Method for preparing nitrogen-doped TiO2 hollow nano material

A hollow nanometer, nitrogen-doped technology, applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve problems such as limiting the efficiency of sunlight utilization, achieve good repeatability, Visible light absorption spectrum and the effect of visible light catalytic activity

Active Publication Date: 2017-05-31
HUAQIAO UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, anatase TiO 2 It is a wide band gap semiconductor material with a band gap of 3.2eV, which indicates that the intrinsic anatase TiO 2 Only absorbs UV light
Because ultraviolet light only accounts for about 4% of sunlight, which greatly limits its utilization efficiency of sunlight

Method used

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  • Method for preparing nitrogen-doped TiO2 hollow nano material
  • Method for preparing nitrogen-doped TiO2 hollow nano material
  • Method for preparing nitrogen-doped TiO2 hollow nano material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1)TiOF 2 Fabrication of nanocubes: synthesis of TiOF by one-step solvothermal reaction 2 nanocube. Add 5.0 mL of tetrabutyl titanate, 1.6 mL of hydrofluoric acid solution and 10 mL of glacial acetic acid into the hydrothermal reaction kettle together. The reaction kettle was sealed and placed in an oven. The reaction temperature was heated from room temperature to 200° C. within 60 minutes, and then the reaction was maintained at 200° C. for 12 hours. After the reaction was over, the reactor was cooled to room temperature. Ultrasonic cleaning with ethanol and centrifugation to obtain white TiOF 2 Nanocube powder, whose composition and structure are characterized as figure 1 shown.

[0026] (2)TiOF 2 The nano-cube powder and urea were weighed and put into two porcelain boats respectively. TiOF 2 The used mass of nanocube is 0.4g, and the mass of urea weighed is 0.1g. Place the two porcelain boats with weighed samples in the middle of the tube furnace one by on...

Embodiment 2

[0029] (1)TiOF 2 The preparation of nanocubes is consistent with that of Example 1.

[0030] (2)TiOF 2 The nanocube and urea scales were taken out and put into two porcelain boats respectively. TiOF 2 The used mass of nanocube is 0.4g, and the mass of urea weighed is 0.25g. Place the two porcelain boats with weighed samples in the middle of the tube furnace one by one, use a vacuum pump to remove the gas in the tube, and then seal the tube furnace. In a sealed state, calcined at 500°C for 10h. After cooling to room temperature, the samples in the porcelain boat were collected to obtain the product.

[0031] refer to figure 2 b. image 3 , the product is characterized by SEM, TEM, XRD as hollow TiO 2 Nano cubic box structure, the size is about 400-500nm. It can be seen through the solid powder ultraviolet-visible absorption spectrum (such as Figure 5 c), the absorption range of the product to visible light is broadened. The signal of N1s in the XPS spectrum is also...

Embodiment 3

[0033] (1)TiOF 2 The preparation of nanocubes is consistent with that of Example 1.

[0034] (2) Sample TiOF 2 The nanocube and urea scales were taken out and put into two porcelain boats respectively. TiOF 2 The mass of the nanocube is 0.4g, and the mass of urea is 0.50g. Place the two porcelain boats with weighed samples in the middle of the tube furnace one by one, use a vacuum pump to remove the gas in the tube, and then seal the tube furnace. In a sealed state, calcined at 600°C for 12h. After cooling to room temperature, the samples in the porcelain boat were collected to obtain the product.

[0035] refer to figure 2 c and image 3 , the product is characterized by SEM, TEM, XRD as hollow TiO 2 Nano cubic box structure, the size is about 400-500nm. It can be seen through the solid powder ultraviolet-visible absorption spectrum (such as Figure 5 d), the absorption range of the product to visible light is broadened, which is wider than the two products with le...

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Abstract

The invention discloses a method for preparing a visible-light-responsive nitrogen-doped TiO2 hollow nano material by adopting a TiOF2 nanocube as a template and urea as a nitrogen source. The TiOF2 nanocube with a cubic structure is obtained by using a solvothermal method. The method comprises the steps that the TiOF2 nanocube powder and different amount of urea are put together in a sealed tubular furnace for heating treatment, NH3 generated from urea decomposition participates in the process that the TiOF2 is heated for decomposition to cause reconstruction of crystal lattices and generate TiO2, so that the N doping is realized; and the products form a hollow cubic box structure, and the surface is formed by TiO2(001) crystal surfaces. According to the method, the doping amount of nitrogen in products can be simply controlled by controlling the use amount of the urea, so that the absorption range and the absorption intensity of the products in a visible-light area can be regulated. The method disclosed by the invention has the advantages that the operation is simple, the applicable reaction temperature is wider, and the use amount and the proportion of the materials can be regulated in a larger range, so that the controllability is good and the universality is very strong.

Description

technical field [0001] The invention relates to a method for preparing visible light-responsive nitrogen-doped titanium dioxide hollow nanomaterials by using titanium oxyfluoride nanocubes as templates. Background technique [0002] The research and development of high-efficiency photocatalytic nanomaterials is an important research direction to develop solar energy utilization and solve the problem of global energy shortage. As we all know, improving the activity of photocatalytic nanomaterials mainly starts from the following three aspects: (1) enhance the separation of photogenerated electrons and holes and inhibit the recombination of excitons; (2) expand the effective specific surface area of ​​photocatalytic materials and increase the photocatalytic surface (3) Improve the absorption efficiency of the photocatalytic material to sunlight. For a long time, structure-controlled synthesis, including morphology control and heterogeneous recombination rich in specific cryst...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J35/00
CPCB01J27/24B01J35/004
Inventor 谢水奋王伟刘凯王媛媛
Owner HUAQIAO UNIVERSITY
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