Method for preparing negative electrode material lithium titanate of lithium battery through spray freeze drying

A technology of spray freeze-drying and negative electrode materials, which is applied in the direction of battery electrodes, circuits, electrical components, etc., can solve the problems of unsatisfactory electrochemical performance, lithium dendrite short circuit, poor conductivity, etc., and achieve excellent high rate discharge characteristics, particle size Uniform distribution and improved conductivity

Inactive Publication Date: 2016-12-07
SOUNDON NEW ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, the anode materials of commercial lithium-ion batteries mostly use carbon anode materials, but carbon anode materials still have some defects: they react with the electrolyte to form a surface passivation film during the first discharge process, resulting in a low initial coulombic efficiency; The electrode potential of the carbon electrode is similar to that of metal lithium. When the battery is overcharged, lithium dendrites will be formed to cause a short circuit, causing safety problems, etc.
[0004] However, lithium titanate is an insulating material with poor conductivity, rapid capacity decay and poor rate performance during high-current charging and discharging, which limits its application.
The existing preparation methods of lithium titanate are mainly spray drying and solid-phase methods, and element doping and surface carbon coating are used in the preparation process, although the above methods can solve the problem of poor electronic conductivity of lithium titanate materials to a certain extent , but its electrochemical performance is still unsatisfactory

Method used

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  • Method for preparing negative electrode material lithium titanate of lithium battery through spray freeze drying
  • Method for preparing negative electrode material lithium titanate of lithium battery through spray freeze drying
  • Method for preparing negative electrode material lithium titanate of lithium battery through spray freeze drying

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] According to the molar ratio Li: (Ti+Nb) = 0.805, Ti: Nb = 4.95: 0.05, weigh Li 2 CO 3 , rutile TiO 2 , Nb 2 o 5 Mix evenly and disperse in distilled water with a solid content of 20%. Transfer the dispersed slurry to a sand mill and grind it for 1 hour, then spray the slurry into a mixture of liquid nitrogen and liquid propane at a volume ratio of 1:1.5. A frozen product is produced in the refrigerant, and the frozen product is vacuum freeze-dried at -60°C for 18 hours to sublimate and disappear the water in the product to obtain a porous spherical lithium titanate precursor. The precursor is placed in an atmosphere furnace under an air atmosphere for 400 After pre-firing at ℃ for 5 hours, switch to nitrogen atmosphere and sinter at 800℃ for 9 hours to obtain the target product porous spherical lithium titanate negative electrode material: Li 4 Nb 0.05 Ti 4.95 o 12 Such as figure 1 shown.

[0022] A 2032 button battery composed of the material in Example 1 and...

Embodiment 2

[0024] According to the molar ratio Li: (Ti+Nd) = 0.82, Ti: Nd = 4.95: 0.05, weigh Li 2 CO 3 , rutile TiO 2 、Nd 2 o 3 Mix evenly and disperse in distilled water with a solid content of 18%. Transfer the dispersed slurry to a sand mill and grind it for 0.5h, then spray the slurry into liquid nitrogen and liquid propane to mix in a volume ratio of 1:2 A frozen product is produced in the refrigerant, and the frozen product is vacuum freeze-dried at -50°C for 16 hours to sublimate and disappear the water in the product to obtain a porous spherical lithium titanate precursor, which is placed in an atmosphere furnace under an air atmosphere Pre-fired at 435°C for 4 hours, then switched to sintering at 775°C for 8 hours under nitrogen atmosphere to obtain the target product porous spherical lithium titanate negative electrode material: Li 4 Nd 0.05 Ti 4.95 o 12 .

[0025] A 2032 button battery composed of the material of Example 2 and metal lithium sheets was tested at 25°C b...

Embodiment 3

[0027] According to molar ratio Li: (Ti+V) = 0.80, Ti: V = 4.95: 0.06, weigh Li 2 CO 3 , rutile TiO 2 , V 2 o 5 Mix evenly and disperse in distilled water with a solid content of 25%. Transfer the dispersed slurry to a sand mill and grind for 1.5 hours, then spray the slurry into liquid nitrogen and liquid propane to mix at a volume ratio of 1:1 The frozen product is produced in the refrigerant, and the frozen product is vacuum freeze-dried at -40°C for 20 hours to sublimate and disappear the water in the product to obtain a porous spherical lithium titanate precursor, which is placed in the atmosphere furnace under the air atmosphere After pre-calcining at 400°C for 4 hours, switch to nitrogen atmosphere and sinter at 850°C for 8 hours to obtain the target product porous spherical lithium titanate negative electrode material: Li 4 V 0.06 Ti 4.94 o 12 .

[0028] A 2032 button battery composed of the material of Example 3 and metal lithium sheets was tested at 25°C by a...

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Abstract

The invention discloses a method for preparing a negative electrode material lithium titanate of a lithium battery through spray freeze drying. The method comprises the steps of weighing ingredients of a Ti compound, a Li compound and a metal oxide M at a stoichiometric ratio, dispersing the ingredients into distilled water, carrying out sanding, carrying out pelletizing through spray freeze drying by employing liquid nitrogen and liquid propane as refrigerants, and then burning to obtain an M-doped and modified lithium titanate material. The method is simple in process and high in controllability; the obtained material is excellent in high-rate capability and can be suitable for industrial production of the lithium titanate negative electrode material.

Description

technical field [0001] The invention relates to a preparation method of a battery electrode material, in particular to a method for preparing lithium titanate, a negative electrode material of a lithium battery, by spray freeze drying. Background technique [0002] At present, the anode materials of commercial lithium-ion batteries mostly use carbon anode materials, but carbon anode materials still have some defects: they react with the electrolyte to form a surface passivation film during the first discharge process, resulting in a low initial coulombic efficiency; The electrode potential of the carbon electrode is similar to that of metal lithium. When the battery is overcharged, lithium dendrites will be formed to cause a short circuit and cause safety problems. [0003] Lithium titanate, as an anode material for lithium-ion batteries that has attracted much attention in recent years, has gradually become a research hotspot. It has many advantages: (1) The crystal struct...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/485H01M4/1391H01M10/0525
CPCH01M4/1391H01M4/485H01M10/0525Y02E60/10
Inventor 陈敏唐泽勋商士波常敬杭刘洪金
Owner SOUNDON NEW ENERGY TECH CO LTD
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