Preparation method of oxide solid electrolyte diaphragm

A solid electrolyte and oxide technology, which is applied in the manufacture of electrolyte batteries, non-aqueous electrolyte batteries, electrolyte immobilization/gelation, etc., can solve problems such as easy damage and deformation, achieve flat and compact finished products, and reduce the chance of contamination , The effect of simple process

Active Publication Date: 2017-02-08
NO 63971 TROOPS PLA
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to solve the problems of pre-pressing the diaphragm before sintering in the traditional solid-state method, easy deformation during the sintering process, and easy damage in the post-processing, etc., and provide a high ionic conductivity with simple process, flat and compact finished product, and easy scale-up Preparation method of oxide solid electrolyte separator

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  • Preparation method of oxide solid electrolyte diaphragm

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example 1

[0014] First press Li 7 La 3 Zr 2 o 12 Proportioning, weigh lithium hydroxide (LiOH, excess 15%) 12.3135g, zirconium oxide (ZrO 2 ) 8.8930g, lanthanum oxide (La 2 o 3 ) 17.4594g, put it in a ball mill tank, add 20ml of absolute ethanol, the ball mill speed is 400 rpm, and ball mill for 10h; the obtained slurry is dried at 120°C for 10h, and then ground to obtain the primary oxide material; the primary material is placed in In the corundum crucible in the temperature-controlled furnace, the temperature was rapidly raised to 1150°C and kept for 10 hours; the raw material after high-temperature treatment was directly crushed and mixed evenly by grinding and ball milling, and LLZO powder was obtained after sieving with a 100-mesh sieve. The average particle size measured by laser particle size analyzer is 10.88 microns; the obtained powder is placed in a corundum crucible, placed in a temperature-controlled furnace, and sintered at a high temperature of 1150°C in air for 15 h...

example 2

[0016] Lithium carbonate (Li 2 CO 3 , excess 10%) 10.3704g, zirconia (ZrO2) 8.8930g, lanthanum oxide (La 2 o 3 ) 17.4594g and tantalum oxide (Ta 2 o 5 ) 1.0525g, put it in a ball mill jar, add 20ml of absolute ethanol, the ball mill speed is 400 rpm, and ball mill for 10h; the obtained slurry is dried at 120°C for 10h, and ground to obtain the primary oxide material; the primary material is placed in a control In the corundum crucible in the heating furnace, the temperature was rapidly raised to 1150°C and kept for 10 hours; the raw material after high temperature treatment was directly pulverized and mixed evenly by grinding, ball milling, etc., and LLZO powder was obtained after sieving with a 100-mesh sieve; The powder is placed in a corundum crucible, placed in a temperature-controlled furnace, and sintered at a high temperature of 1150°C in air for 20 hours to obtain a dense oxide solid electrolyte block; the block is cut into a thickness of 1.490mm by a table mill cu...

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Abstract

The invention relates to a preparation method of an oxide solid electrolyte diaphragm, belonging to the fields of electro chemical engineering and ceramic industry. The method comprises the following steps: by using lithium carbonate or lithium hydroxide as a lithium source, putting previously prepared solid electrolyte powder in a crucible, and directly sintering at high temperature to obtain a compact block; and carrying out cutting and sanding on the block to obtain the solid electrolyte diaphragm sheet. The method avoids the complex mold preforming process in the conventional method; and the mechanical energy is converted into the surface free energy of the powder granules by ball milling, the excessive low-melting-point lithium salt is molten at high temperature to generate the liquid phase which is covered on the powder particle surfaces, and the powder automatic aggregates under the action of surface tension, so that the surface free energy is lowered, thereby forming the compact solid electrolyte block. The method has the advantages of simple technique, smooth and compact finished product and the like, can easily implement large-scale production, and is especially suitable for preparing oxide solid electrolyte diaphragms in the solid secondary battery.

Description

technical field [0001] The invention relates to a preparation method of an oxide solid electrolyte diaphragm, which belongs to the fields of electrochemical engineering and ceramic industry. Background technique [0002] Due to the use of organic electrolytes in traditional lithium-ion batteries, there are potential dangers such as combustion and explosion. The new generation of lithium-ion batteries, the so-called "all-solid-state batteries", uses solid electrolytes instead of flammable organic electrolytes, which fundamentally solves the safety problem of batteries. Solid electrolytes can be broadly classified into polymers and inorganic substances. High molecular polymers have low ionic conductivity at room temperature, making it difficult to apply in all-solid-state batteries. Although inorganic solid electrolytes are difficult to produce on a large scale, they have high ionic conductivity, good selectivity, and long service life, and have become the mainstream of rese...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M2/14H01M10/058H01M50/403
CPCH01M10/058H01M2300/0085H01M50/403Y02E60/10Y02P70/50
Inventor 赵鹏程曹高萍文越华徐艳程杰
Owner NO 63971 TROOPS PLA
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