Lithium lanthanum titanium oxygen LLTO composite solid-state electrolyte material and synthesizing method thereof

一种固态电解质、电解质材料的技术，应用在锂离子电池用高安全性无机复合固态电解质材料及其制备领域，能够解决LLTO电导率低、晶界电导率低、达不到实用要求等问题，达到缩短实验周期、提高总电导率、节省能耗和生产成本的效果

Active Publication Date: 2008-12-17
TSINGHUA UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Its grain conductivity has reached 10 at room temperature -3 S / cm, but its grain boundary conductivity is lower than 10 -5 S / cm, resulting in low conductivity of LLTO, which cannot meet practical requirements

Method used

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  • Lithium lanthanum titanium oxygen LLTO composite solid-state electrolyte material and synthesizing method thereof
  • Lithium lanthanum titanium oxygen LLTO composite solid-state electrolyte material and synthesizing method thereof
  • Lithium lanthanum titanium oxygen LLTO composite solid-state electrolyte material and synthesizing method thereof

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preparation example Construction

[0022] The present invention provides a novel lithium lanthanum titanium oxide composite solid electrolyte material containing an amorphous nano silicon oxide layer (2) at the grain boundary between crystal grains (1) and a synthesis method thereof. The experiment achieved the introduction of the amorphous nano-silicon oxide grain boundary layer (2) by using a wet chemical method. The wet chemical method used inexpensive organic silicide as an additive to be added to the lithium lanthanum titanium oxide solid electrolyte material. At 1-10%, the lithium lanthanum-titanium-oxygen composite solid electrolyte material containing silicon oxide grain boundary layer can be synthesized after sintering.

[0023] The process flow of the present invention is as follows:

[0024] (1) Preparation of LLTO raw material powder: use solid phase method or sol-gel method to prepare Li 3x La 2 / 3-x TiO 3 (x=0~0.16), disperse the raw material powder into ethanol to obtain a turbid liquid a for use;

[...

Embodiment 1

[0033] (1) Preparation of LLTO raw material powder: use solid phase method or sol-gel method to prepare Li 0.5 La 0.5 TiO 3 , Disperse 8 grams of raw material powder into ethanol to obtain turbid liquid a for use;

[0034] (2) Preparation of catalyst: prepare mixed solution b with 80ml water, 320ml ethanol and 800ml ammonia water;

[0035] (3) Preparation of silicon solution: Weigh 0.5 g of ethyl orthosilicate, and disperse it in ethanol to obtain solution c;

[0036] (4) Preparation of the mixed solution: After mixing the turbid solution a and the mixed solution b, drop the solution c into the mixed solution and stir evenly;

[0037] (5) Heating reaction: heating the mixed solution at 250°C for 3 hours;

[0038] (6) Drying: dry at 100°C to obtain composite powder;

[0039] (7) Sintering: After the composite powder is compressed, it is sintered at a high temperature of 1100 for 10 hours to obtain a composite solid electrolyte material.

Embodiment 2

[0041] (1) Preparation of LLTO raw material powder: use solid phase method or sol-gel method to prepare Li 0.5 La 0.5 TiO 3 , Disperse 2 grams of raw material powder into ethanol to obtain turbid liquid a for use;

[0042] (2) Preparation of catalyst: prepare mixed solution b with 80ml water, 240ml ethanol and 400ml ammonia water;

[0043] (3) Preparation of silicon solution: Weigh 0.125 g of ethyl orthosilicate, and disperse it in ethanol to obtain solution c;

[0044] (4) Preparation of the mixed solution: After mixing the turbid solution a and the mixed solution b, drop the solution c into the mixed solution and stir evenly;

[0045] (5) Heating reaction: heating the mixed solution at 200°C for 1 hour;

[0046] (6) Drying: dry at 90°C to obtain composite powder;

[0047] (7) Sintering: After the composite powder is pressed into tablets, it is sintered at a high temperature of 1200°C for 8 hours to obtain a composite solid electrolyte material.

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Abstract

The invention provides a La-Li-Ti-O (LLTO) composite solid electrolyte material containing an amorphous silicon oxidate grain boundary layer and the synthetic method thereof, and belongs to the field of the lithium ion battery. The material is characterized in that: composite ceramics of an amorphous nano-silicon oxidate layer 2 are contained in the position of the grain boundary between materialcrystal grains, and the induction of the amorphous nano-silicon oxidate layer 2 is realized by adopting the wet chemical process, in the wet chemical process, inexpensive organic silicide is adopted as the additive to be added to the LLTO solid electrolyte material, and when the silicone content is 1 to 10 percent, the LLTO composite solid electrolyte material containing the amorphous silicon oxidate grain boundary layer can be synthesized through agglomeration. The electrical conductivity of the grain boundary is obviously improved, thereby improving the total electrical conductivity of the material. The composite solid electrolyte material has the advantages that the preparation process is simple, the operation is easy, the experimental period is greatly shortened, and the synthesis temperature is reduced, the energy consumption and the production cost are saved.

Description

Technical field [0001] The invention belongs to the field of lithium ion batteries, and relates to a high-safety inorganic composite solid electrolyte material for lithium ion batteries and a preparation method thereof. Background technique [0002] With the pressure of energy and the environment, in order to reduce dependence on oil and pollution to the environment, the development of clean and efficient vehicles to replace the existing gasoline and diesel-fueled vehicles has become the development of the automobile industry formulated by all countries in the world. Strategic policy direction. The development of new energy vehicles puts forward higher requirements for the storage of power energy. As a power battery, the battery needs to have a smaller size, lighter weight and higher safety. Lithium-ion batteries are superior to other secondary batteries due to their high working voltage, mass density and energy density. Therefore, lithium-ion batteries are considered to be the b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01B1/06H01B1/08H01M10/36H01M10/40H01M6/18
CPCH01M10/0525H01M10/056H01M10/0562H01M10/0567H01M2300/0088Y02E60/10
Inventor 南策文梅骜冯玉川林元华横石章司南田善隆
Owner TSINGHUA UNIV
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