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Preparation method of rutile type boron-doped titania (B-TiO2) microsphere with exposed high energy crystal face {001}

A rutile type, titanium boride technology, applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve the problems of poor dispersion of doping elements, uneven stress, limited and other problems, Achieve the effect of avoiding the influence of morphology and stability, uniform size, and controllable doping amount

Inactive Publication Date: 2014-03-26
ZHANJIANG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the energy band gap of TiO2 is 3.2 eV, and only ultraviolet light with a wavelength below 380 nm can excite the transition of valence band electrons, while the ultraviolet light in the solar spectrum is less than 5%, and the wavelength is 400 nm. Visible light at -750 nm accounts for about 45%, which fundamentally restricts the practical application of TiO2 photocatalysts
However, the doping amount of B in this method is limited in the titanium dioxide lattice. Due to the excessive doping of B ions, B2O3 will be precipitated from the inside of the titanium dioxide crystal.
The mechano-chemical method has also been reported. Although the preparation process of the mechano-chemical method is simple, the particle size distribution of the product and the degree of dispersion of doping elements are not good due to uneven force.

Method used

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  • Preparation method of rutile type boron-doped titania (B-TiO2) microsphere with exposed high energy crystal face {001}
  • Preparation method of rutile type boron-doped titania (B-TiO2) microsphere with exposed high energy crystal face {001}
  • Preparation method of rutile type boron-doped titania (B-TiO2) microsphere with exposed high energy crystal face {001}

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Experimental program
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Effect test

Embodiment 1

[0029] Add 500 mg of titanium boride (TiB, 99%) to 70 ml of hydrochloric acid solution containing 0.015 mol / L sodium fluoride in a 250 ml beaker, where the concentration of hydrochloric acid is 1.0 mol / L, stir vigorously for 30 min, then Transfer to a 100 ml lined tetrapolyethylene hydrothermal reaction kettle, put it into a constant temperature drying oven at 200 °C, and keep the reaction for 24 h under solvothermal conditions. After the reaction, it was naturally cooled to room temperature, washed three times with distilled water and absolute ethanol, and the product was vacuum-dried in a drying oven at 70 °C for 12 h. B-TiO prepared by this step 2 The diameter of the microspheres is about 3 μm.

Embodiment 2

[0031]Add 1000 mg of titanium boride (TiB, 99%) to 70 ml of hydrochloric acid solution containing 0.015 mol / L sodium fluoride in a 250 ml beaker, where the concentration of hydrochloric acid is 1.5 mol / L, stir vigorously for 15 min, then Transfer to a 100 ml lined tetrapolyethylene hydrothermal reaction kettle, put it into a constant temperature drying oven at 200 °C, and keep the reaction for 18 h under solvothermal conditions. After the reaction, it was naturally cooled to room temperature, washed three times with distilled water and absolute ethanol, and the product was vacuum-dried in a drying oven at 80 °C for 12 h. B-TiO prepared by this step 2 The diameter of the microspheres is about 3.8 μm.

Embodiment 3

[0033] Add 800 mg of titanium boride (TiB, 99%) to 70 ml of hydrochloric acid solution containing 0.015 mol / L sodium fluoride in a 250 ml beaker, where the concentration of hydrochloric acid is 2.0 mol / L, stir vigorously for 40 min, then Transfer to a 100 ml lined PTFE hydrothermal reaction kettle, put it into a constant temperature drying oven at 200 °C, and keep the reaction for 20 h under solvothermal conditions. After the reaction, it was naturally cooled to room temperature, washed three times with distilled water and absolute ethanol, and the product was vacuum-dried in a drying oven at 75 °C for 18 h. B-TiO prepared by this step 2 The diameter of the microspheres is about 4.2 μm.

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Abstract

The invention provides a preparation method of a rutile type boron-doped titania (B-TiO2) microsphere with an exposed high energy crystal face {001} and belongs to the technical field of the preparation of inorganic material. The preparation method comprises the following specific steps: adding titanium boride (TiB) into a hydrochloric acid solution hydrazine containing natrium fluoride (NaF) to obtain a mixed solution, forcefully agitating, then transferring the mixed solution to a reactor with a polytetrafluoroethene lining, keeping the mixed solution at a constant temperature of 200 DEG C for 12-24 hours, naturally cooling the mixed solution to the room temperature so as to obtain a product, filtering the product, respectively washing and settling the product with distilled water and absolute ethyl alcohol for three times, drying the product at a temperature of 60-80 DEG C for 12-24 hours, and finally preparing the B-TiO2 microsphere with the exposed high energy crystal face {001}, of which exposing rate nearly reaches 100 percent. The preparation method is simple in preparation technology and good in repeatability; the prepared B-TiO2 microsphere is controllable and uniform in size and has a diameter of 3-5 micron; the element boron is doped, and is uniform in distribution and controllable in the amount of dopping; in addition, the prepared B-TiO2 microphere has excellent visible light catalytic activity, and is likely to be widely applied in the fields of photolytic water hydrogen preparation, organic contaminant degradation and the like.

Description

technical field [0001] The invention relates to a method for preparing titanium dioxide microspheres, in particular to a method for preparing exposed high-energy crystal plane {001} rutile boron-doped titanium dioxide microspheres, and belongs to the technical field of inorganic material preparation. Background technique [0002] Environmental pollution and energy crisis are two major problems that plague the economic development of the world today. The extensive use of fossil fuels not only causes huge pollution to the global environment and ecology, but also these energy sources are non-renewable resources, and the global storage content is estimated to reach the middle of this century. is about to dry up. Therefore, how to solve the problem of environmental pollution is imminent. Since the discovery of TiO by Honda and Fujishima in 1972 2 Since the single crystal electrode has a certain redox performance under the action of light, scientists have proposed an efficient a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/06B01J35/08
Inventor 周小松金蓓
Owner ZHANJIANG NORMAL UNIV
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