Efficient preparation method of sulfur halide compound solid electrolyte

A solid electrolyte and compound technology, applied in the manufacture of electrolyte batteries, non-aqueous electrolyte batteries, circuits, etc., can solve the problems of insoluble raw materials, long reaction time, low output, etc. The effect of yield

Active Publication Date: 2022-03-11
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

In dry ball milling, the distribution of raw materials is uneven, and it is easy to stick to the inner wall of the ball milling tank and the surface of ball milling beads, and the yield is low; while in wet ball milling, the raw materials do not have enough contact with each other due to the existence of the grinding medium, and the pre-reaction is not thorough enough, so it cannot Obtain the expected crystal phase
The disadvantage of the liquid phase method is that the reaction time is longer, the raw materials are difficult to dissolve, and the ionic conductivity of the obtained solid electrolyte is generally low.

Method used

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  • Efficient preparation method of sulfur halide compound solid electrolyte
  • Efficient preparation method of sulfur halide compound solid electrolyte

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh Li according to the stoichiometric ratio of 5:1:2 2 S, P 2 S 5 and LiCl, then Li 2 S, P 2 S 5 The mass ratio of the total mass of LiCl and the grinding medium is 1:3, and an appropriate amount of ethyl propionate is weighed, and it is successively packed into a zirconia vacuum ball mill jar, and simultaneously, zirconia ball milling beads are added at a ball-to-material ratio of 40:1. And fill it with argon gas of 0.15Mpa to carry out ball milling for 4 hours at a speed of 400r / min. Thereafter, the ball milling tank was evacuated and heated to 120° C. for a second ball milling for 8 hours at a rotational speed of 800 r / min. Thereafter, the ball mill jar was cooled and filled with 0.15Mpa argon to perform ball milling three times for 2 hours at a rotational speed of 300r / min. After the ball milling, the solid electrolyte precursor slurry was dried under the protection of an inert atmosphere at a temperature of 150° C. for 40 h. The dried solid electrolyte pr...

Embodiment 2

[0029] Weigh Li according to the stoichiometric ratio of 5:1:0.8:1.2 2 S, P 2 S 5 , LiCl and LiBr, then press Li 2 S, P 2 S 5 The mass ratio of the total mass of LiCl and LiBr to the grinding medium is 1:3. Weigh an appropriate amount of propylene oxide, put it into a zirconia vacuum ball milling tank in turn, and add zirconia ball milling beads at a ball-to-material ratio of 40:1 , and filled with argon gas of 0.15Mpa to carry out a ball milling, the time is 4h, the rotating speed is 400r / min. Thereafter, vacuumize the ball mill jar and heat it to 150° C. for a second ball mill for 8 hours at a rotational speed of 800 r / min. Thereafter, the ball mill jar was cooled and filled with 0.15Mpa argon to perform ball milling three times for 2 hours at a rotational speed of 300r / min. After the ball milling, the solid electrolyte precursor slurry was dried under the protection of an inert atmosphere at a temperature of 150° C. for 48 h. The dried solid electrolyte precursor was...

Embodiment 3

[0031] Weigh Li according to the stoichiometric ratio of 4.5:1:1.5:1 2 S, P 2 S 5 , LiCl and LiI, then press Li 2 S, P 2 S 5The mass ratio of the total mass of LiCl and LiI to the grinding medium is 1:4. Weigh an appropriate amount of octamethylcyclotetrasiloxane, and put it into a zirconia vacuum ball mill jar in turn, and press the ball-to-material ratio of 40:1 Add zirconia ball milling beads, and fill with argon gas of 0.15Mpa to carry out ball milling for 4 hours at a speed of 400r / min. Thereafter, vacuumize the ball mill jar and heat it to 150° C. for a second ball mill for 12 hours at a rotational speed of 800 r / min. Thereafter, the ball mill jar was cooled and filled with 0.15Mpa argon to perform ball milling three times for 2 hours at a rotational speed of 300r / min. After the ball milling, the solid electrolyte precursor slurry was dried under the protection of an inert atmosphere at a temperature of 150° C. for 36 h. The dried solid electrolyte precursor was s...

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Abstract

The invention discloses a preparation method of an efficient sulfur halide compound solid electrolyte. The preparation method comprises the following steps: weighing Li2S, P2S5 and X-containing lithium salt according to a required stoichiometric ratio; weighing a grinding medium; the preparation method comprises the following steps: adding raw materials into a vacuum ball milling tank, filling argon into the ball milling tank, and performing primary ball milling in a positive pressure state; vacuumizing and heating the ball milling tank, and carrying out secondary ball milling; cooling the ball-milling tank, filling argon, and carrying out third-time ball-milling to obtain uniformly mixed solid electrolyte precursor slurry; drying the solid electrolyte precursor slurry under the protection of an inert atmosphere; and sintering the dried solid electrolyte precursor at high temperature, cooling, grinding and screening to obtain the sulfur halide compound solid electrolyte with high ionic conductivity. The sulfur halide compound solid electrolyte prepared by the invention has relatively high ionic conductivity and a relatively wide electrochemical window. In addition, compared with a traditional preparation method, the method has the potential of large-scale production.

Description

technical field [0001] The invention belongs to the technical field of lithium-ion batteries, and in particular relates to a method for preparing a sulfur-halogen compound solid-state electrolyte. Background technique [0002] The development of electric vehicles can reduce my country's dependence on foreign oil, improve energy security, and support major national development strategies. However, at this stage, the power batteries are all liquid batteries. The lithium dendrites formed during the electrochemical cycle can easily cause the liquid batteries to fail or even short-circuit, which can seriously cause the car to spontaneously ignite. The solid-state battery can avoid this phenomenon and improve the safety of the battery. In addition, the theoretical energy density of the solid-state battery is greater than that of the existing liquid battery, which is an inevitable trend of future development. However, the preparation and large-scale production of solid electrolyte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/547C04B35/622H01M10/052H01M10/0562H01M10/058
CPCC04B35/547C04B35/622H01M10/0562H01M10/058H01M10/052C04B2235/446C04B2235/444C04B2235/6567Y02E60/10Y02P70/50
Inventor 刘芳洋刘汉周张宗良
Owner 湖南恩捷前沿新材料科技有限公司
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