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Preparation method of micron-sized garnet type inorganic solid electrolyte membrane

A garnet-type, inorganic solid technology, applied in the manufacture of electrolyte batteries, electrolytes, non-aqueous electrolyte batteries, etc., can solve problems such as unfavorable battery energy density and power density, limit industrial application prospects, and complex equipment, and achieve low cost, Easy-to-control, simple-to-equip effects

Inactive Publication Date: 2019-02-22
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the preparation methods of garnet-type solid electrolyte sheets or films mainly include traditional solid-state reaction methods, sol-gel methods, and field-assisted sintering methods. Improvement of energy density and power density; methods such as magnetron sputtering, pulsed laser deposition or chemical vapor deposition are mostly suitable for 2D thin-film lithium batteries, which are unlikely to be used in bulk battery systems, and are limited by the characteristics of high cost and complicated equipment The prospect of its industrial application

Method used

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  • Preparation method of micron-sized garnet type inorganic solid electrolyte membrane
  • Preparation method of micron-sized garnet type inorganic solid electrolyte membrane
  • Preparation method of micron-sized garnet type inorganic solid electrolyte membrane

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Experimental program
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Effect test

Embodiment 1

[0029] refer to figure 1 In the process flow shown, the garnet-type solid electrolyte Li prepared by the sol-gel method is first 6.25 Al 0.25 La 3 Zr 2 o 12 The powder was put into an agate mortar, manually ground for 30 minutes, and passed through a 500-mesh sieve. Weigh 6g of the sieved powder and add it into a zirconia ball mill jar, the mass ratio of zirconia balls to powder is 4:1. Then add 2.7 g of ethanol, 2.7 g of butanone and 0.15 g of castor oil, and ball mill at a speed of 300 r / min for 12 h. After the first ball milling, add plasticizer dibutyl phthalate (DBP) and binder polyvinyl butyral (PVB) 0.42g each, and continue ball milling at 300r / min for 24h to obtain stable And evenly dispersed cast slurry. The casting slurry was used as raw material to cast on a casting machine, and the height of the scraper was controlled to be 500 μm. The obtained wet film was vacuum-dried at 45° C. for 24 hours to obtain a casting green body with good processability. The cast...

Embodiment 2

[0031] The garnet-type solid electrolyte Li prepared by the traditional solid-state method 5 La 3 Nb 2 o 12The powder was put into an agate mortar, manually ground for 60 minutes, and passed through a 300-mesh sieve. Weigh 6g of the sieved powder and add it into a zirconia ball mill jar, the mass ratio of zirconia balls to powder is 3:1. Then add 3.2g each of ethanol and toluene and 0.18g of KD-1 dispersant, and ball mill at 400r / min for 18h. After the first ball milling, add plasticizer butyl benzyl phthalate (BBP) and binder PVB 0.45g each, and continue ball milling at 400r / min for 18 hours to obtain a stable and uniformly dispersed casting slurry material. The casting slurry was used as the raw material for casting on a casting machine, and the height of the scraper was controlled to be 300 μm. The obtained wet film was vacuum-dried at 60° C. for 36 hours to obtain a casting green body with good processability. The cast body was hot-pressed at 80°C for 0.5h, cut into ...

Embodiment 3

[0033] The garnet-type solid electrolyte Li prepared by plasma activation sintering 6.4 La 3 Zr 1.4 Ta 0.6 o 12 The powder was put into an agate mortar, manually ground for 45 minutes, and passed through a 300-mesh sieve. Weigh 6g of the sieved powder and add it into a zirconia ball mill jar, the mass ratio of zirconia balls to powder is 2.5:1. Then add 9.0 g of trichlorethylene and 0.12 g of fish oil, and ball mill at a speed of 200 r / min for 24 hours. After the first ball milling, 0.45 g of plasticizer ethylene glycol and 0.36 g of adhesive polymethylacrylate were added, and ball milling was continued for 24 hours at a speed of 300 r / min to obtain a stable and uniformly dispersed casting slurry. The casting slurry was used as raw material to cast on a casting machine, and the height of the scraper was controlled to be 400 μm. The obtained wet film was vacuum-dried at 80° C. for 24 hours to obtain a cast green body with good processability. The cast body was hot-pressed...

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Abstract

The invention relates to a preparation method of a micron-sized garnet type inorganic solid electrolyte membrane. The preparation method comprises the following steps: firstly, mixing garnet type inorganic solid electrolyte with certain particle size with an organic solvent and a dispersant for ball milling, then adding a plasticizer and a binder for secondary ball milling, defoaming obtained slurry, carrying out curtain coating to form a film, drying, carrying out hot-pressing, removing the binder and sintering to form the garnet-type solid electrolyte membrane with the thickness of 20 to 200micrometers. Compared with the existing method, the preparation method has the advantages of low cost, simple equipment, stable process, easy industrialization and the like; and the obtained membraneproduct has high ionic conductivity and controllable thickness.

Description

technical field [0001] The invention relates to the technical field of membrane materials and inorganic solid electrolyte materials, in particular to a method for preparing a micron-sized garnet-type inorganic solid electrolyte membrane. Background technique [0002] In recent years, with the rapid development of renewable energy, the development of new high-efficiency energy storage technologies has become the key to improving energy utilization efficiency and power quality, reducing transmission loss, and promoting the widespread application of renewable energy. Common electrical energy storage technologies mainly include physical energy storage, chemical energy storage, and electromagnetic energy storage. Among them, chemical energy storage including lithium-ion batteries and lead-acid batteries is considered to be the most promising energy storage technology for industrialization. Lithium-ion batteries developed late, but because of their light weight, high specific ener...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/058H01M10/0562C04B35/50C04B35/622C04B35/626
CPCC04B35/50C04B35/622C04B35/62605C04B2235/3203C04B2235/3217C04B2235/3244C04B2235/6025C04B2235/6562C04B2235/6567C04B2235/661H01M10/0562H01M10/058H01M2300/0071Y02E60/10Y02P70/50
Inventor 陈斐曹诗雨查文平沈强张联盟
Owner WUHAN UNIV OF TECH
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