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The synthesis process for the sulfur¨Ccarbon composite by the in situ sulfur deposition route is illustrated in Scheme 1, and the in situ sulfur deposition in aqueous solution involves the following reaction: Na2S2O3 +2HCl¡ú2NaCl+SO2 +H2O+S¡ý First, 0.02 mole of sodium thiosulfate (Na2S2O3, Fisher scientific) was completely dissolved in 750 mL of deionized (DI) water by stirring. Then, 0.1 g of commercial conductive carbon black with a diameter of 30¨C60 nm (Super P) was suspended in the above solution by adding a small amount of isopropyl alcohol (C3H8O, Fisher scientific) under ultrasonic vibrations. The reason for adding isopropyl alcohol is that it enhances the wetting of the hydrophobic carbon nanoparticles in the aqueous solution. A 2 mL of hydrochloric acid (HCl, Fisher Scientific) was then slowly added to the solution to precipitate the sulfur onto the surface and into the interspaces of the nano-sized carbon black. During the in situ sulfur deposition reaction, the sulfur particles grow to a thermodynamically favored size and the carbon nanoparticles in the composite self-assemble, become interconnected with each other, and finally wrap the sulfur. After allowing the reaction mixture to stir for 24 h, the product was filtered and washed several times with DI water, ethanol, and acetone. The sulfur¨Ccarbon composite thus collected was dried in an air-oven at 50 ◦C for 24 h. The sulfur content in the composite was determined by thermogravimetric analysis (TGA) with a Perkin-Elmer TGA 7 Thermogravimetric Analyzer at a heating rate of 5 ◦C/min from 30 to 300 ◦C with flowing air. During this process, all the sulfur volatilizes and the sulfur content could be obtained from the observed weight loss since carbon black does not exhibit any weight loss in this temperature range. The sulfur¨Ccarbon composites with 75 wt.% sulfur as confirmed by the TGA data were employed for further experiments. Wang et al. [22] used a similar solution-based reaction to obtain sulfur, but the carbon was attached to the surface of the sulfur particles by an extra mixing process after the precipitation of sulfur. In other words, only part of the sulfur was slightly connected with the conductive carbon, resulting in a low utilization of the active material. In contrast, the in situ sulfur deposition route used in our study ensures that sulfur contacts with the carbon black closely due to the heterogeneous nucleation of sulfur. In order to have a comparison, pure sulfur was also synthesized by the same reaction route, but carbon black was added after sulfur was precipitated. |
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3Â¥2013-04-22 16:52:14
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2Â¥2013-04-22 16:48:35
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°®ÓëÓêÏÂ: ½ð±Ò+1 2013-04-22 21:11:24
Ó´Ó´william: ½ð±Ò+10, ·ÒëEPI+1, ¡ïÓаïÖú, ·ÒëÒ»°ë£¬¸øÒ»°ëµÄ½ð±Ò 2013-04-22 22:02:52
°®ÓëÓêÏÂ: ½ð±Ò+1 2013-04-22 21:11:24
Ó´Ó´william: ½ð±Ò+10, ·ÒëEPI+1, ¡ïÓаïÖú, ·ÒëÒ»°ë£¬¸øÒ»°ëµÄ½ð±Ò 2013-04-22 22:02:52
|
¸Õ³Ô·¹»ØÀ´£¬·ÁËǰÁ½¶Î£¬¸úÄãרҵ²»Ò»ÑùËùÒÔÓеÄרҵ´Ê²»ÖªµÀÒëµÄ¶Ô²»¶Ô¡£¡£ ¹©²Î¿¼¡ª¡ª The synthesis process for the sulfur¨Ccarbon composite by the in situ sulfur deposition route is illustrated in Scheme 1, and the in situ sulfur deposition in aqueous solution involves the following reaction: Na2S2O3 +2HCl¡ú2NaCl+SO2 +H2O+S¡ý ͨ¹ýÔλÁò³Áµí;¾¶£¨Ó¦¸ÃÊǸöרҵÃû´Ê°É£¬»¹ÊÇͬλÁò£¿£©ºÏ³ÉÁò̼¸´ºÏ²ÄÁϵŤÒÕÒѾÔÚͼ±í1ÖвûÊÍÁË£¬ÔλÁòÔÚË®ÈÜÒºÖеijÁµí°üº¬ÈçÏ·´Ó¦£ºNa2S2O3 +2HCl¡ú2NaCl+SO2 +H2O+S¡ý First, 0.02 mole of sodium thiosulfate (Na2S2O3, Fisher scientific) was completely dissolved in 750 mL of deionized (DI) water by stirring. Then, 0.1 g of commercial conductive carbon black with a diameter of 30¨C60 nm (Super P) was suspended in the above solution by adding a small amount of isopropyl alcohol (C3H8O, Fisher scientific) under ultrasonic vibrations. Ê×ÏÈ£¬0.02moleÁò´úÁòËáÄÆÍ¨¹ý½Á°èÍêÈ«ÈܽâÓÚ750mlÈ¥Àë×ÓË®ÖС£È»ºó£¬°ÑÖ±¾¶30-60nmµÄ0.1gµ¼µçÌ¿ºÚ¼ÓÉÙÁ¿Òì±û´¼£¬ÔÚ³¬ÉùÕñ¶¯ÏÂÐü¸¡ÔÚÉÏÊöÒºÌåÖС£ The reason for adding isopropyl alcohol is that it enhances the wetting of the hydrophobic carbon nanoparticles in the aqueous solution. ¼ÓÒì±û´¼µÄÔÒòÊÇËü¿ÉÒÔÌá¸ßÊèË®ÐÔÄÉÃ×̼ÔÚË®ÈÜÒºÖеÄʪ¶È£¨wettingÊÇÒë³Éʪ¶ÈÂ𣿻¹ÊÇÇ×Ë®¶È£¿ÈÜË®ÐÔ£¿£©¡£ A 2 mL of hydrochloric acid (HCl, Fisher Scientific) was then slowly added to the solution to precipitate the sulfur onto the surface and into the interspaces of the nano-sized carbon black. °Ñ2mlÑÎËỺÂý¼ÓÈëÈÜÒº£¬Ê¹Ö®ÔÚ±íÃæÉϺÍÄÉÃ×̼ºÚÖ®¼ä³Áµí³öÁò¡£ During the in situ sulfur deposition reaction, the sulfur particles grow to a thermodynamically favored size and the carbon nanoparticles in the composite self-assemble, become interconnected with each other, and finally wrap the sulfur. ÔÚÔλÁò³Áµí·´Ó¦ÖУ¬ÁòÔ×Ó³¤µ½ÈÈÁ¦Ñ§ÉÏÎȶ¨µÄ´óС£¬¸´ºÏ²ÄÁÏÖеÄÄÉÃ×̼×Ô×é×°£¬»¥ÏàÁ¬½Ó£¬×îÖÕ°ü¹üסÁò¡£ After allowing the reaction mixture to stir for 24 h, the product was filtered and washed several times with DI water, ethanol, and acetone. ÔÚ°Ñ»ìºÏÎï½Á°è24hºó£¬¹ýÂ˲úÎï²¢·Ö±ðÓÃÈ¥Àë×ÓË®¡¢ÒÒ´¼ºÍ±ûͪϴµÓÈô¸É´Î¡£ The sulfur¨Ccarbon composite thus collected was dried in an air-oven at 50 ◦C for 24 h. °ÑÉÏÊöÊÕ¼¯µÄÁò̼¸´ºÏ²ÄÁÏ50ÉãÊ϶ÈÈÈ¿ÕÆø¸ÉÔï24h¡£ |
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4Â¥2013-04-22 19:09:15
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5Â¥2013-04-22 19:15:05













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