CN101798701A - Method for preparing alumina template by guidance of etching pattern - Google Patents
Method for preparing alumina template by guidance of etching pattern Download PDFInfo
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- CN101798701A CN101798701A CN 201010135291 CN201010135291A CN101798701A CN 101798701 A CN101798701 A CN 101798701A CN 201010135291 CN201010135291 CN 201010135291 CN 201010135291 A CN201010135291 A CN 201010135291A CN 101798701 A CN101798701 A CN 101798701A
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Abstract
The invention discloses a method for preparing an alumina template by guidance of an etching pattern, which is implemented by the following concrete steps: 1, selecting a high-purity aluminum sheet, polishing, performing heat treatment in argon gas, immersing in sodium hydroxide solution, soaking successively by distilled water, alcohol and acetone, rinsing by distilled water, and performing electropolishing in electrolyte prepared from perchloric acid and ethanol; 2, designing a nano-pore pattern, and etching the pattern on the electropolished aluminum sheet obtained in step 1 by a focused ion beam; and 3, using the aluminum sheet after pattern etching in the step 2 as an anode, taking a Pt net as a cathode, and preparing the alumina template by using a primary anodic oxidation method, wherein the anodic oxidation parameters are as follows: maintaining the temperature of electrolyte selected from oxalate, sulfuric acid or phosphoric acid, and controlling applied pressure and anodic oxidation time correspondingly to obtain the alumina template finally. The alumina template prepared by the method in the invention has accurately-regulated aperture and hole pitches.
Description
Technical field
The invention belongs to technical field of nano material, relate to a kind of method of preparing alumina template by guidance of etching pattern.
Background technology
In recent years, anodic oxidation is owing to the nanoporous that can prepare hexagonal array causes extensive concern.This template is cheap and easy to get, and general laboratory can both prepare.As long as with certain density oxalic acid, sulfuric acid or phosphoric acid etc. is electrolytic solution, apply suitable voltage aluminium flake is carried out anodic oxidation, just can obtain the nanohole array of self-assembly, apply voltage by change, the temperature of anodizing time or electrolytic solution can be adjusted the diameter and the degree of depth of nano aperture.
Yet the alumina formwork of anodic oxidation gained has the following disadvantages in the prior art: the one, and nanohole array and hole dimension be strict conformance not; The 2nd, in bigger areal extent (micron order), nano-pattern can occur than large deviation; The 3rd, nano-pattern is difficult to precise treatment.These problems do not solve, and employed AAO template will pass to prepared nano structural material to these defectives, influences the performance of prepared material.
For many years, people take several different methods to improve the order of AAO template, but effect is not ideal.Therefore the template that presses for the preparation high-sequentialization satisfies the application need of aspects such as magnetic storage, opto-electronic device, biosensor.
Summary of the invention
The method that the purpose of this invention is to provide a kind of preparing alumina template by guidance of etching pattern has solved and exists nanohole array and hole dimension inconsistent in the prior art; In bigger areal extent (micron order), the problem than large deviation can appear in nano-pattern.
The technical solution adopted in the present invention is, a kind of method of preparing alumina template by guidance of etching pattern, and this method is specifically implemented according to following steps:
Step 1, the high-purity aluminium flake of selection are raw material, through after the mechanical polishing, in argon atmosphere, 450-550 ℃ of thermal treatment 12-24h, in mass concentration is the sodium hydroxide solution of 0.4%-0.7%, soak 5-15min subsequently, soak with distilled water, alcohol, acetone successively, use the distilled water rinsing again, be to carry out electropolishing in the electrolytic solution formed of 1:3.5-4.5 by perchloric acid and ethanol volume ratio then, the electropolishing voltage control is at 12-15V;
Step 2, according to the scantlings of the structure of the prepared alumina formwork of electrolytic solution design nanoporous pattern, with focused ion beam etching layout on the electropolishing aluminium flake that step 1 obtains;
Step 3, the aluminium flake of finishing etching pattern with step 2 are anode, with the Pt net is negative electrode, adopt an anonizing to prepare alumina formwork, the anodic oxidation parameter is: electrolyte temperature remains on 0-5 ℃, electrolytic solution is selected oxalic acid, sulfuric acid or phosphoric acid for use, corresponding control applies voltage and anodizing time, obtains having the alumina formwork of etching layout at last.
The beneficial effect of the inventive method is, the alumina formwork of preparation, and aperture and pitch of holes adjustment are accurate, and with the regional correlation that does not have etching, the nanohole array of etch areas is almost completely consistent with hole dimension.
Description of drawings
Fig. 1 is the 50nm aperture for layout in the embodiment of the invention 6, high-purity aluminium flake SEM figure of 400nm pitch of holes;
Fig. 2 is the SEM figure of high-purity aluminium flake behind ion beam etching among Fig. 1;
Fig. 3 is the figure of the SEM after the anodic oxidation in the phosphoric acid of 0.2M of the high-purity aluminium flake after the etching among Fig. 2.
Embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
The method of preparing alumina template by guidance of etching pattern of the present invention, implement according to following steps:
Step 1, to select high-purity aluminium flake that purity is 99.999%, thickness is 0.3mm be raw material, through after the mechanical polishing, in argon atmosphere, 450-550 ℃ of thermal treatment 12-24h, in mass concentration is the sodium hydroxide solution of 0.4%-0.7%, soak 5-15min subsequently, soak with distilled water, alcohol, acetone successively, use the distilled water rinsing again, be to carry out electropolishing in the electrolytic solution formed of 1:3.5-4.5 by perchloric acid and ethanol volume ratio then, the electropolishing voltage control is at 12-15V.
Step 2, according to the scantlings of the structure of alumina formwork, the design aperture is 50nm, the pitch of holes nanoporous pattern between 100nm-400nm, with focused ion beam etching layout on the electropolishing aluminium flake that step 1 obtains.
Step 3, the aluminium flake of finishing etching pattern with step 2 are anode, with the Pt net is negative electrode, adopt an anonizing to prepare alumina formwork, the anodic oxidation parameter is: electrolyte temperature remains on 0-5 ℃, electrolytic solution is selected the oxalic acid of 0.3-0.35M for use, applying voltage is 60-65V, and anodizing time is 100-120min; Or select the sulfuric acid of 0.3-0.35M for use, and applying voltage is 25-30V, anodizing time is 10-12min; Or select the phosphoric acid of 0.2-0.25M for use, and applying voltage is 140-150V, anodizing time is 10-12min, obtains nanohole array and the almost completely consistent alumina formwork of hole dimension at last.
Embodiment 1
Step 1, to select high-purity aluminium flake that purity is 99.999%, thickness is 0.3mm be raw material, through after the mechanical polishing, in argon atmosphere, at 450 ℃ of thermal treatment 24h, be that 0.5% sodium hydroxide solution soaks 5min in mass concentration subsequently, successively with distilled water-alcohol-acetone immersion-distilled water rinsing, be to carry out electropolishing in the electrolytic solution formed of 1:4 by perchloric acid and ethanol volume ratio then, electropolishing voltage is 12V.
Step 2, design aperture are that 50nm, pitch of holes are the nanoporous pattern of 100nm, with focused ion beam with this pattern etch on the electropolishing aluminium flake.
Step 3, be anode with the aluminium flake of step 2 etching pattern, with the Pt net is negative electrode, adopt an anonizing to prepare alumina formwork, the anodic oxidation parameter is: electrolyte temperature remains on 0 ℃, electrolytic solution is the oxalic acid of 0.3M, applying voltage is 60V, and anodizing time is 120min, obtains the alumina formwork that pitch of holes is 100nm.
Embodiment 2
Step 1, to select high-purity aluminium flake that purity is 99.999%, thickness is 0.3mm be raw material, through after the mechanical polishing, in argon atmosphere, at 550 ℃ of thermal treatment 12h, be that 0.4% sodium hydroxide solution soaks 15min in mass concentration subsequently, successively with distilled water-alcohol-acetone immersion-distilled water rinsing, be to carry out electropolishing in the electrolytic solution formed of 1:4.5 by perchloric acid and ethanol volume ratio then, electropolishing voltage is 15V.
Step 2, design aperture are that 50nm, pitch of holes are the nanoporous pattern of 100nm, with focused ion beam with this pattern etch on the electropolishing aluminium flake.
Step 3, be anode with the aluminium flake of step 2 etching pattern, with the Pt net is negative electrode, adopt an anonizing to prepare alumina formwork, the anodic oxidation parameter is: electrolyte temperature remains on 5 ℃, electrolytic solution is the sulfuric acid of 0.35M, applying voltage is 30V, and anodizing time is 12min, obtains the alumina formwork that pitch of holes is 100nm.
Embodiment 3
Step 1, to select high-purity aluminium flake that purity is 99.999%, thickness is 0.3mm be raw material, through after the mechanical polishing, thermal treatment 20h in 500 ℃ of following argon gas, be that 0.7% sodium hydroxide solution soaks 10min in mass concentration subsequently, successively with distilled water-alcohol-acetone immersion-distilled water rinsing, be to carry out electropolishing in the electrolytic solution formed of 1:3.5 by perchloric acid and ethanol volume ratio then, electropolishing voltage is 14V.
Step 2, design aperture are that 50nm, pitch of holes are the nanoporous pattern of 100nm, with focused ion beam with this pattern etch on the electropolishing aluminium flake.
Step 3, be anode with the aluminium flake of step 2 etching pattern, with the Pt net is negative electrode, adopt an anonizing to prepare alumina formwork, the anodic oxidation parameter is: electrolyte temperature remains on 2 ℃, electrolytic solution is the phosphoric acid of 0.24M, applying voltage is 140V, and anodizing time is 10min, obtains the alumina formwork that pitch of holes is 100nm.
Embodiment 4
Step 1, to select high-purity aluminium flake that purity is 99.999%, thickness is 0.3mm be raw material, through after the mechanical polishing, in argon atmosphere, at 500 ℃ of thermal treatment 15h, be that 0.5% sodium hydroxide solution soaks 10min in mass concentration subsequently, successively with distilled water-alcohol-acetone immersion-distilled water rinsing, be to carry out electropolishing in the electrolytic solution formed of 1:4 by perchloric acid and ethanol volume ratio then, electropolishing voltage is 13V.
Step 2, design aperture are that 50nm, pitch of holes are the nanoporous pattern of 100nm, with focused ion beam with this pattern etch on the electropolishing aluminium flake.
Step 3, be anode with the aluminium flake of step 2 etching pattern, with the Pt net is negative electrode, adopt an anonizing to prepare alumina formwork, the anodic oxidation parameter is: electrolyte temperature remains on 0 ℃, electrolytic solution is the oxalic acid of 0.35M, applying voltage is 65V, and anodizing time is 100min, obtains the alumina formwork that pitch of holes is 100nm.
Embodiment 5
Step 1, to select high-purity aluminium flake that purity is 99.999%, thickness is 0.3mm be raw material, through after the mechanical polishing, in argon atmosphere, at 500 ℃ of thermal treatment 16h, be that 0.6% sodium hydroxide solution soaks 12min in mass concentration subsequently, successively with distilled water-alcohol-acetone immersion-distilled water rinsing, be to carry out electropolishing in the electrolytic solution formed of 1:4 by perchloric acid and ethanol volume ratio then, electropolishing voltage is 12V.
Step 2, intended diameter are that 50nm, pitch of holes are the nanoporous pattern of 200nm, with focused ion beam with this pattern etch on the electropolishing aluminium flake.
Step 3, being anode with the aluminium flake with etching pattern, is negative electrode with the Pt net, adopts an anonizing to prepare alumina formwork.The anodic oxidation parameter is: electrolyte temperature remains on 3 ℃, and electrolytic solution is the sulfuric acid of 0.33M, and applying voltage is 26V, and anodizing time is 12min.Obtain the alumina formwork that pitch of holes is 200nm thus.
Embodiment 6
Step 1, to select high-purity aluminium flake that purity is 99.999%, thickness is 0.3mm be raw material, through after the mechanical polishing, in argon atmosphere, at 550 ℃ of thermal treatment 12h, be that 0.5% sodium hydroxide solution soaks 15min in mass concentration subsequently, successively with distilled water-alcohol-acetone immersion-distilled water rinsing, be to carry out electropolishing in the electrolytic solution formed of 1:4 by perchloric acid and ethanol volume ratio then, electropolishing voltage is between 15V.
Step 2, design aperture are that 50nm, pitch of holes are the nanoporous pattern of 400nm, and microgram is seen Fig. 1, with focused ion beam with this pattern etch on the electropolishing aluminium flake, microgram is seen Fig. 2.
Step 3, being anode with the aluminium flake with etching pattern, is negative electrode with the Pt net, adopts an anonizing to prepare alumina formwork.The anodic oxidation parameter is: electrolyte temperature remains on 0 ℃, and electrolytic solution is the phosphoric acid of 0.2M, and applying voltage is 145V, and anodizing time is 11min.Obtain the alumina formwork that pitch of holes is 200nm thus, microgram is seen Fig. 3.
Method of the present invention, adopting high-purity aluminium flake is raw material, after mechanical polishing, thermal treatment, cleaning, carry out electropolishing, use the focused-ion-beam lithography pattern then, in oxalic acid, sulfuric acid or phosphoric acid, carry out anodic oxidation at last, obtain the adjustable ordered nano pore array template in aperture.The advantage of the inventive method is that aperture and pitch of holes adjustment are accurate, observes by high resolution scanning electron microscope, and the nanohole array of etch areas is almost completely consistent with hole dimension.
Claims (5)
1. the method for a preparing alumina template by guidance of etching pattern, it is characterized in that: this method is specifically implemented according to following steps:
Step 1, the high-purity aluminium flake of selection are raw material, through after the mechanical polishing, in argon atmosphere, 450-550 ℃ of thermal treatment 12-24h, in mass concentration is the sodium hydroxide solution of 0.4%-0.7%, soak 5-15min subsequently, soak with distilled water, alcohol, acetone successively, use the distilled water rinsing again, be to carry out electropolishing in the electrolytic solution formed of 1:3.5-4.5 by perchloric acid and ethanol volume ratio then, the electropolishing voltage control is at 12-15V;
Step 2, according to the scantlings of the structure of the prepared alumina formwork of electrolytic solution design nanoporous pattern, with focused ion beam etching layout on the electropolishing aluminium flake that step 1 obtains;
Step 3, the aluminium flake of finishing etching pattern with step 2 are anode, with the Pt net is negative electrode, adopt an anonizing to prepare alumina formwork, the anodic oxidation parameter is: electrolyte temperature remains on 0-5 ℃, electrolytic solution is selected oxalic acid, sulfuric acid or phosphoric acid for use, corresponding control applies voltage and anodizing time, obtains having the alumina formwork of etching layout at last.
2. method according to claim 1 is characterized in that, the purity of described high-purity aluminium flake is 99.999%, and thickness is 0.3mm.
3. method according to claim 1 is characterized in that concentration of electrolyte is the oxalic acid of 0.3-0.35M in the described step 3, and applying voltage is 60-65V, and anodizing time is 100-120min.
4. method according to claim 1 is characterized in that concentration of electrolyte is the sulfuric acid of 0.3-0.35M in the described step 3, and applying voltage is 25-30V, and anodizing time is 10-12min.
5. method according to claim 1 is characterized in that concentration of electrolyte is the phosphoric acid of 0.2-0.25M in the described step 3, and applying voltage is 140-150V, and anodizing time is 10-12min.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102764920A (en) * | 2012-07-06 | 2012-11-07 | 河南理工大学 | Processing method for double-side outward-expanded metal micro-hole array |
| CN104233430A (en) * | 2014-07-29 | 2014-12-24 | 中国科学院西安光学精密机械研究所 | Preparation method of nanopore array anodic aluminum oxide film and alumina microchannel plate |
| CN105021502A (en) * | 2015-08-18 | 2015-11-04 | 河南泛锐复合材料研究院有限公司 | Detection method for nano particles |
| CN107059090A (en) * | 2017-04-10 | 2017-08-18 | 福建农林大学 | A kind of device for being used to prepare nano array structure material |
| CN110528059A (en) * | 2019-09-23 | 2019-12-03 | 青海大学 | 8 line aluminium alloy electrolytic polishing liquids of one kind and its preparation and polishing method |
| CN113774436A (en) * | 2021-09-26 | 2021-12-10 | 香港科技大学深圳研究院 | Nickel mold and preparation method and application thereof, antireflection film and preparation method and application thereof |
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| CN1609283A (en) * | 2003-10-21 | 2005-04-27 | 东莞理工学院 | Preparation method of ordered porous anodic alumina template |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102764920A (en) * | 2012-07-06 | 2012-11-07 | 河南理工大学 | Processing method for double-side outward-expanded metal micro-hole array |
| CN102764920B (en) * | 2012-07-06 | 2014-04-02 | 河南理工大学 | Processing method for double-side outward-expanded metal micro-hole array |
| CN104233430A (en) * | 2014-07-29 | 2014-12-24 | 中国科学院西安光学精密机械研究所 | Preparation method of nanopore array anodic aluminum oxide film and alumina microchannel plate |
| CN105021502A (en) * | 2015-08-18 | 2015-11-04 | 河南泛锐复合材料研究院有限公司 | Detection method for nano particles |
| CN107059090A (en) * | 2017-04-10 | 2017-08-18 | 福建农林大学 | A kind of device for being used to prepare nano array structure material |
| 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 |
| CN110528059A (en) * | 2019-09-23 | 2019-12-03 | 青海大学 | 8 line aluminium alloy electrolytic polishing liquids of one kind and its preparation and polishing method |
| CN113774436A (en) * | 2021-09-26 | 2021-12-10 | 香港科技大学深圳研究院 | Nickel mold and preparation method and application thereof, antireflection film and preparation method and application thereof |
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