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Niobium pentoxide yolk structure nano material with controllable core volume and preparation method thereof

A technology of niobium pentoxide egg yolk and niobium pentoxide, applied in chemical instruments and methods, niobium compounds, inorganic chemistry, etc., can solve the negative effects of reducing the utilization rate of electrochemical active sites, material morphology and performance , material collapse or sintering, etc., to improve the conventional preparation method, simplify the preparation process, and enhance the stability

Active Publication Date: 2020-07-31
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the formation of its lattice generally requires high-temperature (> 600 ºC) annealing treatment, and nanomaterials are prone to collapse or sintering at high temperatures, which has a negative impact on the morphology and properties of the material.
Second, Nb2O5 has poor electrical conductivity (~3.4×10-6 S cm- 1), which reduces the utilization rate of its electrochemical active sites and the rate performance of the material

Method used

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  • Niobium pentoxide yolk structure nano material with controllable core volume and preparation method thereof
  • Niobium pentoxide yolk structure nano material with controllable core volume and preparation method thereof
  • Niobium pentoxide yolk structure nano material with controllable core volume and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1) Weigh 0.4 g of NbCl 5 Dissolve in 60 mL of isopropanol and add 0.4 g of TBA aqueous solution (10 wt%) under magnetic stirring. The above solution was transferred to a 100 mL autoclave and kept at 200 ºC for 24 h. After cooling to room temperature, the product was separated by centrifugation and washed several times, and dried at 60 ºC. Nb collected by centrifugation 2 o 5 TEM image see figure 1 as shown in figure 1 It can be seen that the diameter of the nanosphere is about 500 nm, and the surface is not smooth, which is helpful for the coating growth of dopamine hydrochloride.

[0035] 2) Disperse niobium pentoxide nanospheres (80 mg) and dopamine hydrochloride (50 mg) in tris buffer solution under magnetic stirring. After stirring for 6 h, the centrifuged and dried samples were 2 Under protection, heat up to 500 ºC at a rate of 1 ºC / min and keep the temperature constant for 2 h. Samples were collected after cooling. The TEM image of the obtained product i...

Embodiment 2

[0042] 1) Weigh 0.4 g of NbCl 5 Dissolve in 60 mL of isopropanol and add 0.4 g of TBA aqueous solution (10 wt%) under magnetic stirring. The above solution was transferred to a 100 mL autoclave and kept at 200 ºC for 24 h. After cooling to room temperature, the product was separated by centrifugation and washed several times, and dried at 60 ºC.

[0043] 2) Disperse niobium pentoxide nanospheres (80 mg) and dopamine hydrochloride (50 mg) in tris under magnetic stirring. After stirring for 6 h, the centrifuged and dried samples were 2 Under protection, heat up to 500 ºC at a rate of 1 ºC / min and keep the temperature constant for 2 h. Samples were collected after cooling.

[0044] 3) Weigh 1 g of Nb 2 o 5 @NC nanospheres dispersed in 5.25 g hydrofluoric acid dilute solution (4 mol L -1 ) and stirred for 12h, the centrifuged and dried sample was annealed at 700 ºC for two hours, named as T-Nb 2 o 5 @NC-3. The TEM image of the obtained product is shown in Figure 5 as s...

Embodiment 3

[0046] 1) Weigh 0.4 g of NbCl 5 Dissolve in 60 mL of isopropanol and add 0.4 g of TBA aqueous solution (10 wt%) under magnetic stirring. The above solution was transferred to a 100 mL autoclave and kept at 200 ºC for 24 h. After cooling to room temperature, the product was separated by centrifugation and washed several times, and dried at 60 ºC.

[0047] 2) Disperse niobium pentoxide nanospheres (80 mg) and dopamine hydrochloride (50 mg) in tris under magnetic stirring. After stirring for 6 h, the centrifuged and dried samples were 2 Under protection, heat up to 500 ºC at a rate of 1 ºC / min and keep the temperature constant for 2 h. Samples were collected after cooling.

[0048] 3) Weigh 1 g of Nb 2 o 5 @NC nanospheres dispersed in 2.25 g hydrofluoric acid dilute solution (4 mol L -1 ) and stirred for 12h, the centrifuged and dried sample was annealed at 700 ºC for two hours, named as T-Nb 2 o 5 @NC-3. The TEM image of the obtained product is shown in Figure 6 as s...

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Abstract

The invention discloses a niobium pentoxide yolk structure nano material with a controllable core volume and a preparation method thereof. The method comprises the following steps: preparing a niobiumpentoxide template from niobium chloride and tetrabutylammonium hydroxide under a hydrothermal condition, coating the surface of the niobium pentoxide template with dopamine hydrochloride, carrying out carbonization treatment under the protection of nitrogen, and etching the obtained double-layer concentric nanospheres in hydrofluoric acid to remove part of niobium pentoxide cores in order to obtain the nanometer material with an egg yolk structure. The niobium pentoxide core with a controllable hetero-atom carbon shell confinement volume is used, so that the space utilization rate of the nano yolk material can be effectively regulated and controlled, and the problem of volume expansion can be relieved. Heteroatom functional groups on the heteroatom carbon shell are beneficial to infiltration of the electrolyte and transmission of ions.

Description

technical field [0001] The invention relates to the technical field of electrode materials for lithium-ion hybrid capacitors, in particular to a niobium pentoxide egg yolk structure nanomaterial with controllable core volume used in a heteroatom carbon shell confinement of lithium-ion hybrid capacitors and a preparation method thereof. Background technique [0002] With the continuous deepening of research on energy storage devices, lithium-ion hybrid capacitors (HSCs), which combine the advantages of lithium-ion batteries (LICs) and supercapacitors (SCs), have been proposed and have attracted widespread attention. HSC is an energy storage device that combines a lithium-ion intercalation-type Faradaic-behavior negative electrode with an electric double-layer-type non-Faradaic-behavior positive electrode. Existing studies have proved that the combination of two different energy storage mechanisms makes HSCs possess the advantages of both LICs and SCs. Specifically, HSC not o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G33/00H01G11/06H01G11/24H01G11/26H01G11/46H01G11/50
CPCC01G33/00H01G11/24H01G11/26H01G11/46H01G11/50H01G11/06C01P2004/03C01P2004/04C01P2002/85C01P2002/72C01P2004/01C01P2006/40C01P2004/32Y02E60/13Y02E60/10
Inventor 张淮浩练越柏永青王大为赵静
Owner YANGZHOU UNIV
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