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

A method of preparing an arrayed active film enhancing photocatalysis effects is disclosed. The method includes adding a p-type monocrystalline silicon wafer the specific resistance of which is less than 3.0 [omega].cm into an autoclave, filling the autoclave with a corrosive liquid, corroding to prepare a silicon column array, soaking the silicon column array into an ethanol solution of ferrocene, adding the silicon column array into a horizontal tube furnace, performing in-situ growth of carbon nanotubes through a pre-soaked catalyst for 10 min, cooling to room temperature under nitrogen protection to obtain carbon nanotube / silicon column array, and preparing a TiO2 film on the carbon nanotube / silicon column array by adopting a direct-current reactive magnetron sputtering process. The method reasonably utilizes the template function of a micro / nanometer array of a substrate, and the prepared titanium dioxide film rises and falls along with ups and downs of the surface microstructure of the substrate so that bonding is firm. The substrate is formed by arrayed carbon nanotubes and can allow the contact area of the titanium dioxide deposited to the surface of the substrate with an organic solution to be larger so that the catalytic efficiency is higher.

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
CPCB01J21/185B01J35/004B01J37/342
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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