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Preparation method of Zn-N compound doped titanium dioxide nanotube array membrane with visible light activity

A nanotube array and compound doping technology, which is applied in the field of semiconductor nanomaterial modification, can solve the problems of unfavorable photocatalytic reaction, etc., and achieve the effect of high specific surface area and quantum transmission efficiency, high visible light photocatalytic performance, and simple preparation process

Inactive Publication Date: 2018-10-09
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] For the impregnation method to prepare ion-doped TiO 2 The nanotube array membrane still has some shortcomings. During the heat treatment process, metal ions are easily oxidized by oxygen in the air or dissolved oxygen in the immersion solution to form metal oxides. These metal oxides exist in TiO 2 The surface of nanotubes will become the recombination site of photogenerated electrons and holes, which is unfavorable for photocatalytic reactions

Method used

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  • Preparation method of Zn-N compound doped titanium dioxide nanotube array membrane with visible light activity
  • Preparation method of Zn-N compound doped titanium dioxide nanotube array membrane with visible light activity
  • Preparation method of Zn-N compound doped titanium dioxide nanotube array membrane with visible light activity

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Experimental program
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Effect test

Embodiment 1

[0034] (1) Place the pure titanium plate in HF / HNO 3 / H 2 O (volume ratio 1:4:5) polishing solution for 20 s to remove the dense oxide layer on the surface. Then use ethanol and deionized water to ultrasonically clean them for 15 minutes respectively, take them out and wash them, dry them in the air and store them in a desiccator for later use.

[0035] (2) Configure the electrolyte: the electrolyte is composed of 0.55 wt% NH 4 F, 10 wt% H 2 O and ethylene glycol (the remainder) are mixed.

[0036] (3) Using the electrochemical anodizing method, the cleaned titanium plate was used as the anode, the platinum plate was used as the cathode, and the distance between the two electrodes was 20 mm, and the titanium plate was anodized under a DC voltage of 30 V for 1 h. After the reaction, the prepared samples were cleaned with deionized water and dried naturally.

[0037] (4) With absolute ethanol as solvent and anhydrous zinc chloride as solute, prepare 0.001 M zinc chloride etha...

Embodiment 2

[0040] (1) Place the pure titanium plate in HF / HNO 3 / H 2 O (volume ratio 1:4:5) polishing solution for 20 s to remove the dense oxide layer on the surface. Then use ethanol and deionized water to ultrasonically clean them for 15 minutes respectively, take them out and wash them, dry them in the air and store them in a desiccator for later use.

[0041] (2) Configure the electrolyte: the electrolyte is composed of 0.55 wt% NH 4 F, 20 wt% H 2 O and ethylene glycol (the remainder) are mixed.

[0042] (3) Using the electrochemical anodizing method, the cleaned titanium plate was used as the anode and the platinum plate was used as the cathode, with a distance of 30 mm between the two electrodes, and the titanium plate was anodized under a DC voltage of 40 V for 2 h. After the reaction, the prepared samples were cleaned with deionized water and dried naturally.

[0043] (4) With absolute ethanol as solvent and anhydrous zinc chloride as solute, prepare 0.003 M zinc chloride e...

Embodiment 3

[0046] (1) Place the pure titanium plate in HF / HNO 3 / H 2 O (volume ratio 1:4:5) polishing solution for 20 s to remove the dense oxide layer on the surface. Then use ethanol and deionized water to ultrasonically clean them for 15 minutes respectively, take them out and wash them, dry them in the air and store them in a desiccator for later use.

[0047] (2) Configure the electrolyte: the electrolyte is composed of 0.55 wt% NH 4 F, 30 wt% H 2 O and ethylene glycol (the remainder) are mixed.

[0048] (3) Using the electrochemical anodizing method, the cleaned titanium plate is used as the anode, the platinum plate is used as the cathode, and the distance between the two electrodes is 40 mm, and the titanium plate is anodized under a DC voltage of 40 V for 3 h. After the reaction, the prepared samples were cleaned with deionized water and dried naturally.

[0049] (4) With absolute ethanol as solvent and anhydrous zinc chloride as solute, prepare 0.01 M zinc chloride ethanol...

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Abstract

The invention discloses a preparation method of a Zn-N compound doped titanium dioxide nanotube array membrane with visible light activity. According to the method, a pure titanium plate is utilized as a substrate, electrochemical anodizing technology is utilized, the pure titanium plate is utilized as a positive electrode, a platinum plate is utilized as a negative electrode, electrolyte is a mixed solution of NH4F, ethylene glycol and deionized water, anodizing is performed under 20V to 50V direct-current voltage, and the pure titanium plate and the platinum plate are taken out and naturallydried after the reaction finishes; a sample is immersed into a zinc chloride ethanol solution and taken out to be blown and dried; the dried sample is put into a tubular furnace, and the dried sampleis cooled after being calcined to obtain the Zn-N compound doped titanium dioxide nanotube array membrane. By means of the preparation method, zinc and nitrogen can be doped into titanium dioxide lattice at the same time, the side effects caused by zinc ions which are oxidized into metal oxide are overcome, forbidden bandwidth of prepared TiO2 is reduced, and visible light absorption capacity ofthe prepared TiO2 is enhanced. Furthermore, compared with the prior art, the preparation method disclosed by the invention has the advantages of simpleness in operation, low cost, high modifying effect, good industrial application prospect and the like.

Description

technical field [0001] The invention belongs to the technical field of modification of semiconductor nanometer materials, and in particular relates to a preparation method of a Zn-N composite doped titanium dioxide nanotube array film with visible light activity. Background technique [0002] The highly ordered titanium dioxide nanotube array film prepared by electrochemical anodic oxidation has become a popular technology at home and abroad in recent years due to its advantages of high specific surface area, fast carrier transfer rate, high photocatalytic activity, simple preparation and environmental friendliness. One of the hotspots of research. However, TiO 2 The semiconductor has a wide forbidden band (3.2 eV), which can only absorb the ultraviolet light band with a wavelength less than 387.5nm, and the visible light part, which accounts for the vast majority of the solar spectrum, has not been effectively utilized, which greatly limits the ability of TiO 2 practical ...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J37/02B01J37/34C25D11/26B82Y30/00B82Y40/00
CPCC25D11/26B82Y30/00B82Y40/00B01J27/24B01J37/0201B01J37/348B01J35/39
Inventor 陈小泉宋树芳沈文浩
Owner SOUTH CHINA UNIV OF TECH
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