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a li 2 tio 3 Powder material, its preparation method and the li 2 tio 3 Method for preparing spinel lithium titanate from powder material

A technology of powder materials, lithium halite titanate, applied in the direction of nanotechnology, titanate, alkali metal titanate, etc. for materials and surface science, can solve the problem of poor electrolyte compatibility, large volume change, and safety problems and other problems, to achieve the effect of easy large-scale production, simple preparation method, and excellent rate performance

Active Publication Date: 2017-11-03
GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, carbon materials have the following disadvantages: 1. React with the electrolyte to form SEI, resulting in low initial charge and discharge efficiency; 2. Metal lithium is easy to deposit on the surface of the negative electrode, and there is no obvious voltage indication at the end of charging, which is likely to cause safety. Problem; 3. Poor compatibility with electrolyte, such as co-insertion of PC-containing electrolyte in graphite carbon materials, etc.; 4. Large volume changes during charge and discharge, and unsatisfactory cycle stability
It has not been found that lithium titanate (Li 4 Ti 5 o 12 ) of Li 2 TiO 3 Patent documents on materials and their preparation methods

Method used

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  • a li  <sub>2</sub> tio  <sub>3</sub> Powder material, its preparation method and the li  <sub>2</sub> tio  <sub>3</sub> Method for preparing spinel lithium titanate from powder material
  • a li  <sub>2</sub> tio  <sub>3</sub> Powder material, its preparation method and the li  <sub>2</sub> tio  <sub>3</sub> Method for preparing spinel lithium titanate from powder material
  • a li  <sub>2</sub> tio  <sub>3</sub> Powder material, its preparation method and the li  <sub>2</sub> tio  <sub>3</sub> Method for preparing spinel lithium titanate from powder material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Weigh lithium carbonate and nano-titanium dioxide according to the lithium-titanium molar ratio of 2:1, put 73.89g of lithium carbonate and 79.88g of nano-titanium dioxide into a mixing container, add zirconia balls, mix evenly with water for 24 hours as the mixing medium, and dry at 110°C. To obtain a precursor, put the obtained precursor into an alumina crucible, and sinter in a muffle furnace at 400 ° C for 5 hours under an air atmosphere to obtain Li 2 TiO 3 , the particle size of the primary particle is 20nm, the XRD test structure is monoclinic, and the median particle size is D 50 200nm.

Embodiment 2

[0035] Weigh lithium carbonate and metatitanic acid according to the lithium-titanium molar ratio of 2:1, put 73.89g of lithium carbonate and 97.9g of metatitanic acid into a mixing container, add 10 grams of acetylene black, add zirconia balls, and use absolute ethanol as the mixing medium Mix for 24 hours, dry at 110°C to obtain a precursor, put the obtained precursor into an alumina crucible, and treat it at 600°C in an air atmosphere in a muffle furnace for 10 hours to obtain Li 2 TiO 3 , the particle size of the primary particles is 75nm, the XRD test structure is monoclinic, and its XRD pattern is shown in figure 1 , median particle size D 50 is 3 μm.

Embodiment 3

[0037] Weigh lithium carbonate and metatitanic acid according to the lithium-titanium molar ratio of 2:1, put 73.89g of lithium carbonate and 97.91g of metatitanic acid into a mixing container, add 20 grams of polyvinyl alcohol, add zirconia balls, and mix evenly with acetone Dry at 110°C for 24 hours to obtain a precursor, put the obtained precursor into an alumina crucible, and sinter at 700°C in a muffle furnace under an air atmosphere for 5 hours to obtain Li 2 TiO 3 , the particle size of the primary particle is 90nm, the XRD test structure is monoclinic, and the median particle size is D 50 is 10 μm.

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Abstract

The invention discloses an Li2TiO3 powder material, a preparation method of the Li2TiO3 powder material, and a method for preparing spinel lithium titanate (Li4Ti5O12) with the Li2TiO3 powder material. The particle size of a primary particle of the Li2TiO3 powder material is 10-100 nanometers; an XRD (X-Ray Diffraction) testing structure is a monoclinic system or a cubic system; and the median particle size D50 is 50 nanometers-15 micrometers. The preparation method of the Li2TiO3 powder material comprises the steps of taking a lithium compound and a titanium compound at a mole ratio Li / Ti of 2:1 as raw materials, adding a certain amount of carbon or carbon precursor, performing uniform mixing in a medium, performing drying, placing the obtained precursor in a furnace, and performing sintering in an air atmosphere to synthesize the Li2TiO3 material. The method for preparing spinel lithium titanate with the Li2TiO3 powder material comprises the steps of mixing the Li2TiO3 powder material and titanium dioxide or metatitanic acid at a metering ratio of 2:3 (a mole ratio of Ti), adding a certain amount of carbon or carbon precursor, performing the uniform mixing in the medium, performing the drying, placing the obtained precursor in the furnace, and performing the sintering in the air atmosphere to synthesize a spinel lithium titanate material. Obtained spinel lithium titanate is high in purity, fine in primary particle and excellent in electrochemical property.

Description

technical field [0001] The invention relates to a method for preparing spinel lithium titanate (Li 4 Ti 5 o 12 ) of Li 2 TiO 3 Powder material, its preparation method, and use this Li 2 TiO 3 Preparation of spinel lithium titanate (Li 4 Ti 5 o 12 )Methods. Background technique [0002] Since Sony Corporation of Japan developed lithium-ion batteries using petroleum coke as the negative electrode in 1990, carbon materials have attracted people's attention. The varieties include artificial graphite, natural graphite, mesocarbon microspheres, petroleum coke, carbon fiber, etc., which are commercialized Lithium-ion battery main negative electrode material. However, carbon materials have the following disadvantages: 1. React with the electrolyte to form SEI, resulting in low initial charge and discharge efficiency; 2. Metal lithium is easy to deposit on the surface of the negative electrode, and there is no obvious voltage indication at the end of charging, which is like...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/485C01G23/00B82Y30/00
CPCB82Y30/00C01G23/005H01M4/485Y02E60/10
Inventor 卢世刚阚素荣袁敏娟刘菲
Owner GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG