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Method for preparing porous titanium dioxide nanotube array

A technology of titanium dioxide nanotubes and nanotube arrays, which is applied in the field of preparation and stripping of porous ordered titanium dioxide arrays, can solve problems such as tube opening blockage, nanotube array defects, nanotube arrays are easy to aggregate and lodging, and achieve The effect of uniform size and wide application prospects

Inactive Publication Date: 2010-06-23
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve TiO 2 The problem that the nanotube array is easy to aggregate and lodging, the present invention provides a method for forming a porous network membrane structure on the surface of the nanotube array
[0005] The invention solves the problem that a large number of defects are easily generated on the surface of the nanotube array and the nozzle is blocked by using the method of secondary oxidation and mixed electrolyte

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Step 1: Surface treatment of metal titanium: ultrasonic cleaning with water, acetone and ethanol in sequence, rinsing in double distilled water and drying;

[0022] Step 2: Oxidize the cleaned titanium material once in an ethylene glycol electrolyte containing 5wt% ammonium fluoride, the anodic oxidation parameters are voltage 80V, temperature 0°C, time 0.5h, titanium material is the anode, graphite is the cathode ; Then ultrasonically remove the anodic oxide film on the surface in dilute hydrochloric acid solution to obtain a titanium substrate with a flat surface and low defects;

[0023] Step 3: After washing the titanium substrate obtained in Step 2 with double distilled water, add 0.5wt% NH 4 F and 15wt% sulfuric acid in an ethylene glycol mixed electrolyte were subjected to secondary anodization at a voltage of 20V for 10min at a temperature of -5°C to obtain a porous titanium oxide nanotube array.

[0024] Step 4: heat-treat the prepared titanium oxide nanotube ...

Embodiment 2

[0027] Step 1: Surface treatment of metal titanium: ultrasonic cleaning with water, acetone and ethanol in sequence, rinsing in double distilled water and drying;

[0028] Step 2: Oxidize the cleaned titanium material once in an ethylene glycol electrolyte containing 10wt% ammonium fluoride, the anodic oxidation parameters are voltage 60V, temperature 2°C, time 1h, titanium material is the anode, and graphite is the cathode; Then ultrasonically remove the anodic oxide film on the surface in dilute sulfuric acid solution to obtain a titanium substrate with a flat surface and low defects;

[0029] Step 3: After washing the titanium substrate obtained in Step 2 with double distilled water, 4 F and 20wt% hydrofluoric acid in an ethylene glycol mixed electrolyte with a voltage of 60V for secondary anodization for 20h at a temperature of 30°C to obtain a porous titanium oxide nanotube array;

[0030] Step 4: heat-treat the prepared titanium oxide nanotube array at 750°C for 3h to o...

Embodiment 3

[0033] Step 1: Surface treatment of metal titanium: ultrasonic cleaning with water, acetone and ethanol in sequence, rinsing in double distilled water and drying;

[0034]Step 2: Oxidize the cleaned titanium material once in an ethylene glycol electrolyte containing 7wt% ammonium fluoride. The anodic oxidation parameters are voltage 100V, temperature 5°C, and time 2h. The titanium material is used as the anode, and the graphite is used as the cathode; Ultrasonically remove the anodic oxide film on the surface in a dilute phosphoric acid solution to obtain a titanium substrate with a flat surface and low defects;

[0035] Step 3: After washing the titanium substrate obtained in Step 2 with double distilled water, 4 F and 2wt% phosphoric acid in an ethylene glycol mixed electrolyte with a voltage of 100V for 72h and a temperature of 80°C to obtain a porous titanium oxide nanotube array;

[0036] Step 4: heat-treat the prepared titanium oxide nanotube array at 600°C for 2 hours ...

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Abstract

The invention relates to a method for preparing an ordered porous anodic titanium dioxide nanotube array. The method can prepare an ultra-large area defect-free titanium dioxide nanotube array film, the surface layer is the porous shape like an anodic aluminum oxide template, and the lower layer is a nanotube ordered array, thereby overcoming the common problems of easy lodging and aggregation of tubes in the prior art of preparing the anodic titanium dioxide nanotube array and simultaneously solving the problems that the prepared nanotube array film has more surface defect corrosion pits and the sediment blocks tube mouths. The nanotube array can realize the controllable growth by controlling the preparation conditions and the process and obtain the ordered array films with different tube diameters, different wall thicknesses and different tube lengths. The diameter range of the nanotubes is 20-200nm, the wall thickness range is 5-30nm, and the length range of the titanium dioxide tubes is 100nm-1mm. The invention particularly relates to a technology which can effectively and completely strip the titanium dioxide array film, effectively strip a titanium substrate from the TiO2 nanotube array and obtain the different sizes of porous nanotube array self-support films.

Description

technical field [0001] The invention relates to a preparation technology of an anodized titanium nanotube array, in particular to a preparation and stripping method of a porous ordered titanium dioxide array. Background technique [0002] As an n-type semiconductor material with excellent performance, titanium dioxide is widely used in photocatalysts, dye-sensitized solar cells, self-cleaning, photolysis of water, Energy storage and other fields have been widely researched and applied. Especially in recent years, with the development of nanotechnology, TiO with various morphological structures 2 have come out, making TiO 2 The material has become the most widely used nano-photocatalytic material at present, and it also makes it one of the most promising green catalyst materials and photoelectric materials. [0003] At present, research work at home and abroad mainly focuses on TiO 2 In the development of one-dimensional nanomaterials such as nanowires, nanotubes, nanorod...

Claims

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Application Information

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IPC IPC(8): C25D11/26C30B29/16C30B30/02C01G23/047
Inventor 周峰王道爱刘盈刘维民
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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