetric capacity as high as 2495 mAh g-1 at C/3 rate, and capacity retention of 84% after 500 cycles compared with that after 50 cycles. Meanwhile, specific capacities of 1732 and 1264 mAh g-1 were demonstrated after 1200 cycles at rates of 1C and 3C, respectively. Such high specific capacities, excellent cyclability, and rate performance could have contributed to the highly porous 3D architecture of graphene scaffold, which provides not only good electrical conductivity but also mechanical flexibility. The results presented here have paved a new way to synthesize Si-graphene hybrid materials using microwave plasma-enhanced chemical vapor deposition as robust and scalable Si-based anodes for lithium ion batteries. In the fifth section, we report the development of a Sn nanoparticledecorated three-dimensional (3D) foothill-like graphene architecture as the anode electrode in LIBs. 3D graphene scaffold not only acts as an effective pathway for electron/lithium ions transport, but also efficiently buffers the huge volume expansion/shrinkage of Sn particles in the charge/discharge cycling processes. Electrochemical measurements demonstrated that the Sn@3D graphene anode delivered a reversible capacity of 662 mAhg-1 at a current density of 992 mAg-1 after 4000 cycles and 1129 mAhg-1 at 330 mAg-1 after 400 cycles. Its capacity is three times higher than that of the conventional graphite anode, suggesting that the novel Sn@3D graphene structure brings about a significant improvement in the overall performance of a LIB in the aspects of capacity, cycle life, and rate capacity.
    Date of Award2 Oct 2013
    Original languageEnglish
    Awarding Institution
    • City University of Hong Kong
    SupervisorWenjun ZHANG (Supervisor)

    Keywords

    • Graphene
    • Plasma-enhanced chemical vapor deposition

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