Lithium sulfide solid electrolyte material containing silver iodide and silver bromide and preparation method of lithium sulfide solid electrolyte material

A solid electrolyte, silver bromide technology, applied in solid electrolytes, electrolyte battery manufacturing, non-aqueous electrolytes, etc., can solve the problems of low battery coulombic efficiency, hinder lithium ion passing, difficult to maintain charge-discharge cycle, etc., to improve ion conduction. rate, and the effect of improving ion conductivity

Pending Publication Date: 2017-05-17

GUILIN ELECTRICAL EQUIP SCI RES INST

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AI-Extracted Technical Summary

Problems solved by technology

Nevertheless, the applicant believes that this invention is a lithium-ion-free and relies on Ag + The conductive solid electrolyte does not increase the diffusion channel of lithium ions by generating a large number of new atomic vacancies so as to achieve the effect of improving the lithium ion conductivity of the sulfide-based solid electrolyte; the silver ion conductive solid prepared by the method described in the invention The electrolyte is not suitable for use as a solid electrolyte between the positive and negative electrodes of an all-solid lithium battery because: Ag + Migration is not accompanied by electrochemical react...

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Abstract

The invention discloses a lithium sulfide solid electrolyte material containing silver iodide and silver bromide and a preparation method of the lithium sulfide solid electrolyte material. The preparation method comprises the following steps of (1) weighing 35%-50% of lithium sulfide and the balance of phosphorus sulfide according to mass percents under the condition of atmosphere protection and mixing evenly to obtain a lithium-sulfur-phosphorus ternary mixture; (2) taking the lithium-sulfur-phosphorus ternary mixture, the silver iodide which is equivalent to 2%-6% of the mass of the lithium-sulfur-phosphorus ternary mixture and the silver bromide which is equivalent to 1%-5% of the mass of the lithium-sulfur-phosphorus ternary mixture under the conditions of atmosphere protection and safe red light and carrying out ball-milling to obtain an amorphous lithium-sulfur-phosphorus mixture containing the silver iodide and the silver bromide; and (3) sealing the obtained amorphous lithium-sulfur-phosphorus mixture containing the silver iodide and the silver bromide under the conditions of atmosphere protection and red light, and heating the amorphous lithium-sulfur-phosphorus mixture to 100-200 DEG C under a vacuum condition or the condition of atmosphere protection for thermal treatment. According to the method disclosed by the invention, the ion conductivity of the obtained lithium sulfide solid electrolyte material can be effectively improved.

Application Domain

Material nanotechnologySolid electrolytes +3

Technology Topic

Lithium sulfideIon +8

Examples

Experimental program(5)
Comparison scheme(1)

Example Embodiment

[0028] Example 1

[0029] 1) Preparatory mixing process of sulfide:

[0030] According to mass percentage, weigh 40% of lithium sulfide and 60% of phosphorus sulfide in a glove box with low moisture (≤1ppm) and low oxygen content (≤1ppm) with argon atmosphere protection, and mix them with zirconium dioxide After the balls are matched, they are sealed in a ball mill tank. The mass ratio of the zirconia balls to the mixture in the tank is 2:0.7; the sealed ball mill tank is installed in a planetary high-energy ball mill using a dry premixed ball mill, and the ball milling time is In 5 hours, a lithium-sulfur-phosphorus ternary mixture (LiPS mixture for short) is obtained;

[0031] 2) Secondary high-energy ball milling process:

[0032] In a glove box with safety lights (such as red light) with low moisture (≤1ppm) and low oxygen content (≤1ppm) with argon atmosphere protection, silver iodide powder (particle size) equivalent to 2.5% of the mass of the above LiPS mixture 200-250 mesh) and silver bromide powder (particle size 200-250 mesh) equivalent to 1% of the mass of the LiPS mixture is manually stirred and mixed with the LiPS mixture, and the resulting mixture is then mixed with the ball mass ratio of 2:0.7 and the diameter The 3-10mm zirconia ball is sealed in a ball milling jar, sealed, and the sealed ball milling jar is put into a planetary high-energy ball mill for high-energy dry ball milling. The milling time is 36 hours to obtain silver iodide and silver bromide. Amorphous lithium-sulfur-phosphorus mixture;

[0033] 3) In-situ precipitation reaction process:

[0034] Put the resulting amorphous lithium-sulfur-phosphorus mixture containing silver iodide and silver bromide in a glove with safety light (such as red light) with low moisture (≤1ppm) and low oxygen content (≤1ppm) with argon atmosphere protection The box is sealed, and then heated to 150°C for 2 hours under vacuum conditions for heat treatment to obtain a lithium sulfide solid electrolyte material containing silver iodide and silver bromide. During the heat treatment process, part of the silver ions in the cubic structure of silver iodide and silver bromide stabilizes the cubic structure with iodine/bromide ions, and combines with the sulfur in the surrounding lithium sulfide to form nano-scale silver sulfide. At the same time, it is mainly composed of iodine/bromine. A large number of atomic vacancies that can be used for lithium ion diffusion are formed in the cubic structure; on the other hand, ion-conductivity reaction products silver sulfide and lithium iodide/lithium bromide are also formed, thereby further improving the ion conductivity characteristics of the obtained solid electrolyte material.

[0035] After pressing the solid electrolyte powder prepared in this example into a standard sample, using the CHI660 electrochemical workstation, using the AC impedance method, at room temperature 25°C, the ion conductivity of the sample in this embodiment was measured to be 4.2×10 -4 S/cm.

Example Embodiment

[0039] Example 2

[0040] Repeat Example 1, the difference is:

[0041] In step 1), the mass percentages of lithium sulfide and phosphorus sulfide are 50% and 50%, respectively, and the ball milling time is 10 hours.

[0042] After pressing the solid electrolyte powder prepared in this example into a standard sample, using the CHI660 electrochemical workstation, using the AC impedance method, at room temperature 25°C, the ion conductivity of the sample in this embodiment is measured to be 6.0×10 -4 S/cm.

Example Embodiment

[0043] Example 3

[0044] Repeat Example 1, the difference is:

[0045] In step 1), the mass percentages of lithium sulfide and phosphorus sulfide are respectively 50% and 50%, and the time of ball milling is 2 hours;

[0046] In step 2), the particle size of silver iodide and silver bromide powder are both 200-250 mesh, the amount of silver iodide powder added is equivalent to 3.5% of the mass of the LiPS mixture, and the amount of silver bromide powder added is equivalent to 2.5% of the mass of the LiPS mixture;

[0047] After pressing the solid electrolyte powder prepared in this embodiment into a standard sample, using the CHI660 electrochemical workstation, using the AC impedance method, at room temperature 25°C, the ion conductivity of the sample in this embodiment is measured to be 6.2×10 -4 S/cm.

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PUM

Property	Measurement	Unit
Granularity	200.0 ~ 250.0	mesh
Diameter	3.0 ~ 10.0	mm
Ionic conductivity	0.00042	s/cm
tensile		MPa
Particle size		Pa
strength	10

Description & Claims & Application Information

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Lithium sulfide solid electrolyte material containing silver iodide and silver bromide and preparation method of lithium sulfide solid electrolyte material

AI-Extracted Technical Summary

Problems solved by technology

Abstract

Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

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