Hydrothermal synthesis of nano-silicon from a silica sol and its use in lithium ion batteries
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1 Electronic Supplementary Material Hydrothermal synthesis of nano-silicon from a silica sol and its use in lithium ion batteries Jianwen Liang, Xiaona Li, Yongchun Zhu ( ), Cong Guo, and Yitai Qian ( ) Hefei National Laboratory for Physical Science at Microscale and Department of Chemistry, University of Science and Technology of China, Hefei , China Supporting information to DOI /s Figure S1 XRD pattern of agglomerated as-prepared reacted products at a synthesis temperature of 180 C. Figure S2 XRD pattern of agglomerated as-prepared reacted products after immersion in hydrochloric acid. Address correspondence to Yitai Qian, ytqian@ustc.edu.cn; Yongchun Zhu, ychzhu@ustc.edu.cn
2 Figure S3 Nitrogen adsorption and desorption isotherms of porous silicon nanospheres at 77 K. Figure S4 The BJH pore distribution curve of porous silicon nanospheres. Extension experiments Extension experiment 1: Silicon was prepared by reaction of silica aerogel with magnesium and water according to similar procedures to those for the nano-silicon. Typically, silica aerogel (0.6 g), Mg (2 g, mesh) and H 2 O (1.4 g) were mixed and added into a 20 ml stainless autoclave before being sealed. Subsequently, the autoclave was maintained at 200 C for 10 h and cooled to room temperature. The reaction product was immersed in hydrochloric acid (1 mol L 1 ) for several hours to remove MgO. The resulting solution was washed with distilled water and centrifuged (5,000 rpm, 5 min) to collect the silicon. The obtained silicon was dissolved in 10 wt.% dilute HF solution for 10 min to remove unreacted silica and other impurities formed during reduction. The final sample was characterized by XRD, SEM and TEM. XRD (Fig. S5) clearly reveals the presence of a crystalline phase of silicon which means that the hydrothermal reduction reaction can be extended to silica aerogel. SEM (Fig. S6) and TEM (Fig. S7) images reveal that the silicon prepared by using silica aerogel is composed of uniform nanoparticles with a porous structure.
3 Figure S5 XRD pattern of silicon produced from silica aerogel. Figure S6 SEM image of silicon produced from silica aerogel. Figure S7 TEM image of silicon produced from silica aerogel. Extension experiment 2: Silicon was prepared by reduction of silicic acid (hydrated silica) using a similar procedure to that for nano-silicon. Typically, silicic acid (0.57 g), Mg (2.2 g, mesh) and H 2 O (1.33 g) were mixed and added to a 20 ml stainless autoclave which was than sealed. Subsequently, the autoclave was Nano Research
4 maintained at 200 C for 10 h and then cooled to room temperature. The reaction product was immersed in hydrochloric acid (1 mol L 1 ) for several hours to remove MgO. The resulting solution was washed with distilled water and centrifuged (5,000 rpm, 5 min) to collect the silicon. The silicon product was directly characterized by XRD (Fig. S8) without immersion in HF solution. XRD analysis clearly reveals the presence of crystalline phases of silicon and silica (silica can be removed by HF solution), which means that the hydrothermal reduction process can be extended to silicic acid. Figure S8 XRD pattern of silicon produced from silicic acid. Extension experiment 3: An extension experiment involving adjusting the ph of the reaction system was carried out as follows: Hydrochloric acid was add to 10 ml of silica sol (ph 14) to adjust the ph to 9 and then mixed with 11.8g Mg powder and the mixture placed in a 50 ml stainless autoclave which was then sealed. Subsequently, the autoclave was maintained at 150 C for 10 h and then cooled to room temperature. The samples were immersed in hydrochloric acid (1 mol L 1 ) for several hours to remove MgO. The resulting solution was washed with distilled water and centrifuged (5,000 rpm, 5 min) to collect the silicon. The resulting silicon was immersed in 10 wt.% dilute HF solution for 10 min to remove unreacted silica and other impurities during reduction. The brown-black precipitate was collected by centrifugation, washed with deionized water and ethanol and dried overnight at 60 C in a vacuum oven to evaporate the remaining solvent. The yield of the silicon product was about 30%. Figure S9 shows the XRD pattern of the product which confirms that the main component is crystalline silicon. Figure S9 XRD pattern of the as-prepared reacted products at a synthesis temperature of 150 C after adjusting the ph of the silica sol to 9.
5 Figure S10 Cycling properties at 3.6 A g 1 for different test temperatures with the first three cycles activated at 0.72 A g 1 (25 C). Figure S11 Cycling property at 3.6 A g 1 for long term cycling at 40 C after the temperature variation measurement. Nano Research
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