CN104975323A - Sine-surface-shaped aluminum oxide template for preparing nano material and preparation method thereof - Google Patents
Sine-surface-shaped aluminum oxide template for preparing nano material and preparation method thereof Download PDFInfo
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Abstract
A sine-surface-shaped aluminum oxide template for preparing a nano material and a preparation method thereof. Both of an inner surface and an outer surface of the template are sine surfaces. A circular-conical nano pore array is orderly arranged in the vertical direction of the sine surface radially. The size of the circular-conical nano pores and the change rate of the pore size are gradually-varied in the tangential direction of a sine curve and can be regulated by changing the period and the amplitude of the sine surface and anodic oxidation time. The preparation method includes the steps of polishing a sine-surface-shaped high-purity aluminum sheet, performing anodic oxidation, and removing a barrier layer. The sine-surface-shaped aluminum oxide template provides a convenient approach for synthesizing the nano material and the preparation method is simple and available in preparation method.
Description
Technical field:
The present invention relates to the preparation method of sine surface shape alumina formwork for the preparation of nano material and this template.
Background technology:
Along with the development of science and technology, many new subjects constantly rise.Nanomaterial science be wherein one example.The preparation of nano material is the basis of Application of micron.The current method preparing the many employings of nano material has: template, vapour deposition process, photolithography, liquid phase method, ibl etc.And template is wherein a kind of the most basic method.Nearly four kinds more ripe at present of template: carbon nanotube, ion beam etching carbon film, biological micro-micella and alumina formwork.Alumina formwork, owing to having the features such as hole density is large, nanoporous length-to-diameter ratio (bore length/bore dia) is adjustable, becomes one of template be most widely used at present.It is placed on by the fine aluminium sheet of 99.99% in suitable acidic solution (as oxalic acid, sulfuric acid or phosphoric acid etc.), the nano aperture array system obtained by anodic oxidation.Since the beginning of the nineties in last century, people have utilized alumina formwork to successfully synthesize many nano structural materials, as: nanofiber, nanometer rod, nanotube and nano wire etc.These nano materials show the application prospect making us admiring, and some even walks out laboratory stage, as carbon nanotube is used for Flied emission, semiconductor nano laser line generator etc.
But about alumina formwork, what be applied at present is planar shaped alumina formwork, namely its two surfaces are up and down all planes, are unfavorable for the device of nano material practical function.Moreover, the nano aperture in planar shaped alumina formwork presents straight-tube shape and arranged in parallel, utilizes the function singleness of the nano material of this template assemblies.According to existing method, the alumina formwork realizing the radial ordered arrangement of conical nano aperture is impossible.
Summary of the invention:
The present invention, in order to solve the deficiencies in the prior art, provides a kind of sine surface shape alumina formwork preparing nano material and preparation method thereof.Synthesis for nano material provides one approach easily.
The technical scheme that technical solution problem of the present invention adopts is:
The feature of sine surface shape alumina formwork of the present invention is that the inside and outside two sides of template is sine surface, conical nano aperture is along the radial ordered arrangement of sine surface vertical direction, and conical nanoporous pore size and velocity of variation are along the tangential gradual change of sinusoidal line, and can regulate by changing anodizing time.Sine surface shape aluminium flake obtains sine surface shape alumina formwork after polishing, anodic oxidation, removal barrier layer.
Concrete preparation method of the present invention comprises the step of following order:
1. high-purity for planar shaped aluminium flake is covered sine surface die surface, after forging pressing and shaping, obtain sine surface shape aluminium flake, or after sine surface die surface vacuum evaporated aluminium, remove sine surface mould again obtain sine surface shape aluminium flake;
2. sine surface shape aluminium flake polishing 4-5 minute in the mixed solution of ethanol and perchloric acid;
3. aluminium flake deionized water rinsing is taken out 3-5 time;
4. sine surface shape aluminium flake is put into oxalic acid solution Anodic Oxidation 20 hours;
5. the zone of oxidation on sine surface shape aluminium flake is removed;
6. sine surface shape aluminium flake carries out second time anodic oxidation 8 hours in oxalic acid solution;
7. unoxidized aluminium lamination and barrier layer is removed,
8. use deionized water rinsing 3-5 time, at room temperature dry.
Compared with the prior art, the present invention has following technique effect:
1, geometrical property.The surfaces externally and internally of sine surface shape alumina formwork is all sine surface, has greater advantage relative to flat formwork in the device of nano material, such as can make sine surface grating, optical waveguides etc. by sine surface shape template.
2, electrical properties.The electrical properties of the nano wire (pipe, rod) of arranged in parallel, uniform diameter and radial ordered arrangement, conical nano wire (pipe, excellent) has very large difference.Have been found that, the Electronic Transport Properties of different diameter bismuth nano-wire is different, or be semi-metal or for semi-conductor, utilize sine surface shape alumina formwork to assemble and obtain radial ordered arrangement and the nano wire of Diameter Gradual Change (pipe, rod) array, thus the transformation of semi-metal to semi-conductor can be realized on a nano wire, for the device of nano material is laid a good foundation.
3, optical property.Theoretical and experiment proves all, and the nano wire (pipe, rod) of radial ordered arrangement, Diameter Gradual Change has unusual optical property.Such as, the silver nano line array of radiate can realize sub-wavelength super-resolution amplification imaging etc.Utilize sine surface shape alumina formwork to assemble and obtain radial ordered arrangement and the nano wire of Diameter Gradual Change (pipe, rod) array, the optical property of nano material excellence can be realized.
The beneficial effect of this preparation method is embodied in:
The preparation method of sine surface shape alumina formwork is simple to operate, reliable, taper pore size and varying aperture rate can regulate by changing cycle of sine surface, amplitude and anodizing time.
Accompanying drawing illustrates:
Figure is the pictorial diagram of sine surface shape aluminium flake of the present invention after anodic oxidation.
Embodiment:
The inside and outside two sides of the sine surface shape alumina formwork in the present embodiment is all sine surface, conical nano aperture is along the radial ordered arrangement of sine surface vertical direction, the pore size of conical nanoporous and varying aperture rate along the tangential gradual change of sinusoidal line, and can be regulated by the cycle of change sine surface, amplitude and anodizing time.Dotted arrow in figure represents that template sinusoidal line is tangential.
For the alumina formwork in the present embodiment, the concrete steps of its preparation method are:
(1) high-purity for planar shaped aluminium flake is covered sine surface die surface, after forging pressing and shaping, obtain sine surface shape aluminium flake, or after sine surface die surface vacuum evaporated aluminium, remove sine surface mould again obtain sine surface shape aluminium flake;
(2) sine surface shape aluminium flake polishing 4-5 minute in the mixed solution of ethanol and perchloric acid (volume ratio is 5: 1), voltage is 14-15 volt, and temperature is 10 degrees Celsius;
(3) aluminium flake deionized water rinsing is taken out 3-5 time;
(4) sine surface shape aluminium flake is put into 0.3M oxalic acid solution Anodic Oxidation 20 hours, oxidation voltage is 40 volts, and temperature is 5 degrees Celsius;
(5) aluminium flake that (4) obtain is put into the phosphoric acid (1.6%wt) of 1: 1 mixing and the solution of chromic acid (6%wt) by volume, at 60 c, place 2 hours, remove the zone of oxidation on ellipsoid shape aluminium flake;
(6) sine surface shape aluminium flake carries out second time anodic oxidation 8 hours in 0.3M oxalic acid solution, and voltage is 40 volts, and temperature is 5 degrees Celsius;
(7) the sine surface shape alumina wafer (6) obtained puts into saturated mercuric chloride solution 2 hours, removes unoxidized aluminium lamination;
(8) the sine surface shape alumina wafer deionized water rinsing (7) obtained 3-5 time;
(9) (8) are obtained the phosphoric acid solution that sine surface shape alumina wafer puts into 0.1M, place 20 minutes under 30 degrees Celsius, remove barrier layer;
(10) the sine surface shape alumina wafer deionized water rinsing (9) obtained 3-5 time, at room temperature dries.
Experiment shows:
After the sine surface shape alumina formwork obtained at the oxalic acid solution Anodic Oxidation of corresponding conditions completes above step, taper hole presents radial ordered arrangement along sine surface vertical direction.Near the A point shown in figure, its tapered hole is respectively along the minimum and maximum diameter in template surface vertical line direction: 50nm and 74nm, the velocity of variation of nano aperture is 0.60nm/ μm, near the B point shown in figure, its tapered hole is respectively along the minimum and maximum diameter in template surface vertical line direction: 55nm and 70nm, the velocity of variation of nano aperture is 0.50nm/ μm, i.e. and template surface vertical line direction tangential along template sinusoidal line, the aperture of nanoporous and the gradual change of varying aperture rate, also size and the varying aperture rate in tapered hole aperture can be regulated by the cycle and amplitude changing anodizing time and sine surface template, the direct observation of scanning electronic microscope can the feasibility of substantive approach.
Claims (2)
1. prepare the sine surface shape alumina formwork of nano material for one kind, it is characterized in that the inside and outside two sides of template is sine surface, conical nano aperture array is along the radial ordered arrangement of sine surface vertical direction, and conical nanoporous pore size and velocity of variation are along the tangential gradual change of sinusoidal line.
2. the preparation method of the sine surface shape alumina formwork of a preparation nano material according to claim 1, it is characterized in that sine surface shape aluminium flake is that high-purity for planar shaped aluminium flake is covered sine surface die surface, by obtaining after forging pressing and shaping, or after sine surface die surface vacuum evaporated aluminium, remove sine surface mould again obtain.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110528045A (en) * | 2019-08-21 | 2019-12-03 | 歌尔股份有限公司 | The surface treatment method of metal material |
| CN114990663A (en) * | 2022-05-17 | 2022-09-02 | 山东建筑大学 | Parabolic cylindrical aluminum oxide template for preparing nano material, preparation method and application |
| CN114990663B (en) * | 2022-05-17 | 2024-06-07 | 山东建筑大学 | Parabolic cylindrical aluminum oxide template for preparing nano material, preparation method and application |
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| CN114990663B (en) * | 2022-05-17 | 2024-06-07 | 山东建筑大学 | Parabolic cylindrical aluminum oxide template for preparing nano material, preparation method and application |
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