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Preparation and application of aluminium-phosphate-cladded carbon-cladded Li4Ti5O12/TiN

A technology of lithium titanate nitride and carbon coating, which is applied in the field of nanomaterials to achieve high gram capacity, high conductivity, and good industrial application prospects

Inactive Publication Date: 2015-01-07
西安中科新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] At present, the preparation method of carbon-coated lithium titanate coated with phosphate has not been reported.

Method used

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  • Preparation and application of aluminium-phosphate-cladded carbon-cladded Li4Ti5O12/TiN
  • Preparation and application of aluminium-phosphate-cladded carbon-cladded Li4Ti5O12/TiN
  • Preparation and application of aluminium-phosphate-cladded carbon-cladded Li4Ti5O12/TiN

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] The preparation method of the aluminum phosphate-coated carbon-coated lithium titanate nitride comprises the following steps:

[0055] Step 1) preparation of lithium titanate

[0056] Lithium carbonate and rutile titanium dioxide were weighed according to the Li:Ti molar ratio of 0.8:1, mixed with absolute ethanol, and ball milled in an argon atmosphere in a QM-2SP12 ball mill of Nanjing University Instrument Factory for 12 hours. The uniformly mixed sample was placed in a vacuum oven at 80°C, heated and dried for 5 hours, and then cooled to room temperature under vacuum. Put the sample in JQF1400-30 high-temperature atmosphere electric furnace of Shanghai Jiugong Electric Co., Ltd., vacuumize, pass 99.9% nitrogen protective gas, then raise the temperature to 500°C at a speed of 5°C / min, and keep it at this temperature for 1 hour, then Continue to raise the temperature to 850° C. at a rate of 2° C. / min, and keep it at this temperature for 1 hour. After natural cooling,...

Embodiment 2

[0068] The preparation method of the aluminum phosphate-coated carbon-coated lithium titanate nitride comprises the following steps:

[0069] Step 1) The preparation of lithium titanate, the reaction environment and conditions are the same as step 1) of Example 1.

[0070] Step 2) Preparation of carbon-coated lithium titanate, the reaction environment and conditions are the same as step 2) of Example 1.

[0071] Step 3) Preparation of carbon-coated lithium titanate nitride

[0072] 30 grams of the carbon-coated lithium titanate particles prepared in step 2) are mixed in an agate ball mill jar by mass percentage 5:100, and 1.5 grams of brown liquid hydrophilic ionic liquid 1-butylpyridine dinitrile amine salt, and added 300 grams of agate grinding balls, protected by argon, planetary ball grinding for 2 hours, rotating speed 300rpm.

[0073] Take out the previous material and place it in a vacuum drying oven at 80°C for 15 hours, grind it evenly and put it into a crucible, th...

Embodiment 3

[0076] The preparation method of the aluminum phosphate-coated carbon-coated lithium titanate nitride comprises the following steps:

[0077] The reaction environment and conditions of step 1), 2) 3) and 4) are the same as in Example 2, the difference is that in step 3), the nitrogen source is a hydrophilic colorless liquid ionic liquid 1-butyl-3-formazan imidazole dicyanamide salt.

[0078] The product of step 3) is gray carbon-coated lithium titanate nitride powder. The carbon coating contains pyrolytic carbon and carbon nitride (CN X ) compounds. Among them, carbon nitride (CN X ) compounds are highly conductive.

[0079] Material Characterization

[0080] 1) The crystal structure test was carried out on the Shimadzu X-ray diffractometer XRD-7000, using a copper target, the scanning speed was 2° / min, the test accuracy was ±0.04°, and the scanning range was 5-90°.

[0081] The spinel structure carbon-coated lithium titanate XRD spectrum pattern that embodiment 1 step 2...

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Abstract

The invention discloses preparation and application of aluminium-phosphate-cladded carbon-cladded Li4Ti5O12 / TiN. The preparation method for the aluminium-phosphate-cladded carbon-cladded Li4Ti5O12 / TiN comprises the following steps: firstly, preparing Li4Ti5O12 of a spinel structure; then uniformly mixing a carbon source and the Li4Ti5O12, and calcining the mixture in vacuum or protective gas atmosphere to obtain carbon-cladded Li4Ti5O12; then uniformly mixing a nitrogen source and the carbon-cladded Li4Ti5O12, and calcining the mixture of the nitrogen source and the carbon-cladded Li4Ti5O12 in the vacuum or protective gas atmosphere to obtain carbon-cladded Li4Ti5O12 / TiN; and adding aluminium salt and phosphate into the suspending liquid of the carbon-cladded Li4Ti5O12 / TiN, uniformly cladding the particle surfaces of carbon-doped Li4Ti5O12 / TiN with the obtained aluminium phosphate, and calcining the particles of the aluminium-phosphate-cladded carbon-doped Li4Ti5O12 / TiN in the vacuum or protective gas atmosphere to obtain the aluminium-phosphate-cladded carbon-cladded Li4Ti5O12 / TiN. The preparation process of the preparation method disclosed by the invention is simple, no pollution in reaction is achieved, the product homogeneity is good, and the prepared aluminium-phosphate-cladded carbon-cladded Li4Ti5O12 / TiN is high in gram volume, and has a good industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, and in particular relates to the preparation and application of a carbon-coated lithium titanate nitride negative electrode material coated with aluminum phosphate. Background technique [0002] Lithium titanate (Li 4 Ti 5 o 12 ) is a lithium-ion secondary battery negative electrode material with good application prospects. Lithium titanate battery has long life, high rate, safety and excellent high and low temperature performance. [0003] Lithium titanate is a composite oxide composed of metal lithium and low-potential transition metal titanium. It has a spinel structure and a space group of Fd3m. It is non-conductive and can exist stably in the air. As the negative electrode of lithium-ion secondary batteries, during the charging and discharging process, there is no crystal form change, and the volume change is less than 1%, which is called "zero strain material". This stable ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/485H01M4/36
CPCH01M4/36H01M4/485Y02E60/10
Inventor 徐士民李宏斌马毅徐一丹都云刘志坚陈俊桦
Owner 西安中科新能源科技有限公司
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