Method for preparing spherical titanium oxide niobate anode material in large scale by utilizing spray drying method and application thereof to lithium ion battery

A large-scale preparation and spray-drying technology, which is applied to niobium compounds, chemical instruments and methods, and battery electrodes, can solve the problem of low theoretical capacity and achieve low raw material costs, excellent high-rate charge and discharge performance, and safety performance. The effect of broad application prospects

Inactive Publication Date: 2016-04-20
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the past ten years, lithium titanate has attracted widespread attention due to its excellent rate performance and low production cost, and has become a next-generation anode material that is very likely to be commercialized. Howeve...

Method used

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  • Method for preparing spherical titanium oxide niobate anode material in large scale by utilizing spray drying method and application thereof to lithium ion battery
  • Method for preparing spherical titanium oxide niobate anode material in large scale by utilizing spray drying method and application thereof to lithium ion battery
  • Method for preparing spherical titanium oxide niobate anode material in large scale by utilizing spray drying method and application thereof to lithium ion battery

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specific Embodiment approach 1

[0027] Specific implementation method one: disperse tetrabutyl phthalate and niobium ethoxide in equimolar ratio and dissolve in ethanol, fully stir to make it disperse evenly, then add equal volume of distilled water to mix and stir, put it in the spray drier It is sprayed at a flow rate of 10ml / min, and the nozzle temperature is 150°C. figure 1 and figure 2 That is, TiNb prepared by spray drying 2 o 7 The scanning electron microscope image of the nanosphere shows the typical spherical particles at the Chen correlation point of the material. The obtained powder is dried in an oven at 80°C to obtain a white precursor, and then the precursor is calcined in a tube furnace at 900°C in an air atmosphere to obtain spherical TiNb 2 o 7 Negative material.

specific Embodiment approach 2

[0028] Specific embodiment two: Disperse and dissolve titanium isopropoxide (isopropyl titanate) and niobium hydroxide in equal molar ratios in water, where a certain amount of oxalic acid needs to be added in advance to prevent hydrolysis at a concentration of 0.5 mol / L , fully stirred to disperse evenly, sprayed out in a spray dryer at a speed of 5ml / min, and the spraying temperature from spray drying was 180°C. The obtained powder is dried in an oven to obtain a precursor, and then the precursor is calcined in a high-temperature furnace at 1000°C in an air atmosphere to obtain spherical TiNb 2 o 7 Negative material. image 3 and Figure 4 That is the morphology of spherical TNO after calcination.

specific Embodiment approach 3

[0029] Specific embodiment three: Titanium isopropoxide (isopropyl titanate) and niobium hydroxide in equimolar ratio are dispersed and dissolved in water, wherein a certain amount of oxalic acid needs to be added in advance to prevent hydrolysis, the concentration is 0.2mol / L, Thoroughly stir it to disperse it evenly, spray it in the spray dryer at a speed of 20ml / min, the spray temperature from spray drying is 200°C, increase the flow rate and nozzle temperature to obtain the precursor material of large particles, and then Improve its tap density and the energy density of the battery. The obtained powder is dried in an oven to obtain a precursor, and then the precursor is calcined in a high-temperature furnace at 1200°C in an air atmosphere to obtain a larger volume of spherical TiNb 2 o 7 Negative material.

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Abstract

The invention discloses a method for preparing a spherical titanium oxide niobate anode material in a large scale by utilizing a spray drying method and application thereof to a lithium ion battery. The method comprises: 1, dispersing and dissolving a titanium source and a niobium source in an equal molar ratio in a solvent system, and sufficiently stirring to enable the titanium source and the niobium source to be uniformly dispersed; 2, spraying out the mixed solution in a spray dyer according to a certain flow, and drying obtained powder in an oven to obtain a precursor; 3, calcining the precursor in a high-temperature furnace in the air atmosphere at a temperature of 800 to 1,400 DEG C so as to obtain the spherical TiNb2O7 anode material. The spherical titanium-niobium composite oxide TiNb2O7 prepared by the method has excellent electrochemical performance, and has high coulombic efficiency and reversible capacity and excellent high-rate charge/discharge performance and safety performance when being used as a lithium ion battery anode material. The spherical titanium oxide niobate anode material is low in raw material cost, is non-toxic and harmless, and has a very wide application prospect.

Description

technical field [0001] The invention belongs to the technical field of energy storage materials, and relates to a preparation method of a spherical titanium niobate oxide negative electrode material with excellent electrochemical performance and a high-performance lithium-ion secondary battery based on the material as a negative electrode. Background technique [0002] As the traditional fossil energy tends to be exhausted, the search for efficient and clean new green energy has become a research hotspot in the chemical field. Among them, lithium-ion secondary batteries have received more and more attention due to their many advantages. In addition to meeting the power needs of portable devices, the development prospects of lithium-ion batteries in high-power, high-energy power batteries It is even more exciting. Among them, the study of electrode materials is particularly critical. In the past ten years, lithium titanate has attracted widespread attention due to its excel...

Claims

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Application Information

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IPC IPC(8): C01G33/00H01M4/48H01M10/0525
CPCC01G33/00C01P2004/03C01P2004/32C01P2004/61H01M4/48H01M10/0525Y02E60/10
Inventor 尹鸽平娄帅锋高金龙马玉林高云智程新群
Owner HARBIN INST OF TECH
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