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Preparation method of three-dimensional sulfur-doped graphene/sulfur composite material electrode slice

A technology of sulfur-doped graphene and composite materials, which is applied in the field of preparation of lithium-sulfur battery cathode materials, can solve the problems of reducing the utilization rate of sulfur active materials, slow migration speed, and slow electrochemical reaction kinetics, achieving reduction The shuttle effect, the effect of improving the conductivity and reducing the cost

Inactive Publication Date: 2016-07-13
钟玲珑
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This phenomenon, known as the shuttle effect, reduces the availability of sulfur active species
At the same time insoluble Li 2 S and Li 2 S 2 Deposited on the surface of the lithium negative electrode, which further deteriorates the performance of the lithium-sulfur battery; (3) the final product of the reaction, Li 2 S is also an electronic insulator and will be deposited on the sulfur electrode, while lithium ions migrate slowly in solid lithium sulfide, slowing down the electrochemical reaction kinetics; (4) sulfur and the final product Li 2 The density of S is different. When sulfur is lithiated, the volume expands by about 79%, which easily leads to Li 2 Pulverization of S, causing safety problems in lithium-sulfur batteries
The above deficiencies restrict the development of lithium-sulfur batteries, which is also a key issue that needs to be solved in current research on lithium-sulfur batteries.

Method used

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  • Preparation method of three-dimensional sulfur-doped graphene/sulfur composite material electrode slice

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Mix and grind 1 g of graphite oxide and 0.8 g of benzene disulfide, and then put it into a nitrogen-protected muffle furnace at 800 ° C for 120 minutes to react. After the reaction, it is naturally cooled to room temperature to obtain sulfur-doped graphene.

[0019] (2) Add 1g of polyacrylonitrile, 0.7g of sulfur-doped graphene, and 0.3g of graphite oxide into 100mL of N-methylpyrrolidone, stir evenly and ultrasonically react for 30 minutes, then coat the mixed slurry on aluminum foil, Vacuum drying to obtain electrode sheets.

[0020] (3) Put the obtained electrode sheet into an inert gas-protected muffle furnace, slowly raise the temperature to 400°C at a rate of 3°C / min, react for 60 minutes, and cool naturally.

[0021] (4) Completely insert the electrode sheet obtained in (3) into 0.5mol / L Na 2 S 2 o 3 In the solution, stand still for 30 minutes, then slowly add 1mol / L hydrochloric acid dropwise to the solution until the solution pH=6.5, take out the electro...

Embodiment 2

[0023] (1) 1g of graphite oxide and 1.2g of benzene disulfide were mixed and ground, and then placed in a nitrogen-protected muffle furnace at 1200°C for 20 minutes to react. After the reaction, it was naturally cooled to room temperature to obtain sulfur-doped graphene.

[0024] (2) Add 1g of polyacrylonitrile, 0.9g of sulfur-doped graphene, and 0.1g of graphite oxide into 100mL of N-methylpyrrolidone, stir evenly and ultrasonically react for 120 minutes, then coat the mixed slurry on aluminum foil, Vacuum drying to obtain electrode sheets.

[0025] (3) Put the obtained electrode sheet into an inert gas-protected muffle furnace, slowly raise the temperature to 500°C at a rate of 5°C / min, react for 30 minutes, and cool naturally.

[0026] (4) Fully insert the electrode piece obtained in (3) into 2mol / L Na 2 S 2 o 3 In the solution, stand still for 60 minutes, then slowly add 1mol / L hydrochloric acid dropwise to the solution until the solution pH=7.5, take out the electrode ...

Embodiment 3

[0028] (1) Mix and grind 1g of graphite oxide and 1g of benzene disulfide, then put it in a nitrogen-protected muffle furnace at 900°C for 100 minutes, and cool it down to room temperature naturally after the reaction to obtain sulfur-doped graphene.

[0029] (2) Add 1g of polyacrylonitrile, 0.75g of sulfur-doped graphene, and 0.25g of graphite oxide into 100mL of N-methylpyrrolidone, stir evenly and ultrasonically react for 60 minutes, then coat the mixed slurry on aluminum foil, Vacuum drying to obtain electrode sheets.

[0030] (3) Put the obtained electrode sheet into an inert gas-protected muffle furnace, slowly raise the temperature to 450°C at a rate of 4°C / min, react for 45 minutes, and cool naturally.

[0031] (4) Fully insert the electrode piece obtained in (3) into 1mol / L Na 2 S 2 o 3 In the solution, stand still for 50 minutes, then slowly add 1mol / L hydrochloric acid dropwise to the solution until the pH of the solution is 7, take out the electrode sheet, and o...

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Abstract

The invention provides a preparation method of a three-dimensional sulfur-doped graphene / sulfur composite material electrode slice. The preparation method comprises the following steps of step (1) mixing and grinding graphite oxide and benzene disulfide, then placing in a nitrogen protection muffle furnace for reacting, and naturally cooling to room temperature after reaction to obtain sulfur-doped graphene; step (2) adding polyacrylonitrile, the sulfur-doped graphene and graphite oxide into N-methyl pyrrolidone, performing ultrasonic reaction, then coating an aluminum foil with mixed slurry, and drying to obtain an electrode slice; step (3) placing the obtained electrode slice into a muffle furnace protected by inert gas, slowly heating to 400 to 500DEG C, and naturally cooling; step (4) completely inserting the electrode slice obtained in the step (3) into a Na2S2O3 solution, slowly dripping hydrochloric acid into the solution, and drying to obtain a positive electrode slice. The electrode slice prepared by the preparation method provided by the invention can be directly used for a cathode of a lithium sulfur battery without adding any conductive agent and bonding agent, so that the cost of the electrode is greatly reduced.

Description

technical field [0001] The invention relates to the synthesis of nanometer materials, in particular to a preparation method of a cathode material of a lithium-sulfur battery. Background technique [0002] A lithium-sulfur battery is a battery system in which metallic lithium is used as the negative electrode and elemental sulfur is used as the positive electrode. Lithium-sulfur batteries have two discharge platforms (about 2.4V and 2.1V), but their electrochemical reaction mechanism is relatively complicated. Lithium-sulfur batteries have the advantages of high specific energy (2600Wh / kg), high specific capacity (1675mAh / g), and low cost, and are considered to be a promising new generation of batteries. However, at present, there are problems such as low utilization of active materials, low cycle life and poor safety, which seriously restrict the development of lithium-sulfur batteries. The main reasons for the above problems are as follows: (1) elemental sulfur is an elec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/1393
CPCH01M4/1393Y02E60/10
Inventor 钟玲珑肖丽芳
Owner 钟玲珑
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