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Sol-gel method for preparing lithium titanate

A gel method, lithium titanate technology, applied in the direction of electrical components, battery electrodes, circuits, etc., can solve problems affecting the quality of the sol, and achieve the effects of inhibiting hydrolysis, good control, and easy operation

Inactive Publication Date: 2013-11-20
PANZHIHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional sol-gel process is to dissolve butyl titanate in absolute ethanol, but it cannot avoid the hydrolysis of butyl titanate, which affects the formation of sol, affects the chelation process of chelating agent, and thus affects the quality of sol , resulting in impurity TiO 2 High content affects Li 4 Ti 5 o 12 Charge and discharge performance of negative electrode materials

Method used

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  • Sol-gel method for preparing lithium titanate
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  • Sol-gel method for preparing lithium titanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] a. Dissolve 40mL of butyl titanate in 100mL of ethylene glycol to prepare M solution, stir rapidly to make it evenly mixed.

[0038] b. Mix 14.74g of lithium acetate dihydrate with 10mL of citric acid, 12mL of deionized water, and 80mL of absolute ethanol to prepare N solution.

[0039] c. Quickly stir the M solution, and at the same time, quickly drop the prepared N solution into the M solution at a speed of 0.25-0.3mL / s within 5 minutes, the pH value is 5.2, stir vigorously at room temperature for 30 minutes to obtain a transparent sol, and age After 24 hours, a milky white gel was obtained.

[0040] d. Put the gel obtained in step c into a drying oven, dry at a constant temperature of 80° C. for 36 hours to obtain a dry gel, and obtain a precursor after ball milling.

[0041] e. After fully grinding the precursor, use the segmental sintering method: at a heating rate of 5 °C / min, raise the temperature to 600 °C for 6 hours, cool to room temperature and fully grind f...

Embodiment 2

[0046] a. Dissolve 40mL of butyl titanate in 150mL of ethylene glycol to prepare M liquid, stir rapidly to make it evenly mixed.

[0047] b. Mix 14.74g of lithium acetate dihydrate with 10mL of citric acid, 20mL of deionized water, and 120mL of absolute ethanol to prepare N solution.

[0048] c. Quickly stir the M solution, and at the same time, quickly drop the prepared N solution 0.3-0.4mL / s into the M solution within 7 minutes, control the pH value to 5.7, stir vigorously at room temperature for 40 minutes to obtain a transparent sol, and age for 36 hours to obtain Milky white gel.

[0049] d. Put the gel obtained in step c into a drying oven, dry at a constant temperature of 80° C. for 36 hours to obtain a dry gel, and obtain a precursor after ball milling.

[0050] e. After fully grinding the precursor, use the segmented sintering method: at a heating rate of 5 °C / min, raise the temperature to 600 °C for 6 hours, cool to room temperature and fully grind for 0.5 h; then r...

Embodiment 3

[0053] a. Dissolve 40mL of butyl titanate in 80mL of ethylene glycol to prepare M liquid, stir rapidly to make it evenly mixed.

[0054] b. Mix 15.08g of lithium acetate dihydrate with 10mL of citric acid, 12mL of deionized water, and 80mL of absolute ethanol to prepare N solution.

[0055] c. Quickly stir the M solution, and at the same time, quickly drop the prepared N solution into the M solution at 0.25-0.3mL / s within 5 minutes, the pH value is 5.5, stir vigorously at room temperature for 30 minutes to obtain a transparent sol, and age for 24 hours to obtain Milky white gel.

[0056] d. Put the gel obtained in step c into a drying oven, dry at a constant temperature of 120° C. for 24 hours to obtain a dry gel, and obtain a precursor after ball milling.

[0057] e. After fully grinding the precursor, use the segmental sintering method: at a heating rate of 5 °C / min, raise the temperature to 600 °C for 12 hours, cool to room temperature and fully grind for 0.5 h; then raise...

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Abstract

The invention belongs to the technology field of lithium battery, and especially relates to a sol-gel method for preparing lithium titanate. The invention aims to solve the technology problem of uneasy operation control, which causes the instability of gel, in the conventional sol-gel method. In order to solve the technology problem mentioned above, the invention provides a sol-gel method for preparing lithium titanate. The method comprises following steps: step a, dissolving butyl titanate in glycol to prepare a solution; step b, mixing dihydrate lithium acetate, citric acid, absolute ethanol and deionized water together to prepared a solution; step c, dropwise adding the solution obtained in the step b into the solution obtained in the step a, adding ammonia liquor at the same time, then stirring to obtain transparent sol, then ageing to obtain the gel; step d, drying the gel under constant temperature to obtain dry gel, then fully grinding the dry gel to obtain precursors; step e, and finally sintering the precursors in sections to obtain lithium titanate. The preparation method has the advantages of convenient operation, excellent product properties and preferably good application prospect.

Description

technical field [0001] The invention belongs to the technical field of lithium ion batteries, and in particular relates to the preparation of lithium titanate by a sol-gel method. technical background [0002] Lithium-ion battery anode material, spinel Li 4 Ti 5 o 12 (Lithium titanate) has the characteristics of "zero strain" with stable crystal structure and almost no change during charging and discharging. It can discharge quickly, has high safety performance and good cycle performance, so it has become a research topic at home and abroad. hot spot. At present, the sol-gel method has become the most studied method for preparing nano-lithium titanate. The smooth preparation of sol and gel determines the follow-up work of preparing lithium titanate anode materials by sol-gel method, and the properties of sol and gel also determine the composition and properties of the precursor to a certain extent. Therefore, a smooth, stable and reliable sol-gel process is a prerequisi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/485
CPCY02E60/122Y02E60/10
Inventor 王能为崔旭梅黄载春肖博
Owner PANZHIHUA UNIV
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