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Method for preparing titanium niobium oxide

A technology of titanium niobium oxide and niobium source, applied in niobium compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of difficulty in taking into account the performance and production cost of titanium niobium oxide, and achieves increased lithium ion transmission performance, improved Effect of particle morphology, mild reaction conditions

Pending Publication Date: 2022-05-13
CHENGDU SCI & TECH DEV CENT CHINA ACAD OF ENG PHYSICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a method for preparing titanium niobium oxide for the problem that the performance and production cost of the prepared titanium niobium oxide existing in the prior art are difficult to balance

Method used

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  • Method for preparing titanium niobium oxide
  • Method for preparing titanium niobium oxide
  • Method for preparing titanium niobium oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Titanium niobium oxide TiNb 6 o 17 preparation of

[0051] Ethylene glycol is used as a solvent, P123 is used as a surfactant; niobium oxalate is used as a niobium source, and titanium isopropoxide is used as a titanium source;

[0052] S1, add 20ml of ethylene glycol to the beaker, then add 0.1g of P123, 6.456g of niobium oxalate and 0.505ml of titanium isopropoxide into the beaker;

[0053] S2, heated to 160°C, concentrated to form a gel;

[0054] S3, calcining the gel obtained in step S2 at 800° C. for 5 hours in an air atmosphere to obtain a powder, and ball milling and drying the powder to obtain titanium niobium oxide.

[0055] The SEM of the titanium niobium oxide is as figure 1 Shown, XRD test result is as follows figure 2 shown.

[0056] The performance of the obtained titanium niobium oxide is tested, the test method is: the obtained TiNb 6 o 17 Mix it with conductive carbon black and PVDF, add NMP as a solvent and coat it on copper foil to make an el...

Embodiment 2

[0058] Titanium niobium oxide TiNb doped with carbon and oxygen vacancies 6 o 17 preparation of

[0059] Ethylene glycol is used as a solvent, P123 is used as a surfactant; niobium oxalate is used as a niobium source, and tetrabutyl titanate is used as a titanium source;

[0060] S1, add 20ml of ethylene glycol to the beaker, then add 0.2g of P123, 12.912g of niobium oxalate and 1.36ml of tetrabutyl titanate into the beaker;

[0061] S2, heated to 150°C, concentrated to form a gel;

[0062] S3, calcining the gel obtained in step S2 at 500°C for 2 hours in an air atmosphere; then sintering at 900°C for 3 hours in an argon atmosphere to obtain a powder, and ball milling and drying the powder to obtain titanium niobium oxide doped with carbon and oxygen vacancies .

[0063] The SEM of the titanium niobium oxide is as Figure 4 As shown, the TEM test results are as follows Figure 5 As shown, the performance of the obtained titanium-niobium oxide was tested, and the test met...

Embodiment 3

[0066] Titanium niobium oxide TiNb 2 o 7 preparation of

[0067] 1,2-propanediol is used as solvent, P123 is used as surfactant; ammonium niobium oxalate is used as niobium source, and tetrabutyl titanate is used as titanium source.

[0068] S1, add 20ml of 1,2-propanediol to the beaker, then add 0.1g of P123, 7.5g of ammonium niobium oxalate and 3.4ml of tetrabutyl titanate into the beaker;

[0069] S2, heated to 180°C, concentrated to form a gel;

[0070] S3, calcining the gel obtained in step S2 at 900°C for 3 hours in an air atmosphere to obtain a powder, which is ball milled and dried to obtain TiNb 2 o 7 .

[0071] The SEM of the titanium niobium oxide is as Figure 7 Shown, XRD test result is as follows Figure 8 As shown, the rate performance as Figure 9 shown.

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Abstract

The invention relates to the technical field of new energy materials, in particular to a method for preparing titanium niobium oxide. The method comprises the following steps: S1, adding a niobium source and a titanium source into a solvent; the solvent is alcohol or a mixture of alcohol of which the boiling point is greater than 100 DEG C; the niobium source comprises one or two of niobium oxalate and niobium ammonium oxalate, and the titanium source comprises one or two of titanium isopropoxide and tetrabutyl titanate; s2, concentrating the solution obtained in the step S1 at 100-220 DEG C to form gel; and S3, calcining the gel obtained in the step S2 to obtain the titanium niobium oxide. By screening a titanium source, a niobium source and a solvent, when gel is formed, the temperature is controlled to be 100 DEG C or above, and esterification reaction is carried out in a solution, so that titanium and niobium are uniformly distributed in the gel, and uniform distribution and consistent performance of product particles are facilitated. And the preparation process is carried out under normal pressure, the reaction condition is mild, the repeatability is good, and the potential of large-scale production is achieved.

Description

technical field [0001] The invention relates to the technical field of new energy materials, in particular to a method for preparing titanium niobium oxide. Background technique [0002] As an anode material for lithium-ion batteries, titanium niobium oxide (TNO) has attracted extensive attention due to its high safety and high capacity. [0003] Titanium niobium oxide (TNO) is a solid solution of niobium oxide and titanium oxide, which can generally be prepared by calcining niobium oxide and titanium oxide at high temperature. TNO is a semiconductor material with a relatively wide band gap, which can be applied in the field of photocatalysis. At the same time, because its crystal structure is conducive to the intercalation and extraction of ions, it can also be used in lithium-ion batteries, sodium-ion batteries, and supercapacitors. When used as a negative electrode material for lithium-ion batteries, TNO has the advantages of high theoretical specific capacity and high ...

Claims

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Application Information

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IPC IPC(8): C01G33/00
CPCC01G33/00C01P2004/03C01P2002/72C01P2006/40Y02E60/10
Inventor 曾文文詹浩然商云帆卢苏阳梅军杨烨
Owner CHENGDU SCI & TECH DEV CENT CHINA ACAD OF ENG PHYSICS
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