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Preparation method of sulfide solid electrolyte

A solid electrolyte and sulfide technology, applied in the field of lithium-ion batteries, can solve the problems of poor air stability and achieve moderate crystallinity, good water resistance and oxidation resistance, and high safety effects

Pending Publication Date: 2020-11-10
湖南恩捷前沿新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, sulfide solid electrolytes still have disadvantages such as poor air stability.

Method used

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  • Preparation method of sulfide solid electrolyte
  • Preparation method of sulfide solid electrolyte
  • Preparation method of sulfide solid electrolyte

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh 2N pure reagent Li according to the required stoichiometric ratio 2 S, P 2 S 5 and LiCl, put it into a zirconia ball mill jar after mixing, add zirconia balls and ball mill, the ball milling speed is 300rpm, ball mill for 6 hours, then take it out and manually grind it with a mortar for 15min, after sieving through a 300-mesh sieve, you can get a well-mixed Precursor. Place the precursor in the ceramic vibrating tank in the microwave equipment and vibrate and turn over. The schematic diagram of the equipment is shown in Figure 4 As shown, the vibration frequency is 10Hz, the amplitude is 5mm, the temperature is raised to 150°C at a rate of 30°C / min, and the temperature is kept for 10min. After cooling, Li 6 P.S. 5 Cl solid electrolyte powder, please refer to the physical map of solid electrolyte powder figure 1 . from image 3 According to XRD, it can be found that the solid electrolyte powder prepared by this method is argentite-type cubic phase, with goo...

Embodiment 2

[0026] Weigh 2N pure reagent Li according to the required stoichiometric ratio 2 S, P 2 S 5 and LiBr, put it into a zirconia ball mill jar after mixing, add zirconia balls and ball mill, the ball milling speed is 600rpm, ball mill for 6 hours, then take it out and manually grind it with a mortar for 15min, after sieving through a 600-mesh sieve, you can get a well-mixed Precursor. Place the precursor in the ceramic vibrating tank in the microwave equipment and vibrate and flip, the vibration frequency is 20Hz, the amplitude is 5mm, the temperature is raised to 300°C at a rate of 10°C / min, and the temperature is kept for 40min. After cooling, Li 6 P.S. 5 Br solid electrolyte powder, press the obtained powder under a pressure of 200Mpa, hold the pressure for 3min, and obtain a solid electrolyte tablet. The whole process was carried out under an argon protective atmosphere. The lithium electrical conductivity of the solid electrolyte sheet at room temperature is 4×10 -3 S c...

Embodiment 3

[0028] Weigh 2N pure reagent Li according to the required stoichiometric ratio 2 S, P 2 S5, LiCl and SiS 2 , after mixing, put it into a zirconia ball mill jar, add zirconia balls and mill it, the ball milling speed is 800rpm, mill for 8 hours, then take it out and manually grind it with a mortar for 15 minutes, and sieve through a 300-mesh sieve to get a uniformly mixed precursor . Place the precursor in the ceramic vibrating tank of the microwave equipment and vibrate and flip, the vibration frequency is 20Hz, the amplitude is 5mm, the temperature is raised to 300°C at a rate of 15°C / min, and the temperature is kept for 20min. After cooling, Li 5.4 Si 0.2 P.S. 5 Cl solid electrolyte powder, press the obtained powder under a pressure of 200Mpa, hold the pressure for 3min, and obtain a solid electrolyte tablet. The whole process was carried out under an argon protective atmosphere. The lithium electrical conductivity of the solid electrolyte sheet at room temperature is ...

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Abstract

The invention discloses a preparation method of sulfide solid electrolyte, which comprises: (1) weighing Li2S, P2S5 and an X-containing lithium salt according to a required stoichiometric ratio, and uniformly mixing, with the X comprising one or a plurality of Cl, Br and I; (2) grinding and screening the uniformly mixed mixture to obtain a uniformly mixed precursor; and (3) putting the precursor into a ceramic vibration tank in microwave equipment, vibrating and overturning, carrying out microwave sintering at the temperature of 150 to 400 DEG C for 10 min to 1 hour, and cooling to obtain theargyrodite type solid electrolyte containing Li, P, S and X elements. The method is simple in process and low in sintering temperature, product components are easy to control, the argyrodite type cubic phase solid electrolyte stable at the room temperature can be obtained, and the method can be applied to industrial large-scale production.

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 sulfide solid electrolyte. Background technique [0002] With the rapid development of new energy technologies, the demand for secondary battery systems with high energy density and high safety is increasingly urgent. Commercial lithium-ion batteries mostly use liquid organic electrolytes, which are flammable and explosive. Compared with them, solid-state electrolytes are safer. Compared with the traditional liquid electrolyte lithium battery, the all-solid-state lithium secondary battery using the inorganic solid-state electrolyte has the following characteristics in theory: (1) no leakage and combustion of the electrolyte occurs, which improves safety; (2) in the all-solid-state In batteries, the solid electrolyte has dual functions as a separator and an electrolyte; (3) Compared with traditional polymer separators, it has be...

Claims

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Application Information

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IPC IPC(8): C01B25/14C01B25/08H01M10/0525H01M10/0562
CPCC01B25/08C01B25/14C01P2002/72C01P2004/01C01P2006/40H01M10/0525H01M10/0562H01M2300/0068Y02E60/10
Inventor 刘芳洋孙振吕娜蒋良兴贾明
Owner 湖南恩捷前沿新材料科技有限公司
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