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Lithium sulfide solid electrolyte material with addition of lithium-tin alloy and silver bromide and preparation method thereof

A solid electrolyte, silver bromide technology, applied in solid electrolytes, electrolyte battery manufacturing, non-aqueous electrolytes, etc., can solve the problems of reducing the proportion of lithium sulfide, high additive content, inability to diffuse lithium ions, etc., to improve conductivity. Effect

Inactive Publication Date: 2017-05-17
GUILIN ELECTRICAL EQUIP SCI RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The improvement of the ionic conductivity of the solid electrolyte obtained by the invention is also not ideal, and its total conductivity at room temperature is also at 10 -6 S / cm
The applicant believes that in the above invention patents (1) the additives (such as iodide or sulfide, etc.) are stable hexagonal or orthorhombic crystals, and no more atomic vacancies are introduced into the system, so they cannot be lithium ions. Diffusion provides more diffusion channels; (2) The content of additives is too high, which reduces the proportion of lithium sulfide as a lithium ion carrier in the solid electrolyte formulation, directly reducing the density of migratable lithium ions that contribute to lithium ion conduction ; (3) The high content of additives not only did not increase the lithium ion diffusion channels in the solid electrolyte, but hindered the diffusion of lithium ions
Therefore, the ingredients added in the above invention patents did not significantly improve the ion conductivity of the sulfide-based solid electrolyte
[0007] On the other hand, the research on tin-based materials first originated from Japan's Seiko Electronics Industry Company, and then Sanyo Electric, Matsushita Electric, Fuji Film and other companies successively carried out research (such as the invention patents of CN1930726A and CN101887965A), but these studies only use lithium Tin alloy powder, as a battery anode material suitable for lithium ion intercalation, is used as an anode material for thermal batteries, lithium ion batteries, lithium ion capacitors, lithium sulfur batteries, and lithium air batteries to accept the insertion of lithium ions during charging. Related studies involving the enhancement of the density of migratable lithium ions in solid electrolytes by the simultaneous addition of lithium-tin alloys and silver bromide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1) Mixed high energy ball milling process:

[0028] In a glove box protected by an argon atmosphere with low moisture (≤1ppm) and low oxygen content (≤1ppm), the molar ratio of lithium sulfide, phosphorus sulfide, lithium-tin alloy powder and sulfur powder is 4:1:0.1: The proportion of 0.05 ingredients, stirring and mixing, and the zirconia balls with a diameter of 3-10mm are sealed into the ball milling tank. The mass ratio of the zirconia balls in the tank to the mixture is 2:0.7; the sealed ball milling tank In the planetary high-energy ball mill, dry mixing ball milling is adopted, and the ball milling time is 5 hours to obtain the lithium sulfur phosphorus tin mixture;

[0029] 2) Second high energy ball milling process:

[0030] In a glove box protected by an argon atmosphere with low moisture (≤1ppm) and low oxygen content (≤1ppm) with safe lights (such as red light), bromide equivalent to 3% of the mass of the above-mentioned lithium sulfur phosphorous tin mixt...

Embodiment 2

[0038] Repeat Example 1, the difference is:

[0039] In step 1), lithium sulfide, phosphorus sulfide, lithium-tin alloy powder and sulfur powder are mixed in a molar ratio of 2.5:0.5:0.02:0.01, and the ball milling time is 3 hours;

[0040] Step 2) in, the particle size of silver bromide powder is 250-300 order;

[0041] In step 3), the heat treatment is carried out at 60° C., and the heat treatment time is 5 hours.

[0042] After the solid electrolyte powder prepared in this example was pressed into a standard sample, the ion conductivity of the sample in this example was measured to be 4.6×10 by using the AC impedance method at a room temperature of 25°C using a CHI660 electrochemical workstation. -4 S / cm.

Embodiment 3

[0044] Repeat Example 1, the difference is:

[0045] In step 1), lithium sulfide, phosphorus sulfide, lithium-tin alloy powder and sulfur powder are mixed in a molar ratio of 3.0:0.7:0.05:0.02, and the mass ratio of zirconia balls to the mixture is 2:0.5 , the ball milling time is 2 hours;

[0046] In step 2), the particle size of the silver bromide powder is 200 mesh, and the addition amount of the silver bromide powder is equivalent to 5% of the mass of the lithium sulfur phosphorus tin mixture;

[0047] In step 3), the heat treatment is carried out at 150° C., and the heat treatment time is 1 hour.

[0048] After pressing the solid electrolyte powder prepared in this example into a standard sample, the ion conductivity of the sample in this example was measured to be 5.8×10 at a room temperature of 25° C. -4 S / cm.

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Abstract

The invention discloses a lithium sulfide solid electrolyte material with the addition of lithium-tin alloy and silver bromide and a preparation method thereof. The preparation method comprises the following steps: (1) weighing lithium sulfide, phosphorus sulfide, lithium-tin alloy powder and sulfur according to a molar ratio of (2.5 to 4.0) to (0.5 to 1.0) to (0.02 to 0. 1) to (0.01 to 0.05) under an atmosphere protection condition, and uniformly mixing, thus obtaining a lithium-sulfur-phosphorus-tin mixture; (2) taking and putting the lithium-sulfur-phosphorus-tin mixture and the silver bromide which accounts for 1 to 5 percent of the lithium-sulfur-phosphorus-tin mixture in mass percentage in a ball-milling tank under atmosphere protection and safe red light conditions, and carrying out ball milling, thus obtaining an amorphous lithium-sulfur-phosphorus-tin mixture containing the silver bromide; (3) sealing the amorphous lithium-sulfur-phosphorus-tin mixture containing the silver bromide under the atmosphere protection condition, and heating to 60 to 150 DEG C under a vacuum condition for carrying out thermal treatment, thus obtaining the lithium sulfide solid electrolyte material. According to the preparation method disclosed by the invention, the lithium ionic conductivity of the obtained lithium sulfide solid electrolyte material is increased by simultaneously adding the lithium-tin alloy and the silver bromide.

Description

technical field [0001] The invention relates to a lithium sulfide solid electrolyte material, in particular to a lithium sulfide solid electrolyte material added with lithium tin alloy and silver bromide and a preparation method thereof. Background technique [0002] Lithium-ion batteries with high energy density have shown more and more important market prospects as power batteries for electric vehicles and have been widely valued. A general lithium-ion battery is composed of a positive electrode, a negative electrode, a diaphragm, an organic electrolyte, and a sealed casing. Major safety accidents such as fires caused by flammable organic electrolytes occur from time to time. Although many studies have greatly improved the performance of lithium-ion batteries in terms of material modification and battery structure, the safety problems of lithium-ion batteries containing organic electrolytes in use have not been fundamentally resolved. [0003] The use of solid lithium-ion...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/058H01M10/0562B82Y30/00
CPCB82Y30/00H01M10/0562H01M10/058H01M2300/0068Y02E60/10Y02P70/50
Inventor 王振宇朱凌云张天锦王奐然赵霞妍
Owner GUILIN ELECTRICAL EQUIP SCI RES INST
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