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A method of preparation of the array -based activated film that enhances the light catalytic effect

A photocatalytic and thin-film technology, which is applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc. It can solve problems such as poor bonding between the film and the substrate, small active specific surface area of ​​the film, and complex preparation process. , to achieve enhanced photocatalytic performance, stable photocatalytic activity, and simple preparation process

Active Publication Date: 2018-02-27
太湖县市场监督检验所(太湖县功能膜检测研究院)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing titanium oxide film preparation technology still has disadvantages such as complex preparation process, low crystallinity, small active specific surface area of ​​the film, and poor bonding firmness between the film and the substrate.

Method used

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  • A method of preparation of the array -based activated film that enhances the light catalytic effect
  • A method of preparation of the array -based activated film that enhances the light catalytic effect
  • A method of preparation of the array -based activated film that enhances the light catalytic effect

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Experimental program
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Effect test

Embodiment 1

[0026] The preparation method of the arrayed active film with strong photocatalytic effect in this embodiment, the steps are as follows:

[0027] (1) A P-type monocrystalline silicon wafer with a resistivity of 0.015 Ω cm (the sample size is 2.5×2.5 cm 2 ) into the autoclave, and then fill the autoclave with corrosion solution, the corrosion solution is composed of hydrofluoric acid with a concentration of 8.00 mol / l and an aqueous ferric nitrate solution with a concentration of 0.08 mol / l, the solution in the autoclave The volume filling degree is 90%, and it is etched at 140°C for 35 minutes to prepare the substrate material silicon pillar array (Si-NPA). The scanning electron microscope shows figure 1 shown;

[0028] (2) Soak the silicon pillar array (Si-NPA) freshly prepared in step (1) in 0.002 mol / L ferrocene ethanol solution for 30 minutes, then place it in a horizontal tube furnace, and raise the temperature to The temperature was 760°C, and then ethylenediamine was ...

Embodiment 2

[0031] The preparation method of the arrayed active film with strong photocatalytic effect in this embodiment, the steps are as follows:

[0032] (1) A P-type monocrystalline silicon wafer with a resistivity of 0.03 Ωcm (the sample size is 2.5×2.5 cm 2 ) into the autoclave, and then fill the autoclave with corrosion solution. The corrosion solution is composed of hydrofluoric acid with a concentration of 8.00mol / l and an aqueous ferric nitrate solution with a concentration of 0.08 mol / l. The solution in the autoclave The volume filling degree is 90%, etched at 100°C for 40 min, and the substrate silicon pillar array (Si-NPA) is prepared;

[0033](2) Soak the silicon pillar array (Si-NPA) freshly prepared in step (1) in 0.002 mol / L ferrocene ethanol solution for 20 min, then place it in a horizontal tube furnace, nitrogen (60 sccm ) was heated to 800 °C under the protection of nitrogen gas, and then ethylenediamine was brought into the furnace at a rate of 1.5 mL / min to grow c...

Embodiment 3

[0036] The preparation method of the arrayed active film with strong photocatalytic effect in this embodiment, the steps are as follows:

[0037] (1) A P-type monocrystalline silicon wafer with a resistivity of 0.03 Ωcm (the sample size is 2.5×2.5 cm 2 ) into the autoclave, and then fill the autoclave with corrosion solution. The corrosion solution is composed of hydrofluoric acid with a concentration of 15.00mol / l and an aqueous ferric nitrate solution with a concentration of 0.02mol / l. The solution in the autoclave The volume filling degree is 90%, etched at 200°C for 30 min, and the substrate silicon pillar array (Si-NPA) is prepared;

[0038] (2) Soak the freshly prepared silicon pillar array (Si-NPA) in step (1) in 0.002 mol / L ferrocene ethanol solution for 25 min, then place it in a horizontal tube furnace, nitrogen (60 sccm ) to 780°C under the protection of nitrogen gas, then bring ethylenediamine into the furnace at 1.2 mL / min to grow carbon nanotubes in situ at 780°...

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Abstract

The invention discloses a method for preparing an arrayed active film that enhances the photocatalytic effect. A P-type single crystal silicon wafer with a resistivity less than 3.0Ω·cm is placed in an autoclave, and then the autoclave is filled with etching liquid to corrode Finally, a silicon pillar array is prepared; the silicon pillar array is infiltrated into an ethanol solution of ferrocene, and then placed in a horizontal tube furnace. The carbon nanotubes are grown in situ through the pre-infiltration catalyst for 10 minutes, and then cooled to room temperature under nitrogen protection. A carbon nanotube / silicon pillar array was obtained; a TiO2 film was prepared on the carbon nanotube / silicon pillar array using DC reactive magnetron sputtering. The invention makes reasonable use of the template function of the micro / nano array of the substrate. The titanium dioxide film produced fluctuates with the fluctuation of the microstructure on the surface of the substrate, and is firmly bonded. At the same time, the substrate is composed of arrayed carbon nanotubes, which can make its surface The deposited titanium dioxide has a larger area exposed to the organic solution, so the catalytic efficiency is high.

Description

technical field [0001] The invention belongs to the technical field of semiconductor photocatalyst preparation, and specifically relates to a titanium dioxide / carbon nanotube / silicon column array photocatalytic composite film with an array structure, and also relates to a preparation method and application thereof. Background technique [0002] While the rapid development of science and technology has brought people rich material life, it has also led to increasingly serious environmental pollution problems. Although there have been many methods to deal with pollution problems in actual production and application, due to their own limitations, there is still no practical application for some toxic and refractory biochemical wastewater, such as the sewage discharged by pesticide, pharmaceutical, paper and dye enterprises. effective technical methods. Semiconductor photocatalysis technology can solve this problem. [0003] Because photocatalytic materials can directly use su...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J21/18
CPCB01J21/185B01J37/342B01J35/39
Inventor 袁沛文杨晓辉姜卫粉贾敏张巧丽
Owner 太湖县市场监督检验所(太湖县功能膜检测研究院)
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