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Preparation method of sphere-like fast ion conducting material of modified calcium lithium titanate

An ion conductor, calcium lithium titanate technology, applied in the field of preparation of spherical fast ion conductor material modified calcium lithium titanate, can solve the problems of inhibiting development, ion conductivity can not meet the practical requirements, etc., to achieve conductivity Effect of improvement, excellent rate and cycle performance, and excellent electrochemical performance

Inactive Publication Date: 2014-03-12
YANGTZE UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the all-solid polymer electrolyte solves the problem of the mechanical properties of the matrix, its ionic conductivity cannot meet the practical requirements, thus inhibiting its development.

Method used

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  • Preparation method of sphere-like fast ion conducting material of modified calcium lithium titanate
  • Preparation method of sphere-like fast ion conducting material of modified calcium lithium titanate
  • Preparation method of sphere-like fast ion conducting material of modified calcium lithium titanate

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Using the nitrate solution of lithium nitrate, calcium nitrate, n-butyl titanate and cerium oxide as raw materials, according to Li 0.1-z Ce 0.1 Ca 0.8 Ti z o 3 The stoichiometric ratio is mixed in the aqueous solution of ethanol; finally, the complexing agent acetylacetone is added according to 3 times of the theoretical amount, stirred and hydrolyzed for 6 hours at 40°C to obtain a uniform solution, sol or suspension, and then spray-dried. The wind temperature is 120°C, the outlet air temperature is 98°C, and finally in the air atmosphere at 600°C, 700°C, 800°C, and 900°C for 6 hours to obtain the modified calcium lithium titanate-like spherical fast ion conductor material Li 0.1-z Ce 0.1 Ca 0.8 Ti z o 3 , the resulting product was prepared into an all-solid electrolyte and then assembled into a button battery to investigate its battery performance in the voltage range of 2.75-4.25V. Charge and discharge at different rates, the first discharge specific capacit...

Embodiment 2

[0030] Using the nitrate solution of lithium acetate, calcium acetate, n-butyl titanate and cerium oxide as raw materials, according to Li 0.1-z Ce 0.1 Ca 0.8 Ti z o 3 The stoichiometric ratio is mixed in the aqueous solution of ethanol, and then the complexing agent acetylacetone is added according to 3 times the theoretical amount, stirred and hydrolyzed for 6 hours at 40°C to obtain a uniform solution, sol or suspension, and then spray-dried. The wind temperature is 120°C, the outlet air temperature is 98°C, and finally the temperature is kept at 700°C in the air atmosphere for 2 hours, 6 hours, 8 hours and 10 hours respectively, and the modified calcium lithium titanate-like spherical fast ion conductor material Li 0.1-z Ce 0.1 Ca 0.8 Ti z o 3 , the resulting product was prepared into an all-solid electrolyte and then assembled into a button battery to investigate its battery performance in the voltage range of 2.75-4.25V. Charge and discharge at different rates, t...

Embodiment 3

[0035] Using the nitrate solution of lithium oxalate, calcium oxalate, n-butyl titanate and cerium oxide as raw materials, according to Li 0.1-z Y x Ca 0.9-x Ti z o 3 (wherein x=0.05, 0.10, 0.40 and 0.80) the stoichiometric ratio is mixed in the aqueous solution of ethanol, then add the complexing agent acetylacetone by 3 times of the theoretical amount, stir and hydrolyze for 6 hours at 40°C to obtain a uniform solution, The sol or suspension is then spray-dried, the air inlet temperature is 120°C, the air outlet temperature is 98°C, and finally the temperature is kept at 700°C for 6 hours in the air atmosphere to obtain the modified calcium lithium titanate spherical fast ion conductor material Li 0.1-z Y x Ca 0.9-x Ti z o 3 , the resulting product was prepared into an all-solid electrolyte and then assembled into a button battery to investigate its battery performance in the voltage range of 2.75-4.25V. Charge and discharge at different rates, the first discharge sp...

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Abstract

The invention discloses a preparation method of a sphere-like fast ion conducting material of modified calcium lithium titanate. The preparation method is characterized by comprising the following steps: (1) mixing lithium source, calcium sources, titanium sources and a salt solution of a modified material Y according to the stoichiometric proportion of Li0.1-zYxCa0.9-xTizO3 and adding the mixture to ethanol water to obtain a mixed solution; (2) adding a complexing agent to the mixed solution, stirring and hydrolyzing to obtain an intermediate mixed solution; (3) conducting spray drying on the intermediate mixed solution, heating the obtained product under air atmosphere until the temperature of the obtained product is 600-900 DEG C, keeping the temperature for 2-12 hours to obtain the sphere-like fast ion conducting material of modified calcium lithium titanate. According to the invention, the hydrolyzing, complexing and spray drying methods are adopted, so that the reagents are mixed in the solution at a molecular or atomic level, so as to prepare the sphere-like particulate material with uniform particles and good electrochemical performance. The sphere-like fast ion conducting material has the advantages of higher ionic conductivity at the room temperature, high rate capability and good cycle performance.

Description

Technical field: [0001] The invention relates to a preparation method of a spherical fast ion conductor material modified calcium lithium titanate, which belongs to the technical field of preparation methods of polymer lithium ion battery electrolyte materials. Background technique: [0002] Lithium-ion batteries are favored due to their significant advantages such as high voltage, long service life and high energy density. However, because the liquid electrolyte used in it is prone to accidents such as leakage and gas expansion under high temperature conditions, it is imperative to find an electrolyte that can replace the liquid electrolyte. Gel-state polymer electrolyte can absorb a large amount of liquid electrolyte due to its unique electrolyte membrane network structure, and has up to 10 -3 S cm -1 ionic conductivity, but due to the softening effect of the electrolyte, the mechanical properties of the polymer matrix are poor enough to function as a separator. Althoug...

Claims

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Application Information

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IPC IPC(8): H01M10/0562
CPCH01M10/0562H01M2300/0071Y02E60/10
Inventor 肖围梅平缪畅廖海星颜学敏秦少雄高林曲宝龙赵庆美
Owner YANGTZE UNIVERSITY
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