Electric field activated sintering method of solid electrolyte material

A technology of electric field activation sintering and solid electrolyte, applied in chemical instruments and methods, inorganic chemistry, zirconium compounds, etc., can solve the problems of high sintering temperature, low lithium ion conductivity, long sintering time, etc., and achieve low sintering temperature, lithium High ionic conductivity and the effect of improving synthesis efficiency

Inactive Publication Date: 2014-01-08
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a solid electrolyte material Li 7 La 3 Zr 2 o 12 The sintering method, which is mixed by ball milling and then sintered by electric field activation, aims to obtain cubic phase LLZO with high density and high lithium ion conductivity, reduce the sintering temperature and simplify the preparation process

Method used

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  • Electric field activated sintering method of solid electrolyte material
  • Electric field activated sintering method of solid electrolyte material
  • Electric field activated sintering method of solid electrolyte material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Use lithium oxide Li 2 O, lanthanum oxide La 2 o 3 , Zirconia ZrO 2 The powder is used as the raw material powder, and the lanthanum oxide (La 2 o 3 ) was roasted at a constant temperature of 900°C. According to the mass fraction is 9.2%, 60.4% and 30.4% respectively weigh and synthesize 5g required raw material powder lithium oxide (Li 2 O, 99.9%) 0.46g, lanthanum oxide (La 2 o 3 ,99.99%) 3.02g, zirconia (ZrO 2 ,99.9%) 1.52g. Put the above three kinds of powder into a ball mill jar made of zirconia for ball milling, and use zirconia balls as the ball milling medium, use isopropanol as the solvent, and the mass ratio of isopropanol to powder is 3:1, and the milling speed is 100 Ball milling for 36 hours under rpm. The ball-milled powder was put into a vacuum drying oven and dried at 80° C. for 6 hours. Weigh 1.5g of the dried powder and put it into a graphite mold, keep the pressure at 0MPa when the temperature is <800°C, and keep it warm for 5 minutes; then ...

Embodiment 2

[0033] Use lithium oxide Li 2 O, lanthanum oxide La 2 o 3 , Zirconia ZrO 2 The powder is used as the raw material powder, and the lanthanum oxide (La 2 o 3 ) was roasted at a constant temperature of 900°C. According to the mass fraction of 10.1%, 59.8% and 30.1%, respectively weigh and synthesize 5g of the required raw material powder lithium oxide (Li 2 O, 99.9%) 0.505g, lanthanum oxide (La 2 o 3 ,99.99%) 2.99g, zirconia (ZrO 2 ,99.9%) 1.505g. Put the above three kinds of powder into a ball mill jar made of zirconia for ball milling, and use zirconia balls as the ball milling medium, use isopropanol as the solvent, and the mass ratio of isopropanol to powder is 3:1, and the milling speed is 200 Ball milling for 24 hours at rpm. The ball-milled powder was put into a vacuum drying oven and dried at 80° C. for 6 hours. Weigh 1.5g of the dried powder and put it into a graphite mold, keep the pressure at 0MPa when the temperature is <800°C, and keep it warm for 4 minute...

Embodiment 3

[0035] Use lithium oxide Li 2 O, lanthanum oxide La 2 o 3 , Zirconia ZrO 2 The powder is used as the raw material powder, and the lanthanum oxide (La 2 o 3 ) was roasted at a constant temperature of 900°C. According to the mass fraction is 11.8%, 58.7% and 29.5% respectively weigh and synthesize 10g required raw material powder lithium oxide (Li 2 O,99.9%) 1.18g, lanthanum oxide (La 2 o 3 ,99.99%) 5.87g, zirconia (ZrO 2 ,99.9%) 2.95g. Put the above three kinds of powder into a ball mill jar made of zirconia for ball milling, and use zirconia balls as the ball milling medium, use isopropanol as the solvent, and the mass ratio of isopropanol to powder is 6:1, and the milling speed is 300 Ball milling for 12 hours under rpm. The powder after ball milling was put into a vacuum drying oven, and dried at 80° C. for 8 hours. Weigh 1.5g of the dried powder and put it into a graphite mold, keep the pressure at 0MPa when the temperature is <800°C, and keep it warm for 3 minut...

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Abstract

The invention provides an electric field activated sintering method of a solid electrolyte material Li7La3Zr2O12 (LLZO). The electric field activated sintering method comprises the following specific steps: ball-milling with a ball and mixing Li2O, La2O3 and ZrO2 powder, the mass percents of which are respectively 9.2-15.5%, 56.2-60.4% and 28.3-30.4%, wherein a zirconium oxide ball is used as a ball-milling medium, isopropanol is used as a solvent, and the ball-milling time is 12-36 hours; carrying out vacuum drying on ball-milling milled powder for 6-12 hours at the temperature of 80 DEG C; and carrying out electric field activated sintering, wherein the temperature is in the range from 800 to 1230 DEG C, the pressure is 0-100 MpaMPa, and a sintered sample has the room-temperature lithium-ion conductivity greater than 6*10<-4S>S/cm. Compared with a conventional solid-phase synthesis method, the electric field activated sintering method has the advantages that the synthesis reaction and the sintering compact process are completed in one step, the synthetic efficiency is improved to a large extent, the preparation technology is simplified, and the LLZO with the high lithium-ion conductivity is obtained.

Description

Technical field: [0001] The invention belongs to the technical field of preparation of solid electrolyte materials, in particular to a solid electrolyte material Li 7 La 3 Zr 2 o 12 The electric field activated sintering method. Background technique: [0002] With the rapid development of mobile phones, computers, etc., lithium-ion batteries have attracted great attention in the past few decades. Scientists are currently trying to use these batteries to power cars to avoid the carbon dioxide and other pollutants produced by traditional gasoline-powered vehicles. These new applications require lithium-ion batteries to have high safety, high energy density, long life and high temperature resistance. Current lithium-ion batteries based on liquid electrolytes cannot meet these requirements because the organic liquid electrolytes they use are flammable, volatile, leaky and decompose at high temperatures (C.A. Geiger, E. Alekseev, W. Weppner, Inorg. Chem. .2011, 50, 1089-109...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/00
CPCY02E60/10
Inventor 张联盟张艳华陈斐涂溶沈强
Owner WUHAN UNIV OF TECH
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