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a spherical ti 2 nb 10 o 29 Materials and methods of making the same

A spherical, certain amount of technology, applied in the direction of chemical instruments and methods, hybrid/electric double layer capacitor manufacturing, niobium compounds, etc., can solve the problem of long diffusion path of lithium ions, low electrochemical rate performance, large particle size of titanium niobate, etc. problems, to achieve the effect of easy control of product size, high rate cycle performance, and uniform shape

Inactive Publication Date: 2017-12-15
NANYANG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the titanium niobate reported in the literature all adopts the high-temperature solid-phase method. Although the process is simple, the titanium niobate particle size prepared by this method is relatively large (> 1 μm), which makes the diffusion path of lithium ions long and the electrical conductivity of the material is relatively large. Lower chemical rate performance

Method used

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  • a spherical ti  <sub>2</sub> nb  <sub>10</sub> o  <sub>29</sub> Materials and methods of making the same
  • a spherical ti  <sub>2</sub> nb  <sub>10</sub> o  <sub>29</sub> Materials and methods of making the same
  • a spherical ti  <sub>2</sub> nb  <sub>10</sub> o  <sub>29</sub> Materials and methods of making the same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (a) dissolving niobium pentachloride in a certain amount of glacial acetic acid, then adding titanium sulfate according to the atomic ratio titanium / niobium=0.18 under stirring conditions, wherein the concentration of niobium ions is 0.26mol / L;

[0031] (b) Put the mixed solution obtained in step (a) into a stainless steel reaction kettle lined with polytetrafluoroethylene, place it in a constant temperature drying oven, and react at 260° C. for 36 hours;

[0032] (c) naturally cooling to room temperature, washing the obtained precipitate three times with deionized water and ethanol respectively, and then vacuum-drying at 75° C. to obtain a powder;

[0033] (d) Calcining the powder obtained in step (c) at 1230°C for 30 hours to obtain spherical Ti 2 Nb 10 o 29 Material.

[0034] Spherical Ti prepared by Example 1 2 Nb 10 o 29 The XRD pattern of the material is shown in figure 1 As shown, the diffraction peak of the sample is the same as that of Ti in the standard...

Embodiment 2

[0036] (a) dissolving niobium ethanol in a certain amount of glacial acetic acid, and then adding butyl titanate according to the atomic ratio titanium / niobium=0.23 under stirring conditions, wherein the concentration of niobium ions is 2.1mol / L;

[0037] (b) Put the mixed solution obtained in step (a) into a stainless steel reaction kettle lined with polytetrafluoroethylene, place it in a constant temperature drying oven, and react at 120° C. for 72 hours;

[0038] (c) naturally cool to room temperature, wash the obtained precipitate three times with deionized water and ethanol, and then vacuum-dry at 70° C. to obtain a powder;

[0039] (d) Calcining the powder obtained in step (c) at 1110°C for 40 hours to obtain spherical Ti 2 Nb 10 o 29Material.

Embodiment 3

[0041] (a) dissolving niobium oxalate in a certain amount of glacial acetic acid, then adding titanium sulfate according to the atomic ratio titanium / niobium=0.21 under stirring conditions, wherein the concentration of niobium ions is 0.0015mol / L;

[0042] (b) Put the mixed solution obtained in step (a) into a stainless steel reaction kettle lined with polytetrafluoroethylene, place it in a constant temperature drying oven, and react at 280° C. for 30 hours;

[0043] (c) naturally cooling to room temperature, washing the obtained precipitate three times with deionized water and ethanol respectively, and then vacuum-drying at 96° C. to obtain a powder;

[0044] (d) Calcining the powder obtained in step (c) at 710°C for 60 hours to obtain spherical Ti 2 Nb 10 o 29 Material.

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Abstract

The invention discloses a preparation method of a spherical Ti2Nb10O29 material.The preparation method comprises the specific steps that a, a niobium source and a titanium source are dissolved in glacial acetic acid according to a certain proportion; b, the mixed liquid is loaded into a high-pressure reactor to be heated and react; c, washing, drying and calcining are carried out after cooling, and the spherical Ti2Nb10O29 material is obtained.The invention further discloses the spherical Ti2Nb10O29 material prepared through the preparation method.The preparation method and the spherical Ti2Nb10O29 material have the advantages that the method is easy and convenient, and the size of the product is easy to control.The prepared spherical Ti2Nb10O29 material is even in morphology and small in size, a porous structure exists in the material, high tap density is achieved, and the rate charge-discharge circulating performance of Ti2Nb10O29 is greatly improved.

Description

technical field [0001] The application belongs to the field of chemical power sources, in particular, it relates to a spherical Ti as lithium-ion battery or supercapacitor negative electrode material 2 Nb 10 o 29 Materials and their preparation methods. Background technique [0002] With the enhancement of people's awareness of environmental protection and the support of national industrial policies, the electric vehicle industry has flourished in recent years. As an ideal power source for electric vehicles, lithium-ion batteries have the advantages of high energy density, high operating voltage, long service life and low environmental pollution. However, most of the current commercial lithium-ion batteries use graphite-like carbon materials as negative electrodes, which have problems such as slow charging speed and poor safety, which cannot meet the requirements of power batteries for electric vehicles. Therefore, it is urgent to develop high-performance and high-safety...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G33/00H01M4/48H01M4/131H01M4/1391H01M10/0525H01G11/46H01G11/86
CPCC01G33/00C01P2002/72C01P2004/03C01P2004/04C01P2004/32C01P2004/61C01P2004/62C01P2006/40H01G11/46H01G11/86H01M4/131H01M4/1391H01M4/483H01M10/0525Y02E60/10
Inventor 刘光印魏铭郭佳莉赵强毛武涛张瑞雪谢海泉柳文敏马勤阁
Owner NANYANG NORMAL UNIV
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