Lithium sulfide solid electrolyte material with lithium tin alloy and silver chloride and preparation method therefor

A solid electrolyte, silver chloride technology, applied in solid electrolytes, non-aqueous electrolytes, circuits, etc., can solve the problems of reducing the proportion of lithium sulfide, reducing the density of movable lithium ions, and high additive content, and achieving the effect of improving conductivity

Inactive Publication Date: 2017-08-18
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 chloride

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), put the chloride equivalent to 2.5% of the mass of the above-mentioned lithium sulfur phosphoru...

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 chloride powder is 250-300 order;

[0041] In step 3), the heat treatment is carried out at 80° 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 3.7×10 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 chloride powder is 200 mesh, and the addition of the silver chloride 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 100° 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 4.4×10 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 lithium tin alloy and silver chloride and preparation method therefor. The preparation method comprises the following steps of: 1) under the condition of atmosphere protection, weighing and taking the lithium sulfide, phosphorus sulfide, lithium tin alloy powder and sulphur with a mole ratio of 2.5-4.0:0.5-1.0:0.02-0.1:0.01-0.05, and mixing evenly so as to obtain a lithium-sulfur-phosphorus-tin mixture; 2) under the conditions of atmosphere protection and safe red light, taking the lithium-sulfur-phosphorus-tin mixture and the silver chloride of which the quality is equivalent to 1-5% of the quality of the mixture, and putting into a ball mill tank for ball milling so as to obtain an amorphous lithium-sulfur-phosphorus-tin mixture containing the silver chloride; and 3) carrying out sealing on the amorphous lithium-sulfur-phosphorus-tin mixture containing the silver chloride obtained under the condition of atmosphere protection; and carrying out heat treatment under the condition of vacuum by heating up to 80-150 DEG C, thus obtaining the lithium sulfide solid electrolyte material with lithium tin alloy and silver chloride. According to the lithium sulfide solid electrolyte material with lithium tin alloy and silver chloride and preparation method therefor, the lithium tin alloy and the silver chloride are added simultaneously, so that lithium ion conductivity of the solid electrolyte material obtained can be improved.

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 chloride 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-io...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0562H01M10/0525
CPCH01M10/0525H01M10/0562H01M2300/0068Y02E60/10
Inventor 王振宇朱凌云张天锦何旻雁刘鑫雨
Owner GUILIN ELECTRICAL EQUIP SCI RES INST
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