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Preparation method of crystalline state Li-Sn-S series inorganic lithium ion solid electrolyte

A solid electrolyte, inorganic lithium technology, applied in circuits, electrical components, secondary batteries, etc., can solve problems such as corrosion of electrodes, oxidative combustion, liquid leakage, etc., and achieve the effect of short reaction time

Active Publication Date: 2015-07-01
湖南国拓机械有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, the organic electrolyte used in lithium-ion batteries on the market has safety problems such as leakage, corrosion of electrodes, and even oxidative combustion.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] An inorganic solid electrolyte Li 4 SnS 4 The preparation method is as follows:

[0013] In a three-necked flask, 5.0350g (120mmol) LiOH·H 2 O is stirred and dissolved in water, and H is passed into it 2 S gas, the rate is 10mL / min, after 25~35min, the excess H 2 S gas is absorbed with KOH solution, and then 5.259g (15mmol) SnCl 4 ·5H 2 After O was dissolved in 10 mL of water, it was added into a three-necked flask, and the yellow precipitate formed was completely dissolved. Add excess LiOH·H 2 O, adjust the pH between 11 and 12, under the condition of nitrogen atmosphere, react at 45°C for 8h, then add acetone to the flask, and then place it in the environment of 0°C for 48h, until white crystals are precipitated. The precipitate was extracted by filtration and rinsed several times with acetone, and the crystal precipitate was dried in vacuum for 12 hours to obtain a light gray powder, which was then kept at 350°C for 12 hours to remove the crystal water of the ...

Embodiment 2

[0015] In a three-necked flask, 120mmol LiOH·H 2 O was stirred and dissolved in water, and 60 mmol of K was added to it 2 After S, add 15mmol of SnCl 4 ·5H 2 After O was dissolved in 10 mL of water, it was added into a three-necked flask, and the yellow precipitate formed was completely dissolved. The following steps are exactly the same as in Example 1.

Embodiment 3

[0017] In a three-necked flask, 120mmolLiOH·H 2 O is stirred and dissolved in water, and H is passed into it 2 S gas, the rate is 10mL / min, after 25~35min, the excess H 2 S gas is absorbed with KOH solution, and then 15mmol of SnBr 4 ·5H 2 After O was dissolved in 10 mL of water, it was added into a three-necked flask, and the yellow precipitate formed was completely dissolved. Add excess LiOH·H 2 O, adjust the pH between 11 and 12, under the condition of nitrogen atmosphere, react at 80°C for 3h, then add ethanol to the flask, and then place it in the environment of 0°C for 48h, until white crystals are precipitated. Extract the precipitate by filtration, wash it with ethanol several times, dry the crystal precipitate in vacuum for 8 hours to obtain a light gray powder, and then keep it at 320°C for 12 hours to remove the crystal water of the powder product to obtain a crystalline inorganic solid electrolyte Li 4 SnS 4 .

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PUM

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Abstract

The invention provides a preparation method of a crystalline state Li-Sn-S series inorganic lithium ion solid electrolyte. The method comprises the following steps: introducing H2S gas or adding a water-soluble sulfide into a LiOH.H2O aqueous solution in an enclosed container, reacting for a certain time period, and adding an aqueous solution containing a metal Sn element; introducing protective gas for reacting continually, adding an organic reagent, putting the mixture into a low-temperature environment, drying a crystal which is separated out, and removing crystalized water by means of thermal treatment to obtain a product. An all-solid electrolyte is prepared by adopting a novel wet process. Compared with the conventional solid-phase synthesis, the method has the remarkable advantages of short reaction time and controllability of the product morphology.

Description

technical field [0001] The invention relates to a preparation method of a solid electrolyte for an all-solid lithium ion battery, in particular to a preparation method of a crystalline Li-Sn-S inorganic lithium ion solid electrolyte. Background technique [0002] At present, the organic electrolyte used in lithium-ion batteries on the market has safety problems such as leakage, electrode corrosion and even oxidative combustion. Lithium ion inorganic solid electrolyte can well avoid the above problems, and has high lithium ion conductivity (up to 10 -2 S / cm), good chemical stability, large potential window (5 ~ 10V), etc., and can be combined with high specific energy energy storage material sulfur electrodes, it is very promising to develop high specific energy, safety, and high temperature use. New lithium-ion battery. Li-Sn-S inorganic lithium-ion solid electrolyte is a kind of electrolyte material that has been studied more at present. For example, the applicant Toyota ...

Claims

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Application Information

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IPC IPC(8): H01M10/0562
CPCH01M10/0525H01M10/0562Y02E60/10
Inventor 韦伟峰曾小慧丁正平柳佳图陈立宝张大同
Owner 湖南国拓机械有限责任公司
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