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Process for preparing carbon-doped spherical Li4Ti5O12

A spherical and negative electrode material technology, applied in chemical instruments and methods, alkali metal compounds, inorganic chemistry, etc., can solve the problems of poor conductivity and low bulk density, and achieve the effect of high bulk density, simple process flow and good conductivity

Inactive Publication Date: 2008-08-20
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the material has the problems of poor electrical conductivity and low bulk density. Judging from the current research results, these two problems have not been well resolved.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Example 1. Weigh 10g TiCl 4 Put into a beaker, add about 20ml ion-free water, hydrolyze to obtain TiOCl 2 Solution. 0.73g of carbon black (accounting for Li 4 Ti 5 O 12 15% of the mass), added to the prepared solution, and then ball milled to make it evenly mixed. Using kerosene as the dispersion medium, and adding Span 80 with a mass ratio of 2% to kerosene as a surfactant, the resulting mixed solution was slowly added dropwise to the dispersion medium kerosene under stirring, and then continued under stirring. Pass more than 5L of ammonia gas into the dispersion medium, stop stirring, and precipitate the gel. Centrifugal separation, aging the obtained dry gel with ammonia water with a mass volume concentration of 5% for 24 hours, and then wash with ion-free water until no Cl is detected in the washing water - After centrifugation and drying, the carbon-doped gel microspheres are obtained. Weigh Li according to the molar ratio Li:Ti=4:5 2 CO 3 (3.1g), uniformly mixed with ...

Embodiment 2

[0015] Example 2. Weigh 8g TiOSO 4 Put into a beaker, add about 20mL 5mol / L HCl solution to prepare TiOCl 2 Solution. 0.69g of carbon black (accounting for Li 4 Ti 5 O 12 15% of the mass) was added to the prepared solution, and then ball milled to make it evenly mixed. Using kerosene as the dispersing medium, and adding Span 80 with a mass ratio of 1% to kerosene as a surfactant, the resulting mixed solution was slowly added dropwise to the dispersing medium kerosene under stirring conditions, and then continued under stirring conditions Pass more than 5L of ammonia gas into the dispersion medium, stop stirring, and precipitate the gel. Centrifugal separation, aging the obtained xerogel with 10% mass and volume concentration of ammonia water for 30 hours, and then wash with ion-free water until no Cl can be detected in the washing water - After centrifugation and drying, the carbon-doped gel microspheres are obtained. Weigh Li according to the molar ratio Li:Ti=4:5 2 CO 3 (3.0g), ...

Embodiment 3

[0016] Example 3. Weigh 6g TiO 2 ·2H 2 Put O in a beaker, add about 20mL of 5mol / L HCl solution to prepare TiOCl 2 Solution. . 0.71g of carbon black (accounting for Li 4 Ti 5 O 12 15% of the mass) was added to the prepared solution, and then ball milled to make it evenly mixed. Using kerosene as the dispersing medium, and adding Span 80 with a mass ratio of 3% to kerosene as a surfactant, the resulting mixed solution was slowly added dropwise to the dispersing medium kerosene under stirring, and then continued under stirring. Pass more than 5L of ammonia gas into the dispersion medium, stop stirring, and precipitate the gel. After centrifugal separation, the obtained dry gel was aged for 16 hours with ammonia water with a mass and volume concentration of 3%, and then washed with ion-free water until no Cl was detected in the washing water. - After centrifugation and drying, the carbon-doped gel microspheres are obtained. Weigh Li according to the molar ratio Li:Ti=4:5 2 CO 3 (3.1g...

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Abstract

The invention discloses a preparing technology of carbon doping spherical Li4Ti5O12 of Li-ion battery cathode, which comprises the following steps: adopting TiOCl2 solution as raw material liquid; doping certain quantity of carbon black in the raw material liquid evenly with 80-kerosene as dispersion medium; dripping the raw material liquid in the dispersion medium kerosene; inputting ammonia gas in the kerosene to generate gel sedimentation; centrifuging; aging; washing; drying to produce gel microball priority; adding Li to heat protected by inert gas to prepare doped carbon spherical Li4Ti5O12. The invention possesses high cathode piling density, which improves conductivity.

Description

Technical field [0001] The invention relates to a lithium ion battery anode material doped with carbon-doped spherical Li 4 Ti 5 O 12 The preparation process belongs to the technical field of chemical engineering and new material preparation. Background technique [0002] Currently, most of the commercially available anode materials for lithium-ion batteries use graphitized carbon materials. However, the material has poor compatibility with the electrolyte, and the thermal stability of the SEI film formed by the interaction with the electrolyte is poor, which may cause safety problems, thereby limiting the use of lithium-ion batteries in power batteries and areas with higher safety requirements In the application. Spinel type lithium titanate (Li 4 Ti 5 O 12 ) With its excellent cycle performance and high safety, it has attracted more and more attention from researchers in recent years. It is a stress-free insertion material that does not change its structure during charging and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/00C01D15/00H01M4/58H01M4/485
CPCY02E60/12Y02E60/10
Inventor 高剑姜长印应皆荣万春荣何向明李建军王莉任建国蒲薇华
Owner TSINGHUA UNIV