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High energy density spinel structural lithium titanate material and preparation method thereof

A technology of structural lithium titanate and spinel, which is applied in the field of nanomaterial preparation technology and energy, can solve the problems of poor fast charge and discharge performance, affecting the charge and discharge performance of lithium ion battery electrode materials, and low electronic conductivity.

Inactive Publication Date: 2009-11-18
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The initial electronic conductivity of pure spinel lithium titanate is very low, which affects the charge and discharge performance of lithium-ion battery electrode materials, especially the fast charge and discharge performance is very poor

Method used

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  • High energy density spinel structural lithium titanate material and preparation method thereof
  • High energy density spinel structural lithium titanate material and preparation method thereof
  • High energy density spinel structural lithium titanate material and preparation method thereof

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Effect test

Embodiment 1

[0025] Heat treatment of spinel lithium titanate submicron particles in 350°C nitrogen atmosphere to obtain high specific energy spinel structure lithium titanate submicron particles, test its performance, and compare with spinel structure titanium without nitrogen heat treatment The performance of lithium oxide submicron particles is compared:

[0026] Dissolve 3-4g of lithium acetate in 20-40ml of ethanol, add 3g of titanium dioxide powder, stir for 4-6 hours, and then dry at 100°C for 7-10 hours. The dried powder is taken out, ground and sieved, then heat-treated in an air atmosphere at 800°C for 3 hours, and cooled with the furnace. The obtained ordinary spinel lithium titanate submicron particles were heat-treated at 350° C. under a nitrogen atmosphere to obtain high specific energy spinel lithium titanate submicron particles, and their properties were tested. The SEM images of spinel lithium titanate submicron particles and products without nitrogen heat treatment are s...

Embodiment 2

[0031] Using sonochemical hydrothermal method and heat treatment at 350°C under 3% (volume) hydrogen / argon atmosphere to obtain high specific energy spinel structure lithium titanate nanotubes, and test their properties:

[0032] 5g TiO 2 Mix with 70mL of 10M NaOH solution at a power of 0.2-0.5W / cm 2 Under the sonochemical reaction for 30 minutes, and then moved into a 100mL autoclave with Teflon liner for hydrothermal reaction for 24h, the hydrothermal temperature was 150°C. After the reaction, take out the reaction kettle, cool to room temperature naturally, filter after opening the lid of the kettle, wash the product of the hydrothermal method with 0.2M concentration of nitric acid under the condition of pH 3 for 30 minutes, and vacuum filter the product through After drying at 80°C, a white fluffy powder product is obtained, which is H 2 Ti 3 o 7 nanotube. 1.5g H 2 Ti 3 o 7 The nanotubes were mixed with 40mL LiOH aqueous solution, stirred evenly, and then moved int...

Embodiment 3

[0037] Heat treatment in a nitrogen atmosphere at 800°C by a solid-state method to obtain submicron particles of lithium titanate with high specific energy spinel structure, and test its properties:

[0038] Dissolve 3-4g of lithium acetate in 20-40ml of ethanol, add 3g of titanium dioxide powder, stir for 4-6 hours, and then dry at 100°C for 7-10 hours. The dried powder was taken out, ground, sieved, and then heat-treated in a nitrogen atmosphere at 800°C for 3 hours, then cooled in the furnace to obtain high specific energy spinel lithium titanate submicron particles, and its properties were tested. The SEM image of the product is shown in Figure 8 .

[0039] Take 2.4g of high specific energy spinel lithium titanate submicron particles, 0.3g of binder polyvinylidene fluoride (PVDF) and 0.3g of conductive agent acetylene black. After mixing evenly, add about 15ml of dispersant N-methylpyrrolidone (NMP), and stir for 4 hours. Then cast on the aluminum foil by doctor blade ...

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Abstract

The invention relates to a high energy density spinel structural lithium titanate material and a preparation method thereof, belonging to the field of nano material preparation technology and energy. The preparation method comprises the following steps: taking cheap industrially produced titanium dioxide as a raw material and carrying out heat treatment on the titanium dioxide by an ultrasonic chemical water-heating method under reducing atmosphere to prepare a lithium titanate nano tube / wire, or taking lithium salt and titanium dioxide as raw materials and carrying out heat treatment on the lithium salt and titanium dioxide under reducing atmosphere to prepare lithium titanate submicron particulate, or carrying out heat treatment on the prepared spinel structural lithium titanate under reducing atmosphere. The high energy density lithium titanate materials obtained through heat treatment under reducing atmosphere can maintain higher capacity, better cyclical stability and longer service life under heavy current than the lithium titanate materials obtained through heat treatment in air, are suitable for serving as electrode materials of lithium ion batteries, supercapacitors or hybrid batteries and are expected to be applied to electric automobiles, etc.

Description

technical field [0001] The invention relates to spinel structure lithium titanate with high charge and discharge rate and high specific energy, and belongs to the field of nano material preparation technology and energy. Background technique [0002] In recent years, spinel-type lithium titanate has been paid more and more attention as an electrode material for new energy storage batteries. This is because the lattice constant of spinel-type lithium titanate changes little before and after lithium ion insertion and extraction, which is called lithium Ion-intercalated "zero-strain materials" can theoretically have excellent cycle stability. At the same time, spinel lithium titanate has the characteristics of good anti-overcharge performance, thermal stability, good safety and large specific capacity, and is an excellent new lithium-ion battery material. Spinel-type lithium titanate can also be used as an electrode material for supercapacitors, providing it with high power de...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/00H01M4/58H01G9/042
CPCY02E60/12Y02E60/13H01G11/50Y02T10/70
Inventor 唐子龙徐睿张中太
Owner TSINGHUA UNIV