Microwave-Assisted Exfoliated Graphene for High Performance Si/Graphene Anode in Secondary Lithium Ion Battery

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研究生：	謝宜真 Hsieh, Yi Chen
論文名稱：	Microwave-Assisted Exfoliated Graphene for High Performance Si/Graphene Anode in Secondary Lithium Ion Battery 利用微波輔助剝離石墨烯應用於高品質二次矽基鋰離子電池之負極研究
指導教授：	闕郁倫 Chueh, Yu Lun
口試委員:	劉全璞 Liu, Chuan Pu 顏光甫 Yen, Kuang Fu
學位類別：	碩士 Master
系所名稱：	工學院 - 材料科學工程學系 Materials Science and Engineering
論文出版年：	2016
畢業學年度：	104
語文別：	英文
論文頁數：	76
中文關鍵詞：	微波輔助、還原氧化石墨烯、二次鋰離子電池
外文關鍵詞：	microwave assisted, reduced graphene oxide, secondary lithium ion battery
相關次數：	點閱：4 下載：0
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現今，我們將面臨能源危機，科學家都在尋找替代能源解決目前遇到的課題，在交通運輸方面，未來電動車的使用率會大幅增加，以取代石油、燃料的消耗，因此如何改善鋰離子電池已成為科學家爭相研究的課題。
本題目主要是針對鋰離子電池的負極材料進行研究與開發，然而，現今商用的鋰離子電池主要是以石墨為主，欲提高電池的理論克容量與電池的效能，我們開始著手於以「矽」為基底的材料。雖然矽擁有極高的理論克容量值(3579mAh/g)，這個數值約是10倍的石墨，然而卻有一些致命的缺點，例如:高體積膨脹率(400%)、不穩定的SEI層等。本題目是利用低成本的製程方法改善材料的結構與結合導電碳材料，以達到高生命週期與高容量的鋰離子電池。本實驗主要分成兩種製程方式，一種是乾式合成；另一種是濕式合成，兩者各具有其優點，以化學方法再加上微波輔助還原的方式進行合成，並加入奈米矽粉作為電池的負極材料。利用微波剝離所得到的石墨烯，透過傅立葉轉換紅外光譜、X光光電子能譜儀與拉曼光譜進行分析，其碳氧比可以高達14，C=O訊號與OH訊號也明顯減弱。而利用此導電材料所做出來的電池在150圈以後，仍維持約1200mAh/g。
另外，利用溶液的方式進行合成的同時，加入一些添加物像是銅奈米線是可行的，更是可以大大提升電池的效能，此部分在本文中也有做進一部探討。我們相信此低成本的製程技術是非常具有潛力的，並有助於日後商業化二次矽基鋰離子電池的發展與應用。

Owing to its high specific capacity (3579 mAh/g), silicon has become one of the most promising anode material candidates for use in lithium ion batteries. However, a 400% volume change during alloying is currently the biggest challenge toward their commercial application. The addition of graphene offers one potential method to overcome this problem. Due to its excellent mechanical properties, graphene is well suited to act as a buffer layer between silicon facilitating its large volume expansion. Hence, a facile route toward the optimization of graphene reduction is required.
In this work, we demonstrate two different approaches leading to more efficient and low cost processes in order to exfoliate and reduce graphene oxide simultaneously within a few minutes. The difference between the two methods is the starting materials. First, the proposed method, so-called “dry exfoliation method” utilizes silicon carbide as an efficient microwave susceptor heat source. The second method, called “wet exfoliation method” uses graphene oxide solution with the addition of a reducing agent. In both cases, under microwave radiation, graphene oxide undergoes a rapid heating and reduction to graphene. To characterize our materials, we utilize Fourier transform infrared spectroscopy (FTIR) and X-Ray photoelectron spectroscopy (XPS), the loss of C=O peaks and OH peaks confirm the reduction of graphene oxide after treatment. Scanning Electron Spectroscopy (SEM) and Transmission Electron Microscopy (TEM) are used to morphologically characterize the material we synthesized.
The cell performances of two different method of reducing graphene oxide are compared, showing capacity values of 1200mAh/g after 150 cycles for r-GO prepared from wet exfoliation method. Furthermore, by using the wet exfoliation method, additional precursors such as copper nanowires can be easily combined into the solution for further material enhancement. We believe this work presents a highly promising technique toward the low-cost production of reduced graphene oxide suitable for future Si based Li-ion battery applications.

Content
Content    I
Tables    VIII
Abstract    IX
摘要    XI
Acknowledgement    XIII
Chapter 1 Introduction    1
1.1 Lithium ion battery    1
1.1.1 Lithium ion battery overview    1
1.1.2 Working Mechanism of lithium ion battery    2
1.1.3 Developments in Anode Materials for Lithium ion batteries    4
1.1.4 Silicon-based Lithium ion batteries    7
1.2 Introduction of Graphene    11
1.2.1 The properties of graphene    11
1.2.2 The syntheses of graphene    16
1.2.2.1 Mechanical exfoliation method    16
1.2.2.2 The growth of graphene onto silicon carbide substrate    17
1.2.2.3 Chemical vapor deposition (CVD)    18
1.2.2.4 The reduction of graphene oxide (r-GO)    19
1.3 Graphene nanosheets in Lithium ion battery    25
Chapter 2 Motivation    30
2.1 Advantage of silicon-based anode for lithium ion battery    30
2.2 Further commercial application    31
Chapter 3 Material analysis method and technology    33
3.1 Raman Spectroscopy    33
3.2 X-ray Photoelectron Spectroscopy (XPS)    35
3.3 Fourier Transform Infrared Spectroscopy (FTIR)    36
3.4 Scanning Electron Spectroscopy (SEM)    37
3.5 Transmission Electron Microscopy (HR-TEM)    38
3.6 Coin cell testing system (LANHE CT2001A)    39
3.7 Electrochemical Impedance Spectroscopy (EIS)    40
Chapter 4 Results and Discussion    43
4.1 The synthesis of graphene oxide by Modified Hummer ’s method    43
4.2 Dry exfoliation method-thermal reduction    44
4.2.1 Experimental design    44
4.2.2 The mechanism of thermal reduction    46
4.3 Wet exfoliation method-thermal and chemical reduction    46
4.3.1 Experimental design    46
4.3.2 Material Characterization    48
4.3.3 Battery and electrochemical performance    53
4.4 Decorated reduced graphene oxide    57
4.4.1 Design of experiment    57
4.4.2 Material characterization    59
4.4.3 Battery and electrochemical performance    62
Chapter 5 Conclusion and future works    72
Chapter 6 Reference    73

Figures
Figure 1 (a) Comparison of the main three kinds of EVs: light EV, PHEV and full EV, including performance and battery properties (b) Ragone plot    2
Figure 2 Schematic illustration of a typical Lithium ion battery: (a) aluminum current collector; (b) transition metal oxide active material; (c) porous separator soaked with liquid electrolyte; (d) SEI layer formed by cycling; (e) graphite active material; (f) copper current collector    3
Figure 3 Schematic illustration of active materials for the next generation of lithium ion battery    5
Figure 4 Galvanostatic charge/discharge profiles for silicon anode    8
Figure 5 Three failure mechanisms of silicon electrode: (a) material pulverization; (b) morphology and volume change of entire silicon electrode (c) the formation of SEI film    9
Figure 6 Allotropes of carbon which are constructed from graphene. From left to right is fullerene, carbon nanotube and graphite, respectively.    12
Figure 7 A schematic of measuring an effective spring constant of suspended graphene sheet by AFM tip.    13
Figure 8 A plot of the spring constant of the suspended graphene sheet. From the linear fit, we are able to realize an average tension and Young’s modulus.    13
Figure 9 The variation of capacitance retention of graphene/carbon black electrodes as a function of cycle number measured at 200mV/s in 6M KOH aqueous solution. And the inset figure shows CV curve of first and 6000th cycle)    15
Figure 10 Nyquist plots of graphene/carbon black electrodes of first and 6000th cycle (frequency range: 105-10-1 Hz)    15
Figure 11 (a) Graphene visualized by atomic force microscopy (b) Graphene sheet freely suspended on metallic scaffold (c) Relatively large graphene image taken by Scanning electron micrograph    16
Figure 12 Scanning tunneling microscope topographs of nominally epitaxial graphene on SiC(0001).    17
Figure 13 The phase diagrams of Ni-C and C-Cu    18
Figure 14 Timeline for the development of graphene synthesizing by electrochemical techniques, including the breakthrough of monolayer graphene.    20
Figure 15 Schematic diagram of the procedure for the production of thermally reduced graphenes. These thermally reduced graphenes are labelled in the following text as G-ST (Staudenmaier method), G-HO (Hofmann method) and G-HU (Hummers method).21    21
Figure 16 (a) Schematic of the formation process of nano-Si (GS-Si) wrapped with graphene sheet (b) The battery performances of different materials (c) Nyquist plots of the cells with GS-Si and GS/Si electrodes after two cycles    27
Figure 17 (a) Schematic of the formation process of C-Si graphene formation (b) the battery performance of C-Si graphene electrode    28
Figure 18 (a) Schematic of the fabrication silicon_carbon nanocables sandwiched between reduced graphene oxide sheets (b) the capacity and Columbic efficiency of the SiNWs graphene sandwich structure cycled at 0.5C for 100 cycles    29
Figure 19 Ranges of anode and cathode materials with different capacities.    31
Figure 20 Vibrational energy level diagram showing Rayleigh and Raman (Stokes and Antistokes) scattering.    34
Figure 21 Raman spectra of 1-Layer G (red), 2-Layer G (blue), 3-Layer G (green) prepared by the mechanical exfoliation of HOPG, shown for comparison.    35
Figure 22 Different reduction treatments on the GO films by High-resolution XPS analysis. (A) Nonreduced film. (B) Hydrazine-vapor treated film. (C) Hydrazine-vapor plus annealing at 400 °C. (D) Thermal annealing at 1100 °C in vacuum.    36
Figure 23 (a) The signals generated by the electron beams. (b) Schematic diagram of Scanning Electron Spectroscopy    38
Figure 24 The components and structure of TEM    39
Figure 25 Battery testing system (the model of CT2001A)    40
Figure 26 The experiment equipment of BioLogic Science Instruments    41
Figure 27 (a) The equivalent circuit for analysis of the Nyquist plots. (b) Schematic figures of physical/chemical processes involved in batteries.    42
Figure 28 A process flow of synthesizing graphene oxide by modified Hummer’s method.    43
Figure 29 Schematic of the process of synthesizing from graphene oxide to functionalized graphene    44
Figure 30 Schematic of dry exfoliation method    45
Figure 31 (a) Process window of dry exfoliation method (b) A curve for microwave power versus temperature.    45
Figure 32 Schematic of wet exfoliation method    46
Figure 33 The color change of graphene oxide before and after microwave treatment    47
Figure 34 Morphological characterizations of materials from graphite to graphene oxide, and then reduced graphene oxide.    49
Figure 35 The Raman spectrums of materials from graphite to graphene oxide, and then reduced graphene oxide.    51
Figure 36 FTIR and XPS spectra of materials. (a) FTIR spectrum of three materials (b, c, d) The XPS spectra of graphene oxide as synthesized, r-GO synthesized by dry and wet exfoliation method.    52
Figure 37 The detailed equipment of the fabrication of coin cell    54
Figure 38 (a) Battery performances of different electrodes, including carbon black (pristine), graphene oxide and r-GO synthesized by dry and wet exfoliation method (b) Coulombic efficiency of battery performances.    56
Figure 39 (a) Nyquist plots of different batteries including carbon black (pristine) and r-GO synthesized by dry and wet exfoliation methods (b) the value of different internal resistance fitting by equivalent circuit    57
Figure 40 SEM image of copper nanowires as synthesized    58
Figure 41 Morphological characterization of decorated r-GO combining copper nanowires with r-GO    59
Figure 42 (a, b) HR-TEM images of copper nanowire without r-GO, indicating the oxidation of copper nanowire (c, d) HR-TEM images of copper nanowire with r-GO and present that r-GO is the fully cover onto copper nanowire.    60
Figure 43 (a) Raman spectrum of decorated r-GO with single copper nanowire (b) Raman spectrum of decorated r-GO with a group of copper nanowires    62
Figure 44 (a) The comparison of battery performance using different electrodes including pure r-GO synthesized by wet exfoliation, pure Cu nanowire, decorated r-GO and r-GO/Cu mixing (indirectly slurry mixing with r-GO and copper nanowires as synthesized), (b) Coulombic efficiency of battery performances.    64
Figure 45 Rate performance of decorated r-GO at different current rate from 0.1C-2C (0.18A/g-7.2A/g). All the specific capacities reported and C rate used are based on active material: silicon’s weight.    65
Figure 46 (a) Schematic illustration of indirectly slurry mixing with r-GO and copper nanowires as synthesized (b) Schematic illustration decorated r-GO of linking copper nanowire and reduced graphene oxide through the electrostatic interactions.    66
Figure 47 Schematic illustration of copper nanowires with GO powder and GO is covered onto copper nanowires. (a) low Magnification (b) high Magnification    67
Figure 48 Nyquist plots of different electrodes. (a) Comparison of four kinds of electrodes after 2 cycles (b) The electrodes of r-GO (wet) and decorated r-GO show much difference after 50 cycles.    69
Figure 49 Cyclic voltammetry curves of silicon with r-GO (wet) and silicon with decorated r-GO electrodes for the first, second, 50th and 100th cycles.    70
Figure 50 Benchmark of battery performances by using silicon/graphene composite as electrode.    71

Tables 
Table 1 Three types of anode materials for lithium ion battery    7
Table 2 The comparison of several research studies which are published to improve battery performance    11
Table 3 Lists of Young’ s modules of common materials.    14
Table 4 The comparison of different chemical methods of reducing graphene oxide.    23
Table 5 The pros and cons of four different kinds of reducing graphene oxide.    24
Table 6 The comparison of two main methods of graphene oxide reduction.    25
Table 7 The calculation of D/G ratios of graphene oxide as synthesized, r-GO (dry) and r-GO (wet)    51
Table 8 The value of different internal resistance fitting by equivalent circuit    69


                                

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