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High-temperature and high-pressure preparation method of oxygen vacancy-containing spinel structure metal oxide negative electrode material

A spinel structure and negative electrode material technology, applied in chemical instruments and methods, structural parts, titanium compounds, etc., can solve problems that limit the development of metal oxide negative electrode materials, and achieve excellent rate performance and cycle stability.

Pending Publication Date: 2022-06-28
CHANGCHUN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The usual way to introduce oxygen vacancy defects is to heat treatment for a long time in an inert or reducing atmosphere. However, the long-term process limits the industrialization of metal oxide anode materials.

Method used

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  • High-temperature and high-pressure preparation method of oxygen vacancy-containing spinel structure metal oxide negative electrode material
  • High-temperature and high-pressure preparation method of oxygen vacancy-containing spinel structure metal oxide negative electrode material
  • High-temperature and high-pressure preparation method of oxygen vacancy-containing spinel structure metal oxide negative electrode material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A spinel structure LiCrTiO with oxygen vacancies 4 High temperature and high pressure preparation method of negative electrode material:

[0031] S1. Put Li 2 CO 3 ,TiO 2 and Cr 2 o 3 The raw materials are placed in a mortar and thoroughly ground in a molar ratio of 1 to 1.5:1:1 to achieve uniform mixing;

[0032] S2. Mold the uniformly mixed powder in S1, assemble and assemble into a block, and place it in the cavity of a Chinese 420-type six-sided top press, heat and hold the pressure for 40 minutes under the conditions of 0.8GPa, 1073K, and get the product containing Spinel structure LiCrTiO with oxygen vacancies 4 Negative material synthesis blocks;

[0033] S3. The spinel structure LiCrTiO containing oxygen vacancies obtained in S2 4 The negative electrode material synthesis block is crushed and ground into powder, and the spinel structure LiCrTiO containing oxygen vacancies 4 Negative electrode material synthesis blocks are mixed with deionized water and ...

Embodiment 2

[0035] A spinel structure LiCrTiO with oxygen vacancies 4 High temperature and high pressure preparation method of negative electrode material:

[0036] S1. Adopt the same proportioning raw material as in Example 1 and be placed in the mortar and fully grind to realize uniform mixing;

[0037] S2. The uniformly mixed powder in S1 is molded, assembled and assembled into a block, and then placed in the cavity of a Chinese 420-type six-sided top press, respectively, at a pressure of 0.6GPa, 0.8GPa and 1GPa, and a temperature of 1073K for 40 minutes. A spinel structure LiCrTiO containing oxygen vacancies was obtained after pressure relief and cooling 4 Negative material synthesis blocks;

[0038] S3. Adopt the same operation steps as S3 in Embodiment 1.

Embodiment 3

[0040] A spinel structure Li with oxygen vacancies 4 Ti 5 o 12 High temperature and high pressure preparation method of negative electrode material:

[0041] S1. Put Li 2 CO 3 ,TiO 2 Put it in a mortar and grind it fully in a molar ratio of 4 to 4.5:5 with raw materials to achieve uniform mixing;

[0042] S2. Mold the uniformly mixed powder in S1, assemble and assemble into a block, and place it in the cavity of a Chinese 420-type six-sided top press, heat and hold the pressure at 0.8GPa, 1073K for 40 minutes, and obtain a product after decompression and cooling. A kind of spinel structure Li with oxygen vacancies 4 Ti 5 o 12 Negative material synthesis blocks;

[0043] S3. Adopt the same operation steps as S3 in Embodiment 1.

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Abstract

The invention provides a high-temperature and high-pressure preparation method of an oxygen vacancy-containing spinel structure metal oxide negative electrode material. The method comprises the following steps: uniformly mixing raw materials, carrying out compression molding, and assembling to form a synthetic block; placing the assembly block in a cavity of high-temperature and high-pressure synthesis equipment; and keeping the temperature and the pressure for more than 30 minutes under the conditions that the pressure is 0.5-2.0 GPa and the temperature is 773-1473K, so as to prepare the spinel structure metal oxide negative electrode material containing the oxygen vacancy. According to the method, oxygen vacancies are introduced in situ while a sample is synthesized, and long-time sintering in an inert atmosphere is avoided. Compared with the traditional solid-phase synthesis method, the preparation time is shortened, the process is simple, the repeatability is good, and the pressure is controllable.

Description

Technical field: [0001] The invention belongs to the technical field of material preparation, and relates to a high-temperature and high-pressure preparation method of a spinel structure metal oxide negative electrode material containing oxygen vacancies. Background technique: [0002] With the widespread application of lithium-ion batteries in electric and hybrid vehicles, especially large-scale public transportation, the electrochemical limitations of commercial graphite anode materials are gradually emerging, such as pulverization of graphite and lithium dendrites at high current densities. growth etc. Therefore, the development of long-term and safe lithium-ion battery anode materials has attracted extensive attention of researchers. [0003] The excellent cycle stability and safety characteristics of spinel metal oxides make them have the potential for industrial development. However, the low intrinsic conductivity and lithium-ion diffusion coefficient limit its appli...

Claims

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Application Information

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IPC IPC(8): C01G23/00H01M4/485H01M10/0525
CPCC01G23/003H01M4/485H01M10/0525C01P2002/72C01P2004/04C01P2002/85C01P2006/40Y02E60/10
Inventor 秦杰明闫律
Owner CHANGCHUN UNIV OF SCI & TECH
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