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Preparation method of nitrogen (N)-doped titanium dioxide (TiO2) microspheres

A technology of titanium dioxide and microspheres, which is applied in the field of preparation of TiO2 microspheres, can solve the problems of expensive raw materials and reduce raw material costs, and achieve the effects of low cost, good stability and wide application prospects

Inactive Publication Date: 2012-06-27
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Yu, H.K. et al. (see Yu, H.K Chemistry of Materials, 2008. 20(8): p. 2704-2710.) used Tween 20 and Pluronic P123 as surfactants to prepare microspheres with controllable particle size, but the raw material cost It is relatively expensive, so reducing the cost of raw materials is also a big problem

Method used

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  • Preparation method of nitrogen (N)-doped titanium dioxide (TiO2) microspheres
  • Preparation method of nitrogen (N)-doped titanium dioxide (TiO2) microspheres
  • Preparation method of nitrogen (N)-doped titanium dioxide (TiO2) microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Embodiment 1 The mol ratio of hydrochloric acid and tetrabutyl titanate is respectively the TiO when 2:1 2 Microspheres

[0015] Pour the mixture of hydrochloric acid and tetrabutyl titanate with a molar ratio of 2:1 into the mixture of urea, ethanol and water and stir for 2-5 hours. The ratio of ethanol, water and urea is 130:0:1.7. The mixed solution is transferred to a pressure melting bomb and kept at 80-160° C. for 2-10 hours. The bottom precipitate was collected and calcined at 400° C. for 2 hours to obtain N-doped titanium dioxide microspheres. like figure 1 As shown, when M (HCl) :M (TBT) When it is 2:1, most of them are spherical, but there is still a considerable part of TiO 2 powder, and the dispersibility of microspheres is relatively poor.

Embodiment 2

[0016] Embodiment 2 The mol ratio of hydrochloric acid and tetrabutyl titanate is respectively the TiO when 2.6:1 2 Microspheres

[0017] Pour the mixture of hydrochloric acid and tetrabutyl titanate with a molar ratio of 2.6:1 into the mixture of urea, ethanol and water and stir for 2-5 hours. The ratio of ethanol, water and urea is 130:0:1.7. The mixed solution is transferred to a pressure melting bomb and kept at 80-160° C. for 2-10 hours. The bottom precipitate was collected and calcined at 400° C. for 2 hours to obtain N-doped titanium dioxide microspheres. When M (HCl) :M (TBT) is 2.6:1 when ( figure 2 ) to get microspheres with good dispersion, but there is still a part of TiO 2 powder. Comparative Observation of Nitrogen-doped TiO by UV-Vis Absorption Spectroscopy 2 Changes in the spectral response of microspheres and P25 titanium dioxide powder (eg Image 6 Shown), it was found that the absorption intensity of nitrogen-doped microspheres exceeded P25 b...

Embodiment 3

[0018] Embodiment 3 The mol ratio of hydrochloric acid and tetrabutyl titanate is respectively the TiO when 3.3:1 2 Microspheres

[0019] Pour the mixture of hydrochloric acid and tetrabutyl titanate with a molar ratio of 3.3:1 into the mixture of urea, ethanol and water and stir for 2-5 hours. The ratio of ethanol, water and urea is 130:0:1.7. The mixed solution is transferred to a pressure melting bomb and kept at 80-160° C. for 2-10 hours. The bottom precipitate was collected and calcined at 400° C. for 2 hours to obtain N-doped titanium dioxide microspheres. like image 3 Shown when M (HCl) :M (TBT) When it is 3.3:1, it basically forms a ball, and the particle size is relatively reduced, and the dispersion and uniformity are also improved.

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Abstract

The invention discloses a preparation method of nitrogen (N)-doped titanium dioxide (TiO2) microspheres. In the invention, urea is used as a nitrogen source, hydrochloric acid is used as a protecting agent of butyl titanate (TBT), and a solvent heat method (ethanol and water mixing liquid is used as a solvent) is adopted for synthesizing the N-doped TiO2 microspheres. According to the method, TiO2 microspheres with good appearance can be prepared, and in addition, nitrogen elements in the urea is utilized for nitrogen doping, so the visible light absorption of the TiO2 microspheres is obviously improved. The method simultaneously realizes the microsphere preparation and the N doping, the preparation process is simple, the cost is low, and in addition, the application range is wide. The preparation method can be used in the fields of catalysis, dye solar cells, and the like.

Description

technical field [0001] The present invention relates to TiO 2 The technical field of preparation of microspheres, in particular to a kind of N-doped TiO 2 Preparation method of microspheres. Background technique [0002] TiO 2 It is an important inorganic material with unique physical and chemical properties such as large specific surface area, high surface activity, good thermal conductivity, good light absorption performance and good dispersion. It is widely used in photocatalysts, solar cells, gas sensors, etc. field. TiO 2 The forbidden band width is 3.2eV (anatase type), the absorption wavelength is less than 388nm, and the absorption band is limited to the ultraviolet region, which means that TiO 2 Only a small amount of sunlight (3~5%) can be used, but visible light (about 45%), which accounts for the majority of sunlight, cannot be used. In order to expand the absorption in the visible light region and further improve the performance of nanomaterials (see Burda...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02
Inventor 孙小华周生刚李修能侯爽罗志猛
Owner CHINA THREE GORGES UNIV
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