Method for preparing black titanium dioxide by contact type reduction method

A black titanium dioxide, titanium dioxide technology, applied in chemical instruments and methods, catalyst activation/preparation, chemical/physical processes, etc., can solve the problems of difficult to achieve industrialization, high equipment investment costs, complex process conditions, etc. Low requirements and good photocatalytic performance

Active Publication Date: 2015-09-30
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the high-temperature hydrogen reduction method has high process requirements, unsafe factors such as flammability and explosion, and is time-consuming and high-cost; while the hydrogen plasma reduction method has disadvantages such as high equipment investment cost, high energy consumption, and complicated process conditions, it is difficult to The realization of industrialization limits the application of these two modification methods

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  • Method for preparing black titanium dioxide by contact type reduction method
  • Method for preparing black titanium dioxide by contact type reduction method
  • Method for preparing black titanium dioxide by contact type reduction method

Examples

Experimental program
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Effect test

Embodiment 1

[0057] Commercial titanium dioxide (Degussa P25TiO 2 ) as the raw material, calcium hydride as a highly active reducing agent, mixed and ground into the quartz tube, vacuumed to make the pressure inside the quartz tube less than 100Pa, sealed the quartz tube, and put it in a furnace at 400°C for 5 hours, then turned off the heating power, and waited The samples were taken out after cooling naturally in the furnace. The obtained powder was added into 1mol / L hydrochloric acid solution and stirred and pickled for 6 hours to remove residual calcium hydride and calcium oxide, then washed with deionized water until neutral, filtered, and baked at 80°C for 12 hours to obtain black nano titanium dioxide.

[0058] After reduction treatment, the sample turns from white to black, and the absorption spectrum is as follows: figure 2 As shown, the absorption of the treated sample in the visible and infrared regions increased significantly, indicating that the photoresponse range of the sa...

Embodiment 2

[0063] Titanium dioxide nanowires made by hydrothermal method as raw materials (Yin, H.; Ding, G.Q.; Gao, B.; Huang, F.Q.; Xie, X.M.; Jiang, M.H., Mater Res Bull2012, 47(11), 3124-3128 .), metal aluminum is a highly active reducing agent, put it into a quartz tube after mixing and grinding, vacuumize the pressure inside the quartz tube to 50Pa, seal the quartz tube, and put it in a furnace at 700°C for 8 hours, then turn off the heating power, and wait for the sample Take it out after cooling naturally with the furnace. The obtained powder was added into 1 mol / L hydrochloric acid solution and stirred and pickled for 6 hours to remove residual metal aluminum and produced alumina, then washed with deionized water until neutral, filtered, and baked at 80°C for 12 hours to obtain black titanium dioxide nanowires.

[0064] After the reduction treatment, the sample changed from white to black, and the absorption spectrum test showed that the absorption of the treated sample in the v...

Embodiment 3

[0068] The titanium dioxide nanowire array made by anodic oxidation is used as the raw material, and sodium borohydride is used as a highly active reducing agent. The nanowire array is buried in sodium borohydride powder, put into a quartz tube, and the pressure inside the quartz tube is evacuated to 10Pa, and the quartz tube is sealed. dead, and placed in a furnace at 200°C for 72 hours to react, then turn off the heating power, and take out the sample after cooling naturally with the furnace. The surface powder is blown off to obtain a black titanium dioxide nanowire array.

[0069] After the reduction treatment, the sample changed from khaki to black, and the absorption spectrum test showed that the absorption of the treated sample in the visible and infrared regions increased significantly; it showed that the photoresponse range of the sample after the reduction treatment was greatly broadened, and there were high levels in the visible and infrared regions. Absorption.

...

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Abstract

The invention relates to a method for preparing black titanium dioxide by a contact type reduction method. The method comprises preparation by a solid and liquid contact type reduction method. A method provided by the invention comprises the following steps: in a negative-pressure or inert atmosphere, heating a mixed material of reducing agents and titanium dioxide to 200-800 DEG C, keeping the stipulated time, reducing titanium dioxide to obtain black titanium dioxide, wherein the reducing agents are metal oxide, metal hydroboron, and/or high-activity metal. Another method provided by the invention comprises the following steps: dispersing titanium dioxide into water, adding reducing agents into water with dispersed titanium dioxide, stirring for the stipulated time, and reducing so as to obtain black titanium dioxide, wherein the reducing agents are metal hydride, metal hydroboron, and/or high-activity metal. Titanium dioxide prepared by the invention has wide application prospect in the fields of dye-sensitized solar cells, hydrogen generation by water photolysis, and the like.

Description

technical field [0001] The invention relates to a method for preparing black titanium dioxide, in particular to a method for preparing black titanium dioxide powder and film with controllable crystal phase and particle size by a contact reduction method. Background technique [0002] Energy shortage and environmental pollution have become the hot issues of human development in the 21st century and have attracted widespread attention around the world. Solar energy is clean and abundant, and it is the most promising clean energy. If solar energy can be fully and rationally utilized, energy and environmental problems will be greatly alleviated, and fully and rationally utilizing solar energy is an ideal way to solve current energy shortages and environmental pollution. Therefore, titanium dioxide, as a semiconductor material with abundant reserves and stable environmental protection, has broad application prospects in photoelectric conversion, photothermal conversion, photocat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/06B01J37/16
Inventor 黄富强尹浩单玉凤于刘涛张阳
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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