A kind of zirconium scandium composite oxide coated lithium titanate negative electrode material and preparation method thereof

A composite oxide and lithium titanate coating technology, which is applied to battery electrodes, electrochemical generators, structural parts, etc., can solve the problem of increased electrode/electrolyte interface impedance, affecting the application of lithium titanate, and shortening battery life. Problems, to achieve the effect of improving the rate and cycle performance, easy to test, and suppressing water absorption

Active Publication Date: 2019-12-10
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the lithium titanate negative electrode material is easy to produce gas during the battery manufacturing process, which increases the electrode / electrolyte interface impedance, rapidly decays the cycle performance, and shortens the battery life, which greatly affects the application of lithium titanate.

Method used

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  • A kind of zirconium scandium composite oxide coated lithium titanate negative electrode material and preparation method thereof
  • A kind of zirconium scandium composite oxide coated lithium titanate negative electrode material and preparation method thereof
  • A kind of zirconium scandium composite oxide coated lithium titanate negative electrode material and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0026] A method for preparing a zirconium-scandium composite oxide-coated lithium titanate negative electrode material proposed by the present invention comprises the following steps:

[0027] S1. Weigh lithium hydroxide, tetrabutyl titanate, zirconium tetrachloride and scandium nitrate according to the molar ratio of Li:Ti:Zr:Sc=4:5:0.05:0.02 and add them to the solution containing 1wt% Ultrasonic treatment for 1 hour in an absolute ethanol solution of citric acid, wherein the amount of citric acid added is 1 wt% of the theoretically synthesized lithium titanate, then heated to 60° C. and stirred for 2 hours to form a gel;

[0028] S2. Dry the gel obtained in S1 at 100°C and grind it, then pre-calcine at 400°C for 3 hours, then calcinate at 650°C for 5 hours, and cool naturally to room temperature to obtain the Zr 5 sc 2 o 13 Coated lithium titanate negative electrode material.

[0029] Zr prepared in this embodiment 5 sc 2 o 13 The 0.2C rate discharge specific capacity...

Embodiment 2

[0031] A method for preparing a zirconium-scandium composite oxide-coated lithium titanate negative electrode material proposed by the present invention comprises the following steps:

[0032] S1. Weigh lithium acetate, tetraethyl titanate, zirconium nitrate and scandium chloride according to the ratio of Li:Ti:Zr:Sc=4.05:5:0.1:0.04 according to the molar ratio. Ultrasonic treatment in absolute ethanol solution for 1.2h, wherein the amount of citric acid added is 2wt% of the theoretically synthesized lithium titanate, then heated to 65°C and stirred for 4h to form a gel;

[0033] S2. Dry the gel obtained in S1 at 105°C and grind it, then pre-calcine at 450°C for 4 hours, then calcinate at 700°C for 6 hours, and cool naturally to room temperature to obtain the Zr 5 sc 2 o 13 Coated lithium titanate negative electrode material.

[0034] Zr prepared in this embodiment 5 sc 2 o 13The 0.2C rate charging specific capacity of the coated lithium titanate negative electrode mater...

Embodiment 3

[0036] A method for preparing a zirconium-scandium composite oxide-coated lithium titanate negative electrode material proposed by the present invention comprises the following steps:

[0037] S1, according to the molar ratio of Li:Ti:Zr:Sc=4.1:5:0.15:0.06, weigh lithium nitrate, tetraisopropyl titanate, zirconium oxide and scandium oxide and add to the solution containing 5wt% citric acid Ultrasonic treatment in absolute ethanol solution for 1.5h, wherein the amount of citric acid added was 5wt% of the theoretically synthesized lithium titanate, then heated to 75°C and stirred for 6h to form a gel;

[0038] S2. Dry the gel obtained in S1 at 110°C and grind it, then pre-calcine at 500°C for 4 hours, then calcinate at 750°C for 8 hours, and cool naturally to room temperature to obtain the Zr 5 sc 2 o 13 Coated lithium titanate negative electrode material.

[0039] Zr prepared in this embodiment 5 sc 2 o 13 The 0.2C rate charging specific capacity of the coated lithium tit...

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Abstract

The invention provides a zirconium-scandium composite oxide-coated lithium titanate negative electrode material and a preparation method therefor. The zirconium-scandium composite oxide-coated lithium titanate negative electrode material is a Zr<5>Sc<2>O<13>-coated lithium titanate negative electrode material; the preparation method comprises the steps of weighing a lithium source, a titanium source, a zirconium source and a scandium source based on proportion and then adding into an absolute ethyl alcohol solution dissolved with citric acid, heating and stirring to perform a reaction to form gel, and then drying and grinding on the gel, and next, performing pre-sintering and then calcining to obtain the Zr<5>Sc<2>O<13>-coated lithium titanate negative electrode material. In the negative electrode mateirla, the surface of lithium titanate is uniformly coated with Zr<5>Sc<2>O<13> to suppress growth of lithium titanate particles and lower the pH value of the material; in addition, the coating layer on the surface of Zr<5>Sc<2>O<13> material is high in chemical stability, so that structural stability of lithium titanate is effectively maintained and the rate capacity and cycling performance of lithium titanate are improved in the repeated charging-discharging process; and meanwhile, the whole preparation process is simple and easy to test so that the preparation method has wide application prospect.

Description

technical field [0001] The invention relates to the technical field of negative electrode materials for lithium ion batteries, in particular to a lithium titanate negative electrode material coated with zirconium scandium composite oxide and a preparation method thereof. Background technique [0002] Traditional anode materials are mainly carbon materials. Carbon materials have the advantages of good cycle stability and low charge-discharge platform, but there are also some disadvantages, such as the potential safety hazard of lithium dendrite precipitation, and the speed of energy release is not fast enough, so it is not suitable for Equipment that requires instantaneous high current, etc. Compared with carbon materials, lithium titanate (Li 4 Ti 5 o 12 ) has obvious advantages, such as almost "zero volume change" during charging and discharging, good cycle performance, high Coulombic efficiency, and no reaction with electrolyte, etc., so it has become a hot research top...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/48H01M4/485H01M10/0525
CPCH01M4/366H01M4/48H01M4/485H01M10/0525Y02E60/10
Inventor 刘兴亮杨茂萍李道聪
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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