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Nitrogen and fluorine co-doped titanium dioxide/carbon micro-sphere material, preparation method thereof and application of nitrogen and fluorine co-doped titanium dioxide/carbon micro-sphere material in sodium-ion battery

A titanium dioxide, co-doping technology, applied in secondary batteries, battery electrodes, circuits, etc., can solve the problems of limited battery volume specific capacity, low tap density of tubular titanium dioxide, and difficulty in commercialization, etc., to achieve high volume ratio Capacity, increase sodium ion storage, and promote the effect of sodium ion diffusion

Active Publication Date: 2022-01-14
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the material has excellent specific capacity and cycle performance, the tap density of tubular titanium dioxide is very low, which greatly limits the volume specific capacity of the battery.
It is difficult to commercialize under the constraints of today's space conditions

Method used

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  • Nitrogen and fluorine co-doped titanium dioxide/carbon micro-sphere material, preparation method thereof and application of nitrogen and fluorine co-doped titanium dioxide/carbon micro-sphere material in sodium-ion battery
  • Nitrogen and fluorine co-doped titanium dioxide/carbon micro-sphere material, preparation method thereof and application of nitrogen and fluorine co-doped titanium dioxide/carbon micro-sphere material in sodium-ion battery
  • Nitrogen and fluorine co-doped titanium dioxide/carbon micro-sphere material, preparation method thereof and application of nitrogen and fluorine co-doped titanium dioxide/carbon micro-sphere material in sodium-ion battery

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] The preparation method of nitrogen and fluorine co-doped titanium dioxide / carbon microsphere material, the steps are as follows:

[0058] (1) Disperse 1mL of tetrabutyl titanate in 30mL of glycerin solvent, and the concentration is 12g L -1 Cetyltrimethylammonium bromide solution (add 0.5ml tetramethylammonium hydroxide to adjust pH) 30mL, mix well;

[0059] (2) Transfer the above mixed solution to a hydrothermal reaction kettle, heat at 180°C for 12 hours; centrifuge the product, wash it with ethanol and water several times, and dry it in a vacuum oven at 60°C for 12 hours to obtain a titanium source precursor;

[0060] (4) Put the titanium source precursor and ammonium fluoride in a tube furnace, the mass ratio of the titanium source precursor and ammonium fluoride is 1:10, wherein the ammonium fluoride is located in the upstream direction of the gas flow, and is heated at 400 °C under the protection of argon. Heated at ℃ for 2 hours to obtain nitrogen and fluorine c...

experiment example 1

[0062] Morphology and composition test

[0063] The nitrogen, fluorine co-doped titanium dioxide / carbon microsphere material of embodiment 1 has been carried out morphology and composition test, as figure 1 shown. Depend on figure 1 a It can be seen that NF-TiO 2 / C is a porous microsphere with a diameter of 3-8 microns. Depend on figure 1 b high resolution electron microscope and figure 1 The XRD spectrum of c can confirm that the synthesized product is anatase phase titanium dioxide. Depend on figure 1 The X-ray photoelectron spectrum of d shows that the material contains N, F, and C elements. figure 2 is NF-TiO 2 The fine spectrum of / C. figure 2 a is the Ti 2p spectrum of titania, a small amount of Ti 3+ Indicating that there may be oxygen vacancies, figure 2 The C1s spectrum in b shows that N and F elements have been successfully doped into the carbon layer. figure 2 In c-d, it is further confirmed that N and F elements are doped into the titanium dioxide ...

Embodiment 2

[0082] The preparation method of nitrogen and fluorine co-doped titanium dioxide / carbon microsphere material, the steps are as follows:

[0083] (1) Disperse 3mL tetrabutyl titanate in 60mL glycerin solvent, and add the concentration of 12g L -1 Cetyltrimethylammonium bromide solution (add 0.5ml tetramethylammonium hydroxide to adjust pH) 30mL, mix well;

[0084] (2) Transfer the above mixed solution to a hydrothermal reaction kettle, heat at 180°C for 12 hours; centrifuge the product, wash it with ethanol and water several times, and dry it in a vacuum oven at 60°C for 12 hours to obtain a titanium source precursor;

[0085] (4) Put the titanium source precursor and ammonium fluoride in a tube furnace, the mass ratio of the titanium source precursor and ammonium fluoride is 1:10, wherein the ammonium fluoride is located in the upstream direction of the gas flow, and is heated at 400 °C under the protection of argon. Heated at ℃ for 2 hours to obtain nitrogen and fluorine co-...

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Abstract

The invention relates to a nitrogen and fluorine co-doped titanium dioxide / carbon micro-sphere material, a preparation method thereof and an application of the nitrogen and fluorine co-doped titanium dioxide / carbon micro-sphere material in a sodium ion battery. The material is structurally characterized in that the surface of a titanium dioxide sphere is coated with a carbon layer, nitrogen and fluorine are co-doped in titanium dioxide and the carbon layer, the whole material is a porous micro-sphere with the diameter of 3-8 microns, and the surface and the interior of the micro-sphere are both a porous structure; and titanium dioxide is anatase-phase titanium dioxide, the tap density of the material is 1.5-1.6 g cm <-3 >, tetrabutyl carbonate is used as a titanium source, a hydrolysate of tetrabutyl titanate is titanium dioxide, tetramethylammonium hydroxide provides an alkaline environment so as to form a porous structure, and a surfactant is calcined to form a carbon layer to coat the surfaces of titanium dioxide spheres. The doping of nitrogen and fluorine shortens the band gap of titanium dioxide and carbon so as to enhance the conductivity of NF-TiO2 / C. And the doping of nitrogen and fluorine elements promotes the storage and diffusion of sodium ions, and improves the sodium storage performance of titanium dioxide.

Description

Technical field: [0001] The invention provides a nitrogen and fluorine co-doped titanium dioxide / carbon microsphere material, a preparation method thereof and an application in a sodium ion battery, belonging to the technical field of negative electrode materials of the sodium ion battery. Background technique: [0002] Na-ion batteries have been considered as one of the most promising energy storage devices to replace lithium-ion batteries due to the abundance and low price of sodium. At present, a lot of research focuses on improving the gravimetric capacity (capacity divided by mass) of Na-ion batteries, but this is not the only direction that requires efforts. In view of the space constraints in consumer electronics, microelectronics, aerospace and other fields, the volume-specific capacity (capacity divided by battery volume) of batteries should be prioritized and improved to meet the space requirements in practical application scenarios. Usually the positive electrode...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/48H01M4/583H01M4/62H01M10/054
CPCH01M4/366H01M4/483H01M4/583H01M4/625H01M10/054H01M2004/027H01M2004/021Y02E60/10
Inventor 杨剑汪冬冬吕丹
Owner SHANDONG UNIV