PREPARATION METHOD OF FLUORINE-DOPED LAMELLAR BLACK TITANIUM DIOXIDE NANO MATERIAL

Abstract

The method for preparing fluorine-doped lamellar black TiO.sub.2 nanomaterials includes mixing a solution of tetra-n-butyl titanate, n-propanol and hydrofluoric acid together, and then stir the solutions for a period of time. The solution is transferred into an autoclave and reacts at a certain temperature for a period of time. The sample obtained by the reaction is washed and dried. Then, the sample is heated in a protective atmosphere for a period of time so as to produce the fluorine-doped lamellar black TiO.sub.2 nanomaterials. This fluorine-doped lamellar black TiO.sub.2 owns superior optical absorption and electron transport performances.

Claims

1. A method for preparing a fluorine-doped lamellar black TiO.sub.2 nanomaterials, the method comprising the steps of: (1) adding 2030 mL of n-propanol into a beaker, then adding 13 mL of tetrabutyl titanate, and stir it well; (2) adding 0.20.8 mL of hydrofluoric acid into the solution prepared in (1), and then stir it for 1 to 3 hours; (3) transfering the solution prepared in (2) to an autoclave, and leaving the solution to have hydrothermal reaction at 160200 C. for 1224 hours; (4) washing the precipitate obtained after reaction in (3) with deionized water and ethanol, until the filtrate is neutral, and then drying the precipitate; (5) calcining the sample obtained in (4) at 400450 C. in a protective atmosphere for a period of time to obtain the fluorine-doped lamellar black TiO.sub.2 nanomaterials.

2. The method for preparing a fluorine-doped lamellar black TiO.sub.2 nanomaterials as claimed in claim 1, wherein the n-propanol added in Step (1) is 2030 mL, with tetra-n-butyl titanate of 13 mL.

3. The method for preparing a fluorine-doped lamellar black TiO.sub.2 nanomaterials as claimed in claim 1, wherein the hydrofluoric acid added in Step (2) is 0.20.8 mL, with the stirring time of 13 hours.

4. The method for preparing a fluorine-doped lamellar black TiO.sub.2 nanomaterials as claimed in claim 1, wherein reaction temperature of the solution in the autoclave obtained in Step (3) is 160200 C., with the reaction time of 1224 hours.

5. The method for preparing a fluorine-doped lamellar black TiO.sub.2 nanomaterials as claimed in claim 1, wherein the drying temperature for the sample obtained in Step (4) is 5060 C., with drying time of 1220 hours.

6. The method for preparing a fluorine-doped lamellar black TiO.sub.2 nanomaterials as claimed in claim 1, wherein the protective atmosphere used in Step (5) comprises a gas mixture of argon and hydrogen, with the calcination time of 24 hours.

Description

BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS

[0022] FIG. 1 is a contrast diagram of the absorption spectra between a fluorine-doped lamellar black TiO.sub.2 nanomaterials prepared in Embodiment 1 of the present invention and the commercial P25 nanoparticles.

[0023] FIG. 2 is a scanning electron microscope (SEM) image of the fluorine-doped lamellar black TiO.sub.2 nanomaterials prepared in Embodiment 1 of the present invention.

[0024] FIG. 3 is a contrast diagram of F1s signal in x-ray photo electron spectroscopy (XPS) between the fluorine-doped lamellar black TiO.sub.2 nanomaterials prepared in Embodiment 1 of the present invention and the commercial P25 nanoparticles.

DETAILED DESCRIPTION OF THE INVENTION

[0025] A method for preparing a pinecone-shaped TiO.sub.2 nanomaterial provided by the present invention can be implemented as below, and the specific preparing method includes the following steps:

Embodiment 1

[0026] (1) add 25 mL of n-propanol into a beaker, then add 2 mL of tetrabutyl titanate, and stir it well;

[0027] (2) add 0.4 mL of hydrofluoric acid into the solution, and then stir it for 2 hours;

[0028] (3) transfer the solution prepared to an autoclave, and leave it to have hydrothermal reaction at 180 C. for 18 hours;

[0029] (4) wash the precipitate obtained after reaction with deionized water and ethanol, until the filtrate is neutral, and then dry it;

[0030] (5) calcine the sample obtained at 430 C. in a protective atmosphere to obtain the fluorine-doped lamellar black TiO.sub.2 nanomaterials.

Embodiment 2

[0031] (1) add 20 mL of n-propanol into a beaker, then add 1 mL of tetrabutyl titanate, and stir it well;

[0032] (2) add 0.15 mL of hydrofluoric acid into the solution, and then stir it for 1 hour;

[0033] (3) transfer the solution prepared to an autoclave, and leave it to have hydrothermal reaction at 180 C. for 15 hours;

[0034] (4) wash the precipitate obtained after reaction with deionized water and ethanol, until the filtrate is neutral, and then dry it;

[0035] (5) calcine the sample obtained at 450 C. in a protective atmosphere to obtain the fluorine-doped lamellar black TiO.sub.2 nanomaterials.