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Three-dimensional flower-like TiO2 microspheres composed of nanowires and preparation method thereof

A nanowire and flower-like technology is applied in the field of three-dimensional flower-like TiO2 materials and their preparation, which can solve the problems of easy generation of danger, difficulty in obtaining three-dimensional complex structures, severe hydrolysis, etc., and achieves novel appearance, simple process and mild reaction conditions. Effect

Active Publication Date: 2015-04-08
THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The preparation of titanium oxide by hydrothermal experiment often uses titanium tetrachloride or tetrabutyl titanate as the raw material. The chemical properties of the above-mentioned substances are active, the hydrolysis is severe, and it is easy to cause danger.
Some researchers also use titanium oxide powder as a raw material to prepare nano-titanium oxide, but the morphology of titanium oxide obtained in this way is relatively simple, mainly composed of one-dimensional nanowires and nanotubes, and it is difficult to obtain three-dimensional complex structures.

Method used

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  • Three-dimensional flower-like TiO2 microspheres composed of nanowires and preparation method thereof
  • Three-dimensional flower-like TiO2 microspheres composed of nanowires and preparation method thereof
  • Three-dimensional flower-like TiO2 microspheres composed of nanowires and preparation method thereof

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Embodiment 1

[0030] (1) Put 0.1g of metallic Ti powder into 150mL of a mixed solution of hydrogen peroxide and nitric acid, wherein the concentration of hydrogen peroxide is 6M, and the concentration of nitric acid is 0.1M; then condense and reflux in an oil bath at 80°C for 4 hours to obtain an orange color solution;

[0031] (2) Measure 18mL of the orange-yellow solution prepared in step (1), mix it with 42mL of 10M NaOH solution in a PTFE liner with a volume of 100mL and stir for 10min, then hydrothermally react at 150°C for 3h;

[0032] (3) After the reaction, the precipitate was separated by centrifugation, washed with 0.1M nitric acid and deionized water until the pH value was 7; then dried in an oven at 80°C to obtain a three-dimensional flower-like TiO composed of nanowires 2 Material.

[0033] figure 1 , figure 2 The three-dimensional flower-like TiO that this embodiment makes 2 The scanning electron micrographs of the material at different magnifications, it can be seen from...

Embodiment 2

[0036] (1) Put 0.1g of metallic Ti powder into 150mL of a mixed solution of hydrogen peroxide and nitric acid, wherein the concentration of hydrogen peroxide is 5M, and the concentration of nitric acid is 0.1M; then condense and reflux in an oil bath at 80°C for 5 hours to obtain an orange color solution;

[0037] (2) Measure 18mL of the orange-yellow solution prepared in step (1), mix it with 42mL of 10M NaOH solution in a PTFE liner with a volume of 100mL and stir for 10min, then carry out at a temperature of 140°C Hydrothermal reaction, time is 5h;

[0038] (3) After the reaction is completed, the product is centrifuged and washed with 0.1M nitric acid and deionized water until the pH value of the product obtained in step (2) is 7; then dried in an oven at 80°C to obtain the nanowire composition The three-dimensional flower-like TiO 2 Material.

[0039] Figure 4 , Figure 5 Shown is the three-dimensional flower-like TiO prepared in this example 2 The scanning electro...

Embodiment 3

[0043] (1) Put 0.05g of metallic Ti powder into 100mL of a mixed solution of hydrogen peroxide and nitric acid, wherein the concentration of hydrogen peroxide is 5M, and the concentration of nitric acid is 0.1M; then condense and reflux in an oil bath at 90°C for 6 hours to obtain orange-yellow solution;

[0044] (2) Measure 18mL of the orange solution prepared in step (1), mix it with 42mL of 9M NaOH solution in a PTFE liner with a volume of 100mL and stir for 10min, then hydrothermally react at 130°C for 5h;

[0045] (3) After the reaction is completed, the precipitate is separated by centrifugation, washed with 0.1M nitric acid and deionized water until the pH value is 7; then dried in an oven at 80°C, and the nanowires radiating from the center are obtained. flower-like TiO 2 Material.

[0046] Scanning electron microscopy shows that the three-dimensional flower-like TiO prepared in this example 2 Flower-like TiO 2 The particle size of the microsphere is about 5 μm, an...

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Abstract

The invention provides a TiO2 material with a three-dimensional structure and its preparation method and use. The TiO2 material includes a three-dimensional flower-like microsphere structure composed of many TiO2 nanowires radiating from the center. The particle size of the three-dimensional flower-like microspheres is 3~6 μm, and the diameter of the nanowires is 20 ~50nm, length 1.5~3μm. The preparation method of the three-dimensional flower-like TiO2 material includes dissolving metal Ti powder in a mixed solution of H2O2 / HNO3, and performing a hydrothermal reaction with sodium hydroxide at a certain temperature; after the reaction is completed, centrifuge and wash until the solution pH value is reached. to 7 and then dried in the oven. The three-dimensional flower-like TiO2 material of the present invention has higher adsorption performance and photocatalytic performance than Degussa P25 nanometer TiO2 when degrading methylene blue dye.

Description

technical field [0001] The invention relates to a three-dimensional flower-shaped TiO 2 Materials and their preparation methods and uses, in particular to a three-dimensional flower-like TiO composed of nanowires 2 Materials and their methods of preparation and uses. Background technique [0002] Titanium oxide has the advantages of high photocatalytic activity, environmental friendliness, and low cost. It is the most concerned high-efficiency photocatalyst. , metallurgy and other fields. [0003] The three-dimensional micro-nano hierarchical structure has the advantages of both micro- and nano-structures, which suppresses the shortcomings of each structure, and has become a hot spot in the field of material research. Three-dimensional micro-nano TiO 2 The material has high specific surface area, good light absorption and refractive index. The high specific surface area is conducive to the generation and migration of photogenerated carriers and the adsorption of reactan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J21/06C01G23/047B82Y30/00B01J35/02B01J35/00
Inventor 朴玲钰杜利霞江潮吴志娇吴谦
Owner THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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