CN103966642A - Preparation method of highly ordered porous anodic oxide film - Google Patents
Preparation method of highly ordered porous anodic oxide film Download PDFInfo
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- CN103966642A CN103966642A CN201410220482.1A CN201410220482A CN103966642A CN 103966642 A CN103966642 A CN 103966642A CN 201410220482 A CN201410220482 A CN 201410220482A CN 103966642 A CN103966642 A CN 103966642A
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- preparation
- porous anodic
- highly ordered
- ordered porous
- anodic oxidation
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000010407 anodic oxide Substances 0.000 title abstract description 5
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 32
- 230000003647 oxidation Effects 0.000 claims abstract description 28
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 150000001868 cobalt Chemical class 0.000 claims abstract description 12
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 14
- 239000008151 electrolyte solution Substances 0.000 claims description 12
- 238000002203 pretreatment Methods 0.000 claims description 8
- 239000004411 aluminium Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000009826 distribution Methods 0.000 abstract description 6
- 239000011148 porous material Substances 0.000 abstract description 6
- 239000003792 electrolyte Substances 0.000 abstract description 5
- 238000005498 polishing Methods 0.000 abstract description 3
- 229910019167 CoC2 Inorganic materials 0.000 abstract 1
- ZJRWDIJRKKXMNW-UHFFFAOYSA-N carbonic acid;cobalt Chemical compound [Co].OC(O)=O ZJRWDIJRKKXMNW-UHFFFAOYSA-N 0.000 abstract 1
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 abstract 1
- 229910000001 cobalt(II) carbonate Inorganic materials 0.000 abstract 1
- 238000004904 shortening Methods 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 9
- 238000005530 etching Methods 0.000 description 7
- 239000012528 membrane Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910019142 PO4 Inorganic materials 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000007743 anodising Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/045—Anodisation of aluminium or alloys based thereon for forming AAO templates
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Catalysts (AREA)
- Laminated Bodies (AREA)
- Weting (AREA)
Abstract
The invention discloses a preparation method of a highly ordered porous anodic oxide film, which comprises pretreatment and anodic oxidation. And in the step of anodic oxidation, the pretreated pure aluminum is put into electrolyte, and is subjected to anodic oxidation for 1-4 hours at the temperature of-20 ℃ and under the voltage of 80-120V. The electrolyte is an aqueous solution containing phosphoric acid and cobalt salt, and each liter of electrolyte contains 0.1-0.6 mol of phosphoric acid and 0.1-0.8 g of cobalt salt. The cobalt salt being Co 3)2·6H2O、CoCO3、(NH4)2Co(SO4)2·6H2O、CoSO4·7H2O and CoC2O4One kind of (1). The preparation method of the invention only needs to carry out one-time anodic oxidation without electrochemical polishing and treatment after polishing, thus greatly shortening the process flow, improving the production efficiency, being very suitable for industrial mass production, and the obtained porous anodic oxide film has uniform pore size distribution and high orderliness.
Description
Technical field
The invention belongs to field of metal surface treatment technology, be specifically related to a kind of preparation method of highly ordered porous anodic film.
Background technology
Porous anodic alumina films (AAO) is to form the aluminum oxide film with highly regular pore structure at surface of pure aluminum by the method for electrochemical oxidation.Its membrane structure is the closelypacked cylindricality after birth of sexangle, the center of each after birth have one nanometer level microporous.
Porous anodic alumina films is heat and electric good insulator, has the features such as hardness is high, wear resistance is good; Have good solidity to corrosion, its resistance to corrosion is decided by the alloying constituent of thicknesses of layers, composition, porosity and body material; Also very strong with the bonding force of matrix metal, even if rete is bent to fracture with matrix, rete still can keep good combination with matrix metal.
Along with the understanding of people to porous anodic alumina films unique microstructures and property, porous anodic alumina films is widely used in catalysis, magnetic pipe recording material, optics and sealed cell, antibacterial film, separation membrane material, sensor various functions field gradually, becomes the focus of various countries' scholar's research.
At present, that the preparation of porous anodic alumina films mainly adopts is two step anonizings (as Chinese patent literature CN1609283A, CN101007645A, CN101139730A etc.), first aluminium is carried out to pre-treatment, then in acid electrolyte, be oxidized first, oxidization time is generally 1h～5h, then remove by chemical corrosion the oxide film that oxidation produces first, finally in acid electrolyte, carry out again secondary oxidation, oxidization time is generally 2h～12h, obtains porous anodic alumina films.Wherein pre-treatment mainly comprises cleaning and electrochemical etching, and the Main Function of electrochemical etching is to obtain compared with even curface, thereby is conducive to obtain size and the more uniform porous array film that distributes after anodic oxidation.The solution that electrochemical etching adopts is all made up of according to certain volume ratio dehydrated alcohol and perchloric acid.The shortcoming of the method is: (1) anodizing time is longer, thereby causes the production cycle; (2) the oxide film degree of order that oxidation produces is first poor, thus the degree of order of the porous anodic alumina films that impact finally obtains.
Chinese patent literature CN103225096A discloses a kind of preparation method of porous anodic alumina films, comprises nanometer porous rete, anodic oxidation and cleaning and oven dry that pre-treatment, electrochemical etching, removal electrochemical etching form.The electrolytic solution that its Anodic Oxidation adopts is 0.2mol/L～0.6mol/L phosphate aqueous solution.The deficiency of the document is: (1), although also only carry out an anodic oxidation, needed to carry out electrochemical etching and treatment solution membrane removal before oxidation, and therefore technical process is still longer, is not suitable for industrialized production.(2) adopt chromium-containing solution to carry out membrane removal, environment and human body are had to larger harm.(3) in phosphate aqueous solution, carry out anodic oxidation poor effect, the porous anodic alumina films pore size distribution finally obtaining is wider, and the degree of order is poor.
Summary of the invention
The object of the invention is to address the above problem, provide a kind of anodic oxidation effect better and technical process is shorter, be applicable to the preparation method of the highly ordered porous anodic film of industrialized production.
The technical scheme that realizes the object of the invention is: a kind of preparation method of highly ordered porous anodic film, comprises pre-treatment and anodic oxidation; Described anodic oxidation is that pretreated fine aluminium is put into electrolytic solution, anodic oxidation 1～4h at the temperature of-20～20 DEG C, under the voltage of 80～120V; Described electrolytic solution is the aqueous solution that contains phosphoric acid and cobalt salt, contains the phosphoric acid of 0.1～0.6mol and the cobalt salt of 0.1～0.8g in every liter of electrolytic solution.
Described cobalt salt is Co (NO
3)
26H
2o, CoCO
3, (NH
4)
2co (SO
4)
26H
2o, CoSO
47H
2o and CoC
2o
4in one.
Described pre-treatment is first by fine aluminium soaked in absolute ethyl alcohol 1～5min, and the sodium hydroxide solution that is then placed in 30～80 DEG C is removed surperficial natural oxide layer, is placed in immediately salpeter solution and carries out acid-base neutralisation reaction 5～30s after then taking out.
The concentration of described sodium hydroxide solution is 1～3mol/L.
The concentration of described salpeter solution is 1～3mol/L.
The present invention has positive effect: (1) method of the present invention adds a small amount of cobalt salt composition electrolytic solution in phosphate aqueous solution, adopt this electrolytic solution only need carry out an anodic oxidation and without the processing after electrochemical etching and polishing, so greatly shorten technical process, improve production efficiency, very applicable industrialized production.(2) even aperture distribution of the porous anodic oxide film that method of the present invention obtains, has order highly, and anodic oxidation successful is better than prior art.(3) method of the present invention can also be prepared the anode oxide film of respective aperture according to specific needs, has advantages of that pore size is adjustable.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph on the highly ordered porous anodic film surface that makes of embodiment 1.
Fig. 2 is the graph of pore diameter distribution of the highly ordered porous anodic film that makes of embodiment 1.
Embodiment
(embodiment 1)
The preparation method of the highly ordered porous anodic film of the present embodiment is as follows:
1. pre-treatment: first fine aluminium is soaked in dehydrated alcohol to 3min, to remove the organism of surface of pure aluminum, then take out with clear water clean, and be placed in the sodium hydroxide solution that 50 DEG C of concentration are 2mol/L and process 20s, to remove the natural oxide layer of surface of pure aluminum, the salpeter solution that is placed in immediately concentration after then taking out and is 2mol/L carries out acid-base neutralisation reaction 20s, after finally taking out, cleans, dries with clear water.
2. prepare electrolytic solution: by the CoSO of 0.6g
47H
2o joins in the phosphoric acid solution that 300mL concentration is 1mol/L and dissolves, and adds water and supply 1L, obtains electrolytic solution.
3. anodic oxidation: by through step 1. pretreated fine aluminium put in the electrolytic solution that 2. step prepare and carry out anodic oxidation, oxidation voltage is 90V, oxidization time is 1.5h, in anode oxidation process, by recirculated cooling water, oxidizing temperature is controlled to 10 DEG C.
4. after anodic oxidation treatment, use ultrasonic washing with clean water 5min, hot-air seasoning, obtains highly ordered porous anodic film.
The scanning electron microscope (SEM) photograph of the highly ordered porous anodic film that the present embodiment makes is shown in Fig. 1, and graph of pore diameter distribution is shown in Fig. 2.
Can be found out by Fig. 1 and Fig. 2: the porous anodic oxide film even aperture distribution that the present embodiment makes, has order highly.
(embodiment 2～embodiment 5)
The preparation method of each embodiment is substantially the same manner as Example 1, and difference is in table 1.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Cobalt salt | CoSO 4·7H 2O | Co(NO 3) 2·6H 2O | (NH 4) 2Co(SO 4) 2·6H 2O | CoCO 3 | CoC 2O 4 |
| Cobalt salt concentration | 0.6g/L | 0.7g/L | 0.4g/L | 0.1g/L | 0.8g/L |
| Phosphoric acid concentration | 0.3mol/L | 0.4mol/L | 0.2mol/L | 0.1mol/L | 0.6mol/L |
| Oxidation voltage | 90V | 110V | 100V | 120V | 120V |
| Oxidization time | 1.5h | 2h | 2.5h | 1h | 4h |
| Oxidizing temperature | 10℃ | 5℃ | 0℃ | 20℃ | -20℃ |
Claims (5)
1. a preparation method for highly ordered porous anodic film, comprises pre-treatment and anodic oxidation; Described anodic oxidation is that pretreated fine aluminium is put into electrolytic solution, anodic oxidation 1～4h at the temperature of-20～20 DEG C, under the voltage of 80～120V; It is characterized in that: described electrolytic solution is the aqueous solution that contains phosphoric acid and cobalt salt, in every liter of electrolytic solution, contain the phosphoric acid of 0.1～0.6mol and the cobalt salt of 0.1～0.8g.
2. the preparation method of highly ordered porous anodic film according to claim 1, is characterized in that: described cobalt salt is Co (NO
3)
26H
2o, CoCO
3, (NH
4)
2co (SO
4)
26H
2o, CoSO
47H
2o and CoC
2o
4in one.
3. the preparation method of highly ordered porous anodic film according to claim 1 and 2, it is characterized in that: described pre-treatment is first by fine aluminium soaked in absolute ethyl alcohol 1～5min, then the sodium hydroxide solution that is placed in 30～80 DEG C is removed surperficial natural oxide layer, is placed in immediately salpeter solution and carries out acid-base neutralisation reaction 5～30s after then taking out.
4. the preparation method of highly ordered porous anodic film according to claim 3, is characterized in that the concentration of described sodium hydroxide solution is 1～3mol/L.
5. the preparation method of highly ordered porous anodic film according to claim 3, is characterized in that: the concentration of described salpeter solution is 1～3mol/L.
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|---|---|---|---|
| CN201410220482.1A CN103966642B (en) | 2014-05-22 | 2014-05-22 | Preparation method of highly ordered porous anodic oxide film |
| CN201610597073.2A CN106048688B (en) | 2014-05-22 | 2014-05-22 | Preparation method of highly ordered porous anodic oxide film |
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|---|---|---|---|
| CN201410220482.1A CN103966642B (en) | 2014-05-22 | 2014-05-22 | Preparation method of highly ordered porous anodic oxide film |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3717555A (en) * | 1970-11-27 | 1973-02-20 | Fentron Ind Inc | Method of producing an electrolytic coating on aluminum and the product thereof |
| JPS5613497A (en) * | 1979-07-09 | 1981-02-09 | Toshiba Corp | Electrolytic coloring method for aluminum group metal |
| SU1145061A1 (en) * | 1982-12-06 | 1985-03-15 | Белорусский Ордена Трудового Красного Знамени Государственный Университет Им.В.И.Ленина | Electrolyte for electrochemical painting of anodized aluminium black and method of preparing same |
| KR20020069977A (en) * | 2001-02-28 | 2002-09-05 | 주식회사 범일 | Color titanium-zirconium alloy and method for manufacturing the same |
| CN1396063A (en) * | 2001-07-06 | 2003-02-12 | 富士胶片株式会社 | Original plate of plane printing plate |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1325698C (en) * | 2003-10-21 | 2007-07-11 | 东莞理工学院 | Preparation method of ordered porous anodic alumina template |
| CN100460327C (en) * | 2006-01-23 | 2009-02-11 | 中国科学院化学研究所 | Process for preparing highly-hydrophilic alumina film material |
| CN103789808B (en) * | 2012-10-31 | 2017-12-01 | 深圳富泰宏精密工业有限公司 | The surface treatment method and aluminum products of aluminium alloy |
-
2014
- 2014-05-22 CN CN201610597073.2A patent/CN106048688B/en active Active
- 2014-05-22 CN CN201410220482.1A patent/CN103966642B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3717555A (en) * | 1970-11-27 | 1973-02-20 | Fentron Ind Inc | Method of producing an electrolytic coating on aluminum and the product thereof |
| JPS5613497A (en) * | 1979-07-09 | 1981-02-09 | Toshiba Corp | Electrolytic coloring method for aluminum group metal |
| SU1145061A1 (en) * | 1982-12-06 | 1985-03-15 | Белорусский Ордена Трудового Красного Знамени Государственный Университет Им.В.И.Ленина | Electrolyte for electrochemical painting of anodized aluminium black and method of preparing same |
| KR20020069977A (en) * | 2001-02-28 | 2002-09-05 | 주식회사 범일 | Color titanium-zirconium alloy and method for manufacturing the same |
| CN1396063A (en) * | 2001-07-06 | 2003-02-12 | 富士胶片株式会社 | Original plate of plane printing plate |
Non-Patent Citations (2)
| Title |
|---|
| A.GHAHREMANINEZHAD ET AL: "A study on electrochemical growth behavior of the Co-Ni alloy nanowires in anodic aluminum oxide template", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| 马迪 等: "铝箔多孔阳极氧化铝膜的低温制备及其电化学性能", 《材料保护》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103966642B (en) | 2016-08-17 |
| CN106048688A (en) | 2016-10-26 |
| CN106048688B (en) | 2017-11-21 |
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