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Rapid preparation method of three-dimensional ordered macroporous titanium dioxide

A titanium dioxide, three-dimensional ordering technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve problems such as incomplete filling, clogged pores on the surface of materials, and problems with the regularity of material morphology, achieving shortened time and simple structure effective effect

Inactive Publication Date: 2014-03-05
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation of macroporous titanium dioxide materials by the method of filling colloidal crystal templates with precursor liquids has problems in terms of material morphology and regularity.
The main reasons are: first, the precursor liquid is easy to hydrolyze, and it is difficult to control its filling degree; second, the viscosity of the precursor liquid is relatively high, and it is easy to form a covering layer on the surface of the macroporous titanium dioxide, resulting in blockage of the pores on the surface of the material
If the number of fillings is small, the filling will be incomplete, the pore wall will be very thin, and the pore wall will collapse during the calcination process; when the number of fillings is large, it is easy to cover a large amount of titanium dioxide layer on the surface of the colloidal crystal, causing the large pores to be covered. Form a regular macroporous structure that interpenetrates

Method used

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  • Rapid preparation method of three-dimensional ordered macroporous titanium dioxide
  • Rapid preparation method of three-dimensional ordered macroporous titanium dioxide
  • Rapid preparation method of three-dimensional ordered macroporous titanium dioxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Spread the aqueous solution of monodisperse polystyrene microspheres (particle size: 265nm, dispersion coefficient: 0.005) with a mass fraction of 5% on a clean glass slide, evaporate for 4 hours at a humidity of 40% and a temperature of 60°C to prepare polystyrene microspheres. Styrene colloidal crystal film;

[0024] (2) heat-treat the prepared colloidal crystal film at a temperature of 100°C for 30 minutes, and after cooling to room temperature, cover the surface with a layer of glass slides, and fix the two slides firmly with clips to form a "sandwich " double slide of the structure;

[0025] (3) Mix tetrabutyl titanate and absolute ethanol at a volume ratio of 1:5, and magnetically stir for 2 hours to obtain a uniform and transparent precursor solution;

[0026] (4) Put the double glass slide with "sandwich" structure vertically into the precursor solution, and take it out after keeping the vacuum at -0.07MPa for 1min;

[0027] (5) Put the filled double glass...

Embodiment 2

[0031] (1) Spread the aqueous solution of monodisperse polystyrene microspheres (particle size: 310nm, dispersion coefficient: 0.005) with a mass fraction of 5% on a clean glass slide, evaporate for 4 hours at a humidity of 40% and a temperature of 60°C to prepare polystyrene microspheres. Styrene colloidal crystal film;

[0032] (2) heat-treat the prepared colloidal crystal film at a temperature of 100°C for 30 minutes, and after cooling to room temperature, cover the surface with a layer of glass slides, and fix the two slides firmly with clips to form a "sandwich " double slide of the structure;

[0033] (3) Mix tetrabutyl titanate and absolute ethanol at a volume ratio of 1:10, and stir magnetically for 2 hours to obtain a uniform and transparent precursor solution;

[0034] (4) Put the double glass slide with "sandwich" structure vertically into the precursor solution, and take it out after keeping the vacuum at -0.07MPa for 1min;

[0035] (5) Put the filled double glas...

Embodiment 3

[0039] (1) Spread the aqueous solution of monodisperse polystyrene microspheres (particle size: 345nm, dispersion coefficient: 0.005) with a mass fraction of 5% on a clean glass slide, evaporate for 4 hours at a humidity of 40% and a temperature of 60°C to prepare polystyrene microspheres. Styrene colloidal crystal film;

[0040] (2) heat-treat the prepared colloidal crystal film at a temperature of 100°C for 30 minutes, and after cooling to room temperature, cover the surface with a layer of glass slides, and fix the two slides firmly with clips to form a "sandwich " double slide of the structure;

[0041] (3) Mix tetrabutyl titanate and absolute ethanol at a volume ratio of 1:15, and magnetically stir for 2 hours to obtain a uniform and transparent precursor solution;

[0042] (4) Put the double glass slide with "sandwich" structure vertically into the precursor solution, and take it out after keeping the vacuum at -0.07MPa for 1min;

[0043] (5) Put the filled double glas...

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Abstract

The invention provides a rapid preparation method of three-dimensional ordered macroporous titanium dioxide by using a vacuum filling template method. The method is as below: filling a homogeneous transparent sol, formed by mixing anhydrous alcohol and tetrabutyl titanate, into template gaps in vacuum; then placing the template into a constant temperature and humidity chamber and controlling certain humidity and temperature for gelation; taking out the template and conducting natural air-drying for 24 h; and finally calcining the obtained sample under high temperature in a muffle furnace to remove the template, so as to obtain the three-dimensional ordered macroporous titanium dioxide with specific crystal form. Compared with a traditional method, the method provided by the invention is simple, practicable, and convenient for operation and has high efficiency, short filling time and few filling frequencies.

Description

technical field [0001] The invention relates to a method for preparing three-dimensional ordered macroporous titanium dioxide by using a sol-gel method combined with vacuum filtration and filling, and belongs to the technical field of new materials. Background technique [0002] Titanium dioxide is a wide bandgap semiconductor, which has the advantages of cheap, non-toxic, anti-light corrosion, high catalytic activity, strong oxidation ability, good stability, etc. The preparation of porous titanium dioxide with high specific surface area and good catalytic performance has attracted people's attention. Filling colloidal crystal templates with precursor liquid is a simple and effective method to prepare porous titanium dioxide. Its advantage is that colloidal crystal templates of different sizes can be used to synthesize macroporous materials with different pore sizes, and the prepared macroporous materials are interconnected. However, the preparation of macroporous titanium ...

Claims

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Application Information

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IPC IPC(8): C01G23/053C01G23/08
Inventor 刘士荣张晨刘缓缓倪忠斌陈明清
Owner JIANGNAN UNIV
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