Titanium nitride coated lithium titanate material preparation method

A technology for coating lithium titanate and lithium source with titanium nitride, which is applied in the direction of electrical components, battery electrodes, circuits, etc., can solve the problems of difficult control of coating effect, uneven coating, toxic cyanide, etc., and achieve easy embedding and emigration, good coating effect, and the effect of preventing flatulence

Active Publication Date: 2013-11-20
SHENZHEN DYNANONIC
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Problems solved by technology

CN200910310151.6 discloses a method for preparing lithium titanate modified by surface self-growth titanium nitride conductive film, which adopts the method of ball milling and sintering to modify lithium titanate, and it is difficult to control the coating effect by using this method
CN201010530815.2 discloses a preparation method of lithium titanate / titanium nitride composite material, which uses a composite material to modify lithium titanate, and this method will have the problem of insufficient coating uniformity
In addition, nitrogen-containing organic matter may produce toxic cyanide during calcination, which not only pollutes the environment, but also poses safety hazards in the production process

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  • Titanium nitride coated lithium titanate material preparation method
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  • Titanium nitride coated lithium titanate material preparation method

Examples

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preparation example Construction

[0029] The preparation method of titanium nitride coated lithium titanate material comprises the following steps:

[0030] First, the lithium source and the titanium source are dispersed in a solution containing a complexing agent and a hydrolysis inhibitor to obtain a precursor solution. The preparation method of the precursor solution is as follows: dissolve the lithium source and complexing agent in water to form an aqueous solution, then dilute the aqueous solution with any amount of ethanol to form solution A; disperse the titanium source and hydrolysis inhibitor in ethanol to form solution B; Add solution B dropwise to solution A to form a precursor solution. Wherein, the ratio of the amount of substances of lithium source, titanium source, complexing agent and hydrolysis inhibitor is n(Li):n(Ti):n(complexing agent):n(hydrolysis inhibitor)=0.75-0.85: 1: 0.1-0.35: 0.2-0.85. The lithium source includes at least one of lithium oxide, lithium hydroxide, lithium acetate, li...

Embodiment 1

[0037] Dissolve 3.75mol lithium hydroxide (LiOH) in water, and add 0.95mol citric acid (C 6 h 8 o 7 ), and then dilute the solution with ethanol to form solution A; 5mol tetrabutyl titanate (C 16 h 36 o 4 Ti) was mixed with acetic acid and dispersed in ethanol to obtain solution B; then solution B was dropped into solution A drop by drop to obtain a precursor solution.

[0038] The precursor solution was heated to 65° C. and kept for 18 hours to obtain a gel, and the gel was heated at 120° C. for 8 hours to evaporate the solvent to obtain a precursor. Then, the precursor was heated to 750°C in an air atmosphere and kept for 12 hours to obtain nano-lithium titanate powder; keeping the temperature constant, the nano-lithium titanate powder was placed in a mixed gas of nitrogen and ammonia (nitrogen and ammonia The gas volume ratio is 9:1) in an atmosphere at constant temperature for 12 hours to obtain a titanium nitride-coated lithium titanate material.

Embodiment 2

[0040]The difference between this example and Example 1 is: the precursor solution was heated to 60° C. and kept for 10 hours to obtain a gel, and the gel was heated at 125° C. for 8 hours to evaporate the solvent to obtain a precursor. Then, the precursor was heated to 800°C in an air atmosphere and kept for 20 hours to obtain nano-lithium titanate powder; keeping the temperature constant, the nano-lithium titanate powder was placed in a mixed gas of nitrogen and ammonia (nitrogen and ammonia The gas volume ratio is 9:1) in an atmosphere at constant temperature for 12 hours to obtain a titanium nitride-coated lithium titanate material.

[0041] Compared with the product prepared in Example 1, the product prepared in this example has a larger particle size of titanium nitride nano-lithium titanate and a smaller thickness of the titanium nitride coating layer. The color of the product prepared in embodiment 1 is dark blue, as Figure 8 Shown; The color of the product prepared ...

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Abstract

The present invention relates to the technical field of battery materials, particularly to a titanium nitride coated lithium titanate material preparation method, which sequentially comprises: preparing a precursor solution, evaporating a solvent, sintering in an atmosphere containing oxygen, and sintering in an atmosphere containing reduction gas nitrogen. According to the present invention, the titanium nitride coated lithium titanate material prepared by using the preparation method has characteristics of high titanium nitride coating uniformity, good coating effect and good conductivity, and the conductivity problem of application of titanium nitride in electrode materials is solved; and titanium nitride is adopted to separate tetravalent titanium ions and an electrolyte, such that catalysis cracking of the electrolyte by the tetravalent titanium ions can be effectively prevented so as to prevent phenomenon of gas generation. In addition, the preparation process is simple and controllable, and process parameters of the lithium titanate material coated through titanium nitride can be controlled so as to control the coating degree of titanium nitride.

Description

technical field [0001] The invention relates to the technical field of battery materials, in particular to a preparation method of titanium nitride-coated lithium titanate material. Background technique [0002] Lithium titanate is an excellent negative electrode material for lithium batteries. However, when lithium titanate is directly applied to lithium batteries, there are two shortcomings. One is the high resistivity of lithium titanate, and the other is that it will appear after the battery is assembled. Flatulence, leading to potential safety hazards in the application. The deficiencies in the above two aspects can be solved or reduced by modifying lithium titanate. CN200910310151.6 discloses a method for preparing lithium titanate modified by surface self-growth titanium nitride conductive film, which adopts the method of ball milling and sintering to modify lithium titanate, and it is difficult to control the coating effect by using this method. CN201010530815.2 di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/485
CPCY02E60/122Y02E60/10
Inventor 黄斯昭孔令涌程文涛赖玉丽许燕平
Owner SHENZHEN DYNANONIC
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