Preparation method of sulfurized polyacrylonitrile anode material used for lithium secondary battery

A technology of vulcanized polyacrylonitrile and lithium secondary batteries, which is applied in the field of materials, can solve the problems of low sulfur content, poor reproducibility, etc., and achieve the effects of high capacitance, avoiding the generation of impurity phases, and easy access to raw materials

Inactive Publication Date: 2014-08-06
SICHUAN UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

However, limited by the solid-state reaction conditions, polyacrylonitrile and sulfur cannot be mixed evenl

Method used

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  • Preparation method of sulfurized polyacrylonitrile anode material used for lithium secondary battery
  • Preparation method of sulfurized polyacrylonitrile anode material used for lithium secondary battery
  • Preparation method of sulfurized polyacrylonitrile anode material used for lithium secondary battery

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Embodiment 1

[0034] Dissolve 1 g of polyacrylonitrile powder in 30 mL of dimethyl sulfoxide, stir magnetically for 20 minutes, add 4 g of sulfur powder, and then stir magnetically for 20 minutes. After the stirring is completed, the solution is placed in an oil bath at 200° C. for a heating reaction for 12 hours, so that polyacrylonitrile and sulfur are cross-linked and combined to form a homogeneous solution. After the reaction, the solution was transferred to a vacuum oven, and vacuum-dried at 80° C. for 1 hour to remove dimethyl sulfoxide in the solution to obtain a vulcanized polyacrylonitrile material precursor. Then transfer to the muffle furnace and fill with N 2 protection, heating to 450°C for carbonization for 4 hours, and natural cooling to obtain a vulcanized polyacrylonitrile material. As a reference group, 1 g of polyacrylonitrile powder was dissolved in 30 mL of dimethyl sulfoxide, but no sulfur powder was added. Then, according to the above processing flow, the pure polya...

Embodiment 2

[0037] Dissolve 10 g of polyacrylonitrile powder in 350 mL of dimethyl sulfoxide, stir magnetically for 30 minutes, add 45 g of sulfur powder, and then stir magnetically for 30 minutes. After the stirring is completed, the solution is placed in an oil bath at 250° C. for a heating reaction for 18 hours, so that polyacrylonitrile and sulfur are cross-linked and combined to form a homogeneous solution. After the reaction, the solution was transferred to a vacuum oven, and vacuum-dried at 80° C. for 2 hours to remove dimethyl sulfoxide in the solution to obtain a vulcanized polyacrylonitrile material precursor. Then transfer to the muffle furnace and fill with N 2 protection, heating to 500°C for carbonization for 6 hours, and natural cooling to obtain a vulcanized polyacrylonitrile material.

Embodiment 3

[0039] Take 5g polyacrylonitrile fiber, chop it and dissolve it in 150mL dimethyl sulfoxide, stir it magnetically for 45 minutes, add 25g sulfur powder, and stir it magnetically again for 45 minutes. After the stirring, the solution was placed in an oil bath at 250° C. for a heating reaction for 20 hours, so that polyacrylonitrile and sulfur were cross-linked and combined to form a homogeneous solution. After the reaction, the solution was transferred to a vacuum oven, and vacuum-dried at 80° C. for 1.5 hours to remove dimethyl sulfoxide in the solution to obtain a vulcanized polyacrylonitrile material precursor. Then transfer to the muffle furnace and fill with N 2 protection, heating to 450°C for carbonization for 5 hours, and natural cooling to obtain a vulcanized polyacrylonitrile material.

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Abstract

The invention relates to a preparation method of a sulfurized polyacrylonitrile anode material used for a lithium secondary battery, and belongs to the technical field of materials. The preparation method is that sulfur and polyacrylonitrile are dissolved in dimethyl sulfoxide to have a crosslinking conjugation reaction and then are carbonized in a nitrogen environment at a temperature of 500 DEG C to obtain the sulfurized polyacrylonitrile material. The sulfur content of the sulfurized polyacrylonitrile material obtained through the preparation method is remarkably increased, the sulfur is distributed evenly, and the sulfurized polyacrylonitrile material has a graphite crystal structure and is remarkably improved in conductivity and stability. In the electrochemical test, the sulfurizedpolyacrylonitrile material shows the discharge quality specific capacity up to 1312mAh.g<-1> and the sulfur utilization rate up to 98.3%, and keeps 77% of the cycling stability of the maximum performance after 60 cycles under the conditions of 0.5C charge-discharge rate and 45 discharge cycles. The results show that the sulfurized polyacrylonitrile material prepared according to the method is an active material suitable for a lithium sulfur battery.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a method for preparing a positive electrode material of a rechargeable lithium-sulfur battery, in particular to a method for preparing a vulcanized polyacrylonitrile material by a homogeneous solvent method. Background technique [0002] Rechargeable lithium-sulfur batteries work on the principle of a reversible redox reaction between sulfur and lithium. Due to its low cost and high cycle performance, a large number of research institutes and personnel around the world are working on the development of lithium-sulfur batteries in both scientific and industrial fields (Ji et al., 2009; Jeong et al. , 2013; Zhao et al., 72013). At present, the technical bottleneck of lithium-sulfur batteries lies in the design and preparation of sulfur-based cathode materials. Specifically, traditional lithium-sulfur batteries have problems such as the loss of active materials and t...

Claims

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Application Information

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IPC IPC(8): H01M4/60C08J3/24
CPCC08J3/24H01M4/604H01M10/052Y02E60/10
Inventor 杜开峰崔旭东李响张永奎
Owner SICHUAN UNIV
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