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Ultrasonic atomization reparation method of porous Li4Ti5O12 hollow spheres

An ultrasonic atomization and hollow sphere technology, applied in chemical instruments and methods, inorganic chemistry, titanium compounds, etc., can solve the problems of difficult control of product particle size distribution, long sintering time, low production efficiency, etc., to improve high-current charging. Discharge performance and cycle performance, easy mass production, simple operation effect

Active Publication Date: 2017-09-29
FUJIAN NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The existing nanoscale lithium titanate preparation technologies mainly include hydrothermal method, sol-gel method, spray cracking method and template method, etc. These methods have long sintering time, low production efficiency, difficult control of particle size distribution of the product, and difficult cumbersome and costly

Method used

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  • Ultrasonic atomization reparation method of porous Li4Ti5O12 hollow spheres
  • Ultrasonic atomization reparation method of porous Li4Ti5O12 hollow spheres
  • Ultrasonic atomization reparation method of porous Li4Ti5O12 hollow spheres

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Hollow spherical hole Li 4 Ti 5 O 12

[0037] 3.32 g Li 2 CO 3 Dissolve in 20 ml of absolute ethanol, continue stirring at room temperature for 30 minutes, add 29.3 ml of isopropyl titanate dropwise, and continue to stir for 20 minutes to obtain A solution. Dissolve 25.2 grams of oxalic acid and 1.5 grams of sucrose in 400 milliliters of deionized water, and stir thoroughly to obtain a clear solution B; add solution A to solution B dropwise at a rate of 5 drops per second, and continue to stir for 1 hour. Mix the solution with the atomized precursor. The resulting solution was atomized with an ultrasonic atomization system with an oscillation frequency of 2.4MHz, the atomization volume was 0.2 ml per minute, and the atomized droplets produced were loaded into the tube furnace at a temperature of 600 ℃ by a vacuum pump. The moving speed of the drop in the quartz tube is 3 cm / s, and the dried precursor powder is collected by a powder collecting device.

[0038] The collected...

Embodiment 2

[0045] 3.24 g Li 2 CO 3 Dissolve in 30 ml of absolute ethanol, continue to stir at room temperature for 30 minutes, add 29.3 ml of isopropyl titanate dropwise, continue to stir for 30 minutes to obtain A solution. Dissolve 25.2 g of oxalic acid in 300 ml of deionized water, stir thoroughly to obtain a clear solution B; add solution A to solution B dropwise at a rate of 5 drops per second, and continue to stir for 2 hours to obtain an atomized solution Precursor mixed solution. The resulting solution is atomized with an ultrasonic atomization system with an oscillation frequency of 1.7MHz. The amount of atomization is 0.5 ml per minute. The resulting atomized droplets are loaded into a tube furnace at a temperature of 700℃ by a vacuum pump. The moving speed of the drop in the quartz tube is 5 cm / s, and the dried precursor powder is collected by a powder collecting device. The collected precursor powder was placed in a muffle furnace and calcined in an air atmosphere: the temper...

Embodiment 3

[0050] Dissolve 34 ml of butyl titanate in 50 ml of absolute ethanol, continue stirring at room temperature for 20 minutes, add 3 ml of glacial acetic acid dropwise, and continue to stir for 10 minutes to obtain a solution A. Dissolve 38.4 g of citric acid in 300 ml of deionized water, continue stirring at room temperature for 10 minutes, add 5.516 g of lithium nitrate, and continue to stir for 20 minutes to obtain a B solution. The A solution was added dropwise to the B solution at a dropping rate of 3 drops per second, and stirring was continued for 1 hour to obtain a precursor mixed solution for atomization. The resulting solution is atomized with an ultrasonic atomization system with an oscillation frequency of 1.7MHz. The atomization volume is 0.5 ml per minute. The resulting atomized droplets are loaded into a tube furnace at a temperature of 650℃ by a vacuum pump. The moving speed of the drop in the quartz tube is 5 cm / s, and the dried spherical lithium titanate precurso...

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Abstract

The invention relates to an ultrasonic atomization preparation method of porous Li4Ti5O12 hollow spheres. The method is as follows: soluble Li and Ti compounds in the molar ratio of (4-4.3): 5 are dissolved in absolute ethanol to obtain a solution A, a soluble metal ion chelating agent and a carbon-containing compound are dissolved in deionized water to obtain a solution B, the solution A is added to the solution B under stirring condition, stirring is continued for 1 to 3 hours, then the obtained mixed solution is atomized into droplets by an ultrasonic atomizer, the droplets are loaded into a high temperature furnace with the help of a vacuum pumping system, the droplets become precursor powder, and finally the porous hollow spherical lithium titanate material is obtained by calcination in an air or oxygen atmosphere. The method effectively optimizes the space structure and the particle size of the lithium titanate negative electrode material, and effectively improves the high current charge discharge performance and the cycle performance of the Li4Ti5O12 material. At the same time, the method has the advantages of simple operation, high efficiency, low cost and convenient mass production and the like.

Description

Technical field: [0001] The invention relates to a porous Li 4 Ti 5 O 12 The ultrasonic atomization preparation method of hollow sphere belongs to the technical field of lithium ion battery material preparation. technical background [0002] In recent years, with the miniaturization and high performance of digital devices and electronic meters, lithium-ion batteries with high energy density and long cycle life have received increasing attention. The negative electrode material is an important part of lithium-ion batteries and plays a key role in battery performance. Spinel-type lithium titanate is a kind of "zero strain" material, which has the advantages of stable charging and discharging voltage and environmental friendliness. The crystal structure can maintain a high degree of stability during the lithium ion extraction / intercalation process, which can effectively avoid lithium branches The formation of crystals and the decomposition of electrolytes fundamentally eliminate th...

Claims

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Application Information

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IPC IPC(8): C01G23/00H01M4/485H01M10/0525B82Y30/00
CPCB82Y30/00C01G23/005C01P2002/72C01P2004/03C01P2004/34C01P2006/40H01M4/485H01M10/0525Y02E60/10
Inventor 林应斌杨艳敏王智胜王颖峰黄志高
Owner FUJIAN NORMAL UNIV
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