Method for preparing titanium dioxide nano tube array on titanium-substrate material surface

A nanotube array, titanium dioxide technology, applied in the field of nanomaterials, can solve the problems of low pH value, high electrolyte cost, single system, etc., and achieve the effects of low cost, easy operation and large specific surface area

Inactive Publication Date: 2008-06-04
SOUTHWEST JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the currently reported methods, there are usually disadvantages of high electrolyte cost and inconvenient process operation.
Chinese patent application 200510125502.8 uses simple HF acid as the electrolyte, the system is single, the pH value drops quickly, the time for oxidation and corrosion to reach equilibrium is short, and it is difficult to increase the length of nanotubes and control the shape of nanotubes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] A thin titanium dioxide nanotube array layer was prepared on a pure titanium sheet with a diameter of 15 mm and a thickness of 1.5 mm.

[0014] (1) Polish a thin titanium sheet with a diameter of 15mm and a thickness of 1.5mm with 280#, 600#, and 1000# water-resistant silicon carbide sandpaper in sequence, and then ultrasonically clean it in acetone and distilled water for 10 minutes;

[0015] (2) Etch in a mixed solution containing 6.0 mol / L nitric acid and 1 mol / L hydrofluoric acid until no bubbles are generated, then rinse the surface of the sample with distilled water, then quickly dry the sample after etching, and place it in the air for at least 1 Carry out (4) operation after hours.

[0016] (3) Prepare 100mL mixed electrolyte, including ammonium dihydrogen phosphate and 0.4mol / L hydrofluoric acid at a concentration of 1mol / L.

[0017] (4) The voltage is 20V, the distance between the electrodes is 4cm, the temperature of the electrolytic cell is kept at room tem...

Embodiment 2

[0021] A thick titanium dioxide nanotube array layer was prepared on a pure titanium sheet with a diameter of 15 mm and a thickness of 1.5 mm.

[0022] (1) Cut a pure titanium rod with a diameter of 15mm into 1.5mm thick slices, polish it with 280#, 600#, 1000# water-resistant silicon carbide sandpaper in turn, and then ultrasonically clean it in acetone and distilled water for 10 minutes.

[0023] (2) Etch in a mixed solution containing 6.0 mol / L nitric acid and 3 mol / L hydrofluoric acid until no bubbles are generated, then rinse the surface of the sample with distilled water, then quickly dry the sample after etching, and place it in the air for at least 1 Carry out (4) operation after hours.

[0024] (3) Prepare 100 mL of mixed electrolyte solution, including ammonium dihydrogen phosphate with a concentration of 1 mol / L and hydrofluoric acid with a concentration of 0.3 mol / L.

[0025] (4) The voltage is 20V, the distance between the electrodes is 4cm, the temperature of th...

Embodiment 3

[0029] A thin and small-diameter titanium dioxide nanotube array layer was prepared on a pure titanium sheet with a diameter of 15 mm and a thickness of 1.5 mm.

[0030] (1) (2) steps are the same as in Example 2.

[0031] (3) Prepare 100 mL of mixed electrolyte solution, including 10 mL of 30% hydrogen peroxide, 1 mol / L ammonium dihydrogen phosphate and 0.3 mol / L hydrofluoric acid.

[0032] (4) The voltage is 20V, the distance between the electrodes is 4cm, the temperature of the electrolytic cell is kept at room temperature, and the anodic oxidation treatment is performed for 60 minutes, and the electrolyte should be kept stirring continuously during the treatment.

[0033] (5) Carry out heat treatment in an air atmosphere with a heating rate of 3°C / min, from room temperature to 450°C for 3 hours, and then cool to room temperature with the furnace.

[0034] Test results: Titanium dioxide nanotubes regularly grow on the surface of pure titanium, the tube diameter is about 80...

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Abstract

The invention discloses a method by which titanium dioxide nanometer tube array layer is prepared on surface of titanium base material, wherein the titanium base materials undergo the surface pretreatment and receive the electrochemistry anodic oxidation treatment in the electrolyte containing the HF acid, the components of the mixed electrolyte are that the ammonium dihydrogen phosphate is 1 to 3mol/L and the hydrofluoric acid is 0.2 to 0.4mol/L, as a result, the amorphous form titanium dioxide nanometer tube surface structure is achieved; the subsequent heat treatment condition is that under air atmosphere, the rate of temperature rise is 3 DEG C/min, the heat is preserved for 3 hours at the temperature of 450 DEG C, the anatase titanium dioxide nanometer tube array layer is achieved after being cooled in the furnace to the room temperature. The electrolyte system prepared based on the method of the invention can control the balance of oxidation and the corrosion within a relatively long time, thereby preferably realizing the control on the shape of the titanium dioxide nanometer tube. The invention has the advantages of easy operation, low cost and orientated and order distribution of the prepared titanium dioxide nanometer tube array; moreover, the amorphous form titanium dioxide nanometer tube is generated normal to the direction of the base; the tube diameter is 80 to 100nm, the wall thickness is 18 to 21nm, the tube length is 0.7 to 2.0um, thereby the specific surface area is large.

Description

technical field [0001] The invention belongs to the field of nanometer materials, in particular to a method for preparing a titanium dioxide nanotube array layer on the surface of pure titanium or titanium alloy. Background technique [0002] Titanium and titanium alloys are light in weight, high in strength and good in corrosion resistance, and have been widely used in aerospace, machinery manufacturing, biomedical materials and other fields. However, when it is used, it is often necessary to modify its surface. The purpose is to obtain a surface with better performance, such as laser melting TiN and TiC to improve its hardness and wear resistance; to improve the titanium surface by depositing a coating. Excellent corrosion resistance, high temperature resistance and wear resistance; the microstructure of titanium surface can be changed by surface nanometerization, and the mechanical properties can be improved. [0003] Titanium dioxide is an important inorganic functional...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/26
Inventor 冯波初薛基翁杰鲁雄汪建新屈树新
Owner SOUTHWEST JIAOTONG UNIV
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