Topic: Electrochemical Application of Carbon Materials MILD-EXFOLIATED GRAPHITE AS AN ANODE MATERIAL FOR LITHIUM ION BATTERY.

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1 Paper ID: 373 Topic: Electrochemical Application of Carbon Materials MILD-EXFOLIATED GRAPHITE AS AN ANODE MATERIAL FOR LITHIUM ION BATTERY Lin Zou, Yong-Ping Zheng, Feiyu Kang, Wanci Shen, Can Xu Laboratory of Advanced Materials, Department of Materials Science and Engineering, Tsinghua University, Beijing , China Abstract Mild-exfoliated graphite (MEG) with a pyrolysis carbon coating has been prepared by low temperature heating treatment of H 2 SO 4 -Graphite Intercalation Compounds, which was synthesized by a chemical oxidation process under H 2 O 2 addition, and then was coated with carbon film. The volume expansion of MEG was limited to less than 50% by controlling the heating temperature and the duration. XRD results showed that the grain size of MEGs decreases with the increase of treating temperature. The sample treated at 360 for 24 h with carbon coating could accommodate up to 378 mah/g capacity and keep 100% capacity after 100 cycles. The cyclic voltammetry measurement indicated that the differences among the capacities of MEGs treated at different conditions were corresponding to the relative strength of the peak at 0.05 V. The porous structure analysis by BET method showed that the increase of micro-pores could make a great contribution to the enhancement of both the cycle stability and the reversible capacity. Key words: Exfoliated graphite; Battery carbon; Electrodes Corresponding author: Prof. F. Kang fykang@tsinghua.edu.cn; Tel:

2 Introduction Natural graphite has been considered as a promising anode material for lithium ion secondary batteries due to its high reversible capacity, appropriate charge/discharge profile and low cost. However, it suffers from low first cycle efficiency, poor cycle stability and bad compatibility with some electrolytes such as PC [L.J.Fu, et al. 2006]. Many works on modification of natural graphite have been adopted to improve its electrochemical performance, such as mild oxidation [Y.P. Wu, et al. 2002], metals or metal oxides deposition [Young Tae Lee, et al. 2005, Yong Wang, et al. 2004], polymer coating [Basker Veeraraghavan, et al. 2002], carbon coating [Hongyu Wang,et al ], and so on. Nevertheless, the cycle stability is still poor comparing with mesocarbon micro bead (MCMB). The cycle performance of natural graphite is poor due to the change of graphite s volume, about 10% expansion in cycles. The layer structure could be broken during the cycles and then the capacity decreases. Here we report a method to improve the cycle stability remarkably. Graphite are mildly expanded to increase the interlayer distance slightly in advance and to form nanopores structure in the graphite layers, which can act as buffers for the expansion during cycles. Further more, the nanopores may greatly increase the capacity. graphite, H 2 SO 4 and H 2 O 2 is 2.5 : 10 : 1. After 10 min reaction, the H 2 SO 4 -H 2 O 2 -GIC was washed until the ph value became 4 and then was dried at 100. The samples were put in alumina pots and heated at 200, 360 for 24 h, then the mild-exfoliated graphite (MEG) was prepared. The volume expansion of MEGs was limited to less than 50% by controlling the heating temperature and the duration. Finally, the MEGs and phenol formaldehyde resin in a mass ratio of 20:1 was dissolved in ethanol and was stirred to be homogeneous, and then it was dried at 80 and carbonized at 1000 for 4 h, then the carbonized mild-exfoliated graphite (CMEG) was obtained. The SNEG was also coated using the same method for comparison. The working electrode was prepared by casting the slurry of CMEG (90 wt.%) and polyvinylidene fluoride (PVDF 10wt.%) dissolved in N-methylpyrrolidone (NMP) on a copper foil. The foil was then dried at 80 for 8 h and later dried in vacuum at 120 for 12 h. Li foil was used as the counter electrode and 1 M LiPF 6 dissolved in a mixture of ethyl methyl carbonate (EMC) and dimethyl carbonate (DMC) (1:1 in volume) was used as the electrolyte. The working and the counter electrodes were separated with Celgard 2400 separator. The cell was galvanostatically cycled between 0 and 2.00 V vs. Li/Li + at a rate of 0.2 C. Results and Discussion Experimental H 2 SO 4 -H 2 O 2 -GIC was prepared by a traditional chemical method. Spherical natural exfoliate graphite (SNEG) was added and stirred in the mixture of H 2 SO 4 (98%) and H 2 O 2 (30%), which was kept in a vessel surrounded by a mixture of ice and water to prevent the H 2 O 2 from decomposition, with the mass ratio of

3 Fig.1 c) and d) show the morphologies of MEGs. All samples morphologies are similar. Exfoliation of graphite could be observed. The SNEG splits after intercalation/de-intercalation process and the surface becomes unsmooth, which leads to an increase of surface area. The surface area of MEG at for 24 h is m /g, while SNEG is 6.75 m /g. It could enhance its charge/discharge performance at high current because it provided more transfer channels for Li ions, while the first cycle efficiency would decrease because more surface was covered by the solid state-electrolyte interface (SEI) film. XRD patterns of MEGs and SNEG are similar to the standard pattern of graphite-2h. The crystalline size along the c-axis (Lc estimated by the Sherrer s equation) of the MEGs treated at 200 and 360 was calculated as 27.6 and 26.3, while SNEG was 34.9 nm, respectively. It demonstrated that the graphite layer along c-axis was cracked somewhere, so that the grain size of MEGs decreased. It acted as a function of the treating temperature. Figure 2 Electrochemical performance at 0.2 C rate of SNEG, SNEG with carbon coating and CMEG treated at 200 and 300 Fig.2 Figure 1. SEM photographs of graphite shows the. electrochemical performance of SNEG, SNEG with carbon samples. a) and b): SNEG. c) and d): MEG coating treated at 360 temperature. The SNEG s cycle stability is poor.. and CMEGs treated at different It becomes better after carbon coating, the

4 capacity reduces to 260 mah/g after 50 cycles. All the CMEGs show perfect cycle performance. The CMEGs treated at 200 and 360 achieve 344 and 378 mah/g capacity, respectively. Both the CMEGs remain 100% capacity after 100 cycles. Comparing with the SNEG with carbon coating, the carbon coating can improve the cycle performance of SNEG, the remarkable increase of capacity and enhancement of cycle stability are primarily on account of the MEGs structure. CV curve shows an abnormity humps at 0.05 V. This peak locates in the range V, which has been confirmed to be stage 2 and stage 1 zone by several works and no peak in this zone were observed previously, it might relate to the pore structure. Fig. 4 illustrates the pores in graphite layer of MEG treated at 360, in which the dominated pores are around 2 nm and lager pores are also observed. The pore structure acts as buffers for the expansion of graphite in the charge/discharge process which greatly improve the cycle stability. Nanopores also increases the capacity remarkably based on the micropore storage mechanism. Conclusions Fig.3 Cyclic voltammetry curve of CMEG treated at 360. The mild-exfoliated graphite (MEG) with pyrolysis carbon coating has been prepared. XRD results show that the grain size of MEGs decreases with the increase of treating temperature. The sample treated at 360 for 24 h with carbon coating could accommodate up to 378 mah/g capacity and keep 100% capacity after 100 cycles. The cyclic voltammetry measurement showed an abnormity humps at 0.05 V, which might relate to the pore structure. Pore structure is detected by HRTEM, which acts as buffers for the expansion of graphite in the charge/discharge process, greatly improves the cycle stability. Nanopores also increase the capacity remarkably according to the micropore storage mechanism. References Fig.4 HRTEM photograph of graphite layer of MEG treated at 360. Fig. 3 displays the fiftieth cycle scanning at 0.1mV/s between 1.2 V and 0.0 V of the electrodes prepared with CMEG treated at 360. Basker Veeraraghavan, Jason Paul, Bala Haran and Branko Popov Study of polypyrrole graphite composite as anode material for secondary lithium-ion batteries. Journal of Power Sources 109(2): Hongyu Wang and Masaki Yoshio Carbon-coated natural graphite prepared by thermal vapor decomposition process, a candidate anode material for lithium-ion

5 battery. Journal of Power Sources 93(1-2): L.J.Fu, H.Liu, C.Li, Y.P.Wu, E.Rahm, T.Holze, H.Q.Wu Surface modifications of electrode materials for lithium ion batteries. Solid State Science 8: Y.P.Wu, C.Jiang, C.Wan and R.Holze Modified natural graphite as anode material for lithium ion batteries. Journal of Power Sources 111(2): Young Tae Lee, Chong Seung Yoon, Yang-Kook Sun Improved electrochemical performance of Li-dropped natural graphite anode for lithium secondary batteries. Journal of Power Sources 139(1-2): Yong Wang, Jim Y.Lee, Theivanayagam.C.Deivaraj. Tin Nanopartical Loaded Graphite Anode for Li-ion Battery Applications. Journal of The Electrochemical Society 151(11):

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