Unlock instant, AI-driven research and patent intelligence for your innovation.

A low-cost method for large-scale preparation of sulfide solid-state electrolytes

A solid-state electrolyte and sulfide technology, applied in the field of lithium-ion batteries, can solve problems such as difficult dissolution, long reaction time, and low ionic conductivity of solid-state electrolytes, so as to reduce costs and realize the effect of closed-loop process

Active Publication Date: 2022-03-01
高能时代(珠海)新能源科技有限公司
View PDF11 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the solid-phase method is mainly based on heat treatment after high-energy ball milling, but high-energy ball milling itself has a low yield and is not suitable for large-scale industrial production
In the liquid phase method, due to the Li 2 S,P 2 S 5 etc. are not easy to dissolve, while the reaction time is long, and the purity of the synthetic material is low, resulting in generally low ionic conductivity of the obtained solid electrolyte.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A low-cost method for large-scale preparation of sulfide solid-state electrolytes
  • A low-cost method for large-scale preparation of sulfide solid-state electrolytes
  • A low-cost method for large-scale preparation of sulfide solid-state electrolytes

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Weigh 2N (99%) pure reagents Li and P according to the stoichiometric ratio of 3:1, put in excess CS 2 In the solvent, after stirring and mixing, put it into a stirred high-pressure reactor and seal it. Continue to heat up to 300°C, and stop the temperature rise when the pressure reaches 20 atmospheres, and the reaction time is 6 hours. Cool and release the pressure, then filter to obtain Li 3 P.S. 4 and carbon blends. The mixed material was dissolved in THF, then filtered and distilled under reduced pressure to obtain Li 3 P.S. 4 Precursor. Finally put Li 3 P.S. 4 The precursor was sintered at 350 °C for 8 h to obtain the finished Li 3 P.S. 4 solid electrolyte. After passing through a 400-mesh sieve, Li 3 P.S. 4 Solid electrolyte powder.

[0056] All the above processes were carried out under the protective atmosphere of argon.

[0057] figure 1 for Li 3 P.S. 4 XRD pattern of solid electrolyte powder. Press the solid electrolyte powder under a pressur...

Embodiment 2

[0059] combine figure 2 As shown, weigh 2N pure reagent Li, P, CCl according to stoichiometric ratio 6:1:0.25 4 put in excess CS 2 In the solvent, after stirring and mixing, put it into a stirred high-pressure reactor and seal it. Continue to heat up to 350°C, and stop the temperature rise when the air pressure reaches 80 atmospheres, and the reaction time is 12 hours. Cool and release the pressure, then filter to obtain Li 6 P.S. 5 Mixed material of Cl and carbon, CS obtained by filtration 2 Solvents can be recycled. The mixed material was dissolved in THF, then filtered and distilled under reduced pressure to obtain Li 6 P.S. 5 Cl precursor, tetrahydrofuran solvent after vacuum distillation can be recycled. Finally put Li 6 P.S. 5 The Cl precursor was sintered at 450 °C for 8 h to obtain Li 6 P.S. 5 Cl solid electrolyte. After passing through a 400-mesh sieve, Li 6 P.S. 5 Cl solid electrolyte powder finished product.

[0060] All the above processes were car...

Embodiment 3

[0063] Weigh 2N pure reagent Li, P, CCl according to stoichiometric ratio 5.5:1:0.375 4 put in excess CS 2 In the solvent, after stirring and mixing, put it into a stirred high-pressure reactor and seal it. Continue to heat up to 320°C, and stop the temperature rise when the air pressure reaches 120 atmospheres, and the reaction time is 20 hours. Cool and release the pressure, then filter to obtain Li 5.5 P.S. 4.5 Cl 1.5 and carbon blends. The mixed material was dissolved in ethanol, then filtered and distilled under reduced pressure to obtain Li 5.5 P.S. 4.5 Cl 1.5 Precursor. Finally put Li 5.5 P.S. 4.5 Cl 1.5 The precursor was sintered at 500 °C for 12 h to obtain the finished Li 5.5 P.S. 4.5 Cl 1.5 solid electrolyte. After passing through a 400-mesh sieve, Li 5.5 P.S. 4.5 Cl 1.5 Solid electrolyte powder.

[0064] All the above processes were carried out under the protective atmosphere of argon.

[0065] Figure 4 for Li 5.5 P.S. 4.5 Cl 1.5 XRD patter...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
electrical conductivityaaaaaaaaaa
Login to View More

Abstract

The invention discloses a low-cost large-scale method for preparing a sulfide solid-state electrolyte, the method comprising: combining Li, P and CS 2 Mix to get a mixture; alternatively, combine Li, P, CY 4 and CS 2 Mix to obtain a mixture, wherein Y is one or more of Cl, Br, and I; the mixture is placed in a reactor, reacted at a preset pressure and a first preset temperature, and is cooled and filtered to obtain Mixed material; dissolving the mixed material in a polar solvent, and filtering; distilling the filtered solution to obtain a sulfide solid electrolyte precursor, and sintering the sulfide solid electrolyte precursor at a second preset temperature, A sulfide solid electrolyte is obtained. This method not only avoids the expensive Li 2 The use of S, while using a solvent method that can be generated on a large scale. At the same time, the method has cheap raw materials, high solvent recycling rate, and the prepared sulfide solid electrolyte has high ion conductivity.

Description

technical field [0001] The invention belongs to the technical field of lithium ion batteries, and in particular relates to a method for preparing sulfide solid electrolytes on a large scale at low cost. Background technique [0002] With the increasing demand for energy storage systems with high energy density and high safety, Li-ion batteries based on traditional flammable electrolytes are facing great challenges. All-solid-state battery technology has attracted much attention due to the use of non-flammable electrolyte components. [0003] So far, sulfide solid-state electrolytes are considered to be favorable competitors in all-solid-state lithium batteries due to their extremely strong processability and high ionic conductivity. Compared with the oxide solid electrolyte, the synthesis temperature of the sulfide solid electrolyte is lower, the Young's modulus is lower, it is easier to process and densify, and the interface contact with the positive and negative electrode...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/0562H01M10/0525
CPCH01M10/0562H01M10/0525H01M2300/0068Y02E60/10
Inventor 林坚业刘延成
Owner 高能时代(珠海)新能源科技有限公司