CN106048688B - A kind of preparation method of highly ordered porous anodic film - Google Patents
A kind of preparation method of highly ordered porous anodic film Download PDFInfo
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- CN106048688B CN106048688B CN201610597073.2A CN201610597073A CN106048688B CN 106048688 B CN106048688 B CN 106048688B CN 201610597073 A CN201610597073 A CN 201610597073A CN 106048688 B CN106048688 B CN 106048688B
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- highly ordered
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 29
- 230000003647 oxidation Effects 0.000 claims abstract description 24
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000003792 electrolyte Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 12
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004411 aluminium Substances 0.000 claims abstract description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 7
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 239000000498 cooling water Substances 0.000 claims description 2
- 235000011194 food seasoning agent Nutrition 0.000 claims description 2
- 239000005416 organic matter Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 150000001868 cobalt Chemical class 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000009826 distribution Methods 0.000 abstract description 6
- 239000007864 aqueous solution Substances 0.000 abstract description 5
- 229910019167 CoC2 Inorganic materials 0.000 abstract description 3
- ZJRWDIJRKKXMNW-UHFFFAOYSA-N carbonic acid;cobalt Chemical compound [Co].OC(O)=O ZJRWDIJRKKXMNW-UHFFFAOYSA-N 0.000 abstract description 3
- 229910000001 cobalt(II) carbonate Inorganic materials 0.000 abstract description 3
- 239000010407 anodic oxide Substances 0.000 abstract description 2
- 238000005498 polishing Methods 0.000 abstract description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 11
- 239000000243 solution Substances 0.000 description 10
- 239000012528 membrane Substances 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 229910019142 PO4 Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011159 matrix material 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
- 230000002378 acidificating effect Effects 0.000 description 2
- 238000007743 anodising Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 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
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 238000005275 alloying 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
- 230000007812 deficiency Effects 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment 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
Abstract
The invention discloses a kind of preparation method of highly ordered porous anodic film, including pretreatment and anodic oxidation.Anodic oxidation is that pretreated fine aluminium is put into electrolyte, at a temperature of 20~20 DEG C, 80~120V 1~4h of voltage anodic oxygenization.Electrolyte is the aqueous solution containing phosphoric acid and cobalt salt, the phosphoric acid containing 0.1~0.6mol and 0.1~0.8g cobalt salt in every liter of electrolyte.Cobalt salt is Co (NO3)2·6H2O、CoCO3、(NH4)2Co(SO4)2·6H2O、CoSO4·7H2O and CoC2O4In one kind.The preparation method of the present invention need to only carry out an anodic oxidation and without the processing after electrochemical polish and polishing, this substantially reduces technological process, improve production efficiency, it is very suitable for industrialized production, and the even aperture distribution of obtained porous anodic oxide film, the order with height.
Description
The application is Application No. 201410220482.1, and the applying date is on May 22nd, 2014, and invention and created name is
The divisional application of the application for a patent for invention of " preparation method of highly ordered porous anodic film ".
Technical field
The invention belongs to field of metal surface treatment technology, and in particular to a kind of system of highly ordered porous anodic film
Preparation Method.
Background technology
Porous anodic alumina films（AAO）It is to be formed by the method for electrochemical oxidation in surface of pure aluminum with highly regular
The aluminum oxide film of pore structure.Its membrane structure is the closelypacked cylindricality after birth of hexagon, and the center of each after birth has one
It is nanometer level microporous.
Porous anodic alumina films are heat and the good insulator of electricity, have the characteristics that hardness is high, wearability is good；Have very well
Corrosion resistance, its resistance to corrosion is decided by the alloying component of thicknesses of layers, composition, porosity and matrix material；With matrix gold
The adhesion of category is also very strong, even if film layer is bent to fracture with matrix, film layer still can and parent metal remain good combination.
As people are to porous anodic alumina films unique microstructures and the understanding of property, porous anodic aluminium oxide
Film is gradually widely used in catalysis, magnetic pipe recording material, optics and photoelectric cell, antibacterial film, separation membrane material, sensor etc.
Various functions field, turn into the focus of scholars' research.
At present, the preparation of porous anodic alumina films is mainly using two step anodizings（Such as Chinese patent literature
CN1609283A, CN101007645A, CN101139730A etc.）, i.e., first aluminium is pre-processed, then in acidic electrolysis bath
Middle to be aoxidized first, oxidization time is usually 1h~5h, then removes oxide-film caused by oxidation first by chemical attack,
Secondary oxidation is finally carried out in acidic electrolysis bath again, oxidization time is usually 2h~12h, obtains porous anodic alumina films.
Wherein pretreatment mainly includes cleaning and electrochemical polish, and the main function of electrochemical polish is to obtain smoother surface,
So as to obtain size and the porous array film more uniformly spread after being advantageous to anodic oxidation.The solution that electrochemical polish uses is equal
It is made up of absolute ethyl alcohol and perchloric acid according to certain volume ratio.The shortcomings that this method, is：（1）Anodizing time compared with
It is long, so as to cause the production cycle；（2）The oxide-film degree of order caused by oxidation is poor first, porous so as to influence to finally give
The degree of order of anodic alumina films.
Chinese patent literature CN103225096A discloses a kind of preparation method of porous anodic alumina films, including pre- place
Reason, electrochemical polish, remove nanometer porous film layer, anodic oxidation and cleaning and drying that electrochemical polish is formed.Wherein
The electrolyte that anodic oxidation uses is 0.2mol/L~0.6mol/L phosphate aqueous solution.The deficiency of the document is：（1）Although
An anodic oxidation is only carried out, but needs to carry out electrochemical polish and treatment fluid membrane removal, therefore technique stream before the oxidation
Journey is still longer, is not suitable for industrialized production.（2）Membrane removal is carried out using chromium-containing solution, has larger harm to environment and human body.
（3）Progress anodic oxidation effect is bad in phosphate aqueous solution, and the porous anodic alumina films pore-size distribution finally given is wider,
The degree of order is poor.
The content of the invention
It is an object of the invention to solve the above problems, there is provided a kind of anodic oxidation effect preferably and technological process it is shorter,
It is adapted to the preparation method of the highly ordered porous anodic film of industrialized production.
Realizing the technical scheme of the object of the invention is：A kind of preparation method of highly ordered porous anodic film, including
Pretreatment and anodic oxidation；Described anodic oxidation is that pretreated fine aluminium is put into electrolyte, in -20~20 DEG C of temperature
Under degree, 80~120V 1~4h of voltage anodic oxygenization；Described electrolyte is the aqueous solution containing phosphoric acid and cobalt salt, every liter
Phosphoric acid containing 0.1~0.6mol and 0.1~0.8g cobalt salt in electrolyte.
Described cobalt salt is Co (NO3)2·6H2O、CoCO3、(NH4)2Co(SO4)2·6H2O、CoSO4·7H2O and
CoC2O4In one kind.
Described pretreatment is that fine aluminium 1~5min of soaked in absolute ethyl alcohol is first subsequently placed in 30~80 DEG C of hydroxide
In sodium solution remove surface natural oxide layer, then take out after be immediately placed in salpeter solution carry out acid-base neutralization reaction 5~
30s。
The concentration of described sodium hydroxide solution is 1~3mol/L.
The concentration of the salpeter solution is 1~3mol/L.
The present invention has positive effect：（1）The method of the present invention adds a small amount of cobalt salt composition electricity in phosphate aqueous solution
Liquid is solved, an anodic oxidation need to be only carried out using the electrolyte and without the processing after electrochemical polish and polishing, it is so big
Technological process is shortened greatly, production efficiency is improved, is very suitable for industrialized production.（2）The method of the present invention obtains more
The even aperture distribution of hole anode oxide film, has the order of height, and anodic oxidation effect is substantially better than prior art.（3）
The method of the present invention can also prepare the anode oxide film of respective aperture according to specific needs, have pore size adjustable excellent
Point.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph on highly ordered porous anodic film surface made from embodiment 1.
Fig. 2 is the graph of pore diameter distribution of highly ordered porous anodic film made from embodiment 1.
Embodiment
（Embodiment 1）
The preparation method of the highly ordered porous anodic film of the present embodiment is as follows：
1. pre-process：Fine aluminium is first soaked into 3min in absolute ethyl alcohol, to remove the organic matter of surface of pure aluminum, then taken out
Cleaned with clear water, be placed in handling 20s in the sodium hydroxide solution that 50 DEG C of concentration are 2mol/L, to remove the natural of surface of pure aluminum
Oxide layer, it is immediately placed on after then taking out in the salpeter solution that concentration is 2mol/L and carries out carrying out acid-base neutralization reaction 20s, finally
Cleaned after taking-up with clear water, drying.
2. prepare electrolyte：By 0.6g CoSO4·7H2O is added to molten in the phosphoric acid solution that 300mL concentration is 1mol/L
Solution, and add water to supply 1L, obtain electrolyte.
3. anodic oxidation：By through step, 1. pretreated fine aluminium is put into 2. electrolyte that step prepares and carries out anode
Aoxidize, oxidation voltage 90V, oxidization time 1.5h, controlled oxidizing temperature by recirculated cooling water in anode oxidation process
At 10 DEG C.
4. after anodized, with ultrasonic washing with clean water 5min, hot-air seasoning, produce highly ordered porous anodic
Film.
The scanning electron microscope (SEM) photograph of highly ordered porous anodic film is shown in Fig. 1 made from the present embodiment, and graph of pore diameter distribution is shown in figure
2。
It can be seen that by Fig. 1 and Fig. 2：Porous anodic oxide film even aperture distribution made from the present embodiment, there is height
Order.
（2~embodiment of embodiment 5）
The preparation method of each embodiment is substantially the same manner as Example 1, and difference is to be shown in Table 1.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Cobalt salt | CoSO4·7H2O | Co(NO3)2·6H2O | (NH4)2Co(SO4)2·6H2O | CoCO3 | CoC2O4 |
| 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 (1)
1. a kind of preparation method of highly ordered porous anodic film, specific as follows；
1. pre-process：Fine aluminium is first soaked into 3min in absolute ethyl alcohol, to remove the organic matter of surface of pure aluminum, then taken out with clear
Water is cleaned, and is placed in handling 20s in the sodium hydroxide solution that 50 DEG C of concentration are 2mol/L, to remove the Native Oxide of surface of pure aluminum
Layer, it is immediately placed on after then taking out in the salpeter solution that concentration is 2mol/L and carries out carrying out acid-base neutralization reaction 20s, finally taken out
Cleaned afterwards with clear water, drying；
2. prepare electrolyte：By 0.6g CoSO4·7H2O, which is added in the phosphoric acid solution that 300mL concentration is 1mol/L, to be dissolved, and
Add water to supply 1L, obtain electrolyte；
3. anodic oxidation：By through step, 1. pretreated fine aluminium is put into 2. electrolyte that step prepares and carries out anodic oxygen
Change, oxidation voltage 90V, oxidization time 1.5h, controlled oxidizing temperature by recirculated cooling water in anode oxidation process
10℃；
4. after anodized, with ultrasonic washing with clean water 5min, hot-air seasoning, produce highly ordered porous anodic film.
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| CN201610597073.2A CN106048688B (en) | 2014-05-22 | 2014-05-22 | A kind of preparation method of highly ordered porous anodic film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410220482.1A CN103966642B (en) | 2014-05-22 | 2014-05-22 | The preparation method of highly ordered porous anodic film |
| CN201610597073.2A CN106048688B (en) | 2014-05-22 | 2014-05-22 | A kind of preparation method of highly ordered porous anodic film |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1609283A (en) * | 2003-10-21 | 2005-04-27 | 东莞理工学院 | Process for producing ordered porous anodic alumina form |
| CN101007645A (en) * | 2006-01-23 | 2007-08-01 | 中国科学院化学研究所 | Process for preparing highly-hydrophilic alumina film material |
Family Cites Families (6)
| 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 |
| KR100439766B1 (en) * | 2001-02-28 | 2004-07-12 | 주식회사 범일 | Color titanium-zirconium alloy and method for manufacturing the same |
| EP1273439B1 (en) * | 2001-07-06 | 2006-05-17 | Fuji Photo Film Co., Ltd. | Presensitized plate for use in making lithographic printing plate |
| 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 |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1609283A (en) * | 2003-10-21 | 2005-04-27 | 东莞理工学院 | Process for producing ordered porous anodic alumina form |
| CN101007645A (en) * | 2006-01-23 | 2007-08-01 | 中国科学院化学研究所 | Process for preparing highly-hydrophilic alumina film material |
Non-Patent Citations (2)
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| "草酸中纳米孔阵列阳极氧化铝膜的一步法制备及其形貌表征";杨文彬 等;《草酸中纳米孔阵列阳极氧化铝膜的一步法制备及其形貌表征》;20050930;第25卷(第9期);第41-43页 * |
| "铝箔多孔阳极氧化铝膜的低温制备及其电化学性能";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》;20120615;第45卷(第6期);第4-6页 * |
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| CN106048688A (en) | 2016-10-26 |
| CN103966642A (en) | 2014-08-06 |
| CN103966642B (en) | 2016-08-17 |
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