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Ó´Ó´william

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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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Ó´Ó´william

ľ³æ (СÓÐÃûÆø)

ÒýÓûØÌû:
2Â¥: Originally posted by carrieskl at 2013-04-22 16:48:35
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3Â¥2013-04-22 16:52:14
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Ó´Ó´william: ½ð±Ò+10, ·­ÒëEPI+1, ¡ïÓаïÖú, ·­ÒëÒ»°ë£¬¸øÒ»°ëµÄ½ð±Ò 2013-04-22 22:02:52
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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
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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.
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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.
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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.
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After allowing the reaction mixture to stir for 24 h, the product was filtered and washed several times with DI water, ethanol, and acetone.
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The sulfur¨Ccarbon composite thus collected was dried in an air-oven at 50 ◦C for 24 h.
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