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Method for preparing spinel-structured film type lithium titanate cathode material

A spinel structure and negative electrode material technology, applied in chemical instruments and methods, titanium compounds, inorganic chemistry, etc., can solve the problems that the performance of miniaturized batteries cannot meet the application requirements, and achieve simple and easy preparation methods, simple equipment, The effect of cheap and easy-to-obtain raw materials

Inactive Publication Date: 2014-08-27
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] With the continuous development of microelectronic devices towards lightweight and miniaturization, higher requirements are placed on the power supply systems supporting these devices, and the performance of miniaturized batteries is far from meeting the application requirements

Method used

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  • Method for preparing spinel-structured film type lithium titanate cathode material
  • Method for preparing spinel-structured film type lithium titanate cathode material
  • Method for preparing spinel-structured film type lithium titanate cathode material

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preparation example Construction

[0026] The preparation method of spinel structure film type lithium titanate negative electrode material, its steps are:

[0027] (1) Ultrasonically mix ethanol solvent and hydrolysis inhibitor in proportion (5:1~2:1), add lithium source and titanium source in a certain proportion, and simultaneously heat in an oil bath at 40-65°C and magnetically stir until completely dissolved Mix evenly to obtain a mixed solution; add methanol whose volume is 1 / 4~1 / 2 of the total volume of the mixed solution, and perform low-pressure distillation to remove impurity water; stop low-pressure distillation and oil bath heating after 30 minutes, and only magnetically stir for 10-15 hours; Finally, 1-5 drops of ethanolamine are added to form an anhydrous precursor solution, and the total molar concentration of metal ions in the precursor solution is 0.2-1.2 mol / l.

[0028] (2) Drop the precursor solution in step (1) on the surface of the substrate, and evenly coat the substrate on the substrate w...

Embodiment 1

[0039] (1) Ultrasonically mix 20ml of ethanol solvent and 10ml of acetic acid, add 0.55g of lithium acetate and 3.22g of butyl titanate, and simultaneously heat in an oil bath at 40-65°C and magnetically stir until completely dissolved and mixed to obtain a mixed solution; add volume Mix methanol with one-third of the total volume of the mixed solution, and perform low-pressure distillation to remove impurity water; stop low-pressure distillation and oil bath heating after 30 minutes, and only magnetically stir for 12 hours; finally add 3 drops of ethanolamine to form an anhydrous precursor solution, the precursor solution The total concentration of metal ions is 0.4 mol / l.

[0040] (2) Drop the precursor solution in step (1) on Pt / Ti / SiO 2 / Si substrate surface, uniformly coated on the substrate with a spin coating machine, the spin coating rate is 2000rpm, and the time is 40s.

[0041] (3) Place the substrate with the liquid film attached to the surface in step (2) in a tub...

Embodiment 2

[0047] (1) Ultrasonically mix 20ml of ethanol solvent and 10ml of acetic acid, add 0.55g of lithium acetate and 3.22g of butyl titanate, and simultaneously heat in an oil bath at 40-65°C and magnetically stir until completely dissolved and mixed to obtain a mixed solution; add volume Mix methanol with one-third of the total volume of the mixed solution, and perform low-pressure distillation to remove impurity water; stop low-pressure distillation and oil bath heating after 30 minutes, and only magnetically stir for 12 hours; finally add 3 drops of ethanolamine to form an anhydrous precursor solution, the precursor solution The total concentration of metal ions is 0.4 mol / l.

[0048] (2) Drop the precursor solution in step (1) on the SrTiO 3 The surface of the substrate was uniformly coated on the substrate with a spin coating machine, the spin coating rate was 1500 rpm, and the time was 60 s.

[0049] (3) Place the substrate with the liquid film on the surface mentioned in st...

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Abstract

The preparation method of the thin-film lithium titanate negative electrode material with spinel structure belongs to the field of energy and new materials. The invention includes the following steps: (1) Ultrasonic mixing of ethanol solvent and hydrolysis inhibitor, according to Li:Ti=4: Add lithium source and titanium source at an atomic ratio of 5 to 4.5:5, heat at 40-65°C, and magnetically stir until completely dissolved and mixed evenly to obtain a mixed solution; add methanol whose volume is 1 / 4 to 1 / 2 of the volume of the mixed solution , remove impurity water and heat, then stir; finally add 1-5 drops of ethanolamine to form an anhydrous precursor solution; (2) evenly coat the precursor solution obtained in step (1) on the surface of the substrate; (3) apply the surface attachment solution The substrate of the film is pre-fired in a tube furnace to obtain a pre-fired film; (4) The pre-fired film is annealed at high temperature, and the atmosphere is dry oxygen; after the annealing is completed, the temperature is naturally lowered to room temperature to obtain spinel titanic acid Lithium film. The equipment required by the invention is simple, the preparation method is simple and easy, and high-quality samples can be prepared.

Description

technical field [0001] The invention belongs to the fields of energy and new materials, and in particular relates to a method for preparing thin-film lithium titanate by a chemical solution method. Background technique [0002] With the continuous development of microelectronic devices towards lightweight and miniaturization, higher requirements are placed on the power supply systems supporting these devices, and the performance of miniaturized batteries is far from meeting the application requirements. Therefore, it is of great significance to develop high-performance and low-cost thin-film lithium-ion batteries. [0003] Negative thin film material is one of the key technologies of thin film lithium ion battery. Lithium titanate (Li 4 Ti 5 o 12 ) is a high-performance lithium-ion battery anode material that has a long life, can be charged and discharged with a large current, is not easy to react with the electrolyte, and is not easy to precipitate metal lithium. High ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/00
Inventor 熊杰朱聪陶伯万徐鹏举赵晓辉李言荣
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA