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Flower-like niobium pentoxide material and preparation method thereof

A technology of niobium pentoxide and niobium pentachloride, applied in chemical instruments and methods, inorganic chemistry, niobium compounds, etc., to achieve the effects of good dispersion, strong controllability of reaction conditions, uniform and regular morphology

Inactive Publication Date: 2017-03-22
NANYANG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, so far there is no information about the ultrathin Nb 2 o 5 3D flower-like Nb assembled from nanosheets 2 o 5 Reports on materials and their preparation methods

Method used

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  • Flower-like niobium pentoxide material and preparation method thereof
  • Flower-like niobium pentoxide material and preparation method thereof
  • Flower-like niobium pentoxide material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Step 1). Dissolve niobium pentachloride in deionized water under stirring conditions, where the concentration of niobium ions is 0.55 mol / L;

[0031] Step 2). Add hydrofluoric acid to the above aqueous solution of niobium pentachloride, wherein the molar ratio of niobium pentachloride to hydrofluoric acid is 1:0.5, and continue to stir for 16 hours;

[0032] Step 3). Transfer the solution obtained in step 2) to a high-pressure stainless steel reactor, place it in a constant temperature drying oven, and heat and react at 180°C for 24 hours;

[0033] Step 4) Centrifuge the reaction precipitate obtained in step 3), wash it with ethanol and deionized water several times, and then dry it in a vacuum drying oven at a temperature of 80°C;

[0034] Step 5). Place the powder obtained in step 4) in a tube furnace and calcine at 600°C for 1 hour to obtain flower-like Nb 2 O 5 material.

[0035] Such as figure 1 As shown, the diffraction peak of the sample and Nb 2 O 5 The standard diffracti...

Embodiment 2

[0037] Step 1). Dissolve niobium pentachloride in deionized water under stirring conditions, where the concentration of niobium ions is 0.055 mol / L;

[0038] Step 2). Add hydrofluoric acid to the above aqueous solution, wherein the molar ratio of niobium pentachloride to hydrofluoric acid is 1:0.2, and continue to stir for 24 hours;

[0039] Step 3). Transfer the solution obtained in step 2) to a high-pressure stainless steel reactor, place it in a constant temperature drying oven, and heat and react at 178°C for 15 hours;

[0040] Step 4) Centrifuge the reaction precipitate obtained in step 3), wash it with ethanol and deionized water several times, and then dry it in a vacuum drying oven at a temperature of 110°C;

[0041] Step 5). Place the powder obtained in step 4) in a tube furnace and calcinate at 600°C for 1.5 hours to obtain flower-like Nb 2 O 5 material.

Embodiment 3

[0043] Step 1). Dissolve niobium pentachloride in deionized water under stirring conditions, where the concentration of niobium ions is 0.45 mol / L;

[0044] Step 2). Add hydrofluoric acid to the above aqueous solution, wherein the molar ratio of niobium pentachloride to hydrofluoric acid is 1:0.6, and continue to stir for 16 hours;

[0045] Step 3). Transfer the solution obtained in step 2) to a high-pressure stainless steel reactor, place it in a constant temperature drying oven, and heat and react at 185°C for 1 hour;

[0046] Step 4) Centrifuge the reaction precipitate obtained in step 3), wash it with ethanol and deionized water several times, and then dry it in a vacuum drying oven at a temperature of 100°C;

[0047] Step 5). Place the powder obtained in step 4) in a tube furnace and calcinate at 700°C for 0.5 hours to obtain flower-like Nb 2 O 5 material.

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Abstract

The invention discloses a preparation method of a flower-like niobium pentoxide material. The preparation method comprises the following steps that firstly, columbium pentachloride is dissolved in deionized water; then hydrofluoric acid is added; then the obtained solution is put into a high-pressure reaction kettle for a heating reaction; and finally, cooling is conducted, then washing, drying and roasting are conducted, and the flower-like niobium pentoxide material is obtained. The invention further discloses the flower-like niobium pentoxide material prepared through the method. The prepared flower-like niobium pentoxide material is uniform and regular in morphology and good in dispersibility. The prepared flower-like Nb2O5 is composed of a two-dimensional nanosheet with the thickness of 10 to 30 nanometers, the size of the flower is about 1-3 micrometers, and the flower-like Nb2O5 has the potential application value in the fields of photocatalysis, sensitized solar cells, sensors, energy storage and the like; and according to the preparation method and the flower-like niobium pentoxide material, a synthetic process is simple, the controllability of the reaction condition is high, and the flower-like niobium pentoxide material and the preparation method are suitable for industrial production.

Description

Technical field [0001] The invention belongs to the field of inorganic nano materials, and specifically relates to a flower-shaped niobium pentoxide material and a preparation method thereof. Background technique [0002] Niobium pentoxide (Nb 2 O 5 ) With excellent physical and chemical properties, it is widely used in the fields of photosensitive dye batteries, photocatalysis, sensors, capacitors and lithium-ion batteries. During the research process, it was discovered that Nb 2 O 5 The morphology, structure, particle size, etc. have a greater impact on its performance. So far, people have successfully synthesized zero-dimensional nanoparticles, one-dimensional nanowires, nanobelts, nanorods and two-dimensional nanosheet structures of Nb. 2 O 5 Material, and showed good performance. In recent years, micro-nano hierarchical structure materials have become the focus of attention of domestic and foreign scientific researchers due to their unique physical and chemical characterist...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G33/00B82Y40/00
CPCB82Y40/00C01G33/00C01P2002/72C01P2004/03C01P2004/04C01P2004/45C01P2004/61
Inventor 郭佳莉季晓广胡敏吴征刘丹魏铭
Owner NANYANG NORMAL UNIV
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