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Preparation method and use of visible light responsive nitrogen-doped titanium dioxide nano-tube

A titanium dioxide, nanotube technology, applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve problems such as tubular structure damage, achieve complete tubular structure, excellent stability and visible light response performance, The effect of high crystallinity

Active Publication Date: 2010-07-14
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

Ghicov et al prepared TiO by anodic template method 2 nanotube arrays, followed by ion implantation to prepare TiO 2-X N X Nanotube arrays with photocurrent ratios of TiO 2 Nanotube arrays are 8 times higher, but their synthesis method requires special equipment (A.Ghicov, J.M.Macak, H.Tsuchiya, J.Kunze, V.Haeublein, L.Frey, P.Schmuki, NanoLetters, 2006, 6 , (5), 1080-1082.), and the nanotube is a mixed phase with a large diameter (~100nm)
Recently, Y.Wang et al. 2 Nanotubes were used as titanium source, and TiO was prepared by high-temperature ammonium solution 2-X N X nanotubes, but the tubular structure of the resulting material is severely damaged, and the transmission electron microscope photos show that the product is a fractured nanorod (Yan Wang, Caixia Feng, Zhensheng Jin, Jiwei Zhang, Jianjun Yang and Shunli Zhang, Journal of Molecular Catalysis A: Chemical, 2006, 260(1-2):1-3)

Method used

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  • Preparation method and use of visible light responsive nitrogen-doped titanium dioxide nano-tube

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Experimental program
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Effect test

Embodiment 1

[0032] Weigh 3.2 grams of commercial anatase TiO 2 , added to 75mL of 10M NaOH solution, stirred vigorously for 30 minutes, then transferred to a 100mL Teflon-lined autoclave, and treated at 160°C for 24 hours, the resulting white precipitate was washed with deionized water Wash with 0.2M hydrochloric acid to neutralize, and obtain metatitanic acid nanotubes. The newly prepared metatitanic acid nanotubes were dispersed in ammonia water, ultrasonically treated for 20 minutes, then moved into a 100mL Teflon-lined autoclave with a filling degree of 80%, treated at 120°C for 12 hours, and the product was taken out After suction filtration and water washing, the obtained white precipitate was dried at 60°C, then dried at 120°C, and finally roasted at 250-600°C for 2 hours to obtain a series of light yellow TiO 2-X N X nanotube product. XRD (X-ray), FESEM (Field Emission Scanning Electron Microscope) and TEM (Transmission Electron Microscope) showed that it was anatase phase TiO ...

Embodiment 2

[0035] Weigh 3.2 grams of commercial anatase TiO 2 , added to 75mL of 10M NaOH solution, stirred vigorously for 30 minutes, then transferred to a 100mL Teflon-lined autoclave, and treated at 160°C for 24 hours, the resulting white precipitate was washed with deionized water Wash with 0.2M hydrochloric acid to neutralize, and obtain metatitanic acid nanotubes. Disperse the new metatitanic acid nanotubes in the water / alcohol mixed solution of 20% ammonium chloride by weight fraction, stir for 7 hours, move into the autoclave of the polytetrafluoroethylene lining of 100mL volume, and the filling degree is 80%, treated at 120°C for 3 hours, a yellow precipitate was obtained, the product was taken out, filtered, washed with water, dried at 60°C, and then dried at 120°C to obtain a series of light yellow TiO 2-X N X nanotube product. XRD, FESEM and TEM showed that it was anatase phase TiO 2-X N X nanotube. The nanotubes can be further roasted at 250-1000°C under an inert atmos...

Embodiment 3

[0038] Weigh 4 grams of commercial metatitanic acid nanotubes, disperse them in hydrazine hydrate, stir for 4 hours, move into a 100mL Teflon-lined autoclave with a filling degree of 80%, and treat them at 120°C for 12 hours, the product After being taken out, filtered and washed with water, the obtained white precipitate was dried at 60°C, then dried at 120°C, and finally roasted at 250-450°C for 2 hours to obtain a series of light yellow TiO 2-X N X nanotube product. XRD, FESEM and TEM showed that it was anatase phase TiO 2-X N X nanotube. Among them, the specific surface area of ​​the sample calcined at 250°C for 2 hours is 300m 2 / g, the specific surface area of ​​the sample calcined at 450°C for 2 hours is 140m 2 / g.

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Abstract

The invention discloses a preparation method of a nitrogen-doped titanium dioxide nanotube with response to visible lights, and comprises the following steps: a. metallic titanium or titaniferous compounds are used for preparing a metatitanic acid nanotube with a hydrothermal or solvothermal method; b. the metatitanic acid or titanium dioxide nanotube that is prepared by step a or a commercial metatitanic acid or titanium dioxide nanotube is dispersed in a water solution with nitrogen sources or a water and alcohol mixed solution, and agitated or ultrasonically processed for 10 minutes to 10 hours; c. serum that is obtained by step b is placed into a reaction kettle with polyfluortetraethylene lining and processed by sealed heating for 10 minutes to 10 days, and the reaction temperature is 50 to 350 DEG C; and d. the product obtained by step c is washed by deionized water, dried and baked, thus obtaining the nitrogen-doped titanium dioxide nanotube. The preparation method of the nitrogen-doped titanium dioxide nanotube of the invention has simplicity, cleanness and environmental protection, is applicable to batch preparation, and has low cost and strong adaptability, wide application of the prepared nitrogen-doped titanium dioxide nanotube.

Description

technical field [0001] The invention relates to a method for preparing titanium dioxide nanotubes, in particular to a method for preparing visible light-responsive nitrogen-doped titanium dioxide nanotubes, and also relates to the application of the titanium dioxide nanotubes prepared by the method. Background technique [0002] Titanium dioxide (TiO 2 ) is non-toxic, harmless, resistant to acid and alkali corrosion, has good absorption of ultraviolet light and photocatalytic activity of ultraviolet light, so TiO powder, film and monolithic etc. 2 Materials have been widely used and researched in the storage and utilization of solar energy, photoelectric conversion, photochromism, deodorization, sterilization, mildew resistance, self-cleaning and photocatalytic degradation of pollutants in the atmosphere and water. TiO 2 The optoelectronic and catalytic properties of sap mainly depend on its crystal form, size and semiconductor band gap energy (Band gap, Eg). Natural or s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J21/06
Inventor 蒋政朱庆山杨帆张涯远李洪钟
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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