Method for preparing electrochemical anodic oxidation of large pipe diameter TiO2 nanometer tube

A technology of anodizing and large diameter, which is applied in the field of surface treatment for expanding the diameter of TiO2 nanotubes, and achieves the effects of less process parameters, less environmental damage and easy adjustment.

Inactive Publication Date: 2008-11-05
SOUTHWEST JIAOTONG UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

This suggests that there is a finite range for increasing the nanotube diameter by increasing the voltage

Method used

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  • Method for preparing electrochemical anodic oxidation of large pipe diameter TiO2 nanometer tube

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Experimental program
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Effect test

Embodiment 1

[0020] Embodiment 1, with the technical pure titanium after cleaning, pickling, drying: place the anode of electrochemical anodic oxidation reaction, take graphite as counter electrode; In hydrofluoric acid water system, add phosphoric acid as activator (partition The ratio is 0.15mol / LHF-0.5mol / LH 3 PO 4 ), and were oxidized twice under the voltage conditions of 20V and 25V respectively. Each oxidation time is 1 hour. After oxidation, the samples were removed and stored dry. Observe the surface morphology of the sample by SEM: the nanotubes are arranged in an orderly and compact manner, the nanotubes have a complete shape, the maximum diameter of the nanotubes is about 220nm, and the average diameter of the nanotubes is about 200nm.

Embodiment 2

[0021] Embodiment 2, with the commercially pure titanium after cleaning, pickling, drying: place the anode of electrochemical anodic oxidation reaction, take graphite as counter electrode; In hydrofluoric acid water system, add phosphoric acid as activator (partition The ratio is 0.15mol / LHF-1mol / LH 3 PO 4 ), and were oxidized twice under the voltage conditions of 20V and 25V respectively. Each oxidation time is 1 hour. After oxidation, the samples were removed and stored dry. Observe the surface morphology of the sample by SEM: the nanotubes are arranged in an orderly and compact manner, the nanotubes have a complete shape, the maximum diameter of the nanotubes is about 220nm, and the average diameter of the nanotubes is about 200nm.

Embodiment 3

[0022] Embodiment 3, with the industrial pure titanium after cleaning, pickling, drying: place the anode of electrochemical anodic oxidation reaction, take graphite as counter electrode; In hydrofluoric acid water system, add phosphoric acid as activator (partition The ratio is 0.15mol / LHF-2mol / LH 3 PO 4 ), and were oxidized twice under the voltage conditions of 20V and 25V respectively. Each oxidation time is 1 hour. After oxidation, the samples were removed and stored dry. Observe the surface morphology of the sample by SEM: the nanotubes are arranged in an orderly and compact manner, the nanotubes have a complete shape, the maximum diameter of the nanotubes is about 250nm, and the average diameter of the nanotubes is about 200nm.

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Abstract

The invention discloses an electrochemical anode oxidizing method for preparing a TiO2 nanotube with large caliber, which takes preprocessed pure titanium as an anode of the electrochemical anode oxidizing reaction and a pot lead as a counter electrode. In a hydrofluoric acid and water system, phosphoric acid is added as an activating agent, the concentration of the hydrofluoric acid is 0.15 mol per liter, and the concentration of the phosphoric acid is 0.5 to 4 mol per liter; oxidation is implemented twice under the conditions with voltage of 15 to 20 V and 23 to 28 V respectively, thus obtaining a TiO2 nanotube array with large caliber surface. Without destroying the permutation and the formation of the TiO2 nanotube, the electrochemical anode oxidizing method for preparing the TiO2 nanotube with large caliber can enlarge the caliber of the TiO2 nanotube to 280 nm, and has simple and convenient operations as well as low cost.

Description

technical field [0001] The present invention relates to a kind of expanded TiO 2 Surface treatment methods for nanotube diameters. Background technique [0002] Titanium dioxide has good photoelectric, photosensitive, gas sensitive, pressure sensitive and other characteristics, and has important application prospects in high-tech fields such as solar cells, photocatalytic degradation of pollutants, various sensors, and biological implant materials. research hotspot. TiO 2 The preparation methods of nanotubes currently reported include template method, chemical treatment method and electrochemical anodic oxidation method. [0003] template method [0004] Using porous anodized alumina (PAA) as a template, Li Xiaohong et al. successfully prepared anatase-type TiO with length, pore diameter and tube wall thickness adjustable according to the template by sol-gel method. 2 nanotube. The diameter of the nanotube is (100nm), the tube wall is relatively thick (10nm), and the d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/26
Inventor 冯波刘达理高玲
Owner SOUTHWEST JIAOTONG UNIV
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