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Preparation method for spherical lithium titanate material

A lithium titanate, spherical technology, applied in the field of preparation of spherical lithium titanate negative electrode material, can solve the problems of high cost, long time, complicated steps, etc., and achieve the effect of uniform particle size and excellent electrochemical performance.

Active Publication Date: 2014-03-26
PEKING UNIV +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention mainly aims at the disadvantages of uneven mixing, high heat treatment temperature, long time in the process of solid-phase synthesis, cumbersome steps and high cost in liquid-phase synthesis, and provides a spherical shape with regular shape, excellent performance and suitable for Preparation method of spherical lithium titanate negative electrode material for high-power lithium-ion power battery produced on an industrial scale

Method used

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  • Preparation method for spherical lithium titanate material
  • Preparation method for spherical lithium titanate material
  • Preparation method for spherical lithium titanate material

Examples

Experimental program
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Effect test

Embodiment 1

[0033] 1. Synthesis of spherical titania

[0034] Prepare a titanium sulfate aqueous solution with a concentration of 0.2 mol / liter. Measure 1 liter of the prepared titanium sulfate aqueous solution and 1 liter of n-propanol in a 2 liter reaction vessel, mix well, and then add 10 grams of polyvinylpyrrolidone K30 to fully dissolve them. Put the reaction vessel at a temperature of 80°C, hydrolyze the mixed solution for 100 minutes to obtain spherical titanium dioxide hydrate, then transfer the obtained material to a solid-liquid separator for solid-liquid separation, and wash the solid obtained from solid-liquid separation with deionized water The pH of the product to wash water was 6. Place the resulting solid product in a desiccator to dry, then transfer it to an alumina crucible, raise the temperature in a muffle furnace at a rate of 300°C / hour to a furnace at 700°C, keep the temperature constant for 2 hours, and stop heating , naturally cooled to room temperature in the f...

Embodiment 2

[0040] 1. Synthesis of spherical titania

[0041] Spherical titanium dioxide was prepared under the same conditions as in Example 1.

[0042] 2. Synthesis of spherical lithium titanate

[0043] The heat treatment temperature of 800° C. is replaced by a heat treatment temperature of 850° C., and other conditions are the same as in Example 1. The XRD test shows that the material is lithium titanate with a single spinel structure; the SEM observation shows that the product particles are uniform and spherical; the tap density of the material is 1.2g / cm 3 , by particle size analysis particle D 50 It is about 1.3 μm.

[0044] 3. Electrochemical properties of spherical lithium titanate materials

[0045] The battery was assembled under the same conditions as in Example 1. The charge and discharge voltage is 1.0-2.5V. Under 0.2C current discharge, the discharge specific capacity is about 160mAh / g, the average capacity decay rate per cycle is less than 0.04%, and the discharge spe...

Embodiment 3

[0047] 1. Synthesis of spherical titania

[0048] Spherical titanium dioxide was prepared under the same conditions as in Example 1.

[0049] 2. Synthesis of spherical lithium titanate

[0050] The heat treatment temperature of 800° C. is replaced by a heat treatment temperature of 900° C., and other conditions are the same as in Example 1. The XRD test shows that the material is lithium titanate with a single spinel structure; the scanning electron microscope (SEM) observation shows that the product particles are uniform and spherical; the tap density of the material is 1.2g / cm 3 , by particle size analysis particle D 50 It is about 1.8 μm.

[0051] 3. Electrochemical properties of spherical lithium titanate materials

[0052] The battery was assembled under the same conditions as in Example 1. The charge and discharge voltage is 1.0-2.5V, and the discharge specific capacity is about 155mAh / g under 0.2C current discharge, and the average capacity decay rate per cycle is ...

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Abstract

The invention discloses a preparation method for a spherical lithium titanate material. The preparation method comprises the following steps of: mixing spherical titanium dioxide and aqueous solution of a lithium compound; performing hydrothermal reaction at the temperature of between 90 and 110 DEG C for 15 to 25 hours; drying and grinding the obtained intermediate; and sintering the intermediate at the high temperature of between 700 and 900 DEG C for 1 to 5 hours to obtain the spherical lithium titanate material. The spherical lithium titanate material prepared by the method has uniform granularity, tap density of 1.0 to 1.2 g / cm<3> and high electrochemical properties, and is an ideal negative electrode material for a high-power lithium ion power cell. The preparation method is simple and practical, low in cost and suitable for industrialized large-scale production.

Description

technical field [0001] The invention belongs to the field of lithium ion secondary battery materials, and in particular relates to a preparation method which can be used as a spherical lithium titanate negative electrode material for lithium ion power batteries. Background technique [0002] The automobile industry is an important pillar industry of the national economy and a landmark industry that reflects the country's competitiveness. my country has become the world's largest automobile production and sales country, and my country's automobile production and sales will maintain a rapid growth momentum for a long period of time in the future. It is estimated that by 2020, the number of automobiles will exceed 200 million. The annual consumption of fuel oil will exceed 400 million tons, and the resulting energy security and environmental problems will become more prominent. Therefore, vigorously developing energy-saving and new-energy vehicles and accelerating the industria...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/00H01M4/1391
CPCY02E60/122Y02E60/10
Inventor 闫慧其鲁张鼎朱智李卫王健郎宇琪
Owner PEKING UNIV
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