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Preparation method of independent and ordered titanium dioxide nanotube arrays among tubes

A nanotube array and titanium dioxide technology is applied in the field of preparation of nanotube arrays, which can solve the problems of reducing the specific surface area of ​​the product, damage to the inner and outer walls of the nanotube, reducing the use value of the product, etc., achieving uniform structure distribution, simple and easy process operation, excellent Effects of Photocatalytic and Photovoltaic Properties

Inactive Publication Date: 2011-10-12
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, this preparation method has shortcomings. First, the prepared TiO 2 Although the nanotube array has a gradient structure, the interfacial stress between the gradients will cause the tube wall at the gradient to fall off, which not only causes damage to the inner and outer walls of the nanotubes, but also easily blocks the nanotubes, reducing the specific surface area of ​​the product. It is greatly reduced, resulting in a sharp decline in its mechanical properties, which greatly reduces the use value of the product; secondly, in addition to the above defects, the surface of the product—the array film is also faced with the difficulty of removing the barrier layer produced after the anodic oxidation is completed. technical challenge

Method used

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  • Preparation method of independent and ordered titanium dioxide nanotube arrays among tubes
  • Preparation method of independent and ordered titanium dioxide nanotube arrays among tubes
  • Preparation method of independent and ordered titanium dioxide nanotube arrays among tubes

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Embodiment 1

[0019] The concrete steps of preparation are:

[0020] Step 1, first put the metal titanium sheet as an anode in a water-based electrolyte solution with a stirring temperature of 25°C, ammonium fluoride, sulfuric acid and water with a molar ratio of 0.12:1.6:48, and adjust the DC voltage to 0.8V / The rate of s was increased from 0V to 20V and kept for 25 minutes, and then the metal titanium sheet that had been anodized for the first time was taken out and washed with water; after that, the metal titanium sheet that had been anodized and cleaned for the first time was used as an anode and placed at a temperature of 25°C , in an organic electrolyte with a molar ratio of ammonium fluoride, water and ethylene glycol of 0.06:1.09:15.5, adjust the DC voltage to rise from 0V to 60V at a rate of 0.8V / s and keep it for 1h; wherein, the metal titanium sheet The purity is 99.9%. The water in the water-based electrolyte and organic electrolyte, as well as the water for cleaning the first ...

Embodiment 2

[0023] The concrete steps of preparation are:

[0024] Step 1, first put the metal titanium sheet as an anode in a water-based electrolyte solution with a stirring temperature of 28 ° C, ammonium fluoride, sulfuric acid and water with a molar ratio of 0.13:1.7:49, and adjust the DC voltage to 0.9V / The rate of s was raised from 0V to 20V and kept for 26 minutes, and then the metal titanium sheet that had been anodized for the first time was taken out and washed with water; after that, the metal titanium sheet that had been anodized and cleaned for the first time was used as an anode and placed at a temperature of 28°C , in an organic electrolyte with a molar ratio of ammonium fluoride, water and ethylene glycol of 0.07:1.1:16.5, adjust the DC voltage to rise from 0V to 60V at a rate of 0.9V / s and keep it for 1.1h; among them, the metal titanium sheet The purity is 99.99%. The water in the water-based electrolyte and organic electrolyte, as well as the water used to clean the f...

Embodiment 3

[0027] The concrete steps of preparation are:

[0028] Step 1, first put the metal titanium sheet as the anode in the water-based electrolyte with the molar ratio of ammonium fluoride, sulfuric acid and water at 30°C under stirring, and adjust the DC voltage at 1V / s The rate is raised from 0V to 20V and kept for 27 minutes, and then the metal titanium sheet that has been anodized for the first time is taken out and washed with water; after that, the metal titanium sheet that has been anodized and cleaned for the first time is placed as an anode at a temperature of 30°C. Ammonium fluoride, water and ethylene glycol in the organic electrolyte with a molar ratio of 0.08:1.15:17.5, adjust the DC voltage from 0V to 60V at a rate of 1V / s and keep it for 1.2h; wherein, the purity of the titanium sheet 99.9%, the water in the water-based electrolyte and organic electrolyte, and the water used to clean the first anodized titanium sheet are deionized water, and the counter electrodes fo...

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Abstract

The invention discloses a preparation method of independent and ordered titanium dioxide nanotube arrays among tubes, comprising the following steps of: feeding a metallic titanium sheet as an anode in water-based electrolyte prepared from ammonium fluoride, sulfuric acid and water with the temperature of 25-35DEG C by stirring; adjusting direct current voltage to be 20V improved from 0V at the speed rate of 0.8-1.2V / s and maintaining for at least 25 minutes; taking out the metallic titanium sheet and washing, and feeding the metallic titanium sheet as the anode into organic electrolyte prepared from ammonium fluoride, water and glycol with the temperature of 25-35DEG C; and adjusting direct current voltage to be 60 V improved from 0V at the speed rate of 0.8-1.2V / s and maintaining for at least one hour; feeding a metallic titanium sheet subjected to anodic oxidation twice in glycol; and ultrasonically oscillating until a grey matter falls off the surface of the metallic titanium sheet completely to obtain the independent and ordered titanium dioxide nanotube arrays among the tubes with the outer diameter of 150-200nm and the thickness of the tube wall of 10-15nm. The preparation method can be widely applied to preparation of the titanium dioxide nanotube arrays which have no barrier layers on the surfaces and have smooth and flat tube wall surfaces and can be applied to the fields of photocatalysis, clean energy, and the like.

Description

technical field [0001] The invention relates to a preparation method of a nanotube array, in particular to a preparation method of an independent and ordered titanium dioxide nanotube array between tubes. Background technique [0002] Titanium dioxide is an important semiconductor functional material, which belongs to the electronic conductivity type (n-type) semiconductor, and is widely used in the degradation of pollutants because of its large forbidden band width, high redox potential and strong photocatalytic activity. , Dye-sensitized solar cells, fuel cells and resistive memory devices. The high specific surface area, strong adsorption, one-dimensional charge transport properties, and effective composite support of low-dimensional micro-nano materials make titanium dioxide nanotube arrays have better performance and application prospects than titanium dioxide. In order to obtain titanium dioxide nanotube arrays, people have made some attempts and efforts, such as a ki...

Claims

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Application Information

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IPC IPC(8): C01G23/053
Inventor 和星亮梁长浩胡小晔
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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