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Plastic crystal-ceramic composite solid electrolyte and low-temperature hot-pressing preparation method thereof

A solid electrolyte and ceramic composite technology, which is applied in the manufacture of electrolyte batteries, non-aqueous electrolyte batteries, chemical instruments and methods, etc., can solve the problems of consumption of solid electrolyte powder, interdiffusion of elements, increase of interface impedance, etc., to avoid elements Effects of interdiffusion and side reactions, high ionic conductivity, and reduced grain boundary resistance

Inactive Publication Date: 2021-03-19
SHANGHAI INST OF SPACE POWER SOURCES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Oxide solid electrolytes usually need to be sintered at high temperature (≥900°C) to densify to reduce grain boundary resistance, which not only consumes energy, but also causes lithium to volatilize and decompose, resulting in a decrease in the ionic conductivity of the solid electrolyte
Although buried powder sintering can suppress the volatilization of lithium elements and keep the original chemical composition of the solid electrolyte as much as possible, but it will consume a large amount of solid electrolyte powder, which is not conducive to reducing production costs
In addition, high-temperature sintering treatment will also lead to the interdiffusion of elements and even side reactions between solid electrolyte positive electrode materials, which will increase the interface impedance, which is not conducive to the performance of solid-state batteries.
[0004] The cold press sintering method can achieve a certain densification of the ceramic powder at a low temperature (-4 S / cm, additives such as water or organic solvents that affect battery performance are also required in the low-temperature sintering process

Method used

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  • Plastic crystal-ceramic composite solid electrolyte and low-temperature hot-pressing preparation method thereof
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  • Plastic crystal-ceramic composite solid electrolyte and low-temperature hot-pressing preparation method thereof

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preparation example Construction

[0031] The invention provides a method for preparing a plastic crystal-ceramic composite solid electrolyte at low temperature by hot pressing, comprising the following steps:

[0032] Step 1, weighing oxide ceramic powder and plastic crystal solid electrolyte, and mixing them uniformly to obtain a mixed powder; the plastic crystal solid electrolyte includes: plastic crystal and lithium salt;

[0033] Step 2, placing the mixed powder in a mold and paving;

[0034] Step 3, compressing the mixed powder, and at the same time, heat-treating the mixed powder, the heating temperature is lower than 600°C, so that the plastic crystal solid electrolyte absorbs heat and melts; then lower the temperature, the plastic crystal The solid electrolyte is solidified and formed to obtain the plastic crystal-ceramic composite solid electrolyte.

[0035] The mass fraction of the oxide ceramic powder of the present invention in the mixed powder is 30-100%, preferably 60-94%. The mass fraction of ...

Embodiment 1

[0042] Weigh CH by stoichiometric ratio 3 COOLi, Al(NO 3 ) 3 9H 2 O, (C 4 h 9 O) 4 Ti and 85wt%H 3 PO 4(inwater), CH 3 COOLi excess 5mol%. (C 4 h 9 O) 4 Ti was dropped into deionized water for hydrolysis, and then centrifuged to obtain a white precipitate, which was dissolved in 2M oxalic acid solution at 60°C to obtain a colorless and transparent solution. The rest of the raw materials were added to the above colorless transparent solution, and after being fully dissolved, the water was evaporated to dryness at 80°C, and the obtained white precipitate was dried overnight in a blast oven at 80°C. The white precipitate was properly ground in an agate mortar, using absolute ethanol as a dispersant, ball-milled with a planetary ball mill at 450r / min for 12h, and then the dried powder was pre-calcined at 400°C for 2h. Subsequently, the calcined powder was ball-milled for 12 hours with a planetary ball mill at 400 r / min, also using absolute ethanol as a dispersant. Fi...

Embodiment 2

[0048] The difference between this embodiment and embodiment 1 is that during the low-temperature hot pressing process, the temperature of the press molding is changed to 140° C., and other conditions remain unchanged.

[0049] In Example 2 of the present invention, a plastic crystal-ceramic composite solid electrolyte 2 was prepared. Depend on Figure 4 with Figure 5 It can be seen that the ionic conductivity of plastic crystal-ceramic composite solid electrolyte 2 is 1.67×10 -4 S / cm, its relative density is 92.44%.

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Abstract

The invention discloses a plastic crystal ceramic composite solid electrolyte and a low-temperature hot-pressing preparation method thereof. The method comprises the following steps of step 1, weighing oxide ceramic powder and the plastic crystal solid electrolyte, and uniformly mixing to obtain mixed powder; the plastic crystal solid electrolyte comprising a plastic crystal and a lithium salt, step 2, putting the mixed powder into a mold, and flattening the mixed powder; 3, the mixed powder being subjected to compression molding, meanwhile, the mixed powder being subjected to heat treatment,the heating temperature being lower than 600 DEG C, and the plastic crystal solid electrolyte absorbing heat to be molten; and then reducing the temperature to solidify and mold the plastic crystal solid electrolyte to obtain the plastic crystal ceramic composite solid electrolyte. According to the method, densification of the solid electrolyte can be realized at a relatively low temperature, thesolid electrolyte has relatively high ionic conductivity, and the processing time, energy loss and volatilization of a lithium element at a high temperature are greatly reduced.

Description

Technical field [0001] The invention relates to the field of new energy materials, and in particular to a plastic crystal-ceramic composite solid electrolyte and a low-temperature hot pressing preparation method thereof. Background technique [0002] As an energy storage device, the development of high-energy-density batteries has received widespread attention. Due to their flammability and narrow electrochemical stability window, batteries using organic liquids as electrolytes are not only limited in their energy density, but also pose safety risks of combustion and explosion. Therefore, people hope to develop solid electrolytes that are non-flammable and have high electrochemical stability to replace organic electrolytes and develop all-solid-state batteries. From the perspective of electrochemical stability window and ionic conductivity, oxide solid electrolytes have great development prospects in the application of all-solid-state batteries. [0003] Oxide solid electr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0562H01M10/052H01M10/058H01M10/42C01B25/45
CPCC01B25/45H01M10/052H01M10/0562H01M10/058H01M10/4235Y02E60/10Y02P70/50
Inventor 吴洁朱蕾汤卫平高靖雄田文生吴勇民周罗增
Owner SHANGHAI INST OF SPACE POWER SOURCES
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