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a li 7 la 3 zr 2 o 12 Preparation method of solid electrolyte

A technology of solid electrolyte and preparation steps, which is applied to circuits, electrical components, secondary batteries, etc., can solve the problems of complex precursor preparation process, large particle size of material particles, and high sintering temperature, and achieves short test period and simple preparation method. , the effect of low sintering temperature

Active Publication Date: 2022-07-19
HARBIN INST OF TECH AT WEIHAI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the precursor preparation process of this method is complicated, the particle size of the obtained material is large, and the uniformity is poor, and the sintering temperature is too high

Method used

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  • a li <sub>7</sub> la <sub>3</sub> zr <sub>2</sub> o <sub>12</sub> Preparation method of solid electrolyte
  • a li <sub>7</sub> la <sub>3</sub> zr <sub>2</sub> o <sub>12</sub> Preparation method of solid electrolyte

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) 0.5820 g of lanthanum oxide, 0.6984 g of lithium carbonate, and 0.65 g of zirconium oxynitrate hydrate were placed in a beaker containing ethanol to obtain a suspension;

[0027] (2) under stirring, 15% dilute nitric acid was added to the suspension of step (1) to obtain a colorless transparent sol;

[0028] (3) Evaporating and drying the sol in step (2) in a water bath at 80° C. for 4 h to obtain a gel;

[0029] (4) drying the gel in step (3) at 200° C. for 2 h, and pyrolyzing to obtain a precursor;

[0030] (5) The sol-gel precursor in step (4) was ground uniformly, sintered at 800 °C for 6 h, and cooled naturally to obtain 1.0 g of LLZO solid electrolyte material with a cube-like structure.

[0031] figure 1 It is the XRD pattern of the garnet-type solid electrolyte LLZO prepared according to Example 1. Depend on figure 1 It was found that the prepared product had a tetragonal crystal structure (PDF#40-0894).

[0032] figure 2 This is a scanning electron m...

Embodiment 2

[0034] (1) Place 0.6893 g of lanthanum hydroxide, 0.3498 to 0.4050 g of lithium hydroxide, and 0.2753 g of zirconium nitrate hydrate in a beaker containing ethanol to obtain a suspension;

[0035] (2) under stirring, 40% dilute nitric acid was added to the suspension of step (1) to obtain a colorless transparent sol;

[0036] (3) Evaporating and drying the sol in step (2) in a water bath at 100° C. for 3 h to obtain a gel;

[0037] (4) drying the gel in step (3) at 200° C. for 2 h, and pyrolyzing to obtain a precursor;

[0038] (5) The sol-gel precursor in step (4) was ground uniformly, sintered at 750 °C for 6 h, and cooled naturally to obtain 1.0 g of LLZO solid electrolyte material.

Embodiment 3

[0040] (1) Place 0.5820 g of lanthanum oxide, 0.6775-0.6984 g of lithium carbonate, and 0.6500 g of zirconium oxynitrate hydrate in a beaker containing ethanol to obtain a suspension;

[0041] (2) under stirring, 30% dilute nitric acid was added to the suspension of step (1) to obtain a colorless transparent sol;

[0042] (3) Evaporating and drying the sol in step (2) in a water bath at 100° C. for 3 h to obtain a gel;

[0043] (4) drying the gel in step (3) at 200° C. for 4 h, and pyrolyzing to obtain a precursor;

[0044] (5) The sol-gel precursor in step (4) was ground uniformly, sintered at 850 °C for 6 h, and cooled naturally to obtain 1.0 g of LLZO solid electrolyte material.

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Abstract

The invention relates to a synthetic solid electrolyte material cubic Li 7 La 3 Zr 2 O 12 The preparation method belongs to the technical field of electrochemical energy. Li prepared by the present invention 7 La 3 Zr 2 O 12 The precursor was synthesized by a non-hydrolyzable sol-gel method. The precursor was evaporated at 80-100 °C, dried at 200 °C, ground, and then heated to 700-900 °C in a muffle furnace and sintered for 4-12 h to obtain cubes with a size of 3-10 μm. stacked Li 7 La 3 Zr 2 O 12 electrolyte material. The raw materials of the invention are cheap and easy to obtain, the process is simple, the operation is convenient, and the environment is friendly, and the morphology of the synthesized products is regular and orderly. Li prepared by this method 7 La 3 Zr 2 O 12 The material has good thermal and chemical stability.

Description

technical field [0001] The present invention relates to a cubic Li 7 La 3 Zr 2 O 12 The invention discloses a method for preparing a solid electrolyte non-hydrolyzable sol-gel, belonging to the technical field of chemical power sources. Background technique [0002] Garnet-type solid electrolyte Li 7 La 3 Zr 2 O 12 (LLZO) is a kind of solid electrolyte. It has the characteristics of low electronic conductivity, small grain boundary resistance, good thermal and chemical stability, and the ionic conductivity will increase with the increase of temperature. focus on. [0003] Among the many public preparation methods of LLZO, there are many methods such as high temperature solid phase method, sol-gel method, co-precipitation method and so on. The high-temperature solid-phase method has been widely used in practical production due to its simple method and convenient operation. The sol-gel method has the characteristics of small product particle size, low reaction temper...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/0562C04B35/50C04B35/624
CPCH01M10/0562C04B35/50C04B35/624C04B2235/3203C04B2235/3244Y02E60/10
Inventor 刘海萍曹菲曹立新毕四富
Owner HARBIN INST OF TECH AT WEIHAI
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