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Method for preparing titanium dioxide nanotube membrane

A technology of titanium dioxide and nanotubes, applied in nanostructure manufacturing, nanotechnology, nanotechnology, etc., can solve problems affecting special applications, difficulty in ultrasonic power and application time, difficulty in obtaining titanium dioxide nanotube films, etc., to achieve wide application, Improved photocatalytic performance and rapid solution exchange

Inactive Publication Date: 2010-06-02
LANZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are two main problems in the preparation of TiO2 nanotube films by anodic oxidation: first, the obtained TiO2 nanotube films always have an impenetrable layer between the bottom of the nanotubes and the titanium substrate after anodization. Titanium dioxide barrier layer, its thickness is usually 10-100nm
The second is that the obtained titanium dioxide nanotube film is always firmly bound on the titanium substrate, and it is difficult to obtain an independent titanium dioxide nanotube film, which also affects some of its special applications.
Since the key step of this method is still to use ultrasonic means to transform TiO 2 The nanotube film is mechanically peeled off from the substrate, with the same disadvantages as other mechanical peeling methods
For example, due to TiO 2 The nanotube film itself is relatively fragile, and it is extremely difficult to control the power and application time of ultrasonic waves when using ultrasonic stripping operations, and it is also difficult to avoid partial rupture of the film due to excessive ultrasonic waves; in addition, if the ultrasonic power is used improperly, the obtained All nanotubes in the film are transparent at both ends

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  • Method for preparing titanium dioxide nanotube membrane
  • Method for preparing titanium dioxide nanotube membrane
  • Method for preparing titanium dioxide nanotube membrane

Examples

Experimental program
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Effect test

Embodiment 1

[0015] The pure titanium plate was cut into a substrate with a size of 3.0 cm × 1.0 cm and a thickness of 250 μm, which were ultrasonically cleaned with acetone, isopropanol, methanol and deionized water in sequence, and then cleaned in HF and HNO 3 Chemical polishing in a mixed solution with a volume ratio of 1:8, N 2 Dry and set aside. At room temperature, with a titanium sheet as the anode and an aluminum sheet as the counter electrode, take 85ml (NH 4 F(0.25wt%)+H 2 O(0.3vol%)+HOCH 2 CH 2 OH) electrolyte, after applying a constant voltage of 60V for anodic oxidation for 2 hours, the surface of the titanium substrate will produce a titanium dioxide layer with a predetermined thickness, and then reduce the oxidation voltage at a rate of 1V / 15s to continue oxidation. After 0, reapply a pulse high voltage of 80V to continue oxidation for 6min, and the titanium dioxide film can fall off from the substrate by itself. Take out the sample sheet and wash it with deionized wate...

Embodiment 2～4

[0017] Similar to Example 1, the difference is that the pure titanium plate is cut into a substrate with a size of 3.0 cm × 1.0 cm and a thickness of 250 μm, which is cleaned with acetone, isopropanol, methanol and deionized water in sequence, and then cleaned in HF and HNO 3 Chemical polishing in a mixed solution with a volume ratio of 1:8, N 2 Dry and set aside. At room temperature, with a titanium sheet as the anode and an aluminum sheet as the counter electrode, take 85ml (NH 4 F(0.25wt%)+H 2 O(0.3vol%)+HOCH 2 CH2 OH) electrolyte solution, apply a voltage of 60V for anodic oxidation for 2h. Thereafter, the oxidation voltage gradually decreased from 60V at intervals of 1V / 15s until the voltage was 1V, and finally applied another 65V (example 2), 70V (example 3), 75V (example 4), and took out the sample and cleaned it with deionized water , air dry. image 3 For the TiO that obtains according to embodiment example 2 2 Scanning electron microscope (SEM) photographs of n...

Embodiment 5～7

[0018] Embodiments 5 to 7: Similar to Embodiment 1, the difference is that the pure titanium plate is cut into a substrate with a size of 3.0 cm × 1.0 cm and a thickness of 250 μm, and is cleaned sequentially with acetone, isopropanol, methanol and deionized water , then in HF and HNO 3 Chemical polishing in a mixed solution with a volume ratio of 1:8, N 2 Dry and set aside. At room temperature, with a titanium sheet as the anode and an aluminum sheet as the counter electrode, take 85ml (NH 4 F(0.25wt%)+H 2 O(0.3vol%)+HOCH 2 CH 2 OH) electrolyte solution, apply a voltage of 60V for anodic oxidation for 2h. Thereafter, the oxidation voltage was gradually reduced from 60V at intervals of 1V every 15s until the voltage was 1V, and finally an 80V pulse high voltage oxidation was applied for 10s (Example 5), 30s (Example 6), and 90s (Example 7). Figure 4 For the corresponding obtained TiO 2 Scanning electron microscope (SEM) photographs of nanotube films. It can be seen fr...

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Abstract

The invention discloses a method for preparing a titanium dioxide (TiO2) nanotube membrane with two permeable ends of a nanotube thereof. The method for preparing the titanium dioxide nanotube membrane comprises the following steps of: firstly, generating a titanium dioxide membrane with a required thickness on the surface of a titanium substrate material in a mode of electrolytic oxidation; secondly, thinning a barrier layer at the bottom of the titanium dioxide nanotube membrane by adopting gradual voltage-lowering oxidation; and finally, applying a high-voltage pulse higher than an anode oxidation voltage to continue oxidizing after finishing the last process until the titanium dioxide nanotube membrane with two permeable ends is shed from the substrate.

Description

technical field [0001] The present invention relates to a kind of titanium dioxide (TiO 2 ) Preparation method of nanotube thin film. The titanium dioxide nanotube film of the present invention is first cleaned and chemically polished on the surface of the titanium base material, then the base material is put into the electrolyte, and the metal plate is used as the counter electrode to carry out electrochemical anodic oxidation, until the surface of the base material is formed Titanium dioxide film of desired thickness. Background technique [0002] Since Fujishima, Japan discovered the photocatalytic water splitting of titanium dioxide single crystal electrodes in 1972 [Nature, 1972, 238(5358): 37-38.], photocatalytic technology has received extensive attention. Photocatalytic technology has the potential to solve the energy crisis and environmental pollution problems of human beings in the future. Photocatalytic technology can be carried out at normal temperature and pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/26B82B3/00
Inventor 张浩力徐华谢克锋李自夏
Owner LANZHOU UNIVERSITY
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