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Preparation method of sulfur composite positive electrode material and all-solid-state lithium-sulfur battery

A composite positive electrode material, lithium-sulfur battery technology, applied in the direction of lithium batteries, positive electrodes, battery electrodes, etc., can solve the problems of large interface impedance, poor solid-solid contact, poor cycle performance, etc.

Active Publication Date: 2020-10-20
湖南恩捷前沿新材料科技有限公司
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  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation method of a sulfur composite positive electrode material and an all-solid-state lithium-sulfur battery, aiming at solving the problem of sulfur element and conductive carbon (electron-conducting agent) inside the sulfur composite positive electrode material in the existing all-solid-state lithium-sulfur battery. Electrolyte (ionic conductive agent) has technical problems such as poor solid-solid contact, large interface impedance, poor cycle performance and low charge and discharge capacity

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  • Preparation method of sulfur composite positive electrode material and all-solid-state lithium-sulfur battery

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preparation example Construction

[0027] The invention provides a method for preparing a sulfur composite cathode material for an all-solid-state lithium-sulfur battery, comprising the following steps:

[0028] (1) Uniformly mixing the conductive carbon and the sulfide solid electrolyte by ball milling to obtain mixed conductor powder, wherein the ball milling speed is 100-500 rpm, the ball milling time is 0.5-10 hours, and the ball milling is completed under the protection of an inert atmosphere;

[0029] (2) Screening the mixed conductor powder of step (1) with a sieve to obtain the sieved mixed powder;

[0030] (3) Place the sulfur element in the high temperature zone of the tube furnace, place the sieved mixed powder obtained in step (2) in the drum sieve in the low temperature zone of the tube furnace, start the high and low temperature zone and roll the drum sieve, and after a certain period of time, the sulfur vapor will Deposited on the mixed powder and cooled to room temperature to obtain a sulfur com...

Embodiment 1

[0037] (1) Preparation of sulfide solid electrolyte Li 6 P.S. 5 Cl

[0038] Weigh 2N pure reagent Li according to the required stoichiometric ratio 2 S, P 2 S 5 After mixing with LiCl, put it into a zirconia ball mill tank, add zirconia balls and mill it at a speed of 300rpm for 6h, and then take out the milled powder and sieve it with a 300-mesh sieve to obtain a uniformly mixed precursor. Place the precursor in the ceramic vibration tank in the microwave equipment and vibrate and turn over, the vibration frequency is 20Hz, the amplitude is 5mm, keep it at 300°C for 10min, and obtain Li 6 P.S. 5 Cl solid electrolyte powder.

[0039] The obtained powder was pressed under a pressure of 200 MPa for 3 minutes to obtain a solid electrolyte sheet. The whole process was carried out under an argon protective atmosphere. The lithium conductivity of the solid electrolyte sheet at room temperature is 3.5×10 -3 Scm -1 .

[0040] (2) Preparation of sulfur composite cathode mate...

Embodiment 2

[0045] (1) Preparation of sulfide solid electrolyte Li 6 P.S. 5 Cl

[0046] The Li 6 P.S. 5 The Cl electrolyte was also synthesized by microwave sintering. The preparation method is the same as in Example 1.

[0047] (2) Preparation of sulfur composite cathode materials

[0048] Weigh 55mg carbon nanotubes and 100mgLi respectively 6 P.S. 5 The Cl solid electrolyte was placed in a ball mill jar, and ball milled at 300 rpm for 3 h in an Ar atmosphere. After ball milling, the powder was sieved in a 2000-mesh sieve to obtain a uniformly mixed powder. Then, weigh 1.5g of elemental sulfur and place it in a quartz crucible, and place it in a high-temperature zone; then spread the sieved mixed conductor powder in a drum sieve in a low-temperature zone. The diameter of the drum sieve is 40 mm, and the length is 100 mm. The size is 5000 mesh, and the rotating speed of the trommel screen is 60rpm. The temperature in the high-temperature zone was 350°C, and the temperature in the...

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Abstract

The invention discloses a preparation method of a sulfur composite positive electrode material and an all-solid-state lithium-sulfur battery. The method comprises the following steps of ball-milling and mixing conductive carbon and sulfide solid electrolyte, and sieving to obtain uniformly mixed conductor powder, and placing elemental sulfur in a high-temperature area of a vacuum tube furnace, placing the mixed conductor powder in a low-temperature area of the vacuum tube furnace, uniformly depositing sulfur vapor in the turned mixed powder, and cooling to room temperature to obtain the sulfurcomposite positive electrode material. The sulfur composite positive electrode material prepared by the method is small in sulfur particle size and large in specific surface area, and is in uniform and close contact with mixed powder, and the obtained all-solid-state lithium-sulfur battery is small in overall impedance, high in active substance utilization rate, low in capacity loss and stable incycle performance.

Description

technical field [0001] The invention belongs to the technical field of lithium-ion batteries, and in particular relates to a preparation method of a sulfur composite cathode material and an all-solid-state lithium-sulfur battery. Background technique [0002] Among various battery technologies, lithium-ion batteries have the characteristics of high specific energy, high efficiency and long life, which make them stand out among many types of batteries and occupy the portable electronics market. The widely used traditional lithium-ion battery mainly uses liquid organic electrolyte, which has high ionic conductivity and good wettability, but its narrow temperature window greatly limits the application environment of the battery, and the narrow electrochemical stability window not only limits the battery The increase in energy density can also easily lead to various safety issues. Traditional lithium-ion batteries can no longer meet the increasing energy density and safety requ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/38H01M4/62H01M10/052
CPCH01M4/362H01M4/38H01M4/624H01M4/625H01M10/052H01M2004/021H01M2004/028Y02E60/10
Inventor 刘芳洋孙振胡雅琪蒋良兴贾明
Owner 湖南恩捷前沿新材料科技有限公司
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