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1 Supporting Information MoS 2 Nanosheets Vertically Grown on Graphene Sheets for Lithium Ion Battery Anodes Yongqiang Teng 1, Hailei Zhao 1, 2,*, Zijia Zhang 1, Zhaolin Li 1, Qing Xia 1, Yang Zhang 1, Lina Zhao 1, Xuefei Du 1, Zhihong Du 1, Pengpeng Lv 1, Konrad Świerczek 3 1 School of Materials Science and Engineering, University of Science and Technology Beijing, Beijing , China 2 The Beijing Municipal Key Laboratory of New Energy Materials and Technologies, Beijing , China 3 AGH University of Science and Technology, Faculty of Energy and Fuels, Department of Hydrogen Energy, al. A. Mickiewicza 30, Krakow, Poland * Corresponding author: address: hlzhao@ustb.edu.cn
2 Fig. S1. XRD patterns recorded for the obtained MoS 2 /G and MoS 2 /G without H 2 C 2 O 4 added during the synthesis. For MoS 2 /G material obtained during synthesis with no H 2 C 2 O 4 added, a presence of graphite-related peaks can be noticed. The main visible peak (~33 deg) corresponds to MoS 2, which is weaker and broader when H 2 C 2 O 4 adding. Fig. S2. FESEM images of MoS 2 /G without H 2 C 2 O 4 added during the synthesis.
3 As shown in the Fig. S2, lack of the assistance of H 2 C 2 O 4 made MoS 2 growing and GO sheets restacking separately. The formed morphology was like graphite. Fig. S3. TG curve of MoS 2 /G composite recorded on heating with a heating rate of 10 o C min -1 in air. In order to determine the amount of graphene in the MoS 2 /G composite, TG analysis was performed for the sample in flowing air. As shown in Fig. S3, the first weight loss (~5.2%) in the range of approximately o C is caused by the removal of residual oxygen-containing groups, and the following one (~16.1%) is ascribed to the oxidation of MoS 2 to MoO 3 and the decomposition of graphene. The total weight loss was measured to be 21.3%. Based on the assumption that all the MoS 2 is converted into MoO 3 at 700 o C, the carbon content estimated for MoS 2 /G is 7.4 wt.%.
4 Fig. S4. XRD pattern of the sample after TGA measurement. XRD measurement (Fig. S4) for the residual product after TGA test reveals that all the MoS 2 has been converted to MoO 3 after TGA test, indicating the complete oxidation of MoS 2 in TGA measurement. Fig. S5. Gas chromatography-mass spectrum (a) and FTIR spectrum (b) of collected gaseous products during heat treatment of MoS 2 /G composite. Gas chromatography-mass and FTIR measurement show that the gaseous product is mainly composed of CO 2 and SO 2 (Fig. S5), revealing that the carbon and sulfur components of MoS 2 /G sample are oxidized to CO 2 and SO 2 in flowing air. In Fig. S5b, the peaks at 2330 and 1340 cm -1 correspond to antisymmetric and symmetry
5 stretching vibration modes of CO2, and another two distinct peaks at 1415 and 1200 cm-1 belong to two modes of SO2. Fig. S6. FESEM images of (a, b) MoS2/G composite before heat treatment and (c, d) MoS2/G composite after heated HNO3 treatment. Compared with the precursor of MoS2/G composite (Figs. S6a and b), the morphology of MoS2/G composite was hardly any change at all. Heat treatment was found to make no difference on the morphology. Furthermore, after successful removing of the MoS2 NSs by reaction with heated HNO3, smooth graphene sheets could be observed again, confirming formation of the MoS2/G heterostructure and that the structure of graphene is not destroyed during hydrothermal process (Figs. S6c and d).
6 Fig. S7. HRTEM images of the MoS 2 /G sample. Fig. S8. STEM image and element mapping images of MoS 2 /G composite. Many MoS 2 sheets with (002) plane exposure distribute randomly on the graphene surface (Fig. S7). STEM mapping reveals a homogenous elemental distribution on graphene surface (Fig. S8), due to the relatively low resolution.
7 Fig. S9. (a) and (b) FESEM images of MoS 2 /graphene mixture. The synthesis procedure of MoS 2 /graphene mixture was the same as in the case of the other composite, but rgo instead of GO was used. The rgo sheets own little oxygen-containing functional group. So, it is difficult to make close contact between MoS 2 particles and rgo sheets. As shown in Fig. S9, smooth graphene sheets and aggregated MoS 2 particles can be observed. Table S1. EDX elemental (S and Mo) composition analysis of the red square region in Figure 4a. Element Weight % Atomic % Detector Uncert. % Correction k-factor S(K) Mo(K)
8 Fig. S10. Charge-discharge curves of the first 5 cycles of MoS 2 /G composite. Fig. S11. Charge-discharge curves recorded at 100 ma g -1 for the 1 st, 10 th, 20 th, 30 th and 40 th cycle for bare MoS 2 electrode. For comparison, the galvanostatic charge-discharge profiles of bare MoS 2 electrode at the same current density were displayed. Obviously, the specific capacity showed a marked fall with an increasing cycle number.
9 Fig. S12. Cycling performance of MoS 2 /graphene mixture and bare MoS 2 electrodes at a current density of 1000 ma g -1. Table S2. Summary of electrochemical performance data of the reported relevant MoS 2 electrode materials. Anode materials Current density (ma g -1 ) Cycle number Reversible capacity (mah g -1 ) Reversible capacity after (X) cycles at a current density of (Y) ma g -1 (mah g -1 ) Reference MoS 2 /3DGN (35, 1000) 1 SL-MoS 2 -GNS (20,1000) 2 MoS 2 /C nanoflowers (30,1000) 3 MoS 2 /ACF cloth (200,500) 4 MoS 2 -Graphene-Carb on Nanotube Macroporous MoS 2 -AC Micro-spherical MoS 2 -G (100,1000) (250,1500) (250,1000) 7
10 MoSx/MWNTs (30,1000) 8 MoS2/G (400,1000) This work Fig. S13. FESEM images of (a, b) MoS2/G electrode and (c, d) bare MoS2 electrode after 130 cycles performed with a current density of 100 ma g-1. References 1. Cao, X.; Shi, Y.; Shi, W.; Rui, X.; Yan, Q.; Kong, J.; Zhang, H. Preparation of MoS2-Coated Three-Dimensional Graphene Networks for High-Performance Anode Material in Lithium-Ion Batteries. Small 2013, 9, Wang, Z.; Chen, T.; Chen, W.; Chang, K.; Ma, L.; Huang, G.; Chen, D.; Lee, J. Y.
11 CTAB-Assisted Synthesis of Single-Layer MoS 2 -Graphene Composites as Anode Materials of Li-Ion Batteries. J. Mater. Chem. A 2013, 1, Hu, L.; Ren, Y.; Yang, H.; Xu, Q. Fabrication of 3D Hierarchical MoS 2 /Polyaniline and MoS 2 /C Architectures for Lithium-Ion Battery Applications. ACS Appl. Mater. Interfaces 2014, 6, Wang, C.; Wan, W.; Huang, Y.; Chen, J.; Zhou, H. H.; Zhang, X. X. Hierarchical MoS 2 Nanosheet/Active Carbon Fiber Cloth as a Binder-Free and Free-Standing Anode for Lithium-Ion Batteries. Nanoscale 2014, 6, Zhu, C.; Mu, X.; van Aken. P. A.; Maier, J.; Yu, Y. Fast Li Storage in MoS 2 -Graphene-Carbon Nanotube Nanocomposites: Advantageous Functional Integration of 0D, 1D, and 2D Nanostructures. Adv. Energy Mater. 2015, 5, Choi, S. H.; Kang, Y. C. Polystyren-Templated Aerosol Synthesis of MoS 2 -Amorphous Carbon Composite with Open Macropores as Battery Electrode. ChemSusChem 2015, 8, Kalluri, S.; Seng, K. H.; Guo, Z.; Du, A.; Konstantinov, K.; Liu, H. K.; Dou, S. X. Sodium and Lithium Storage Properties of Spray-Dried Molybdenum Disulfide-Graphene Hierarchical Microspheres. Sci. Rep. 2015, 5, Shi, Y.; Wang, Y.; Wong, J. I.; Tan, A. Y. S.; Hsu, C. L.; Li, L. J.; Lu, Y. C.; Yang, H. Y. Self-Assembly of Hierarchical MoS x /CNT Nanocomposites (2<x<3): towards High Performance Anode Materials for Lithium Ion Batteries. Sci. Rep. 2013, 3, 2169.
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