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Preparation method of sulfide solid electrolyte

A solid electrolyte and sulfide technology, applied in solid electrolytes, non-aqueous electrolytes, circuits, etc., can solve the problems of high price, low purity of lithium sulfide, and difficulty in industrialized production, and achieve the effect of low price and easy industrialization.

Inactive Publication Date: 2018-07-27
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] This sulfide-based solid electrolyte is mainly prepared from lithium sulfide, phosphorus pentasulfide and additives through high-energy ball milling and post-heat treatment. The solid electrolyte obtained from these conventional methods shows excellent lithium ion conductivity, but the high lithium sulfide raw material The cost and the existing lithium sulfide preparation method all need solvents, the efficiency of the solid-liquid separation process is low, the cost is high, and the solvent is toxic and harmful, it is expensive and difficult to realize industrial production, and the lithium sulfide obtained by this method has a low purity. Disadvantages of high energy consumption

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Dry the raw materials of sulfur powder, lithium hydride, phosphorus pentasulfide and lithium phosphate in a vacuum drying oven at 100°C for 12h. Under the protection of argon atmosphere, 2.24g of sulfur powder, 1.12g of lithium hydride, 6.66g of phosphorus pentasulfide and 0.116g of lithium phosphate were pre-ground in a mortar for 10 minutes, and then added to a sealed ball mill jar. The mass ratio is 20:1, and the ball is milled for 60h under the condition of 400r / min at room temperature. After the ball milling reaction, in an inert atmosphere, the powder was taken out from the ball mill jar, added to the crucible, and sintered in a high-temperature tube furnace in a nitrogen atmosphere of 80 mL / min. The sintering temperature was 300 °C, and the sintering time was 4h. The powder is taken out from the crucible to obtain a sulfide solid electrolyte.

Embodiment 2

[0025] Dry the raw materials of sulfur powder, lithium hydride, phosphorus pentasulfide and lithium phosphate in a vacuum drying oven at 80°C for 18h. Under the protection of argon atmosphere, 2.56g of sulfur powder, 1.28g of lithium hydride, 4.44g of phosphorus pentasulfide and 0.116g of lithium phosphate were pre-ground in a mortar for 10 minutes, and then added to a sealed ball mill jar. The mass ratio is 30:1, and the ball is milled at room temperature for 48h under the condition of 500r / min. After the ball milling reaction, in an inert atmosphere, the powder was taken out from the ball mill jar, added to the crucible, and sintered in a high-temperature tube furnace under a nitrogen atmosphere of 40 mL / min. The sintering temperature was 260 °C, and the sintering time was 3h. The powder is taken out from the crucible to obtain a sulfide solid electrolyte.

Embodiment 3

[0027] The raw materials of sulfur powder, lithium hydride, phosphorus pentasulfide and lithium phosphate were dried in a vacuum drying oven at 60°C for 24h. Under the protection of argon atmosphere, 2.4g of sulfur powder, 1.2g of lithium hydride, 5.55g of phosphorus pentasulfide, and 0.116g of lithium phosphate were pre-ground in a mortar for 10 minutes, and then added to a sealed ball mill. The mass ratio is 40:1, and the ball is milled for 36h under the condition of 300r / min at room temperature. After the ball milling reaction, in an inert atmosphere, the powder was taken out from the ball mill jar, added to the crucible, and sintered in a high-temperature tube furnace under a nitrogen atmosphere of 60 mL / min. The sintering temperature was 280 °C, and the sintering time was 5h. The powder is taken out from the crucible to obtain a sulfide solid electrolyte.

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PUM

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Abstract

The invention provides a preparation method of sulfide solid electrolyte and belongs to the field of solid electrolyte. The preparation method comprises the following steps: (1) putting raw materialsincluding sulfur powder, lithium hydride, phosphorus pentasulfide and lithium phosphate into a vacuum drying box and drying; (2) under the protection of an inert atmosphere and weighing the dried rawmaterials in percentage by mass respectively: 15 percent to 40 percent of the sulfur powder, 5 percent to 20 percent of the lithium hydride, 50 percent to 70 percent of the phosphorus pentasulfide and0 to 10 percent of the lithium phosphate; pre-grinding in a mortar for 5 to 20min; adding the raw materials into a sealed ball milling pot; carrying out ball milling at room temperature and at a rotary speed of 200 to 600r / min for 24 to 60h; (3) after ball milling reaction is finished, taking the powder out from the ball milling pot under the inert atmosphere; adding the powder into a crucible and sintering in a high-temperature tubular furnace under a nitrogen atmosphere, wherein the sintering temperature is 200 to 400 DEG C and the sintering time is 2 to 6h; taking the powder out from the crucible to obtain the sulfide solid electrolyte. The preparation method of the sulfide solid electrolyte, provided by the invention, has the characteristics of simple technology, low raw material costand easiness for industrialized production.

Description

technical field [0001] The invention belongs to the field of solid electrolytes, and in particular relates to a solid electrolyte material that can be used in an all-solid-state lithium ion battery and a preparation method thereof. Background technique [0002] The vigorous development of mobile electrochemical systems for high-energy-density Li-ion batteries, traditional systems using organic liquid electrolytes require improvements in safety and durability. This leads to the need for suitable solid electrolytes. In solid-state electrolytes, based on Li 2 S-P 2 S 5 The systemic sulfide solid electrolyte was demonstrated to have ionic conductivity at 25 °C comparable to the currently used liquid electrolytes. [0003] This sulfide-based solid electrolyte is mainly prepared from lithium sulfide, phosphorus pentasulfide and additives through high-energy ball milling and post-heat treatment. The solid electrolyte obtained from these conventional methods exhibits excellent l...

Claims

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Application Information

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IPC IPC(8): H01M10/0562H01M10/0525
CPCH01M10/0525H01M10/0562H01M2300/0068Y02E60/10
Inventor 薛文东胡凯王兴宇戎马屹飞王玉田白立雄李勇
Owner UNIV OF SCI & TECH BEIJING
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