Preparation method of graphene/zirconium dioxide hollow sphere/sulfur composite material

A technology of zirconium dioxide and composite materials, which is applied in the field of preparation of positive electrode materials for lithium-sulfur batteries, can solve the problems of slow migration speed, reduced utilization rate of sulfur active materials, slow electrochemical reaction kinetic speed, etc., and achieves improved electronic conductivity. efficiency and ionic conductivity, and the effect of improving electrochemical performance

Inactive Publication Date: 2016-06-29
钟玲珑
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  • Abstract
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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 graphene/zirconium dioxide hollow sphere/sulfur composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Weigh 100 mg of nano-calcium carbonate powder and add it to absolute ethanol, and ultrasonicate for 20 minutes to form a suspension.

[0020] (2) Weigh 200mg of zirconium oxychloride and 40mg of yttrium chloride and dissolve in 100mL of deionized water to prepare an aqueous solution.

[0021] (3) Slowly add the aqueous solution obtained in (2) into the suspension in a 90°C water bath for 3 hours, then add ammonia water to adjust the value, then add 100mg polyethylene glycol, and continue stirring the reaction mixture. After aging for a while at room temperature, a white precipitate was obtained, which was filtered, washed, and dried to obtain a white solid. After the reaction mixture was stirred for 3 hours, it was aged at room temperature for 12 hours to obtain a white precipitate, which was filtered, washed and dried to obtain a white solid.

[0022] (4) Put the obtained white solid into a muffle furnace, heat up to 500°C at a rate of 1°C / min in an air atmosphere...

Embodiment 2

[0025] (1) Weigh 100 mg of nano-calcium carbonate powder and add it to absolute ethanol, and ultrasonicate for 60 minutes to form a suspension.

[0026] (2) Weigh 20mg of zirconium oxychloride and 16mg of yttrium chloride and dissolve in 100mL of deionized water to prepare an aqueous solution.

[0027] (3) Slowly add the aqueous solution obtained in (2) into the suspension in a 90°C water bath for 5 hours, then add ammonia water to adjust the value, then add 100mg polyethylene glycol, and continue stirring the reaction mixture for 10 hours , aged at room temperature for 24 hours to obtain a white precipitate, which was filtered, washed and dried to obtain a white solid.

[0028] (4) Put the obtained white solid into a muffle furnace, raise the temperature to 550°C at a rate of 5°C / min in an air atmosphere, calcine and react for 3 hours, put it into a 10% acetic acid solution after cooling and stir React for 0.5 hours, filter, wash with water, and dry to obtain hollow zirconia...

Embodiment 3

[0031] (1) Weigh 100 mg of nano-calcium carbonate powder and add it to absolute ethanol, and ultrasonicate for 30 minutes to form a suspension.

[0032] (2) Weigh 100mg of zirconium oxychloride and 40mg of yttrium chloride and dissolve in 100mL of deionized water to prepare an aqueous solution.

[0033] (3) Slowly add the aqueous solution obtained in (2) into the suspension in a 90°C water bath for 4 hours, then add ammonia water to adjust the value, then add 100mg polyethylene glycol, and continue stirring the reaction mixture for 6 hours , aged at room temperature for 15 hours to obtain a white precipitate, which was filtered, washed and dried to obtain a white solid.

[0034] (4) Put the obtained white solid into a muffle furnace, raise the temperature to 525°C at a rate of 3°C / min in an air atmosphere, calcine and react for 5 hours, put it into a solution with a volume concentration of 6% after cooling, and stir for reaction After 4 hours, filter, wash with water, and dry...

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Abstract

The invention provides a preparation method of a graphene / zirconium dioxide hollow sphere / sulfur composite material. The preparation method comprises the following steps of (1) weighing and adding nano calcium carbonate to absolute ethyl alcohol, carrying out ultrasound to form a suspension liquid; (2) weighing and dissolving zirconyl chloride and yttrium chloride in deionized water, and preparing to an aqueous solution; (3) adding the aqueous solution obtained in the step (2) into the suspension liquid in water bath, and adding an ammonia water adjustment value to obtain a white solid; (4) placing the white solid in a muffle, cooling the white solid, placing the white solid in an acetate solution, stirring the mixture solution and removing calcium carbonate to obtain hollow zirconium dioxide; and (5) adding the obtained hollow zirconium dioxide, elemental sulfur and graphene into carbon disulfide to obtain the composite material. A sulfur-based material is coated with zirconium dioxide hollow spheres in the graphene / zirconium dioxide hollow sphere / sulfur composite material, the dissolving of a discharging product polysulfide can be prevented, volume expansion can be reduced, and the electrochemical performance of the graphene / zirconium dioxide hollow sphere / sulfur composite material is improved.

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): H01M4/36H01M4/38H01M4/62H01M10/0525
CPCH01M4/366H01M4/38H01M4/625H01M4/628H01M10/0525Y02E60/10
Inventor 钟玲珑肖丽芳
Owner 钟玲珑
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