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Preparation method of high-capacity lithium titanate material

A lithium titanate, high-capacity technology, applied in titanate, alkali metal titanate, chemical instruments and methods, etc., can solve the problems of low battery energy density, limited application of lithium titanate, complicated process, etc. Cost control, easy industrial production application, effect of shortening growth time

Inactive Publication Date: 2017-11-07
JIANGSU TOP FINE NEW RAW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, lithium titanate also has shortcomings. The lithium titanate material obtained in the existing research has a low stacking capacity, resulting in low battery energy density, which limits the application of lithium titanate. Therefore, improving the material tap density is the main reason for lithium titanate One of the research directions
[0004] Patent CN201010177934.4 discloses a preparation method of spherical lithium titanate, which can increase the tap density of the material, but this method has special requirements for equipment, and the process is complicated, which significantly increases the production cost

Method used

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Embodiment 1

[0021] Lithium carbonate and anatase titanium dioxide are selected as raw materials, lithium fluoride is used as a flux, the ratio of Li / Ti (mol%) is 0.80:1, the content of lithium fluoride is 1wt% of the mass of TiO2, and ethanol is used as a dispersant , ethanol: solid powder (wt%) = 0.7:1, after ball milling on a ball mill for 6 hours, dry in an oven with 21.6% oxygen gas at 40°C to obtain a precursor. Treat the precursor at 500°C for 2 hours in an atmosphere with an oxygen content of 10%, then heat it up to 800°C after cooling, keep it in an atmosphere with an oxygen content of 21.6% for 8 hours, and finally lower it to room temperature to obtain Li4Ti5O12 sample. The particle size of the obtained material is uniform, and the tap density is 1.20g / cm3. Compared with the tap density (0.78g / cm3) of lithium titanate prepared under the same conditions without adding flux, the density is significantly improved. A button battery was prepared with a lithium metal sheet as the cou...

Embodiment 2

[0023] Lithium nitrate and rutile titanium dioxide are selected as raw materials, boric acid is used as a flux, and the ratio of Li / Ti (mol%) is 0.82:1, and the content of boric acid is 0.5wt% of the mass of TiO2. Ethanol is used as a dispersant, ethanol: solid Powder (wt%)=0.8:1 After ball milling on a ball mill for 6 hours, the precursor was dried at 60° C. by passing a gas containing 0.1% oxygen in an oven. Treat the precursor at 500°C for 2 hours in an atmosphere with an oxygen content of 0.01%, then heat it up to 800°C for 8 hours in an atmosphere with an oxygen content of 99% after cooling, and finally get a Li4Ti5O12 sample after cooling down to room temperature . The obtained material particles are smooth and uniform in size, and the tap density is 1.36g / cm3, which is significantly higher than the tap density (0.80g / cm3) of lithium titanate prepared under the same conditions without adding flux. A button battery was prepared with metal lithium sheet as the counter ele...

Embodiment 3

[0025] Lithium hydroxide and anatase titanium dioxide are selected as raw materials, lithium tetraborate is used as a flux, and the ratio of Li / Ti (mol%) is 0.84: the content of lithium tetraborate is 0.5wt% of the mass of TiO2 for batching, and methanol is used as a dispersant , Methanol: solid powder (wt%) = 1: 1. After ball milling on a ball mill for 6 hours, the precursor was dried in an oven with 21.6% oxygen-containing gas at 50°C. Treat the precursor at 500°C for 2 hours in an atmosphere with an oxygen content of 21.6%, then heat it up to 800°C for 8 hours in an atmosphere with an oxygen content of 0.1% after cooling, and finally lower it to room temperature to obtain Li4Ti5O12 sample. The obtained material particles are smooth and uniform in size, and the tap density is 1.48g / cm3, which is significantly higher than the tap density (0.82g / cm3) of lithium titanate prepared under the same conditions without adding flux. A button battery was prepared with a metal lithium ...

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Abstract

The invention relates to a preparation method of a high-capacity lithium titanate material, mainly aiming at solving the problem that a lithium titanate material in existing technology production at present has a small capacity. The specific method comprises the following steps: carrying out ball milling on a lithium source, a titanium source, a fluxing agent and a dispersant according to a certain ratio and mixing materials; after drying, carrying out low-temperature pre-sintering; after cooling, carrying out high-temperature calcining to generate lithium titanate. The preparation method provided by the invention has the characteristics that the fluxing agent is added in a material mixing process; in a high-temperature sintering process, particles can be in more compact contact and the interfacial tension among the particles is reduced; the growth and development of crystals are better so that the volume density of the material is improved. The method has a simple process flow; the raw materials are easy to obtain; prepared lithium titanate has a large particle size and a high capacity and has good electrochemical performance.

Description

technical field [0001] The invention relates to the field of preparation of energy materials, in particular to a preparation method of lithium titanate, a negative electrode material of a lithium ion battery. Background technique [0002] Due to the advantages of high energy density, long cycle life, and no memory effect, lithium-ion batteries have always been a hot spot in the research and development of batteries. They have been applied in portable appliances, electric vehicles, energy storage and other fields and have good application prospects. At present, commercial lithium-ion battery anode materials generally use carbon anode materials, but because the redox potential of carbon anode materials is very close to the electrode potential of lithium, lithium ions are easily precipitated on the surface of carbon anodes to form lithium dendrites when the battery is overcharged. It may cause a short circuit of the battery and cause safety problems, and the carbon material wil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/00H01M4/485H01M10/0525
CPCC01G23/005C01P2004/03C01P2006/11C01P2006/40H01M4/485H01M10/0525Y02E60/10
Inventor 廖向阳谢宏伟王镇朱贤荣
Owner JIANGSU TOP FINE NEW RAW MATERIAL CO LTD
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