CN104975319B - Prepare cylinder spiral shape alumina formwork of nano material and preparation method thereof - Google Patents
Prepare cylinder spiral shape alumina formwork of nano material and preparation method thereof Download PDFInfo
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- CN104975319B CN104975319B CN201410152801.XA CN201410152801A CN104975319B CN 104975319 B CN104975319 B CN 104975319B CN 201410152801 A CN201410152801 A CN 201410152801A CN 104975319 B CN104975319 B CN 104975319B
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Abstract
A kind of cylinder spiral shape alumina formwork for preparing nano material and preparation method thereof.It is characterized in that the inside and outside two sides of alumina formwork is cylinder helical plane, centered on cylinder helical plane axis, conical nano aperture is along face of cylinder radial radiation shape ordered arrangement, and the pore size of conical nano-pore and varying aperture rate can be adjusted by changing anodizing time and cylindrical screw radius surface.Its preparation method is to obtain the high-purity aluminium flake of cylinder spiral shape after polishing, anodic oxidation, removal barrier layer.Synthesis of the cylinder spiral shape alumina formwork to nano material in the present invention provides a kind of convenient way, its preparation method simple possible.
Description
Technical field：
The present invention relates to for preparing the cylinder spiral shape alumina formwork of nano material and the preparation method of the template.
Background technology：
With the continuous development of scientific technology, many new subjects constantly rise.Nanomaterial science is wherein one.Receive
The preparation of rice material is the basis of Application of micron.Preparing the method that nano material uses more at present has：Template, gas phase are sunk
Area method, photoetching process, liquid phase method, ibl etc..And template therein is a kind of most basic method.At present compared with into
About four kinds of ripe template：CNT, ion beam etching carbon film, the micro- micella of biology and alumina formwork.Alumina formwork
Due to having the characteristics that hole density is big, nano-pore draw ratio (hole length/bore dia) is adjustable, it is the widest to become current application
One of general template.It is that 99.99% fine aluminium piece is placed in appropriate acid solution (such as oxalic acid, sulfuric acid or phosphoric acid),
The nano aperture array system obtained by anodic oxidation.Since the beginning of the nineties in last century, people utilize alumina formwork
Many nano structural materials are successfully synthesized, such as：Nanofiber, nanometer rods, nanotube and nano wire etc..These nano material exhibitions
Reveal the application prospect for making us admiring, some have even walked out laboratory stage, as CNT is used for Flied emission, semiconductor
Nanowire lasers etc..
But on alumina formwork, what is be applied at present is planar shaped alumina formwork, i.e. its two tables up and down
Face is all plane, is unfavorable for the device that nano material realizes function.Moreover, the nano-pore in planar shaped alumina formwork
Straight-tube shape and arranged in parallel is presented in hole, and the function using the nano material of this template assemblies is single.According to existing method,
Realize that the alumina formwork of the radial ordered arrangement of conical nano aperture is impossible.
The content of the invention：
The present invention is in order to solve the deficiencies in the prior art, there is provided a kind of cylinder spiral shape oxidation aluminum dipping form for preparing nano material
Plate and preparation method thereof.A kind of convenient way is provided for the synthesis of nano material.
The technical proposal for solving the technical problem of the invention is：
The characteristics of cylinder spiral shape alumina formwork of the present invention is that the inside and outside two sides of template is cylinder helical plane, with cylinder
Centered on helicoid axis, conical nano aperture is along cylinder helical plane radial radiation shape ordered arrangement, and conical nanometer
The pore size and varying aperture rate in hole can be adjusted by changing anodizing time and cylindrical screw radius surface.Cylinder spiral
Shape aluminium flake obtains cylinder spiral shape alumina formwork after polishing, anodic oxidation, removal barrier layer.
The specific preparation method of the present invention is included following steps in sequence：
It is cylinder spiral shape aluminium flake by forging pressing and shaping 1. the high-purity aluminium flake of bar shaped is wound on into cylinder mold surface, or
In cylinder mold surface vacuum AM aluminum metallization, along spiral wire cutting aluminium film, then remove cylinder mold and obtain cylinder spiral shape aluminium
Piece；
2. cylinder spiral shape aluminium flake polishes 4-5 minutes in the mixed liquor of ethanol and perchloric acid；
3. take out aluminium flake deionized water rinsing 3-5 times；
4. cylinder spiral shape aluminium flake is put into oxalic acid solution Anodic Oxidation 20 hours；
5. remove the oxide layer on cylinder spiral shape aluminium flake；
6. cylinder spiral shape aluminium flake carries out second of anodic oxidation 8 hours in oxalic acid solution；
7. remove unoxidized aluminium lamination and barrier layer,
8. with deionized water rinsing 3-5 times, dry at room temperature.
Compared with the prior art, the present invention has following technique effect：
1st, geometrical property.The surfaces externally and internally of cylinder spiral shape alumina formwork is all cylinder helical plane, relative to plane mould
Plate has greater advantage in terms of the device of nano material, for example spiral shape fiber waveguide can be made by cylinder spiral shape template
Deng.
2nd, electrical properties.Arranged in parallel, uniform diameter nano wire (pipe, rod) and radial ordered arrangement, cone are received
The electrical properties of rice noodles (pipe, rod) have very big difference.It has been found that the Electronic Transport Properties of different-diameter bismuth nano-wire are not
Together, or be semimetal or be semiconductor, using cylinder spiral shape alumina formwork can assemble to obtain radial ordered arrangement and
Nano wire (pipe, rod) array of Diameter Gradual Change, so as to realize transformation of the semimetal to semiconductor on a nano wire, it is
The device of nano material is laid a good foundation.
3rd, optical property.Theoretical and experiment is all it was demonstrated that radial ordered arrangement, the nano wire (pipe, rod) of Diameter Gradual Change
With unusual optical property.For example the silver nano line array of radial arrangement can realize that sub-wavelength super-resolution zooms into picture
Deng.It can assemble to obtain conical nano wire (pipe, rod) battle array of radial ordered arrangement using cylinder spiral shape alumina formwork
Row, it is possible to achieve the excellent optical property of nano material.
This preparation method has the beneficial effect that：
The preparation method of cylinder spiral shape alumina formwork is simple to operate, reliable, taper pore size and varying aperture rate
It can be adjusted by changing anodizing time and cylinder radius surface.
Brief description of the drawings：
Fig. 1 is pictorial diagram of the cylinder spiral shape aluminium flake of the present invention after anodic oxidation.
Embodiment：
The inside and outside two sides of cylinder spiral shape alumina formwork in the present embodiment is all cylinder helical plane, with cylinder helical plane
Centered on axis, conical nano aperture is big along cylinder helical plane radial radiation shape ordered arrangement, the aperture of conical nano-pore
Small and varying aperture rate can be adjusted by changing anodizing time and cylindrical screw radius surface.
For the alumina formwork in the present embodiment, its preparation method concretely comprises the following steps：
(1) the high-purity aluminium flake of bar shaped is wound on cylindrical die surface, is cylinder spiral shape aluminium flake by forging pressing and shaping, or
In cylinder mold surface vacuum AM aluminum metallization, along spiral wire cutting aluminium film, then remove cylinder mold and obtain cylinder spiral shape aluminium
Piece；
(2) cylinder spiral shape aluminium flake polishes 4-5 minutes, electricity in the mixed liquor of ethanol and perchloric acid (volume ratio 5: 1)
It is 10 degrees Celsius to press as 14-15 volts, temperature；
(3) aluminium flake deionized water rinsing 3-5 times is taken out；
(4) cylinder spiral shape aluminium flake being put into 0.3M oxalic acid solutions Anodic Oxidation 20 hours, oxidation voltage is 40 volts,
Temperature is 5 degrees Celsius；
(5) by the aluminium flake that (4) obtain be put into by volume 1: 1 mixing phosphoric acid (1.6%wt) and chromic acid (6%wt) it is molten
In liquid, at 60 c, 2 hours are placed, remove the oxide layer on aluminium flake；
(6) cylinder spiral shape aluminium flake carries out second of anodic oxidation 8 hours in 0.3M oxalic acid solutions, and voltage is 40 volts
Spy, temperature are 5 degrees Celsius；
(7) the cylinder spiral shape alumina wafer that (6) obtain is put into saturation mercuric chloride solution 2 hours, removes and do not aoxidize
Aluminium lamination；
(8) the cylinder spiral shape alumina wafer deionized water rinsing obtained (7) 3-5 times；
(9) (8) are obtained into cylinder spiral shape alumina wafer to be put into 0.1M phosphoric acid solution, 20 is placed under 30 degrees Celsius
Minute, remove barrier layer；
(10) the cylinder spiral shape alumina wafer deionized water rinsing obtained (9) 3-5 times, dries at room temperature.
Experiment shows：
Above step is completed in the cylinder spiral shape alumina formwork that the oxalic acid solution Anodic Oxidation of corresponding conditionses obtains
Afterwards, the minimum and maximum of its bellmouth a diameter of 67nm and 83nm, and taper hole is centered on cylinder helical plane axis, along circle
Radial ordered arrangement is radially presented in post helicoid, and the rate of change of nano aperture is 0.44nm/ μm, changes cylinder spiral shape template
Cylinder radius and anodizing time can adjust the size and varying aperture rate in bellmouth aperture, SEM
Directly observation can be with the feasibility of substantive approach.
Claims (1)
- A kind of 1. preparation method of the cylinder spiral shape alumina formwork of nano material, it is characterised in that the tool of its preparation method Body step is：(1) the high-purity aluminium flake of bar shaped is wound on cylindrical die surface, is cylinder spiral shape aluminium flake by forging pressing and shaping, or Person along spiral wire cutting aluminium film, then removes cylinder mold and obtains cylinder spiral shape in cylinder mold surface vacuum AM aluminum metallization Aluminium flake；(2) cylinder spiral shape aluminium flake polishes 4-5 minutes in the ethanol and the mixed liquor of perchloric acid that volume ratio is 5: 1, and voltage is 14-15 volts, temperature are 10 degrees Celsius；(3) aluminium flake deionized water rinsing 3-5 times is taken out；(4) cylinder spiral shape aluminium flake is put Enter 0.3M oxalic acid solutions Anodic Oxidation 20 hours, oxidation voltage is 40 volts, and temperature is 5 degrees Celsius；(5) (4) are obtained Aluminium flake is put into the 1.6%wt phosphoric acid of 1: 1 mixing and the solution of 6%wt chromic acid by volume, at 60 c, places 2 Hour, remove the oxide layer on aluminium flake；(6) cylinder spiral shape aluminium flake carries out second of anodic oxidation 8 in 0.3M oxalic acid solutions Hour, voltage is 40 volts, and temperature is 5 degrees Celsius；(7) the cylinder spiral shape alumina wafer that (6) obtain is put into saturation chlorination 2 hours in mercury solution, remove unoxidized aluminium lamination；(8) the cylinder spiral shape alumina wafer deionized water rinsing for obtaining (7) 3-5 times；(9) (8) are obtained into cylinder spiral shape alumina wafer to be put into 0.1M phosphoric acid solution, 20 points is placed under 30 degrees Celsius Clock, remove barrier layer；(10) the cylinder spiral shape alumina wafer deionized water rinsing obtained (9) 3-5 times, dries in the air at room temperature It is dry.
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| CN107059090B (en) * | 2017-04-10 | 2018-09-28 | 福建农林大学 | A kind of device being used to prepare nano array structure material |
| CN114990664B (en) * | 2022-05-17 | 2024-04-16 | 山东建筑大学 | Elliptic cylindrical alumina template for preparing nano material, preparation method and application |
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| CN102892930A (en) * | 2010-03-25 | 2013-01-23 | 三菱丽阳株式会社 | Anodizing device, treatment tank, method for producing roll-shaped mold for imprinting, and method for producing article having plurality of protruding parts on surface |
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| JP2013168537A (en) * | 2012-02-16 | 2013-08-29 | Meidensha Corp | Electric double layer capacitor |
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| CN102892930A (en) * | 2010-03-25 | 2013-01-23 | 三菱丽阳株式会社 | Anodizing device, treatment tank, method for producing roll-shaped mold for imprinting, and method for producing article having plurality of protruding parts on surface |
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