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Li4Ti5O12, Li(4-alpha)Zalpha Ti5O12 or Li4ZbetaTi(5-beta)O12 particles, processes for obtaining same and use as electrochemical generators

a technology of electrochemical generators and processes, applied in the field of li4ti5o12, li(4-alpha)zalpha ti5o12 or li4zbetati(5-beta)o12 particles, can solve the problems of limiting the sacrificial capacity was very small, and the electrical capacity and the size of the particles were limited

Inactive Publication Date: 2004-10-14
HYDRO QUEBEC CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Residual impurities of the TiO.sub.2, Li.sub.2TiO.sub.3 and / or other type in the mixture limit the electrode capacity and limit the size of the particles.
However, the sacrificial capacity was very slight when carbon was replaced with a spinel material.

Method used

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  • Li4Ti5O12, Li(4-alpha)Zalpha Ti5O12 or Li4ZbetaTi(5-beta)O12 particles, processes for obtaining same and use as electrochemical generators
  • Li4Ti5O12, Li(4-alpha)Zalpha Ti5O12 or Li4ZbetaTi(5-beta)O12 particles, processes for obtaining same and use as electrochemical generators
  • Li4Ti5O12, Li(4-alpha)Zalpha Ti5O12 or Li4ZbetaTi(5-beta)O12 particles, processes for obtaining same and use as electrochemical generators

Examples

Experimental program
Comparison scheme
Effect test

example 1

Preparation in the Presence of Heptane of Particles of Li.sub.4T.sub.5O.sub.12 Coated with Carbon

[0128] 23 g of TiO.sub.2 with anatase structure (commercialized by the Kronoss Company, Varennes, Canada under the name XP-406) are mixed with 10 grams of Li.sub.2CO.sub.3 (Aldrich, Canada) and with 20 grams of Shawinigan black. An excess of carbon black is used to ensure complete transformation of the CO.sub.2 and lower the synthesis temperature.

[0129] This ternary mixture is placed in a steel container and heptane is added in a powder / liquid ratio of around 35 g / 150 ml. The heptane is used to reduce the heat and the friction between the particles of powder and the balls and leaves the product inert. Stainless steel balls are added to homogenize the ternary mixture. After 2 hours of intimate co-milling, a powder with fine particle size is obtained. The success of the co-milling depends on lowering the synthesis temperature. The heating of this co-milled mixture is carried out in two ste...

example 2

Dry Preparation of Particles of Li.sub.4Ti.sub.5O.sub.12 Coated with Carbon

[0130] 23 g of TiO.sub.2 with anatase structure (XP-406 from the Kronos Company, Varennes) are mixed with 10 grams of Li.sub.2CO.sub.3 (Aldrich, Canada) and with 20 g of Shawinigan black. Again an excess of carbon black is used to ensure complete transformation of the CO.sub.2 and lower the synthesis temperature. This ternary mixture is placed in a dry container with stainless steel balls.

[0131] After 2 hours of intimate milling, a powder with a fine particle size is obtained. Heating of this co-milled mixture is carried out in two steps, at 400.degree. C. and then at 600.degree. C. The X-ray spectrum reveals the presence of a spinel structure for the Li.sub.4Ti.sub.5O.sub.12 particles thus synthesized.

example 3

Dry Preparation and Characterization of Nano-particles of Li.sub.4T.sub.5O.sub.12 Coated with Carbon

[0132] 23 g of TiO.sub.2 with anatase structure (XP-406 from the Kronos Company, Varennes) are mixed with 10 grams of Li.sub.2CO.sub.3 (Aldrich, Canada) and with 2 grams of Shawinigan black. A 6-gram excess of carbon black is again used to ensure complete transformation of the CO.sub.2 and to lower the synthesis temperature. This ternary mixture is subject to high-energy mechanical milling (using a shaker mill machine of the type SPEX 8000) in the presence of stainless steel balls in a ball:powder ratio of 10:1. The milling period can vary between 3 minutes and 3 hours, which in the case of the present example is 2 hours. Heating of the co-milled mixture is carried out in two steps. The first step consists of rapid heating to 400.degree. C. in air. The second step consists of slow heating to 600.degree. C. This completes the transformation of the product into Li.sub.4Ti.sub.5O.sub.12 ...

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Abstract

Synthesis process for new particles of Li4Ti5O12, Li(4-alpha)ZalphaTi5O12 or Li4ZbetaTi(5-beta)O12, preferably having a spinel structure, wherein beta is greater than 0 and less than or equal to 0.5 (preferably having a spinel structure), alpha representing a number greater than zero and less than or equal to 0.33, Z representing a source of at least one metal, preferably chosen from the group made up of Mg, Nb, Al, Zr, Ni, Co. These particles coated with a layer of carbon notably exhibit electrochemical properties that are particularly interesting as components of anodes and / or cathodes in electrochemical generators.

Description

[0001] The present invention relates to new particles based on Li.sub.4Ti.sub.5O.sub.12, based on Li.sub.(4-.alpha.)Z.sub..alpha.Ti.sub.-5O.sub.12, or based on Li.sub.4Z.sub..beta.Ti.sub.(5-.beta.)O.sub.12.[0002] The present invention also relates to processes that make it possible to prepare these particles and to their use, especially in the area of electrochemical devices such as electrochemical generators.DESCRIPTION OF PRIOR ART[0003] Marketing of the lithium-ion battery by Sony, in 1990, was reported by Naguara and Tozawa, Prog. Batt. Solar Cells, 9 (1990), 209. It made possible an expansion and a significant breakthrough of batteries into the area of portable devices (telephone, computer). The technology of Li-ion batteries is based on lithium intercalation electrodes, in particular the anode which is made of graphite. At the time of the first charge, a passivation film is formed on the carbon surface. The chemistry and the composition of this passivation film are complex. Th...

Claims

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Application Information

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IPC IPC(8): C01G23/00H01G9/00H01G9/025H01G11/00H01M4/02H01M4/04H01M4/131H01M4/136H01M4/36H01M4/48H01M4/485H01M4/50H01M4/505H01M4/52H01M4/525H01M4/58H01M4/62H01M4/66H01M4/74H01M6/16H01M10/0525H01M10/0562H01M10/0565H01M10/36
CPCB82Y30/00Y10T428/2982C01G23/005C01P2002/77C01P2002/88C01P2004/03C01P2004/64C01P2006/40H01G9/155H01M4/02H01M4/0471H01M4/131H01M4/136H01M4/366H01M4/485H01M4/505H01M4/525H01M4/5825H01M4/625H01M4/661H01M4/745H01M10/0525H01M10/0562H01M10/0565H01M2300/004H01M2300/0082H01M2300/0085Y02E60/122Y02E60/13C01G23/003Y02E60/10H01G11/06H01G11/50H01G11/46H01G11/86Y02P70/50H01G11/04H01M4/623
Inventor ZAGHIB, KARIMGAUTHIER, MICHELBROCHU, FERNANDGUERFI, ABDELBASTMASSE, MONIQUE
Owner HYDRO QUEBEC CORP
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