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Preparation method of Fe-C-TiO2 nano tube array

A Nanotube Array, Titanium Oxide Nanotube Technology

Inactive Publication Date: 2009-06-10
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the applied anodic oxidation voltage is generally only in the range of 10-25V, beyond this voltage range, the nanotube-like structure cannot be formed, which limits the diameter of the nanotube to a certain extent, and the nanotubes prepared in the aqueous solution system The tube wall is thin and easy to break
200410021589.X discloses a preparation method of titanium dioxide nanotube arrays with a high aspect ratio. The solute of the electrolyte is fluoride and supporting electrolyte, the solvent is water, and alcohol additives are added. This kind of nanotube is still relatively short, only 250 nanometers long, the specific surface area is not large enough, and it can only absorb light in the ultraviolet region, so it cannot make full use of natural sunlight.
At present, there is no report on the simultaneous modification of titanium dioxide nanotube arrays prepared by anodic oxidation with multiple elements at home and abroad.

Method used

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  • Preparation method of Fe-C-TiO2 nano tube array
  • Preparation method of Fe-C-TiO2 nano tube array
  • Preparation method of Fe-C-TiO2 nano tube array

Examples

Experimental program
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Effect test

Embodiment 1

[0035] (1) Polish the surface of the Ti base material, clean it and set aside;

[0036] (2) Organic electrolyte preparation:

[0037] Measure 1.47mL of 40% hydrofluoric acid (HF) solution by mass, mix it evenly with 28.53mL of anhydrous dimethyl sulfoxide (DMSO), and prepare a DMSO solution with 2% by mass of HF ;

[0038] (3) Preparation of titanium oxide nanotube arrays:

[0039] Using a titanium sheet (1*4cm) with a purity of more than 99.9% as the anode and a platinum sheet (1*2cm) as the cathode, electrolyze for 2 hours at a DC voltage of 45V to produce a titanium oxide nanotube with a length of 5 microns; The amorphous titanium oxide nanotube array prepared above was calcined under aerobic condition at 450° C. for 5 h to crystallize it.

[0040] (4) C-TiO 2 Preparation of composite nanotube arrays:

[0041] With step (3) gained TiO 2 The nanotube array was placed in a graphite tank in an oxygen-free vacuum system, 0.2 g of polyethylene glycol was added as a carbon ...

Embodiment 2

[0045] (1) Polish the surface of the Ti base material, clean it and set aside;

[0046] (2) Organic electrolyte preparation:

[0047] Measure 2.21mL of hydrofluoric acid (HF) solution with a mass percentage of 40%, and mix it with 27.79mL of anhydrous dimethyl sulfoxide (DMSO) to prepare a DMSO solution with a mass percentage of HF of 3%. ;

[0048] (3) Preparation of titanium oxide nanotube arrays: using a titanium sheet (1*4cm) with a purity of more than 99.9% as an anode and a platinum sheet (1*2cm) as a cathode, electrolyze it for 1 hour at a DC voltage of 60V to obtain Nanotubes 12 microns long. The titania nanotube array prepared above was calcined at 500° C. under aerobic conditions for 6 h to crystallize it.

[0049] (4) C-TiO 2 Preparation of composite nanotube arrays:

[0050] With step (3) gained TiO 2 The nanotube array was placed in a graphite tank in an oxygen-free vacuum system, 0.4 g of polyethylene glycol was added as a carbon source, heated to 600° C. u...

Embodiment 3

[0054] (1) Polish the surface of the Ti base material, clean it and set aside;

[0055] (2) Preparation of organic electrolyte:

[0056] Measure 0.375mL of 40% hydrofluoric acid (HF) solution by mass, mix it evenly with 29.625mL of anhydrous dimethyl sulfoxide (DMSO), and prepare a DMSO solution with 0.5% by mass of HF ;

[0057] (3) Preparation of titanium oxide nanotube arrays: use a titanium sheet (1*4cm) with a purity of more than 99.9% as an anode, and a platinum sheet (1*2cm) as a cathode, and electrolyze it for 4 hours at a DC voltage of 35V to obtain Nanotubes 2 microns long. The amorphous titania nanotube arrays prepared above were calcined under aerobic conditions at 400 °C for 4 h to crystallize them.

[0058] (4) C-TiO 2 Preparation of composite nanotube arrays:

[0059] With step (3) gained TiO 2 The nanotube array is placed in a graphite tank in an oxygen-free vacuum system, 0.05 g of polyethylene glycol is added as a carbon source, heated to 500° C. under ...

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Abstract

The invention relates to a method for preparing an Fe-C-TiO2 nanotube array, which comprises: firstly, preparing a titanium oxide nanotube array on a Ti substrate material by electrolysis in a mixed solution of hydrofluoric acid and dimethyl sulfoxide, and roasting the obtained titanium oxide nanotube array for crystallization molding; secondly, calcinating the TiO2 nanotube array in an oxygen-free vacuum system, and taking polyethylene glycol as a carbon source to prepare a C-TiO2 composite nanotube array; and thirdly, electroplating the C-TiO2 composite nanotube array in an FeSO4 electroplate liquid, and preparing the Fe-C-TiO2 nanotube array. The method has the advantages that the method has simple and mature technology and convenient operation, can effectively strengthen the absorption capacity and the electronic conduction capacity of the final product, namely the titanium oxide nanotube array, widen the absorption range of the titanium oxide nanotube array in a visible light region, improve the photoelectric conversion efficiency of the titanium oxide nanotube array and realize industrialized mass production, and has wide potential application prospect in the fields of degradation and nontoxic treatment of toxic and harmful pollutant, sewage purification and so on.

Description

technical field [0001] The present invention relates to a preparation method of high-efficiency environmental functional nanomaterials, in particular to a Fe-C-TiO 2 Preparation method of nanotube arrays. Background technique [0002] Titanium dioxide nanotube arrays prepared by anodic oxidation have excellent characteristics such as large specific surface area and adjustable pore size. Its special nanotube-like structure has become a research hotspot in the scientific field of various countries. The electrolyte for preparing titanium dioxide nanotube arrays by anodic oxidation is usually an inorganic aqueous solution system. Since various ions migrate relatively fast in the aqueous solution, the electrochemical anodic oxidation is also fast, and nanotube arrays can be formed in a relatively short period of time. . However, the applied anodic oxidation voltage is generally only in the range of 10-25V, beyond this voltage range, the nanotube-like structure cannot be formed,...

Claims

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Application Information

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IPC IPC(8): B01J37/03B01J21/06C25D11/26C30B29/62C30B30/02
Inventor 罗胜联杨丽霞肖燕蔡青云
Owner HUNAN UNIV
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