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Method for preparing surface self-grown titanium nitride conducting film modified lithium titanate

A technology of lithium titanate and titanium nitride, used in circuits, electrical components, battery electrodes, etc., can solve problems such as poor electronic conductivity, achieve firm and tight contact, improve electronic conductivity, and improve high-rate charge-discharge performance. Effect

Inactive Publication Date: 2010-06-09
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] For Li 4 Ti 5 o 12 The problem of poor electronic conductivity of the material itself, the purpose of the present invention is to propose a method for preparing lithium titanate modified by a surface self-grown titanium nitride conductive film, which can prepare Li 4 Ti 5 o 12 / TiN core-shell electrode material to improve the electronic conductivity of the material

Method used

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  • Method for preparing surface self-grown titanium nitride conducting film modified lithium titanate
  • Method for preparing surface self-grown titanium nitride conducting film modified lithium titanate
  • Method for preparing surface self-grown titanium nitride conducting film modified lithium titanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] According to urea: Li 4 Ti 5 o 12 1.23 g of urea was added at a mass ratio of 5%, ball milled and mixed in absolute ethanol medium for 2 h, and then put into a vacuum drying oven at 70° C. for 8 h. After drying in an atmosphere furnace in N 2 Under a protective atmosphere, the temperature was raised to 800°C at a rate of 2°C / min for 30 minutes, and then cooled with the furnace. The resulting product is Li 4 Ti 5 o 12 / TiN composite electrode material.

[0026] Material performance characterization:

[0027] The crystal structure of the material was analyzed with a Rigaku 3014 X-ray diffractometer in Japan, and the morphology of the material was observed with a transmission electron microscope TEM (PhilipsCM12).

[0028] Electrochemical performance test:

[0029] Both the electrode sheet and the lithium half-cell assembly are prepared as follows: the Li prepared in Example 1 4 Ti 5 o 12 / TiN composite electrode material, conductive carbon black, and binder ar...

Embodiment 2

[0034] According to urea: Li 4 Ti 5 o 12 0.74 g of urea was added at a mass ratio of 3%, ultrasonically mixed in an anhydrous ethanol medium for 1 h, and then placed in a vacuum drying oven at 100° C. for 8 h. After drying in an atmosphere furnace in N 2 Under a protective atmosphere, the temperature was raised to 850°C at a rate of 5°C / min for 30 minutes, and then cooled with the furnace. The resulting product is Li 4 Ti 5 o 12 / TiN composite electrode material.

[0035] The electrochemical performance test is the same as in Example 1.

[0036] The Li prepared by embodiment 2 method and proportioning 4 Ti 5 o 12 The / TiN composite electrode material has a gram capacity of 160.4mAh / g at 0.2C charge and discharge current, 159.3mAh / g at 0.5C charge and discharge current, and 130mAh / g at 3C charge and discharge current. When charging and discharging at 1C, the capacity retention rate of the material for 100 cycles is ≥94%.

Embodiment 3

[0038] According to urea: Li 4 Ti 5 o 12 2.5 g of urea was added at a mass ratio of 10%, ball milled and mixed in an acetone medium for 2 h, and then dried in a vacuum oven at 120° C. for 8 h. After drying in an atmosphere furnace in N 2 Under a protective atmosphere, the temperature was raised to 850°C at a rate of 3°C / min and kept for 10 minutes, and then cooled with the furnace. The resulting product is Li 4 Ti 5 o 12 / TiN composite electrode material.

[0039] The electrochemical performance test is the same as in Example 1.

[0040] The Li prepared by embodiment 3 method and proportioning 4 Ti 5 o 12 The / TiN composite electrode material has a gram capacity of 159.5mAh / g at 0.2C charge and discharge current, 158.1mAh / g at 0.5C charge and discharge current, and 125mAh / g at 3C charge and discharge current. When charging and discharging at 1C, the capacity retention rate of the material for 100 cycles is ≥92%.

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Abstract

The invention relates to a method for preparing a surface self-grown titanium nitride conducting film modified lithium titanate, which comprises the following steps of: uniformly mixing lithium titanate powder with solid nitrogen source in proportion in a dispersion medium in a mode of ultrasound or ball milling, drying the obtained slurry at the temperature of between70 and 120 DEG C, raising temperature to 600 to 900 DEG C in the inert protective atmosphere after grinding, preserving the heat for 10min to 1h, and then cooling together with a furnace to obtain the surface self-grown titanium nitride conducting film modified lithium titanate. Through heat nitrogen reaction, a layer of high-conductive film TiN is self-grown on the surface of the lithium titanate; the TiN film is firmly combined with the lithium titanate; and the prepared high-conductive Li4Ti5O12 / TiN material has high multiplying power of charge-discharge property and excellent circulating property. The preparation method has the advantages of low cost, simple operation and safety, and easy realization of mass production.

Description

technical field [0001] The invention belongs to the technical field of new energy materials, and specifically relates to a negative electrode material for lithium-ion batteries, in particular to the technology of using a solid nitrogen source material to self-grow a layer of highly conductive titanium nitride film on the surface of lithium titanate through pyrolysis and nitriding reaction . Background technique [0002] In today's world, with the shortage of global oil resources and the aggravation of atmospheric pollution, energy-saving and environmentally friendly hybrid electric vehicles (HEV) and pure electric vehicles (EV) are currently receiving special attention and great development. The demand for large-capacity, high-power, and high-safety chemical power supplies for electric vehicles is increasingly urgent. Lithium-ion batteries have become one of the main power sources for electric vehicles due to their high energy density, high operating voltage, and no memory ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/1391H01M4/62
CPCY02E60/12Y02E60/122Y02E60/10
Inventor 李劼张治安高宏权王新宇赖延清
Owner CENT SOUTH UNIV
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