Titanium dioxide nano-pore array thin film and preparation thereof

A nanohole array, titanium dioxide technology, applied in the direction of titanium dioxide, chemical instruments and methods, titanium oxide/hydroxide, etc., can solve the problem of not being able to manufacture a large-area ordered hole array titanium dioxide film, and ordering holes cannot be made from it Array titanium dioxide thin film, unable to manufacture ordered hole array titanium dioxide thin film and other problems, to achieve the effect of easy peeling and transfer of substrate, fast and easy heat treatment, and wide adjustable range of process parameters

Inactive Publication Date: 2009-08-12
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are deficiencies in both the manufacturing method and the finished product. First, it is impossible to produce a titanium dioxide film with an ordered hole array, especially a large-area ordered hole array titanium dioxide film; The pore diameter and pore spacing in the porous titanium dioxide film are random, determined by the porous particles of the template, and cannot be effectively controlled artificially
Although there is also anodic oxidation method used to prepare alumina porous templates, filled with sol-gel and removed after heat treatment to obtain titanium dioxide porous arrays, such as "preparation of One-dimensionally oriented nano-TiO2

Method used

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  • Titanium dioxide nano-pore array thin film and preparation thereof
  • Titanium dioxide nano-pore array thin film and preparation thereof
  • Titanium dioxide nano-pore array thin film and preparation thereof

Examples

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Embodiment 1

[0015] Embodiment 1: complete preparation successively according to the following steps: the first step, the aluminum flake that purity is 99.9% is 10 in vacuum degree -3 Pa, after annealing at 400°C for 7 hours, first place one side of it in an acid solution with a concentration of 0.1M as an anode, anodize it at a DC voltage of 25V and a temperature of 0°C for 7 hours, and then place it at a temperature of 50 Soak in a mixed solution of 4wt% phosphoric acid and 2wt% chromic acid at ℃ for 12h; wherein, the acid solution is oxalic acid solution. Next, the anodized side was subjected to the second anodic oxidation for 24 hours under the same process conditions to obtain an approximate figure 1 a andfigure 1 Porous alumina template with a pore diameter of 20 nm shown in b. In the second step, first mix absolute ethanol, glacial acetic acid and tetrabutyl titanate with a concentration of 0.5M according to the volume ratio of 0.8:0.5:0.3 and stir evenly to obtain a mixed solution...

Embodiment 2

[0016] Embodiment 2: finish preparation successively according to the following steps: the first step, the aluminum flake that purity is 99.9% is 10 in vacuum degree -3 Pa, after annealing at 450°C for 6 hours, first place one side of it in an acid solution with a concentration of 0.2M as an anode, anodize it at a DC voltage of 60V and a temperature of 2°C for 6 hours, and then place it at a temperature of 55 Soak in a mixed solution of 5wt% phosphoric acid and 1.8wt% chromic acid at ℃ for 11 hours; wherein, the acid solution is oxalic acid solution. Then, the anodized side was subjected to the second anodic oxidation for 23 hours under the same process conditions to obtain an approximate figure 1 a and figure 1 Porous alumina template with a pore diameter of 50 nm shown in b. In the second step, first mix absolute ethanol, glacial acetic acid and tetrabutyl titanate with a concentration of 0.55M according to the volume ratio of 0.9:0.4:0.4 and stir evenly to obtain a mixed ...

Embodiment 3

[0017] Embodiment 3: complete preparation successively according to the following steps: the first step, the aluminum flake that purity is 99.99% is 10 in vacuum degree -4 Pa, after annealing at a temperature of 500°C for 6 hours, first place one side of it in an acid solution with a concentration of 0.3M as an anode, anodize it at a DC voltage of 95V and a temperature of 3°C for 6 hours, and then place it at a temperature of 60 Soak in a mixed solution of 6wt% phosphoric acid and 1.5wt% chromic acid at ℃ for 10h; wherein, the acid solution is oxalic acid solution. Next, the anodized side is again subjected to the second anodic oxidation under the same process conditions for 21 hours to obtain the following figure 1 a and figure 1 Porous alumina template with a pore diameter of 80 nm shown in b. In the second step, first mix absolute ethanol, glacial acetic acid and tetrabutyl titanate with a concentration of 0.6M according to the volume ratio of 1:0.3:0.5 and stir evenly to...

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Abstract

The invention discloses a titanium dioxide nanometer hole array film and a preparation method thereof. A hole in the film is an ordered through hole array; the diameter of the through hole thereof is 15 to 130 nm, the hole pitch thereof is 25 to 200 nm, and the porosity thereof is 30 to 40 percent; the thickness of the film is 10 to 1000 nm; the preparation method comprises the following steps: step 1, obtaining a porous aluminum oxide template with the hole diameter of 20 to 150 nm by using the secondary oxidation process; step 2, preparing precursor solution by using absolute ethyl alcohol, glacial acetic acid, butyl titanate and water, then adding polyethylene glycol into the precursor solution after the pH value of the precursor solution is adjusted to 2 to 3 by using nitric acid, and finally obtaining precursor sol; and step 3, firstly coating the precursor sol on the porous aluminum oxide template for at least one time and thermally insulating and drying the precursor sol for at least one time, then placing the aluminum oxide template coated with the precursor sol after being annealed into strong alkaline solution to corrupt the porous aluminum oxide template, and finally preparing the titanium dioxide nanometer-hole array film. The invention can be widely applied to the fields of sensors, catalysis, photo catalysis, photonic crystal, etc.

Description

technical field [0001] The invention relates to a nanohole array film and a preparation method thereof, in particular to a titanium dioxide nanohole array film and a preparation method thereof. Background technique [0002] Titanium dioxide is a wide bandgap semiconductor that plays a very important role in our lives. With people's increasing concern in cleanliness, energy, sensor devices, etc., its excellent catalytic and photocatalytic properties and its application in dye-sensitized solar cells have attracted more and more attention. Oxide semiconductor nanofilms with hole array structure have become more and more research hotspots because of their large specific surface area and excellent properties in various aspects. Many properties of titanium dioxide are directly related to its specific surface area. The specific surface area of ​​titanium dioxide film with a pore array structure is much larger than that of conventional films. Due to its periodic pore array structur...

Claims

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Application Information

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IPC IPC(8): C01G23/047B01J21/06
Inventor 金震费广涛庄重
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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