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Preparation method and application of aluminum fluoride-coated carbon-coated lithium titanate nitride

A technology of lithium titanate nitride and aluminum fluoride is applied in the field of nanomaterials to achieve the effects of low equipment requirements, high gram capacity, and high conductivity

Inactive Publication Date: 2015-02-18
西安中科新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] The preparation method of carbon-coated lithium titanate nitride coated with aluminum fluoride has not been reported yet

Method used

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  • Preparation method and application of aluminum fluoride-coated carbon-coated lithium titanate nitride
  • Preparation method and application of aluminum fluoride-coated carbon-coated lithium titanate nitride
  • Preparation method and application of aluminum fluoride-coated carbon-coated lithium titanate nitride

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Embodiment 1

[0047] A method for preparing aluminum fluoride-coated carbon-doped lithium titanate nitride, comprising the following steps:

[0048] Step 1) Preparation of spinel lithium titanate 1

[0049] 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 the high-temperature atmosphere electric furnace of Shanghai Jiugong Electric Co., Ltd., evacuate it, 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, and then continue to The temperature was raised to 850° C. at a rate of 2° C. / min, and kept at this temperature for 1 hour. After natural cooli...

Embodiment 2

[0059] The preparation method of the aluminum phosphate-coated carbon-coated lithium titanate nitride comprises the following steps:

[0060] Step 1), 2) 3) and 4) the reaction environment and conditions are the same as in Example 2, the difference is that in step 3), the nitrogen source is ionic liquid 1-ethyl-3-methylimidazole dinitrile amine salt (C 8 h 11 N 5 ).

[0061] The product of step 3) is gray carbon-coated lithium titanate nitride powder. The carbon coating contains pyrolytic carbon 3 and carbon nitride 4 (CN X ) compounds. Among them, carbon nitride (CN X ) compounds are highly conductive.

Embodiment 3

[0063] The preparation method of the aluminum phosphate-coated carbon-coated lithium titanate nitride comprises the following steps:

[0064] Step 1), 2) 3) and 4) reaction environment and condition are the same as embodiment 2, difference is, in step 3), nitrogen source is ionic liquid 1-butyl-3-methyl-pyridine dinitrile amine Salt (C 12 h 16 N 4 ).

[0065] 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.

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Abstract

The invention discloses a preparation method and application of aluminum fluoride-coated carbon-coated lithium titanate nitride. The preparation method comprises the following steps: preparing lithium titanate with a spinel structure; mixing a carbon source with the lithium titanate till the mixture is uniform, and carrying out calcination in a vacuum or a shielding gas atmosphere to obtain carbon-coated lithium titanate; uniformly mixing a nitrogen source with the carbon-coated lithium titanate, and carrying out calcination in a vacuum or a shielding gas atmosphere to obtain carbon-coated lithium titanate nitride; adding aluminum salt and ammonium fluoride into a turbid liquid of the carbon-coated lithium titanate nitride, completely evaporating the mixed solution, and conducting calcination on the uniformly mixed particles in a vacuum or a shielding gas atmosphere to obtain aluminum fluoride-coated carbon-coated lithium titanate nitride. The preparation method provided by the invention has the advantages that the preparation process is simple, pollution is avoided during reactions, the product uniformity is excellent, the obtained aluminum fluoride-coated carbon-coated lithium titanate nitride is high in capacity per gram, and the industrial application prospect is wide.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, in particular to the preparation and application of aluminum fluoride-coated carbon-coated lithium titanate nitride. 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 and dense structure can provide access for limit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/485H01M4/62
CPCH01M4/485H01M4/624H01M4/628H01M10/0525Y02E60/10
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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