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Preparation method for nitrogen-doped porous carbon sphere-sulfur composite positive material

A nitrogen-doped porous carbon, composite cathode material technology, applied in battery electrodes, electrical components, circuits, etc., can solve the problems of insufficient infiltration of sulfur salt solution, low sulfur content of composite materials, etc., and achieve high mechanical stability. High stability and simple operation effect

Inactive Publication Date: 2013-07-24
SHENZHEN RES INST CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is also a problem with this method. The sulfur salt solution cannot fully infiltrate the pore structure of the carbon material, resulting in the in-situ deposition of a lot of sulfur into the pore structure of the carbon material, resulting in a low sulfur loading of the composite material.

Method used

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  • Preparation method for nitrogen-doped porous carbon sphere-sulfur composite positive material
  • Preparation method for nitrogen-doped porous carbon sphere-sulfur composite positive material
  • Preparation method for nitrogen-doped porous carbon sphere-sulfur composite positive material

Examples

Experimental program
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Effect test

Embodiment 1

[0029] 1. Preparation of nitrogen-doped porous carbon spheres:

[0030] Weigh 30g biuret, 20g silica sol (SiO 2 Average particle size 7 nm, SiO 2 The concentration is 20 wt%), dissolved in 200 mL deionized water, and ultrasonically mixed for 1 h at 20 °C to make a spray solution. Put the spray solution into an argon gas stream spray pyrolyzer, spray pyrolyze at 400 °C, the atomization volume through the spray system is 0.5 mL / min, the medium gas atomization pressure is 1 MPa, collect the product, and obtain the nitrogen doped solution. Heteropyrolytic carbon-silica spherical composites. The complex was added to a hydrofluoric acid solution with a mass fraction of 10% and stirred at room temperature for 24 h to remove the template, then filtered with suction, washed three times with deionized water and absolute ethanol, and dried at 100°C to obtain nitrogen-doped Porous carbon spheres, whose SEM morphology is shown in Figure 1, the structure of carbon spheres doped with nitrog...

Embodiment 2

[0036] 1. Preparation of nitrogen-doped porous carbon spheres:

[0037] Weigh 40g triethanolamine, 30g silica sol (SiO 2 The particle size is 2 nm, the concentration is 30 wt%), dissolved in 200 mL deionized water, and ultrasonically mixed at 30 °C for 0.5 h to make a spray solution. Put the spray solution into an argon gas flow spray pyrolyzer, spray pyrolyze at 500 °C, the atomization volume through the spray system is 1 mL / min, the medium gas atomization pressure is 10 MPa, and the product is collected to obtain nitrogen-doped Pyrolytic carbon-silica spherical composite. The complex was added to a hydrofluoric acid solution with a mass fraction of 20% and stirred at room temperature for 12 h to remove the template, then suction filtered, washed repeatedly with deionized water and absolute ethanol, and dried at 100°C to obtain nitrogen-doped porous carbon spheres.

[0038] two, Preparation of nitrogen-doped porous carbon sphere-sulfur composite cathode material:

[003...

Embodiment 3

[0042] 1. Preparation of nitrogen-doped porous carbon spheres:

[0043] Weigh 35g dipropylamine, 25g silica sol (SiO 2 The particle size is 10 nm, the concentration is 40 wt%), dissolved in 200 mL deionized water, and ultrasonically mixed at 40 °C for 2 h to make a spray solution. Put the spray solution into the argon gas flow spray pyrolyzer, spray pyrolysis at 600 °C, the atomization volume through the spray system is 10 mL / min, the medium gas atomization pressure is 20 MPa, and the product is collected to obtain nitrogen-doped Pyrolytic carbon-silica spherical composite. The complex was added to a 30% hydrofluoric acid solution by mass and stirred at room temperature for 8 h to remove the template, then suction filtered, washed repeatedly with deionized water and absolute ethanol, and dried at 120°C to obtain nitrogen-doped porous carbon ball.

[0044] two, Preparation of nitrogen-doped porous carbon sphere-sulfur composite cathode material:

[0045] Put 0.4 g of the ...

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Abstract

The invention discloses a preparation method for a nitrogen-doped porous carbon sphere-sulfur composite positive material. The preparation method comprises the following steps of: performing spray pyrolysis on a nitrogen-containing carbon source, silica sol and de-ionized water to obtain a spherical nitrogen-doped pyrolytic carbon-silicon dioxide composite, adding the composite into excessive hydrofluoric acid for reaction, and washing and drying the reactants to obtain nitrogen-doped porous carbon spheres; and adding a sulfosalt solution into the nitrogen-doped porous carbon spheres under a vacuum condition, adding glycerin, which is taken as a dispersing agent, into the carbon spheres, adding an acid solution to the carbon spheres under magnetic stirring, and filtering and washing the mixture, and performing vacuum drying on the washed mixture to obtain the nitrogen-doped porous carbon sphere-sulfur composite positive material. The sulfur content of the prepared composite material is 50 to 90 percent, sulfur particles are more uniformly distributed in porous structures of the porous carbon spheres, and carbon and sulfur particles are more closely bound. The material is high in mechanical stability, specific discharge capacity and cycle performance. The method is simple in process, easy to operate, pollution-free and suitable for industrial implementation and batch production.

Description

Technical field [0001] The present invention involves a preparation method of a lithium sulfur battery positive electrode material, which specifically involves a preparation method for a nitrogen doped porous carbon ball-sulfur composite positive material. Background technique [0002] With the widespread application of lithium -ion batteries in portable electronic products, electric vehicles, and incoming mixed electric vehicles, it is urgent to develop higher energy density batteries.Due to the increase in the capacity of lithium ion batteries, the energy density of lithium -ion batteries is difficult to increase significantly.At the same time, the voltage platform of positive materials to increase energy density will cause security problems.Turning the positive material from "deserture mechanism" to "conversion reaction chemical mechanism" is expected to obtain high -scale and high -ratio energy materials.Summer sulfur is one of the most promising positive materials. Sulfur an...

Claims

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Application Information

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IPC IPC(8): H01M4/58
CPCY02E60/10
Inventor 张治安李强张凯赖延清贾明李劼
Owner SHENZHEN RES INST CENT SOUTH UNIV
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