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Soft chemical synthesis method for preparing sodium ion solid electrolyte

A technology of solid electrolyte and synthesis method, which is applied in the field of soft chemical synthesis of sodium ion solid electrolyte, which can solve the problems of high cost, collapse of crystal structure, and inability to obtain pure phase exchange products, so as to reduce difficulty and avoid damage Effects of sexual influence, variety and quantity

Active Publication Date: 2021-03-26
SHANGHAI INST OF SPACE POWER SOURCES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, on the one hand, due to the high temperature and strong destructiveness of molten salt, it is easy to cause the crystal structure of the product to collapse during the ion exchange process, and the exchange product of pure phase cannot be obtained; on the other hand, using ionic liquid as the exchange medium , the reaction conditions are relatively mild, and high-purity exchange products can be obtained, but the cost is high

Method used

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  • Soft chemical synthesis method for preparing sodium ion solid electrolyte
  • Soft chemical synthesis method for preparing sodium ion solid electrolyte

Examples

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Embodiment 1

[0027] Weigh n-butyl titanate (C 4 h 9 O) 4 Ti, Al(NO 3 ) 3 9H 2 O, 85 wt% H 3 PO 4 (inwater) and 5mol% excess CH 3 COOLi. Will (C 4 h 9 O) 4 Ti was fully hydrolyzed by adding deionized water, and centrifuged with ethanol to remove the organic matter produced by hydrolysis. Then, add the white precipitate obtained by hydrolysis into 2M aqueous oxalic acid solution. After the precipitate is completely dissolved, add the rest of the raw materials and heat and stir at 80°C to obtain a clear and transparent solution. Drying in an oven overnight gave a white precipitate. The precipitate was heat-treated at 400°C for 2h, then ball milled at 450r / min for 12h with a ball mill, and finally calcined at 750°C for 12h to obtain Li 1.3 Al 0.3 Ti 1.7 (PO 4 ) 3 White powder.

[0028] Weigh Li with a molar ratio of 1:40 1.3 Al 0.3 Ti 1.7 (PO 4 ) 3 The powder and anhydrous sodium acetate were placed in a mortar and mixed evenly, then the mixed powder was poured into an a...

Embodiment 2

[0034] In a dry room, weigh Li with a molar ratio of 1:40 7 La 3 Zr 2 o 12 The powder and anhydrous sodium acetate were placed in a mortar and mixed evenly, then the mixed powder was poured into an alumina crucible, and heat treated at 240°C for 2h. Afterwards, centrifuge four times with diethyl ether to remove sodium acetate, then centrifuge four times with absolute ethanol to remove lithium acetate produced by ion exchange reaction, and finally dry the product in a drying room at 60-80°C. The above steps were repeated several times until the ion exchange reaction reached equilibrium.

Embodiment 3

[0036] Weigh Li with a molar ratio of 1:40 0.5 La 0.5 TiO 3 The powder and anhydrous sodium acetate were placed in a mortar and mixed evenly, then the mixed powder was poured into an alumina crucible, and heat treated at 240°C for 2h. Afterwards, centrifuge five times with deionized water to remove excess sodium acetate and lithium acetate produced by exchange, and finally remove water by centrifuging with ethanol, and dry the product at 60-80°C. The above steps were repeated several times until the ion exchange reaction reached equilibrium.

[0037] The principle of the present invention is that the crystal structure of the lithium-ion solid electrolyte is composed of an anion skeleton and lithium ions, and the lithium ions in the skeleton have high mobility. Under the driving force of temperature and concentration difference, they can interact with sodium ions The sodium ions of the exchanger rapidly generate Li + / Na + In the exchange reaction, lithium ions are extract...

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Abstract

The invention discloses a soft chemical synthesis method for preparing a sodium ion solid electrolyte, which comprises the following steps of: 1, uniformly mixing a lithium ion solid electrolyte and asolid-phase sodium ion exchanger to obtain mixed powder; 2, carrying out heat treatment on the mixed powder to synthesize a sodium ion solid electrolyte; wherein the lithium ion solid electrolyte andthe sodium ion exchanger are kept in a solid-phase state in the heat treatment process; 3, dissolving the redundant sodium ion exchanger and the synthesized by-product by adopting a solvent, and centrifuging to obtain a solid product containing the sodium ion solid electrolyte; and 4, drying the obtained solid product, uniformly mixing the dried solid product with a sodium ion exchanger, and repeating the step 2-3 several times to improve the content of the sodium ion solid electrolyte in the solid product. The sodium ion solid electrolyte is synthesized through solid-phase exchange between the lithium ion solid electrolyte and the sodium ion exchanger under the low-temperature heat treatment condition, the method is simple and convenient, the cost is low, and industrial application is easy.

Description

technical field [0001] The invention relates to the field of new energy materials, in particular to a soft chemical synthesis method for preparing sodium ion solid electrolytes. Background technique [0002] In nature, because sodium is more abundant than lithium, sodium-ion batteries have the advantage of lower cost and more sustainable development. Similar to lithium-ion batteries using organic electrolytes, sodium-ion batteries using organic liquids as electrolytes also have safety issues. Solid electrolytes have high thermal stability and wide electrochemical window. Using sodium-ion solid electrolytes to replace organic electrolytes to develop all-solid-state sodium batteries can not only effectively solve safety problems, but also improve the energy density of batteries. [0003] Compared with lithium-ion electrolytes, there are much fewer types and quantities of sodium-ion solid electrolytes, especially those with high ionic conductivity. Na 3 Zr 2 Si 2 PO 12 an...

Claims

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Application Information

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IPC IPC(8): H01M10/0562H01M10/054
CPCH01M10/054H01M10/0562H01M2300/0071Y02E60/10
Inventor 吴洁高靖雄朱蕾吴勇民周罗增汤卫平
Owner SHANGHAI INST OF SPACE POWER SOURCES
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