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A preparing method of a glass ceramic type solid electrolyte

A technology of solid electrolyte and glass ceramics, which is applied in the preparation of Li1+xAlxTi2-x3 glass ceramic solid electrolyte and the field of solid electrolyte preparation, which can solve the problems of low ion conductivity, complicated preparation process, and long sintering time, and achieve sintering The time is short, the preparation method is simple and easy, and the effect of improving the synthesis efficiency

Inactive Publication Date: 2017-03-15
CHINA UNIV OF GEOSCIENCES (WUHAN)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The invention provides a method for preparing a glass-ceramic solid electrolyte, which solves the shortcomings of the prior art such as complicated preparation process, long sintering time, and low ion conductivity.

Method used

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  • A preparing method of a glass ceramic type solid electrolyte
  • A preparing method of a glass ceramic type solid electrolyte
  • A preparing method of a glass ceramic type solid electrolyte

Examples

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Effect test

Embodiment 1

[0025] Weigh 6.2wt% Li 2 CO 3 , 4.9 wt% Al 2 o 3 , 19.9 wt% TiO 2 and 69.0wt% (NH 4 ) 2 HPO 4 The powder is manually ground for 5 minutes, and then the planetary ball mill is used for 0.5 hours. The ball milling medium is zirconia spheres with a diameter of 1 mm and 4 mm. The solvent is absolute ethanol, and the mass ratio of solvent to raw material is 1:1. After ball milling, put it into a vacuum drying oven and dry at 100°C for 10 hours. Put the dried powder into an agate mortar and grind it manually for 30 minutes. The uniformly mixed raw materials are put into an alumina crucible with a purity of 99% for high-temperature melting. First keep the temperature at 700°C for 1 hour, then raise the temperature to 1550°C for 2 hours, and obtain the required glass slag after water quenching. Grind the glass slag manually for 5 minutes, and then use dry ball milling to obtain glass powder. The ball milling medium is 1mm and There are two kinds of 4mm zirconia spheres, the b...

Embodiment 2

[0027] Weigh 6.2wt% Li 2 CO 3 , 4.9 wt% Al 2 o 3 , 20.3wt% TiO 2 and 68.6wt% (NH 4 ) 2 HPO 4 Powder, first manually grind for 5 minutes, and then use planetary ball mill wet ball for 1 hour, the ball milling medium is two kinds of zirconia spheres with a diameter of 1mm and 4mm, the solvent is absolute ethanol, the mass ratio of solvent to raw material is 1:1, ball milling Then put it into a vacuum drying oven and dry it at 100°C for 10h. Put the dried powder into an agate mortar and grind it manually for 30 minutes. The uniformly mixed raw materials are put into an alumina crucible with a purity of 99% for high-temperature melting. First keep the temperature at 700°C for 2 hours, then raise the temperature to 1550°C for 2 hours, and obtain the required glass slag after water quenching. Grind the glass slag manually for 5 minutes, and then use dry ball milling to obtain glass powder. The ball milling time is 10 hours. The ball milling medium is 1mm and 4mm zirconia sp...

Embodiment 3

[0029] Weigh 5.7wt% Li 2 CO 3 , 4.5 wt% Al 2 o 3 , 20.1wt% TiO 2 and 69.7wt% (NH 4 ) 2 HPO 4 The powder is manually ground for 5 minutes, and then the planetary ball mill is used for 0.5 hours. The ball milling medium is zirconia spheres with a diameter of 1 mm and 4 mm. The solvent is absolute ethanol, and the mass ratio of solvent to raw material is 1:1. After ball milling, put it into a vacuum drying oven and dry at 100°C for 10 hours. Put the dried powder into an agate mortar and grind it manually for 30 minutes. The uniformly mixed raw materials are put into an alumina crucible with a purity of 99% for high-temperature melting. First keep the temperature at 700°C for 1 hour, then raise the temperature to 1550°C for 2 hours, and obtain the required glass slag after water quenching. Grind the glass slag manually for 5 minutes, and then use dry ball milling to obtain glass powder. The ball milling medium is 1mm and There are two kinds of 4mm zirconia spheres, the ma...

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Abstract

A preparing method of a glass ceramic type solid electrolyte is disclosed. The chemical formula of the solid electrolyte is Li<1+x>Al<x>Ti<2-x>(PO4)3, wherein 0<=x<=0.5. The preparing method includes weighing Li<2>CO3, Al<2>O3, TiO2 and (NH4)<2>HPO4 powder according to a mass ratio, grinding each raw material, fully mixing the ground raw materials, adding the mixture to a crucible, heating the mixture to melt the mixture, performing water quenching to obtain glass splinters, grinding the glass splinters firstly, then subjecting the glass splinters to ball milling in a dry ball mill to obtain glass powder, adding the glass powder to a specific graphite die, and rapidly heating the glass powder under protection of an inert gas by utilizing high-intensity pulse current (assistant by an electric field) to crystallize the glass. The glass ceramic type solid electrolyte with excellent properties is prepared through controlling the heating rate, synthetic temperature, insulation temperature and other process parameters.

Description

technical field [0001] The invention provides a preparation method of a solid electrolyte, in particular to a Li 1+x al x Ti 2-x (PO 4 ) 3 (0≤x≤0.5) A method for preparing a glass-ceramic solid electrolyte belongs to the technical field of battery material preparation. Background technique [0002] In recent decades, with the advancement of science and the development of civilization, the demand for energy is increasing day by day. On the one hand, traditional fossil energy is not enough to support the sustainable development of human society. On the other hand, a series of environmental problems caused by it, such as acid rain and greenhouse effect, seriously endanger human health. Therefore, it is imminent to seek clean and efficient renewable energy. Common renewable energy sources such as solar energy, tidal energy, and wind energy are generally limited by the environment and geographical location, resulting in energy consumption and unbalanced access, resulting in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0562H01M10/0525C03B32/02C03B19/06C03C10/02
CPCH01M10/0525H01M10/0562C03B19/063C03B32/02C03C10/009H01M2300/0068H01M2300/002Y02E60/10
Inventor 靳洪允段姗姗侯书恩刘敏
Owner CHINA UNIV OF GEOSCIENCES (WUHAN)
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