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Method for titania film growth in fluorine-based aqueous solution

A titanium dioxide, aqueous solution technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of increasing the supersaturation of the solution, unable to control the film orientation, unable to use the growth temperature, etc., to improve the crystallinity and realize the large-scale industry. The effect of less production and raw material consumption

Inactive Publication Date: 2009-05-27
UNIV OF JINAN
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Problems solved by technology

However, this process also has obvious deficiencies: (1) due to the use of F ion trapping agent to greatly increase the supersaturation of the solution, a large amount of precipitation occurs during growth, and the utilization rate of raw materials is low; (2) it is impossible to use a growth temperature higher than 70 ° C temperature, the crystallinity of the film is poor; (3) the orientation of the film cannot be controlled, and the substrate must be modified to improve the crystallinity and crystal orientation

Method used

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  • Method for titania film growth in fluorine-based aqueous solution
  • Method for titania film growth in fluorine-based aqueous solution
  • Method for titania film growth in fluorine-based aqueous solution

Examples

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Embodiment 1

[0032] The seed layer was deposited on the substrate by the sol-gel method. Preparation of the gel: dissolve 0.1M butyl titanate in 50ml of ethanol, stir evenly, add 2ml of acetylacetone, and stir for 2 hours; continue to add 1ml of water and stir A stable and uniform pale yellow sol was obtained after 1 hour.

[0033] The coating method adopts spin coating method. The sol is coated on the cleaned ITO conductive glass substrate at a rotation speed of 3000rpm for 30s. After drying the wet film at 120℃ for 60 minutes, it is transferred to a muffle furnace at 450℃ and kept for 1h. , take out and naturally cool to room temperature to obtain a seed layer with a thickness of 30 nm.

[0034] Place the seed layer in growth solution for growth: formulation containing 0.05M ammonium hexafluorotitanate (AHFT) and 0.05M ammonium fluoride (NHFT) 4 F) growth solutions, stabilized for 2 h and pretreated at 95 °C for 6 h, respectively. The above seeded ITO substrate was placed vertically in...

Embodiment 2

[0039] Other conditions are the same as those in Example 1, except that the substrate is a single crystal silicon substrate and the growth time is 24h. The surface morphology of the obtained titanium dioxide film is similar to that of Example 1, and the cross-sectional morphology is as follows. Figure 5 shown. The thickness of the film is about 700 nm, which is thicker than the 300 nm film grown on ITO, indicating that the film has a relatively uniform growth rate in the growth solution. The density, crystal structure and crystallographic orientation of the films are similar to those grown on ITO.

Embodiment 3

[0041] The other conditions are the same as in Example 1, except that the substrate is ITO and the growth temperature is 75°C. The surface morphology of the obtained titanium dioxide film is similar to that of Example 1, and the cross-sectional morphology is as follows. Figure 6a shown. The thickness of the film is about 300 nm, showing a state of particle orientation accumulation, and the half-width of the (001) diffraction peak of the film in XRD is significantly larger than that of the film obtained at 95 °C, indicating that temperature is the main factor affecting the crystallinity. The better the crystal quality. In addition, using the detection method in Example 1, it was found that under the same conditions, methyl orange was degraded by 40%, which indicated that the crystallinity of the film decreased and the catalytic efficiency decreased.

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Abstract

The invention relates to a method for preparing an anatase titania film with high compactness and high catalytic activity on various matrixes. The method mainly comprises the following steps: firstly, precipitating a titania seed layer with an amorphous form on a matrix; secondly, placing the seed layer in a titanium salt solution which contains a titanium salt stabilizer and has the mol concentration of 0.01 to 0.2mol.L<-1> for growth; and cleaning and drying the grown film to obtain a product. The method improves the compactness of the film and enables the film to have the light transmittance as high as more than 80 percent in the visible light area; and the method also realizes the epitaxial growth of the film in a single c axis direction and greatly improves the crystallinity. In addition, the method adopts a low temperature process and cheap raw material and has little raw material consumption and a simple process, thereby greatly reducing the production cost. The prepared film has potential application prospect in the fields of solar cells, antifog and self-cleaning coating, interference coating, gratings, and microelectronic and electroluminescent devices.

Description

technical field [0001] The invention relates to a method for growing a titanium dioxide film in a fluorine-based aqueous solution, which can grow anatase TiO on various substrates 2 The thin film can increase the density of the titanium dioxide thin film and improve the crystal quality and crystal orientation of the thin film, and belongs to the technical field of preparation methods of semiconductor coating materials. Background technique [0002] Titanium dioxide is a semiconductor material with a wide band gap (3.2 eV), which has good transmittance in the visible light region, and can absorb sunlight in the near-ultraviolet light region and show good photocatalytic activity. In addition, TiO 2 The film material also has excellent acid resistance, alkali corrosion resistance and high mechanical strength, and shows good adaptability in various environments. Therefore, TiO2 thin film materials can be widely used in the fields of photocatalytic degradation, solar cells, opt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/053C03C17/25C04B41/00
Inventor 武卫兵胡广达
Owner UNIV OF JINAN
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