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Low-temperature manufacturing method of lithium ion battery negative material rutile-type titanium dioxide microsphere

A lithium-ion battery, rutile technology, applied in the direction of titanium dioxide, battery electrodes, titanium oxide/hydroxide, etc., can solve the problems of difficult control of product morphology, poor electrochemical performance, easy introduction of impurities, etc., to avoid high temperature Solid-phase reaction process, good crystallinity, and the effect of shortening the diffusion path

Inactive Publication Date: 2015-06-03
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the one hand, the high-temperature solid-phase method will make the morphology of the product difficult to control, resulting in poor electrochemical performance; on the other hand, the high-temperature solid-phase method puts forward higher requirements for equipment and causes a large waste of energy.
However, some researchers used the liquid phase method to synthesize rutile titanium dioxide electrode materials with special morphology, but most of them used surfactants or templating agents in the preparation process, which brought troubles to the subsequent processing and easily introduced impurities.

Method used

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  • Low-temperature manufacturing method of lithium ion battery negative material rutile-type titanium dioxide microsphere
  • Low-temperature manufacturing method of lithium ion battery negative material rutile-type titanium dioxide microsphere
  • Low-temperature manufacturing method of lithium ion battery negative material rutile-type titanium dioxide microsphere

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Experimental program
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Effect test

Embodiment 1

[0024] A low-temperature preparation method of rutile-type titanium dioxide microspheres, a lithium-ion battery negative electrode material, comprising the following steps:

[0025] 1) Measure 5mL of tetrabutyl titanate, 35mL of acetic acid and 10mL of ethylene glycol, mix well to obtain a mixed solution, and fully magnetically stir the mixed solution at room temperature for 30 minutes to obtain a reaction precursor;

[0026] 2) The reaction precursor solution was hydrothermally reacted at 150° C. for 18 hours, and then centrifuged after natural cooling; the hydrothermal reaction was carried out by placing the reaction precursor solution in a hydrothermal reaction kettle lined with polytetrafluoroethylene, The filling ratio of the hydrothermal reactor used is 30% to 70%;

[0027] 3) Wash the precipitate obtained by centrifugation for 3 times with deionized water, then with absolute ethanol for 3 times, and then dry at 60° C. for 2 hours to obtain rutile titanium dioxide micros...

Embodiment 2

[0030] A low-temperature preparation method of rutile-type titanium dioxide microspheres, a lithium-ion battery negative electrode material, comprising the following steps:

[0031] 1) Measure 6mL of tetrabutyl titanate, 30mL of acetic acid and 40mL of ethylene glycol, mix well to obtain a mixed solution, and fully magnetically stir the mixed solution at room temperature for 20 minutes to obtain a reaction precursor;

[0032] 2) The reaction precursor solution was hydrothermally reacted at 170° C. for 10 hours, and then centrifuged after natural cooling; the hydrothermal reaction was carried out by placing the reaction precursor solution in a hydrothermal reaction kettle lined with polytetrafluoroethylene, The filling ratio of the hydrothermal reactor used is 30% to 70%;

[0033] 3) Wash the precipitate obtained by centrifugation for 3 times with deionized water, then with absolute ethanol for 3 times, and then dry at 50° C. for 3 hours to obtain rutile titanium dioxide micros...

Embodiment 3

[0036] A low-temperature preparation method of rutile-type titanium dioxide microspheres, a lithium-ion battery negative electrode material, comprising the following steps:

[0037] 1) Measure 2mL of tetrabutyl titanate, 10mL of acetic acid and 30mL of ethylene glycol, mix well to obtain a mixed solution, and fully magnetically stir the mixed solution at room temperature for 10 minutes to obtain a reaction precursor;

[0038] 2) The reaction precursor solution was hydrothermally reacted at 150° C. for 24 hours, and then centrifuged after natural cooling; the hydrothermal reaction was carried out by placing the reaction precursor solution in a hydrothermal reaction kettle lined with polytetrafluoroethylene, The filling ratio of the hydrothermal reactor used is 30% to 70%;

[0039] 3) The precipitate obtained by centrifugation was first washed once with deionized water, then washed twice with absolute ethanol, and then dried at 70° C. for 2 hours to obtain rutile titanium dioxid...

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Abstract

The invention discloses a low-temperature manufacturing method of a lithium ion battery negative material rutile-type titanium dioxide microsphere, and belongs to the technical field of the manufacturing of a lithium ion battery negative material. The method comprises the following steps: (1) uniformly mixing tetrabutyl titanate, acetic acid and ethylene glycol according to the volume ratio of 1 to (5-20) to (2-15) so as to obtain a mixed solution to obtain a mixed solution; fully stirring the mixed solution uniformly so as to obtain a reaction precursor solution; (2) carrying out hydrothermal reaction on the reaction precursor solution at 120-220 DEG C for 10-24h, cooling and centrifuging; and (3) cleaning a centrifuged deposit and drying so as to obtain the rutile-type titanium dioxide microsphere. By manufacturing the titanium dioxide electrode material by virtue of a hydrothermal process, the method disclosed by the invention can be used for effectively avoiding phase transformation from anatase to rutile-type TiO2 and omitting a high-temperature solid-phase reaction process, and lithium titanate powder which is high in purity and good in crystallization is manufactured within a short time; and meanwhile, the manufacturing method by virtue of the hydrothermal method is simple in process, moderate in condition, free of special process equipment and easy in industrial production.

Description

technical field [0001] The invention belongs to the technical field of preparation of negative electrode materials of lithium ion batteries, and in particular relates to a low-temperature preparation method of rutile-type titanium dioxide microspheres, which are negative electrode materials of lithium ion batteries. Background technique [0002] Lithium-ion batteries have been widely used due to their high voltage, high specific energy, and long storage time. However, the anode materials of lithium-ion batteries currently used in commercialization are graphite materials, which easily form SEI films during use, which leads to certain safety hazards. As an alternative material for Li-ion anode materials, TiO has attracted extensive attention due to its small volume expansion (3%) and high discharge plateau potential (about 1.7 V) during Li-ion intercalation / extraction. [0003] There are four crystal forms of titanium dioxide: [Li Xiaojie, Chen Tao, Li Ruiyong, Wang Zhanlei, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/48C01G23/053
CPCC01G23/053H01M4/48H01M10/0525Y02E60/10
Inventor 曹丽云惠亚妮黄剑锋欧阳海波许占位李嘉胤费杰李翠艳
Owner SHAANXI UNIV OF SCI & TECH
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