Tantalum-doped cubic garnet structure Li7La3Zr2-xTaxO12 material and preparation method thereof

A garnet and cubic technology, which is applied in the field of lithium-ion battery electrolyte materials, can solve problems such as cost increase, energy consumption, and Li element loss, and achieve the effects of energy saving, good crystal form, and reduced content requirements

Active Publication Date: 2016-01-13
SHANGHAI POWER ENERGY STORAGE BATTERY SYST ENG TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The mainstream preparation methods in the industry tend to be solid-phase methods, but in the existing solid-state reactions, long-term high-temperature heating (often at 900°C and above, 6-12h or longer) will not only cause a large amount of energy consumption, It will also cause a large amount of Li element to be lost at high temperature, which will significantly increase the cost of production and processing.

Method used

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  • Tantalum-doped cubic garnet structure Li7La3Zr2-xTaxO12 material and preparation method thereof
  • Tantalum-doped cubic garnet structure Li7La3Zr2-xTaxO12 material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0026] (1) Weigh lanthanum zirconate, lanthanum oxide, lithium acetate and lithium tantalate. The molar ratio of lanthanum zirconate to lanthanum oxide is 7:5, the molar ratio of lanthanum zirconate to lithium acetate is 1:8, and the molar ratio of lanthanum zirconate to lithium acetate is 1:8. The molar ratio to lithium tantalate is 7:2 to comply with Li 7 La 3 Zr 1.75 Ta 0.25 O 12 The molar ratio of the elements in the molecular formula. The above materials were successively placed in a glass beaker and a complexing agent was added and stirred for 6 hours.

[0027] (2) After the mixing is uniform, the stirrer starts to heat, and the temperature is gradually raised to 80 °C and kept at a temperature until the excess water is removed, and the final paste is the precursor of the high-temperature solid-phase treatment.

[0028] (3) Pre-heat the precursor at 400°C for 3 hours in a tube furnace to remove cyclodextrin and a small amount of residual water, and take out the prod...

Embodiment 2

[0033] (1) Weigh lanthanum zirconate, lanthanum oxide, lithium acetate and lithium tantalate. The molar ratio of lanthanum zirconate to lanthanum hydroxide is 7:10, the molar ratio of lanthanum zirconate to lithium acetate is 1:8, and the zirconate The molar ratio of lanthanum to lithium tantalate was 7:2 to match the Li 7 La 3 Zr 1.75 Ta 0.25 O 12 molar ratio. The above materials were successively placed in a glass beaker and a complexing agent was added and stirred for 4 hours.

[0034] (2) After the mixing is uniform, the stirrer starts to heat, and the temperature is gradually raised to 80 °C and kept at a temperature until the excess water is removed, and the final paste is the precursor of the high-temperature solid-phase treatment.

[0035] (3) Pre-heat the precursor at 400°C for 3 hours in a tube furnace to remove cyclodextrin and a small amount of residual water, and take out the product, fully grind it with an agate mortar, and then roast it in a tube furnace at...

Embodiment 3

[0038] (1) Weigh lanthanum zirconate, lanthanum oxide, lithium nitrate and lithium tantalate. The molar ratio of lanthanum zirconate to lanthanum oxide is 7:5, the molar ratio of lanthanum zirconate to lithium nitrate is 1:8, and the molar ratio of lanthanum zirconate to lithium nitrate is 1:8. The molar ratio to lithium tantalate is 7:2 to comply with Li 7 La 3 Zr 1.75 Ta 0.25 O 12 molar ratio. The above materials were successively placed in a glass beaker and a complexing agent was added and stirred for 4 hours.

[0039] (2) After the mixing is uniform, the stirrer starts to heat, and the temperature is gradually raised to 80 °C and kept at a temperature until the excess water is removed, and the final paste is the precursor of the high-temperature solid-phase treatment.

[0040] (3) Pre-heat the precursor at 400°C for 4 hours in a tube furnace to remove cyclodextrin and a small amount of residual water, and take out the product, fully grind it with an agate mortar, and...

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Abstract

The invention discloses a tantalum-doped cubic garnet structure Li7La3Zr2-xTaxO12 material and a preparation method thereof. The preparation method comprises the steps that 1, lanthanum zirconate, a lanthanum source, a lithium source and a doped element being a tantalum source are weighed; the materials are placed in a container successively, a complexing agent is added into the container, and then stirring is performed for 4-6 h; 2, the temperature is gradually increased to 80 DEG C and kept till excessive moisture is removed, and a precursor processed in a high-temperature solid-phase mode is obtained; 3, the precursor is preheated for 3-5 h at the temperature of 400 DEG C, and a product is taken out, sufficiently and evenly ground and roasted for 1.5-5 h at the temperature of 900 DEG C to obtain a primary roasted product, wherein the value of x is 0.25-0.6. The method is simple in process, the requirement for the content of the doped materials is lowered, energy consumption and lithium high-temperature losses are reduced in the preparation process due to the fact that the roasting time is shortened, energy is saved, the cost is greatly reduced, and the preparation method is quite suitable for large-scale production.

Description

technical field [0001] The present invention relates to a kind of preparation method of inorganic oxide, especially a kind of tantalum doped cubic garnet structure Li 7 La 3 Zr 2-x Ta x o 12 The invention discloses a material preparation method, belonging to the field of lithium ion battery electrolyte materials. Background technique [0002] In 2007, the Weppner research group reported for the first time Li with a garnet structure 7 La 3 Zr 2 o 12 Materials (Murugan, R.; Thangadurai, V.; Weppner, W. Angewandte Chemie 2007, 46 (41), 7778.), the impedance test results show that the conductivity of the material at room temperature can reach 10 -4 S cm -1 The order of magnitude is suitable for the practical application level of all-solid-state lithium batteries. [0003] Thus the garnet structure Li 7 La 3 Zr 2 o 12 The material has begun to come into people's sight and is used as a solid electrolyte material for solid-state batteries to improve some safety haza...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0562H01M10/0525
CPCH01M10/0525H01M10/0562H01M2300/0068H01M2300/0071H01M2300/0085Y02E60/10
Inventor 王婷解晶莹王可王久林罗英
Owner SHANGHAI POWER ENERGY STORAGE BATTERY SYST ENG TECH
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