CN107130219A - A kind of preparation method of ultra-thin through hole anodic aluminum oxide film - Google Patents

A kind of preparation method of ultra-thin through hole anodic aluminum oxide film Download PDF

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CN107130219A
CN107130219A CN201710281727.5A CN201710281727A CN107130219A CN 107130219 A CN107130219 A CN 107130219A CN 201710281727 A CN201710281727 A CN 201710281727A CN 107130219 A CN107130219 A CN 107130219A
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nano tube
film
alumina nano
aluminum oxide
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CN107130219B (en
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李佳红
张文军
徐鸣
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Huazhong University of Science and Technology
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Huazhong University of Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • C23C14/16Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/06Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C25D11/10Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/16Pretreatment, e.g. desmutting
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/18After-treatment, e.g. pore-sealing
    • C25D11/24Chemical after-treatment

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Abstract

Correlative technology field is prepared the invention belongs to nano material, it discloses a kind of preparation method of ultra-thin through hole anodic aluminum oxide film, is comprised the following steps:(1) after the surface of aluminium substrate is handled successively, one layer of aluminium film is deposited on the surface of the aluminium substrate;(2) anodic oxidation reactionses are carried out to the aluminium substrate, to obtain alumina nano tube film;(3) after the alumina nano tube film is protected, then the aluminium substrate is arranged at full closes CuCl2Carry out being reacted to give the alumina nano tube film of one end closing in solution;(4) phosphoric acid solution is added dropwise on the surface of the alumina nano tube film away from the carrier, so that the phosphoric acid solution and the alumina nano tube on the neighbouring barrier layer react;(5) surface of the alumina nano tube film is rinsed, to obtain ultra-thin through hole anodic aluminum oxide film.Above-mentioned preparation method is simply easily repeated, and reduces experimental cost, and be easy to large-scale production.

Description

A kind of preparation method of ultra-thin through hole anodic aluminum oxide film
Technical field
Correlative technology field is prepared the invention belongs to nano material, more particularly, to a kind of ultra-thin through hole anodic oxidation The preparation method of aluminium film.
Background technology
Fine aluminium piece can prepare a kind of regular nano-porous alumina structure by anodic oxidation reactionses, control nanometer The structural parameters of pipe include:Anodic oxidation voltage, time, Arrays Aluminum Films in Acid Solution and concentration.Such a nanotube has electrical insulating property, light Permeable, chemical stability, biologically inert and biocompatibility, be respectively provided with terms of optics, electrochemistry, biology Potential application.For anodizing, it can just pass through simple preparation process under cheap and easy appointed condition Prepare the nano-pore structure of high-sequential.Just because of this high-sequential and porous nano-pore structure and structure can Control property so that alumina nanohole more is gone to synthesize other orderly materials, such as Template synthesis nanometer as template Line, nanotube, nano particle.During these nano-arrays are synthesized, the thickness of anodised aluminium nanotube layer is to closing weight Will, such as when the thickness of nanotube layer is larger, nano particle to be deposited can not enter backing material by alumina nano tube. Therefore, when the thickness of only alumina nano tube reaches below 1000nm, material prepares some nano dots, nano-pore as template Etc. structural system.In addition, alumina nano tube is prepared as after through-hole structure, can be applied to gas phase, liquid phase separation with And the field such as sensor.
In recent years, the preparation of ultra-thin through hole anodised aluminium nano-pore template is increasingly paid attention to by researchers, such as Patent CN104726920 discloses preparation and its transfer method technology of a kind of ultra-thin through hole anodised aluminium, the preparation and Its transfer method generates orderly aluminium oxide nano pore structure using anodizing twice, under polystyrene PS protection, Aluminium substrate and barrier layer are removed, ultra-thin nanohole alumine nano-pore structure is obtained, the alumina formwork distribution that the method is obtained is equal Even, aperture is consistent, but step is relatively complicated, and the nano-pore thickness prepared is difficult accuracy controlling.Correspondingly, this area is present The technical need for the preparation method for developing a kind of simple ultra-thin through hole anodic aluminum oxide film of Making programme.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, the invention provides a kind of ultra-thin through hole anodised aluminium is thin The preparation method of film, its preparation characteristic based on existing ultra-thin through hole anodic aluminum oxide film, for ultra-thin through hole anodic oxidation The preparation method of aluminium film is designed.The preparation method regulates and controls the thickness of aluminium film by sputtering time, and regulation and control are simple, It is easily achieved;Certain thickness aluminium film is deposited in aluminum flake surface using magnetron sputtering embrane method, combined between aluminium film and aluminium substrate Power is stronger, is evenly distributed, and is easy to react continuous and stable progress in anode oxidation process.In addition, being 5% with mass percent Phosphoric acid solution progressively dissolve alumina nano tube, due to the inhibition between alumina nano tube interface, prevent phosphoric acid molten Further dissolving of the liquid to sedimentary alumina nano tube, method is simply easily repeated, and reduces experimental cost, is also allowed for extensive Production.
To achieve the above object, the invention provides a kind of preparation method of ultra-thin through hole anodic aluminum oxide film, it is wrapped Include following steps:
(1) aluminium substrate is provided, the surface of the aluminium substrate carried out successively after electrochemical polish, cleaning and drying, One layer of aluminium film is deposited on the surface of the aluminium substrate using magnetron sputtering embrane method;
(2) anodic oxidation reactionses are carried out to the aluminium substrate using anodizing, to obtain alumina nano tube Film, anodizing time is 30 minutes;
(3) surface of the alumina nano tube film is covered using the common scraps of paper, and will be described common with copper adhesive tape The scraps of paper are pasted after fixation, then the aluminium substrate is arranged at into full conjunction CuCl2Reacted to remove the aluminium substrate, obtained in solution The alumina nano tube film closed to one end;
(4) the alumina nano tube film is transferred on carrier, and the openend of the alumina nano tube film On the surface for being attached at the carrier, the surface of the alumina nano tube film away from the carrier is barrier layer, described Phosphoric acid solution is added dropwise on barrier layer, so that the phosphoric acid solution and the alumina nano tube on the neighbouring barrier layer react;
(5) surface of the alumina nano tube film is rinsed, the acidity of the alumina nano tube film surface is removed Ion, to obtain ultra-thin through hole anodic aluminum oxide film.
Further, sputtering time is 347~3472s, and aluminium film thickness is 100~1000nm, and sputtering power is 200W, is splashed Firing rate rate is 0.288nm/s.
Further, the thickness of the alumina nano tube be 2.696 μm, the alumina nano tube film it is a diameter of 1~3cm, it is alumina nano tube array structure, and the average caliber of the alumina nano tube is 40~120nm.
Further, the electrolyte of anodic oxidation is oxalic acid solution, the mass percent of the oxalic acid solution for 3%~ 5%.
Further, the common scraps of paper are circle, its a diameter of 1~3cm.
Further, the carrier is any of slide, smooth silicon chip and smooth metal piece.
Further, the mass percent of the phosphoric acid solution is 5%.
Further, anodic oxidation voltage is 40~60V, and electric current is 15~20mA.
In general, by the contemplated above technical scheme of the present invention compared with prior art, what the present invention was provided is super The preparation method of thin through hole anodic aluminum oxide film mainly has the advantages that:
(1) thickness of aluminium film is regulated and controled by sputtering time, regulation and control are simple, it is easy to accomplish;
(2) certain thickness aluminium film is deposited on the surface of aluminium substrate using magnetron sputtering embrane method, aluminium film and aluminium substrate it Between adhesion it is stronger, be evenly distributed, be easy to react continuous and stable progress in anode oxidation process;
(3) aluminum oxide film is protected using the circle scraps of paper and copper adhesive tape, CuCl is closed full2Aluminium substrate is removed in solution, is grasped Make easy, experiment repetitive rate is high, and the integrity degree of the aluminum oxide film formed is higher;
(4) alumina nano tube is progressively dissolved for 5% phosphoric acid solution with mass percent, due to aluminium oxide nano area within a jurisdiction Inhibition between face, prevents further dissolving of the phosphoric acid solution to sedimentary alumina nanohole, and method is simply easily repeated, Experimental cost is reduced, large-scale production is also allowed for.
Brief description of the drawings
Fig. 1 is the flow of the preparation method for the ultra-thin through hole anodic aluminum oxide film that better embodiment of the present invention is provided Figure;
The cross-sectional scans Electronic Speculum of the alumina nano tube film obtained in the step of Fig. 2 is first embodiment of the invention three Figure;
Fig. 3 is the cross-sectional scans Electronic Speculum for the ultra-thin through hole anodised aluminium nanotube that first embodiment of the invention is obtained Figure;
Fig. 4 is the cross-sectional scans Electronic Speculum for the ultra-thin through hole anodised aluminium nanotube that second embodiment of the invention is obtained Figure;
In Fig. 5 is that intermediate product in first to the 8th embodiment of the invention removes sweeping for the barrier layer after aluminium substrate Retouch electron microscope;
After Fig. 6 is the bottom surface through hole of the ultra-thin anode aluminum oxide film obtained in first to the 8th embodiment of the invention Scanning electron microscope (SEM) photograph.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and It is not used in the restriction present invention.As long as in addition, technical characteristic involved in each embodiment of invention described below Not constituting conflict each other can just be mutually combined.
Referring to Fig. 1, the preparation method for the ultra-thin through hole anodic aluminum oxide film that better embodiment of the present invention is provided, institute State preparation method and simplify flow and technique, improve the efficiency and success rate of experiment, be the nano junctions such as nano dot and nano-pore The preparation of structure system provides more effective and controllable template.
The preparation method of described ultra-thin through hole anodic aluminum oxide film is mainly included the following steps that:
Step one carries out electrochemical polish, cleaning there is provided an aluminium substrate, by the surface of the aluminium substrate and dried successively Afterwards, one layer of aluminium film is deposited on the surface of the aluminium substrate using magnetron sputtering embrane method.In present embodiment, sputtering time is 347~3472s, aluminium film thickness is 100~1000nm;Sputtering power is that 200W, sputter gas mass flow are 35sccm, sputtering Speed is 0.288nm/s.
Step 2, carries out an anodic oxidation reactionses to the aluminium substrate using anodizing, is received with obtaining aluminum oxide Mitron film, anodizing time is 30 minutes.In present embodiment, the thickness of the obtained alumina nano tube is 2.696 μm, a diameter of 1~3cm of alumina nano tube film, control voltage is 40~60V, and electric current is 15~20mA;0~ At a temperature of 20 DEG C, the oxalic acid solution that configuration quality percentage is 3%~5% is the electrolyte of anodic oxidation, with aluminium after plated film Piece is anode, and graphite is negative electrode;The alumina nano tube film is alumina nano tube array structure, alumina nano tube Average caliber is 40~120nm.
Step 3, is covered the surface of the alumina nano tube film using the common scraps of paper, and will be described with copper adhesive tape After common scraps of paper stickup is fixed, the aluminium substrate is arranged at full conjunction CuCl2Reacted to remove aluminium substrate in solution, obtained The alumina nano tube film of one end closing.Specifically, the common scraps of paper are used to protect the alumina nano tube film;Institute Alumina nano tube film one end opposite with its blind end is stated for openend;The common scraps of paper are circular paper, its diameter For 1~3cm;In other embodiments, the common scraps of paper can not also dissolve in CuCl from other2Solution and energy and aluminium flake The covering being brought into close contact is replaced.
Step 4, the alumina nano tube film is transferred on carrier, and the alumina nano tube film is opened Mouth end is attached on the surface of the carrier, and the surface of the alumina nano tube film away from the carrier is barrier layer, Phosphoric acid solution is added dropwise on the barrier layer, so that the phosphoric acid solution and the alumina nano tube film on the neighbouring barrier layer are sent out Raw reaction.Specifically, the mass percent of the phosphoric acid solution is 5%;The carrier can be slide, smooth silicon chip, light Sliding sheet metal;The reaction time of the phosphoric acid solution and the alumina nano tube film is 330 minutes;Due to aluminium oxide nano Inhibition between the face of area within a jurisdiction, prevents further dissolving of the phosphoric acid solution to the alumina nanohole of sedimentary, method It is simple easily to repeat, experimental cost is reduced, and be easy to large-scale production.
Step 5, rinses the surface of the alumina nano tube film, removes the alumina nano tube film surface Acid ion, to obtain ultra-thin through hole anodic aluminum oxide film.
First embodiment
(1) by fine aluminium piece (purity is 99.99%, and size is 2cm × 2cm × 1mm) in perchloric acid and the mixed liquor of ethanol (volume ratio 1:4) electrochemical polish is carried out in, polishing voltage is 15~18V, and electric current is 1A, and polishing time is 3min;After polishing Aluminium flake deionized water be cleaned by ultrasonic and dry.
(2) one layer of uniform aluminium film is deposited using the aluminum flake surface of magnetron sputtering embrane method after a polish, sputtering power is 200W, sputter gas mass flow is 35sccm, and regulated obtained sputter rate is 0.288nm/s, and sputtering time is 694s.
(3) it is anode by the aluminium flake after plated film, graphite flake is negative electrode, enters in mass percent is 3% oxalic acid solution Row anodic oxidation reactionses.Anodizing temperature is 20 DEG C, and voltage is 40V, and electric current is 20mA, and oxidization time is 30min.Reaction knot Shu Hou, obtains thickness for 2.696 μm, a diameter of 1cm alumina nano tube film.
(4) surface of alumina nano tube film is covered with a diameter of 2cm circle scraps of paper, further will using copper adhesive tape The scraps of paper and aluminum flake surface close adhesion.Configure saturation CuCl2Solution, aluminium substrate is dissolved and removed, dissolution time is 30s, is obtained The alumina nano tube transparent membrane of bottom surface closing.
(5) aluminum oxide film is placed on smooth carrier, opening surface is fitted with smooth carrier surface, with alumina barrier layer For upper surface, the phosphoric acid solution that mass percent is 5% is added dropwise, surface alumina oxide nanotube is gradually dissolved, after 330min, clearly Aluminum oxide film surface is washed, obtained transparent membrane is ultra-thin through hole anodic aluminum oxide film.
Second embodiment
The second embodiment and the first embodiment are essentially identical, and difference is the second embodiment The step of (2) in sputtering time be 1041s, deposit the thick aluminium films of 300nm in aluminum flake surface.
3rd embodiment
3rd embodiment and the first embodiment are essentially identical, and difference is the 3rd embodiment The step of (2) in sputtering time be 1389s, deposit the thick aluminium films of 400nm in aluminum flake surface.
4th embodiment
4th embodiment and the first embodiment are essentially identical, and difference is the 4th embodiment The step of (2) in sputtering time be 1736s, deposit the thick aluminium films of 500nm in aluminum flake surface.
5th embodiment
5th embodiment and the first embodiment are essentially identical, and difference is the 5th embodiment The step of (2) in sputtering time be 2083s, deposit the thick aluminium films of 600nm in aluminum flake surface.
6th embodiment
6th embodiment and the first embodiment are essentially identical, and difference is the 6th embodiment The step of (2) in sputtering time be 2430s, deposit the thick aluminium films of 700nm in aluminum flake surface.
7th embodiment
7th embodiment and the first embodiment are essentially identical, and difference is the 7th embodiment The step of (2) in sputtering time be 2778s, deposit the thick aluminium films of 800nm in aluminum flake surface.
8th embodiment
8th embodiment and the first embodiment are essentially identical, and difference is the 8th embodiment The step of (2) in sputtering time be 3125s, deposit the thick aluminium films of 900nm in aluminum flake surface.
Aluminium substrate after plated film generates orderly aluminium oxide nano pore structure after anodic oxidation, as shown in Fig. 2 anodic oxygen Change after 30min, the thickness of nanotube is 2.696 μm, a diameter of 42nm, the aluminium film of the primary aluminum piece and sedimentary institute after anodic oxidation There is obvious interface between the alumina nanohole of generation, the interface prevents phosphoric acid solution to the aluminium oxide nano of sedimentary The further dissolving in hole.By upper strata nanohole array after acid leach solution, having obtained average thickness as shown in Figure 3 is 210nm nanohole alumine film.When Fig. 4 is that deposition of aluminum film is 300nm in second embodiment, obtained ultra-thin through hole anode The scanning electron microscopic picture of alumina nano tube, can occur a certain degree of expansion after being anodized due to aluminium, thus obtain as Thickness shown in figure is 312nm aluminium oxide nano pore structure.Fig. 5 is the scanning electron microscope (SEM) photograph for removing barrier layer bottom surface after aluminium substrate Piece, now bottom is the nano-pore structure of closing, after the aluminium oxide nano aperture layer of phosphoric acid solution dissolving reaction surface, is led to The anodic aluminum oxide film in hole, Fig. 6 is the scanning electron microscope (SEM) photograph after the bottom surface through hole of anodic aluminum oxide film, and now bottom is to open The aluminium oxide nano pore structure of mouth, nano-pore average diameter is 49nm.It can be seen that, the embodiment of the present invention is prepared for the super of different-thickness Thin through hole anodic aluminum oxide film.
The preparation method for the ultra-thin anode aluminum oxide film that the present invention is provided, it regulates and controls the thickness of aluminium film by sputtering time Degree, regulation and control are simple, it is easy to accomplish;Certain thickness aluminium film, aluminium film and aluminium are deposited in aluminum flake surface using magnetron sputtering embrane method Adhesion is stronger between substrate, is evenly distributed, and is easy to react continuous and stable progress in anode oxidation process.In addition, using matter Amount percentage progressively dissolves alumina nano tube for 5% phosphoric acid, due to the inhibition between alumina nano tube interface, prevents Further dissolving of the phosphoric acid solution to sedimentary alumina nano tube, method is simply easily repeated, and reduces experimental cost, also just In large-scale production.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, it is not used to The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the invention etc., it all should include Within protection scope of the present invention.

Claims (8)

1. a kind of preparation method of ultra-thin through hole anodic aluminum oxide film, it is characterised in that this method comprises the following steps:
(1) aluminium substrate is provided, the surface of the aluminium substrate is carried out successively after electrochemical polish, cleaning and drying, used Magnetron sputtering embrane method deposits one layer of aluminium film on the surface of the aluminium substrate;
(2) anodic oxidation reactionses are carried out to the aluminium substrate using anodizing, to obtain alumina nano tube film, Anodizing time is 30 minutes;
(3) surface of the alumina nano tube film is covered using the common scraps of paper, and with copper adhesive tape by the common scraps of paper Paste after fixing, then the aluminium substrate is arranged at full conjunction CuCl2Reacted in solution to remove the aluminium substrate, obtain one The alumina nano tube film that end seal is closed;
(4) the alumina nano tube film is transferred on carrier, and the openend of the alumina nano tube film is attached In on the surface of the carrier, the surface of the alumina nano tube film away from the carrier is barrier layer, is stopped described Phosphoric acid solution is added dropwise on layer, so that the phosphoric acid solution and the alumina nano tube on the neighbouring barrier layer react;
(5) surface of the alumina nano tube film is rinsed, the acid ion of the alumina nano tube film surface is removed, To obtain ultra-thin through hole anodic aluminum oxide film.
2. the preparation method of ultra-thin through hole anodic aluminum oxide film as claimed in claim 1, it is characterised in that:Sputtering time is 347~3472s, aluminium film thickness is 100~1000nm, and sputtering power is 200W, and sputter rate is 0.288nm/s.
3. the preparation method of ultra-thin through hole anodic aluminum oxide film as claimed in claim 1, it is characterised in that:The aluminum oxide The thickness of nanotube is 2.696 μm, a diameter of 1~3cm of the alumina nano tube film, and it is alumina nano tube array Structure, the average caliber of the alumina nano tube is 40~120nm.
4. the preparation method of the ultra-thin through hole anodic aluminum oxide film as described in claim any one of 1-3, it is characterised in that:Sun The electrolyte of pole oxidation is oxalic acid solution, and the mass percent of the oxalic acid solution is 3%~5%.
5. the preparation method of the ultra-thin through hole anodic aluminum oxide film as described in claim any one of 1-3, it is characterised in that:Institute It is circle, its a diameter of 1~3cm to state the common scraps of paper.
6. the preparation method of the ultra-thin through hole anodic aluminum oxide film as described in claim any one of 1-3, it is characterised in that:Institute It is any of slide, smooth silicon chip and smooth metal piece to state carrier.
7. the preparation method of the ultra-thin through hole anodic aluminum oxide film as described in claim any one of 1-3, it is characterised in that:Institute The mass percent for stating phosphoric acid solution is 5%.
8. the preparation method of the ultra-thin through hole anodic aluminum oxide film as described in claim any one of 1-3, it is characterised in that:Sun Pole oxidation voltage is 40~60V, and electric current is 15~20mA.
CN201710281727.5A 2017-04-26 2017-04-26 A kind of preparation method of ultra-thin through-hole anodic aluminum oxide film Expired - Fee Related CN107130219B (en)

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CN114232051A (en) * 2021-12-16 2022-03-25 深圳拓扑精膜科技有限公司 Preparation method of nano-pore metal structure
CN115369404A (en) * 2022-07-22 2022-11-22 深圳华越再生医学生物科技有限公司 Aluminum oxide film and preparation method and application thereof

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CN101386985A (en) * 2008-10-14 2009-03-18 北京大学 Method for preparing AAO formwork on transparent electrode and corresponding device
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CN108865971A (en) * 2018-03-14 2018-11-23 深圳拓扑精膜科技有限公司 A kind of separation method and its separator of excretion body
CN114232051A (en) * 2021-12-16 2022-03-25 深圳拓扑精膜科技有限公司 Preparation method of nano-pore metal structure
CN115369404A (en) * 2022-07-22 2022-11-22 深圳华越再生医学生物科技有限公司 Aluminum oxide film and preparation method and application thereof

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