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Method for preparing black titanium dioxide through auxiliary hydrogenation of hydrogen plasma

A technology of black titanium dioxide and titanium dioxide, which is applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of narrow photoresponse range of titanium dioxide materials, difficulty in industrialization, complex process, etc., achieve remarkable reduction effect, controllable particle size, The effect of high photocatalytic performance

Active Publication Date: 2013-07-24
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still some problems in titanium dioxide photocatalytic materials, which greatly restrict its practical application and promotion. At present, one of the main problems restricting the photocatalytic efficiency of titanium dioxide is the narrow photoresponse range of titanium dioxide materials.
However, the hydrogen reduction method is complicated in process, has unsafe factors such as flammability and explosion, and has disadvantages such as long time consumption and high cost, making it difficult to realize industrialization, which limits the application of this modification method

Method used

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  • Method for preparing black titanium dioxide through auxiliary hydrogenation of hydrogen plasma
  • Method for preparing black titanium dioxide through auxiliary hydrogenation of hydrogen plasma
  • Method for preparing black titanium dioxide through auxiliary hydrogenation of hydrogen plasma

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Use commercial titanium dioxide (P25) as raw material, put it into a closed tube furnace, vacuumize the whole system to 0.1Pa, and then inject H into the system 2 After 10 minutes, exhaust the remaining oxygen in the system. After heating the sample to 500°C, continue to feed hydrogen and adjust the gas flow to keep the system pressure at 100Pa, then turn on the RF power to start the plasma, and slowly increase the power to 200W. After 8 hours of reaction, turn off the radio frequency power supply and the heating power supply in turn, and after the sample cools down, turn off the gas flow.

[0045] TEM images of the treated samples as figure 2 As shown, it can be seen that after the hydrogenation is completed, an amorphous layer with a thickness of about 2 nm is formed on the surface of the sample.

[0046] After hydrogenation treatment, the sample changed from white to black, and the absorption spectrum was as follows: image 3 As shown, the absorption of the sampl...

Embodiment 2

[0052] Titanium dioxide microspheres made by hydrothermal method were used as raw materials (Lü, X.; Ding, S.; Xie, Y.; Huang F.; Eur.J.Inorg.Chem., 2011, 2879-2883), and put into a closed In the tube furnace, after the whole system is evacuated to 0.1Pa, Ar / H is introduced into the system 2 Mixed gas (molar ratio 1:1) for 10 minutes, exhaust the remaining oxygen in the system. After heating the sample to 300°C, continue to feed Ar / H into the system 2 Mix the gas and adjust the gas flow to keep the system pressure at 100Pa, then turn on the RF power to start the plasma, and slowly increase the power to 200W. After 12 hours of reaction, turn off the radio frequency power supply and the heating power supply in turn, and after the sample cools down, turn off the gas flow.

[0053] After hydrogenation treatment, the sample changes from white to black, and the absorption spectrum test shows that the absorption of the treated sample in the visible and infrared regions increases si...

Embodiment 3

[0057] Use commercial titanium dioxide (P25) as raw material, put it into a closed tube furnace, vacuumize the whole system to 0.1Pa, and then inject H into the system 2 After 10 minutes, exhaust the remaining oxygen in the system. After heating the sample to 500°C, continue to feed hydrogen into the system and adjust the gas flow to keep the system pressure at 100Pa, then turn on the RF power to start the plasma, and slowly increase the power to 200W. After 4 hours of reaction, turn off the radio frequency power supply and the heating power supply in turn, and after the sample cools down, turn off the gas flow.

[0058] After hydrogenation treatment, the sample changed from white to black. After the treatment, the absorption of the sample in the visible and infrared regions increased significantly. It can be calculated that the absorption of the sample in the visible region (400-760nm) and infrared region (>760nm) accounted for the entire 22% and 20% of the solar spectrum. ...

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Abstract

The invention relates to a method for preparing black titanium dioxide through auxiliary hydrogenation of hydrogen plasma. The method comprises the following steps of placing the titanium dioxide into a closed system, and vacuum pumping the closed system to ensure the pressure of the closed system to be less than 30Pa; inputting a mixed atmosphere of hydrogen and argon into the closed system; heating the titanium dioxide, and adjusting the mixed atmosphere so as to ensure the pressure in the closed system to be 50 to 500Pa; and starting a radio-frequency power supply to generate the active hydrogen plasma to process the titanium dioxide within a specified time, and utilizing the hydrogen molecules ionized by the radio-frequency power supply to generate the active hydrogen plasma which is used for reducing the titanium dioxide to the black titanium dioxide.

Description

technical field [0001] The invention relates to a method for preparing black titanium dioxide powder and film, in particular to a method for preparing black titanium dioxide powder and film with controllable crystal phase and particle size through hydrogen plasma-assisted hydrogenation. Background technique [0002] With the increasingly severe environmental pollution and energy crisis, solar energy, as the most promising clean energy, has received extensive attention. Titanium dioxide is a semiconductor material with abundant reserves and environmental protection. Since the phenomenon of continuous hydrogen production on the surface of titanium dioxide photoelectrodes was discovered in 1972 (Fujishima, A.; Honda, K.; Nature 238, 37-38), semiconductor photoelectric materials based on titanium dioxide have been Catalytic technology has received great attention and has made great progress. It can be used to degrade organic pollutants, crack water to produce hydrogen, antibacte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/047
Inventor 黄富强汪宙杨重寅林天全尹浩
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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