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Sulfide solid electrolyte and preparation method thereof and equipment

A solid-state electrolyte and sulfide technology, which is applied in circuits, electrical components, secondary batteries, etc., can solve problems affecting the performance of sulfide solid-state electrolytes, low reproducibility of sulfide solid-state electrolytes, and unsuitability for large-scale industrial production. , to achieve the effect of reducing the chance of raw materials in contact with water and air, reducing the production and preparation cycle, and eliminating the need for vacuum distillation

Inactive Publication Date: 2018-11-23
桑德新能源技术开发有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] (1) There are many operating steps, which are not suitable for large-scale industrial production;
[0011] (2) The raw material has a high probability of contact with water vapor, and is prone to side reactions, which may affect the performance of the sulfide solid electrolyte, especially its conductivity to lithium ions
[0012] (3) The reproducibility of sulfide solid electrolytes with high ionic conductivity is low, and the lithium ion conductivity needs to be further improved

Method used

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  • Sulfide solid electrolyte and preparation method thereof and equipment

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preparation example Construction

[0040] A preparation method of a sulfide solid state electrolyte, the preparation method is that the reaction raw materials are placed in an anhydrous and oxygen-free sealed container to be ground, heated by microwave radiation for a certain period of time, and then cooled to obtain the sulfide solid state electrolyte.

[0041] Specifically, the reaction raw materials and abrasives are placed together in the sealed container, and the sealed container is filled with inert gas, such as argon, etc.; the sealed container is driven to move, so that the reaction raw materials are ground by the abrasives in the sealed container; When the sealed container is in a sealed state, the material in the sealed container is directly heated and reacted by microwave radiation for a period of time, and after cooling, a sulfide solid electrolyte is prepared. Preferably, the sealed container is a ball mill, the driving device is a planetary ball mill, and the rotation speed is set to be 100-3000rpm...

Embodiment 1

[0053] Take Li 2 S.P 2 S 5 As raw material, in an argon glove box with a molar ratio of 75:25 (Li 2 S:P 2 S 5 ) weighing 3.827gLi 2 S, and 6.164gP 2 S 5 , put it into the corundum ball mill jar, then add corundum crushed beads with a particle size of 3mm, and finally seal the ball mill jar.

[0054] The above-mentioned ball mill jar was placed in a ball mill, and mixed at a low speed of 800 rpm for 5 minutes, and then, the rotation speed was increased to 1800 rpm for 2 h. After completion, the ball mill jar was transferred to the microwave oven in the glove box, set under high heat conditions (power 1000W, frequency 2450MHz), microwave heating for 30 minutes. In the glove box, pass the material in the tank through a titanium mesh screen (16 mesh) to separate the corundum pulverized beads, and the obtained sulfide solid powder can be used to prepare a solid-state lithium battery electrolyte layer.

[0055] The lithium ion conductivity was measured by the AC impedance m...

Embodiment 2

[0057] Take Li 2 S.P 2 S 5 , LiCl as raw material, in an argon glove box with a molar ratio of 72:20:8 (LiCl 2 S:P 2 S 5 : LiCl) weighing 3.312gLi 2 S, 4.446gP 2 S 5 And 0.340g LiCl, put it into a teflon tank, then put zirconia crushed beads with a particle size of 3mm, and finally seal the teflon tank.

[0058] The above-mentioned polytetrafluoroethylene tank was placed in a ball mill, and crushed at a low speed of 800 rpm for 10 minutes, then, the rotation speed was increased to 1800 rpm, and mixed for 2 hours. The ball mill jar was transferred to a microwave oven in a glove box and heated for 30 minutes under high heat conditions (set power 800W, frequency 2450MHz). In the glove box, pass the material in the tank through a titanium mesh screen (16 mesh) to separate the corundum pulverized beads, and the obtained sulfide solid powder can be used to prepare a solid-state lithium battery electrolyte layer.

[0059] The lithium ion conductivity was measured by the AC i...

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Abstract

The invention relates to a preparation method of a sulfide solid electrolyte. The preparation method comprises the following steps of putting reaction raw materials into a water-free oxygen-free sealed container, and grinding the reaction raw materials, carrying out microwave radiation heating for a certain time, and then cooling to obtain the sulfide solid electrolyte. In the preparation process,the reaction raw materials are all contained in one sealed container, and replacement of the container is not needed in the middle of the process, so that industrial production can be realized easily; the probability of contact with water and air is lowered, and the occurrence of side reactions is reduced; the reaction is carried out in a microwave heating condition, so that rapid heating and cooling and realized; on one hand, the glassy state and the amorphous state in the synthesized product are relatively more, and the channels for rapid migration of the lithium ions are increased, so thatthe conductivity of the lithium ions is improved; and on the other hand, relatively more point defects and / or plane defects exist in the synthesized products, the channels for rapid migration of thelithium ions are increased, and the conductivity of the lithium ions is improved. Experiments prove that the lithium ion conductivity of the sulfide solid electrolyte prepared according to the methodcan reach 8*10<-4>s / cm to 6*10<-3>s / cm at the room temperature.

Description

technical field [0001] The invention relates to the technical field of electrolytes for batteries, in particular to a method for preparing a sulfide solid state electrolyte of a lithium ion battery. Background technique [0002] Commercial lithium-ion batteries contain liquid organic electrolytes with low ignition points, which are prone to safety problems such as liquid leakage, flammability and explosion, which largely limit the application fields of liquid lithium-ion batteries. With the popularization of large-scale energy storage devices such as electric vehicles and smart grids, higher requirements are placed on the energy density and safety performance of lithium-ion batteries. [0003] Compared with commercial lithium-ion batteries, all-solid-state lithium-ion batteries use inorganic solid-state electrolytes instead of liquid organic electrolytes, which can better solve the safety problems of lithium-ion batteries. Inorganic solid electrolytes can well inhibit the g...

Claims

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Application Information

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IPC IPC(8): H01M10/0562
CPCH01M10/0562Y02E60/10
Inventor 陈渊周美丽倪海芳
Owner 桑德新能源技术开发有限公司
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