Preparation method of lithium ion secondary battery with nanometer lithium titanate simultaneously doped at A and B site

A nano-lithium titanate and secondary battery technology, applied in battery electrodes, nanotechnology, nanotechnology, etc., can solve problems such as poor discharge performance at high rates, achieve improved bulk phase conductivity, good cycle stability, and improved The effect of mixing uniformity

Inactive Publication Date: 2015-06-24
SHANGHAI NAT ENG RES CENT FORNANOTECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the defect of poor discharge performance at high rates that exists in the preparation of lithium titanate negative electrode materials in the prior art, and to provide a sol that is simultaneously doped with rare earth metals at the A and B positions and combined with a two-component chelating agent Method for preparing composite material lithium titanate with excellent electrochemical performance by gel method

Method used

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  • Preparation method of lithium ion secondary battery with nanometer lithium titanate simultaneously doped at A and B site
  • Preparation method of lithium ion secondary battery with nanometer lithium titanate simultaneously doped at A and B site
  • Preparation method of lithium ion secondary battery with nanometer lithium titanate simultaneously doped at A and B site

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Embodiment 1

[0031] Firstly, 300 mL of ethanol and 30 mL of water were premixed according to the volume ratio of 1:0.1 to form a mixed solution, and then 15 mL of HNO 3As the inhibitor of follow-up reaction; Li and the compound of Ti, carry out batching according to the mol ratio of Li:Ti=4.2:5, take the tetra-n-butyl titanate (analytical pure) of 25.52 g, the lithium carbonate of 2.33 g ( analytically pure), added to the previous alcohol-water-acid mixture, stirred by a magnetic heating stirrer until completely dissolved; then added 0.3292 g of lanthanum nitrate and 0.257 g of zirconium nitrate, stirred, and dissolved; then 20 g of ethylenediaminetetra Add acetic acid and 30 g of citric acid to the premixed metal ion solution, mix well, add 100 mL of ammonia water dropwise to adjust the pH value to 8, and continue stirring; after the above mixed solution is stirred evenly to form a sol, heat and stir at 80 °C to the gel state, and then dried in a blast oven at 240°C to obtain a black and ...

Embodiment 2

[0033] According to the volume ratio of 1:0.1, 300 mL of ethanol and 30 mL of water were premixed to form a mixed solution, and then 15 mL of HCl was added as an inhibitor of the subsequent reaction; the compound of Li and Ti was mixed according to the molar ratio of Li:Ti=4.2:5 For batching, 21.31 g of tetraisopropyl titanate (analytical pure) and 6.43 g of lithium acetate (analytical pure) were weighed, added to the previous alcohol-water-acid mixture, and stirred by a magnetic heating stirrer until all Dissolve; then add 0.3292 g of lanthanum nitrate and 0.3321 g of neodymium nitrate, stir and dissolve; then add 20 g of ethylenediaminetetraacetic acid and 40 g of citric acid into the pre-mixed metal ion solution, mix well and add dropwise 100 Adjust the pH value to 9 with mL ammonia water, and continue to stir; after the above mixed solution is stirred evenly to form a sol, heat and stir at 80°C until it reaches a gel state, and then dry it in a blast oven at 240°C to obtain...

Embodiment 3

[0035] Premix 300 mL of ethanol and 60 mL of water according to the volume ratio of 1:0.2 to form a mixed solution, and then add 30 mL of HNO 3 As the inhibitor of follow-up reaction; Li and the compound of Ti, carry out batching according to the mol ratio of Li:Ti=4.4:5, take the tetra-n-butyl titanate (analytically pure) of 25.52 g, the lithium nitrate of 4.55 g ( analytically pure), added to the previous alcohol-water-acid mixture, stirred by a magnetic heating stirrer until completely dissolved; then added 0.3292 g of lanthanum nitrate and 0.3419 g of gadolinium nitrate, stirred and dissolved; then 20 g of ethylenediaminetetra Add acetic acid and 60 g of citric acid to the premixed metal ion solution, mix well, add 110 mL of ammonia water dropwise to adjust the pH to 7, and continue stirring; after the above mixed solution is stirred evenly to form a sol, heat and stir at 80°C to the gel state, and then dried in a blast oven at 240°C to obtain a black and fluffy lithium ti...

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Abstract

The invention provides a preparation method of lithium ion secondary battery with nanometer lithium titanate simultaneously doped at A and B sites. By using sol-gel method, soluble compounds of Li and Ti are prepared according to a mol ratio Li / Ti=0.8-1.0, and the mixture is added into an alcohol-water mixed solvent mixed with a hydrolysis inhibitor, and a dual component chelating agent and metal ions are added, after stirring, heating and gelling, a sintered precursor is obtained; after ball milling and thermal insulation of the obtained precursor, Li4Ti5O12 with A and B site simultaneously doped is obtained. Li4Ti5O12 and carbon source are mixed in an aqueous solution containing emulsifier, finally, the uniform mixture of lithium titanate and carbon source is heated, and a Li4Ti5O12 / C combined electrode with rare earth elements simultaneously doped at A and B site is obtained. The lithium titanate prepared by the method has good dispersion effect, uniform carbon coating and high conductivity. The initial discharge specific capacity of the Li4Ti5O12 / C composite material prepared by the method at room temperature at 1C multiplying power reaches to 178 mAh / g, and the discharge specific capacity at 20C multiplying power still maintains about 110 mAh / g, so that the composite material has excellent multiplying power performance and circulating stability and can be widely applied in the fields of portable instrument and power battery.

Description

technical field [0001] The present invention relates to a preparation method of lithium titanate, a nanocomposite electrode material for a lithium ion secondary battery, in particular to a preparation method of a carbon-coated composite electrode material lithium titanate in which A and B positions of rare earth metal ions are simultaneously doped . Background technique [0002] Lithium-ion secondary batteries have the advantages of high energy density, no memory effect, and small self-discharge. They dominate the energy storage battery market and are widely used in portable electronic products such as notebook computers, mobile phones, PDAs, and digital cameras. With the development of new technologies and the depletion of fossil resources, this type of secondary energy storage battery has been gradually applied in the field of energy-saving clean vehicles such as electric bicycles and electric vehicles. Among the existing battery systems, lithium secondary batteries a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/485H01M4/62C01G23/00B82Y30/00
CPCY02E60/10
Inventor 张春明王丹汪元元吴晓燕何丹农
Owner SHANGHAI NAT ENG RES CENT FORNANOTECH
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