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Lithium titanate/titanium black anode material and preparation method thereof

A technology of titanium suboxide and negative electrode materials, applied in chemical instruments and methods, titanium compounds, inorganic chemistry, etc., can solve the problems of aggravating battery self-discharge, easy structure changes, electrolyte corrosion, etc., and achieve high specific capacity and high rate Excellent charge and discharge performance and stable performance

Active Publication Date: 2012-06-13
北京盟固利新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

By enhancing the conductive network of the matrix, its conductivity can also be improved, as in Li 4 Ti 5 o 12 The introduction of Ag and Cu into the matrix can increase the conductivity of the matrix by two orders of magnitude, but the price of Ag is relatively expensive, and Cu is a magnetic substance, which aggravates the self-discharge phenomenon of the battery
(3) Coating modification, mainly carbon coating, mainly coating carbon conductive agent outside the grains to improve the conductivity between grains, but the structure of carbon materials is prone to change when lithium ions are embedded, resulting in When it is discharged with a large current, the cycle performance is poor
And it is easily corroded by electrolyte at high current density

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Dextrin and lithium titanate (Li 4 Ti 5 o 12 ) into methanol, the carbon content in dextrin is the same as lithium titanate (Li 4 Ti 5 o 12 ) The ratio of the amount of substance is 1: 4, adopt ball mill ball milling 2h to mix;

[0032](2) drying the mixture in step (1) at 100°C for at least 12 hours to obtain a mixture;

[0033] (3) ball milling the mixture for 1 hour to obtain a fine powder;

[0034] (4) Put the fine powder in a vacuum carbon tube furnace, evacuate the furnace to below 50Pa, and fill the furnace with nitrogen to wash the furnace 2 to 3 times, and slowly raise the temperature at a heating rate of 3°C / min under the condition of vacuuming To the synthesis temperature of 1050 ° C, keep warm for 3 hours;

[0035] (5) Cool down to room temperature at 12° C. / min, carry out classified crushing, and sieve to obtain the product—lithium titanate / titanium oxide negative electrode material.

[0036] The chemical formula in the obtained lithium titanate...

Embodiment 2

[0039] (1) Dextrin and lithium titanate (Li 4 Ti 5 o 12 ) into absolute ethanol, the carbon content in dextrin is the same as that of lithium titanate (Li 4 Ti 5 o 12 ) The ratio of the amount of substance is 1: 16, adopt ball mill ball milling 4h to mix;

[0040] (2) drying the mixture at 100°C for at least 12 hours to obtain a mixture;

[0041] (3) ball milling the mixture for 1 hour to obtain a fine powder;

[0042] (4) Put the fine powder in a vacuum carbon tube furnace, evacuate the furnace to below 50Pa, and fill the furnace with argon to wash the furnace 2 to 3 times, and slow down the heating rate at 5°C / min under vacuum Raise the temperature to the synthesis temperature of 1100°C and keep it warm for 2 hours;

[0043] (5) Cool down to room temperature at 15°C / min, carry out classified crushing, and sieve to obtain the product.

[0044] The chemical formula in the obtained lithium titanate / titania negative electrode material is 0.96Li 4 Ti 5 o 12 -0.05Ti 4 ...

Embodiment 3

[0047] (1) Combine dextrin with lithium titanate (Li 4 Ti 5 o 12 ) into citric acid, the carbon content in dextrin is the same as lithium titanate (Li 4 Ti 5 o 12 ) The ratio of the amount of substance is 1: 8, adopt ball mill ball milling 4h to mix;

[0048] (2) drying the mixture at 90°C for at least 12 hours to obtain a mixture;

[0049] (3) ball milling the mixture for 1 hour to obtain a fine powder;

[0050] (4) Put the fine powder in a vacuum carbon tube furnace, evacuate the furnace to below 50Pa, and fill the furnace with argon to wash the furnace 2 to 3 times, and slow down the heating rate at 5°C / min under vacuum Raise the temperature to the synthesis temperature of 1000°C and keep it warm for 4 hours;

[0051] (5) Cool down to room temperature at 10°C / min, carry out classified crushing, and sieve to obtain the product.

[0052] The chemical formula in the obtained lithium titanate / titanium oxide negative electrode material is 0.92Li 4 Ti 5 o 12 -0.1Ti 4 ...

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Abstract

The invention relates to a lithium titanate / titanium black anode material and a preparation method thereof belonging to the technical field of lithium ion batteries. The lithium titanate / titanium black anode material has a chemical formula of (1-0.8x)Li4Ti5O12-xTi4O7, wherein x is more than 0,03 and is not more than 0.30. The lithium titanate / titanium black anode material can be synthesized by adopting two methods, the first method is as follows: lithium titanate is carbonized in vacuum, a compact titanium black high-conductive membrane is formed on the surface of the lithium titanate through controlling temperature, reaction time and pressure to have higher multiplying power performance; and the second method is as follows: Ti4O7 is directly added in the lithium titanate, and the lithium titanate / titanium black anode material is synthesized under an inert atmosphere at high temperature. The lithium titanate / titanium black anode material has a simple manufacture process and is beneficial to industrialized production. Compared with the current marketized anode material, the lithium titanate / titanium black anode material has higher electrical conductivity and corrosion resistance and higher large-current discharge cycling performance; and multiplying power charge and discharge performances and cycling performance of a lithium ion power battery can be further improved.

Description

technical field [0001] The invention belongs to the technical field of lithium ion batteries, in particular to a lithium titanate / titanium oxide negative electrode material and a preparation method thereof. Background technique [0002] As lithium-ion batteries are widely used in pure electric vehicles, hybrid vehicles and other portable electronic devices, higher requirements are placed on the high power and high energy density of lithium-ion batteries. Among them, the safety performance of batteries and the electrochemical performance of negative electrode materials have been widely concerned. Spinel Li 4 Ti 5 o 12 It is a "zero strain" insertion material, which has become a new material to replace carbon negative electrodes due to its excellent cycle performance and stable structure. [0003] For the practical application of lithium-ion batteries, especially in the field of power batteries, which is attracting worldwide attention, the high-rate working characteristics...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/485C01G23/00
CPCY02E60/122Y02E60/10
Inventor 朱晓沛江卫军吴剑文王浩然张春玲孙春胜庞自钊白珍辉
Owner 北京盟固利新材料科技有限公司
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