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Method for manufacturing spinelle lithium titanate for lithium ionic cell cathode material

A lithium-ion battery and negative electrode material technology, applied in battery electrodes, chemical instruments and methods, circuits, etc., can solve the problems of low initial charge and discharge efficiency, poor uniformity, and no obvious voltage indication, etc., to improve the performance of high-current charge and discharge , easy mass production, and excellent electrochemical performance

Inactive Publication Date: 2009-03-25
GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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. Lithium metal 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 easy to cause safety. 3. Poor compatibility with the electrolyte, such as co-insertion of PC-containing electrolytes in graphite carbon materials, etc.; 4. Large volume changes during charging and discharging, and unsatisfactory cycle stability
[0003] Lithium titanate (Li 4 Ti 5 o 12 ) preparation methods generally include traditional high-temperature solid-phase method, sol-gel method, etc. The traditional high-temperature solid-phase method is based on TiO 2 with Li 2 CO 3 Or LiOH is synthesized at a high temperature of 800°C to 1000°C, and the reaction time is generally 12 to 24 hours. The advantage of this method is that the process is simple and easy to produce on a large scale. The gel method generally uses the organic alkoxide of titanium and lithium as the precursor, and the target product is prepared by hydrolysis and sol-gel process. Compared with the traditional high-temperature solid-phase method, the product has high chemical purity, good uniformity, and finer particles. , but this method uses organic compounds to increase the cost, and the operation is complicated, so it is not suitable for large-scale production

Method used

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  • Method for manufacturing spinelle lithium titanate for lithium ionic cell cathode material
  • Method for manufacturing spinelle lithium titanate for lithium ionic cell cathode material
  • Method for manufacturing spinelle lithium titanate for lithium ionic cell cathode material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Take by weighing 93.5 g of metatitanic acid 93.5 g of purity 98% and lithium acetate (CH 3 COOLi.2H 2 (0) 84.88g was put into a mixing container, 19.82g of acetylene black was added, uniformly mixed in an ethanol medium for 10 hours, dried at 80°C, then put into an alumina crucible, treated at 300°C in a muffle furnace for 10 hours, and then Synthesized at 700°C for 15 hours to obtain lithium titanate with spinel structure. The electrochemical performance test specific capacity is 156mAh / g, and the ratio of 1C / 0.1C specific capacity is 91%. The particle morphology of the spinel structure lithium titanate that embodiment 1 obtains is as follows figure 1 As shown, the particle size of its particles is less than 500 nm. The cycle curve of the spinel structure lithium titanate that embodiment 1 obtains is as follows Image 6 shown. The rate performance of the spinel structure lithium titanate that embodiment 1 obtains is as follows Figure 7 shown, and Figure 8 Comp...

Embodiment 2

[0029] Take by weighing 93.5 g of metatitanic acid 93.5 g of purity 98% and lithium hydroxide (LiOH.H 2 O) 36.38g was put into a mixing container, 20g of polyvinyl alcohol was added, uniformly mixed in the mixture medium of ethanol and water for 20 hours, dried at 120°C, then put into an alumina crucible, and treated at 400°C in a muffle furnace for 8 hours, and then synthesized at 600°C for 25 hours to obtain spinel lithium titanate. The electrochemical performance test specific capacity is 152mAh / g, and the ratio of 1C / 0.1C specific capacity is 93%. The particle morphology of the spinel structure lithium titanate that embodiment 2 obtains is as follows figure 2 As shown, the particle size of its particles is less than 500 nm.

Embodiment 3

[0031] Weigh 93.5g of metatitanic acid with a purity of 98% and lithium carbonate with a purity of 98% and 31.05g of lithium carbonate according to the lithium-titanium molar ratio of 0.88, put them into a mixing container, add 14g of graphite, and mix uniformly in an acetone medium for 30 hours. Dry it, then put it into an alumina crucible, treat it in a muffle furnace at 500°C for 5 hours, and then synthesize it at 800°C for 5 hours to obtain spinel lithium titanate. The electrochemical performance test specific capacity is 153mAh / g, and the ratio of 1C / 0.1C specific capacity is 88%. The XRD spectrum pattern of the spinel structure lithium titanate that embodiment 3 obtains is as Figure 4 shown. The charge-discharge curve of the spinel structure lithium titanate that embodiment 3 obtains is as follows Figure 5 shown.

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Abstract

The invention provides a method for preparing spinel lithium titanate used for the negative electrode materials of lithium ion batteries, which comprises the following steps of: mixing compounds of metatitanic acid and lithium according to an atomic ratio of lithium to titanium between 0.8 and 0.88; adding into carbon or powder former body of the carbon; carrying out an even mixing for 5 to 72 hours in a medium and then drying the mixture; carrying out treatment for 2 to 20 hours under the temperature between 200 and 500 DEG C; then synthesizing for 2 to 72 hours under the temperature between 600 and 900 DEG C, to acquire spinel-structure lithium titanate for the negative electrode materials of the lithium ion batteries. Adopting the cheap metatitanic acid as the raw materials and adding into the carbon or powder former body of the carbons, the method for preparing spinel lithium titanate for the negative electrode materials of the lithium ion batteries realizes the synthesis of spinel-structure lithium titanate with grains diameter less than 500 nanometers under lower temperatures and greatly improves the rate capacity, while the traditional high-temperature solid state method, with a sintering temperature generally between 800 and 100 DEG centigrade, only produces larger lithium carbonate particles at micron levels. With simple technique and strong operability, the method for preparing spinel lithium titanate for the negative electrode materials of the lithium ion batteries is easy to realize large-scale production.

Description

technical field [0001] The invention mainly relates to a spinel lithium titanate (Li 4 Ti 5 o 12 ) preparation method, which belongs to the technical field of lithium ion battery negative electrode material preparation. 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. Lithium metal 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 easy to cause safety. 3. Poor compatibility wit...

Claims

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Application Information

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IPC IPC(8): C01G23/00C01D15/00H01M4/58
CPCY02E60/10
Inventor 卢世刚阚素荣伍乐李文成张向军庞静金维华王昌胤刘莎
Owner GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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