CN105887156B - The preparation method of the porous anodic alumina films of high-sequential - Google Patents
The preparation method of the porous anodic alumina films of high-sequential Download PDFInfo
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- CN105887156B CN105887156B CN201610261245.9A CN201610261245A CN105887156B CN 105887156 B CN105887156 B CN 105887156B CN 201610261245 A CN201610261245 A CN 201610261245A CN 105887156 B CN105887156 B CN 105887156B
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 49
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000004411 aluminium Substances 0.000 claims abstract description 33
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 24
- 230000003647 oxidation Effects 0.000 claims abstract description 21
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229960004063 propylene glycol Drugs 0.000 claims abstract description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 18
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 12
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 2
- 235000011194 food seasoning agent Nutrition 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 229910000423 chromium oxide Inorganic materials 0.000 claims 1
- 238000004140 cleaning Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 3
- 229940117975 chromium trioxide Drugs 0.000 description 10
- GAMDZJFZMJECOS-UHFFFAOYSA-N chromium(6+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Cr+6] GAMDZJFZMJECOS-UHFFFAOYSA-N 0.000 description 10
- 239000003792 electrolyte Substances 0.000 description 8
- 238000009826 distribution Methods 0.000 description 6
- 239000012530 fluid Substances 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 4
- 238000007743 anodising Methods 0.000 description 4
- 238000005868 electrolysis reaction Methods 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000010306 acid treatment Methods 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 230000005518 electrochemistry Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003892 spreading Methods 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
- C25D11/16—Pretreatment, e.g. desmutting
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/16—Polishing
- C25F3/18—Polishing of light metals
- C25F3/20—Polishing of light metals of aluminium
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Catalysts (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
- Printing Plates And Materials Therefor (AREA)
- Manufacturing Of Magnetic Record Carriers (AREA)
- Photoreceptors In Electrophotography (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a kind of preparation methods of the porous anodic alumina films of high-sequential, have steps of：1. being pre-processed to surface of pure aluminum；2. carrying out electrochemical polish to pretreated fine aluminium；The electrochemical polish solution is made of 1,2 propylene glycol and perchloric acid according to 9: 1~2: 1 volume ratio；3. removing the nanometer porous film layer of surface of pure aluminum；4. carrying out anodic oxidation 1h~5h；5. cleaning and drying.The present invention forms nanometer porous film layer in surface of pure aluminum using electrochemical polish, substantially reduces the production cycle by selecting suitable electrochemical polish solution and suitable electrochemical polish condition.And the present invention may finally obtain the porous anodic alumina films of high-sequential.
Description
The application is application No. is 201310188114.9, and the applying date is on May 17th, 2013, and invention and created name is
The divisional application of the application for a patent for invention of " preparation methods of porous anodic alumina films ".
Technical field
The invention belongs to field of metal surface treatment technology, and in particular to a kind of preparation side of porous anodic alumina films
Method.
Background technology
Aluminium is the active metal of comparison, in air can about hundreds of nanometers of one thickness of self-assembling formation oxidation film, this layer of oxygen
It is amorphous to change film, and thin porous, mechanical strength is low, cannot be satisfied the requirement of functionalized application.
In order to obtain the oxidation film layer of specific function, it is necessary to handle aluminium surface, typically in the electrolytic solution, by aluminium
Electrolysis processing is carried out as anode, to obtain oxidation film in aluminium surface.According to the difference of electrolyte, densification can be respectively obtained
（Or blocking）Anodic alumina films and porous anodic alumina films.It is fine and close（Or blocking）Anodic alumina films are in neutral electrolyte
In anodic oxidation carried out to aluminium obtain, it is a kind of fine and close, unformed, in homogeneous thickness pellumina, this oxidation
Aluminium film has good dielectric properties, can be used as the anode foils of aluminium electrolutic capacitor.Porous anodic alumina films be then oxalic acid,
What anodic oxidation obtained is carried out to aluminium in acidic electrolysis bath of phosphoric acid, the sulfuric acid etc. itself with certain oxidability, it is by one layer
It is in six side's solid matter periodic structures, porous anodic alumina films master close to the barrier layer of metal and outer layer Woelm Alumina composition
It is used for filter membrane and prepares the template of nano material.
Currently, 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 for the first time, oxidization time is usually 1h~5h, and the oxidation film for aoxidizing generation for the first time is then removed 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 includes mainly cleaning and electrochemical polish, and the main function of electrochemical polish is to obtain smoother surface,
To be conducive to the porous array film for obtaining size after anodic oxidation and more uniformly spreading.The solution that electrochemical polish uses is equal
It is made of according to certain volume ratio absolute ethyl alcohol and perchloric acid.The disadvantages of this method is：（1）Anodizing time compared with
It is long, so as to cause the production cycle；（2）The oxidation film degree of order for aoxidizing generation for the first time is poor, finally obtained porous to influence
The degree of order of anodic alumina films.
Invention content
It is an object of the invention to solve the above problems, provide that a kind of production cycle is shorter, porous anode of high-sequential
The preparation method of pellumina.
Realizing the technical solution of the object of the invention is：A kind of preparation method of porous anodic alumina films has following step
Suddenly：1. being pre-processed to surface of pure aluminum；2. using step 1. pretreated fine aluminium as anode and with as cathode platinum electricity
Pole is put into togerther in electrochemical polish solution, and anode and cathode spacing is made to be 50mm~70mm, then at ambient temperature（0 DEG C~
40 DEG C, similarly hereinafter）, in 80mA/cm2~160mA/cm2Current density under carry out electrochemical polish 10s~90s, in fine aluminium
Surface forms nanometer porous film layer；The electrochemical polish solution is by 1,2- propylene glycol and perchloric acid according to 9: 1~2: 1
Volume ratio forms；Or 1. pretreated fine aluminium is put into togerther electrochemistry as anode and with the graphite as cathode using step
In polishing solution, electrochemical polish 10s~90s is carried out under the voltage of 15V~50V, to form nanoscale in surface of pure aluminum
Porous membrane layer；The electrochemical polish solution is made of absolute ethyl alcohol and perchloric acid according to 10: 1~3: 1 weight ratio；3. will
2. step is immersed in 0.5h~6h in 50 DEG C~90 DEG C for the treatment of fluid after the fine aluminium washing after electrochemical polish, it is pure to remove
The nanometer porous film layer of aluminium surface；4. by being put into electrolyte after step 3. treated fine aluminium washing, 60V~140V's
Anodic oxidation 1h~5h is carried out at a temperature of voltage and -10 DEG C~20 DEG C；5. being carried out to the fine aluminium after step 4. anodic oxidation
Cleaning and drying.
Above-mentioned steps 3. described in treatment fluid be every liter of chromium trioxide containing 10g~25g and 10mL~35mL
The aqueous solution of phosphoric acid.
Above-mentioned steps 4. described in electrolyte be 0.2mol/L~0.6mol/L phosphate aqueous solution.
Above-mentioned steps 1. described in surface of pure aluminum carry out pretreatment be will through oil removing and washing after fine aluminium be placed in 60
DEG C~80 DEG C of aqueous slkali in 30s~60s, take out and wash, then be placed in dipping 30s~60s, taking-up in dilute nitric acid solution and go forward side by side
Row is cleaned by ultrasonic 5min~10min.The aqueous slkali is the aqueous solution of every liter of sodium hydroxide containing 15g~30g.Described
The percent by volume of dilute nitric acid solution is 10%~30%.
Above-mentioned steps 5. described in cleaning be with deionized water be cleaned by ultrasonic 5min~10min；The drying is heat
Wind is dried.
The good effect that the present invention has：（1）The present invention is by the suitable electrochemical polish solution of selection and suitably
Electrochemical polish condition forms nanometer porous film layer in surface of pure aluminum using electrochemical polish, is equivalent to two step anodic oxidations
Oxidation for the first time in method, but for the first time oxidization time of the electrochemical polish time of 10s~90s compared to 1h~5h, greatly shorten
Production cycle.（2）The nanometer porous film layer that the electrochemical polish of the present invention obtains also has big, high-sequential of range etc. excellent
Point may finally obtain the porous anodic alumina films of high-sequential.（3）The method and process of the present invention is simple, and cost is relatively low.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph on porous anodic alumina films surface made from embodiment 1.
Fig. 2 is the graph of pore diameter distribution of porous anodic alumina films made from embodiment 1.
Fig. 3 is the scanning electron microscope (SEM) photograph on porous anodic alumina films surface made from embodiment 5.
Fig. 4 is the graph of pore diameter distribution of porous anodic alumina films made from embodiment 5.
Specific implementation mode
（Embodiment 1）
The preparation method of the porous anodic alumina films of the present embodiment has steps of：
1. being pre-processed to surface of pure aluminum：
First, fine aluminium is put into absolute ethyl alcohol and impregnates 5min, to remove the greasy dirt when machining of surface.Then, it uses
Clear water washes fine aluminium, to remove the dust and dirt of surface of pure aluminum.Then, the fine aluminium after clear water being washed is placed in 60 DEG C of alkali
30s in solution, to remove the natural thin oxide layer of surface of pure aluminum, the aqueous slkali is every liter and contains 20g sodium hydroxides
Aqueous solution.Followed by, by fine aluminium take out and washed again with clear water, be placed in percent by volume for 25% dilute nitric acid solution in
Impregnate 30s.Finally, fine aluminium is taken out and is cleaned by ultrasonic 5min with deionized water.
2. using step 1. pretreated fine aluminium as anode and with the platinum electrode as cathode be put into togerther electrochemistry throw
In light solution, and anode and cathode spacing is made to be 60mm, then at ambient temperature（The present embodiment is 10 DEG C）, in 120mA/cm2's
Electrochemical polish 60s is carried out under current density, to form nanometer porous film layer in surface of pure aluminum；
Above-mentioned electrochemical polish solution is made of 1,2- propylene glycol and perchloric acid according to 4: 1 volume ratio.
3. 3h in 60 DEG C for the treatment of fluid is immersed in after the fine aluminium after step 2. electrochemical polish is washed with clear water, to go
Except the nanometer porous film layer of surface of pure aluminum.
Above-mentioned treatment fluid is the aqueous solution of every liter of chromium trioxide containing 20g and the phosphoric acid of 30mL.
4. by step, 3. treated is put into electrolyte after fine aluminium washed with clear water, in the voltage of 110V and 5 DEG C
At a temperature of carry out anodic oxidation 1h.
Above-mentioned electrolyte is the phosphate aqueous solution of 0.4mol/L.
5. being cleaned by ultrasonic 10min, then hot-air seasoning to the deionized water of the fine aluminium after step 4. anodic oxidation.
The scanning electron microscope (SEM) photograph on porous anodic alumina films surface made from the present embodiment is shown in that Fig. 1, graph of pore diameter distribution are shown in Fig. 2,
From Fig. 1 and Fig. 2：The pore-size distribution of porous anodic alumina films made from the present embodiment is highly uniform, and average pore size is
320nm or so, porosity is up to 30%.
（2~embodiment of embodiment 4）
The preparation method of each embodiment is substantially the same manner as Example 1, and difference is shown in Table 1.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Electrochemical polish solution | 1,2- propylene glycol: perchloric acid 4: 1 | 1,2- propylene glycol: perchloric acid 5: 1 | 1,2- propylene glycol: perchloric acid 6: 1 | 1,2- propylene glycol: perchloric acid 2: 1 |
| Anode and cathode spacing | 60mm | 60mm | 60mm | 70mm |
| Current density | 120mA/cm2 | 150mA/cm2 | 100mA/cm2 | 160mA/cm2 |
| Electrochemical polish temperature | 10℃ | 5℃ | 0℃ | 30℃ |
| The electrochemical polish time | 60s | 50s | 40s | 90s |
| Treatment fluid | Every liter of chromium trioxide containing 20g and 30mL phosphoric acid | Every liter of chromium trioxide containing 15g and 25mL phosphoric acid | Every liter of chromium trioxide containing 25g and 35mL phosphoric acid | Every liter of chromium trioxide containing 10g and 30mL phosphoric acid |
| Treatment temperature | 60℃ | 60℃ | 70℃ | 80℃ |
| Processing time | 3h | 2h | 5h | 4h |
| Electrolyte | 0.4mol/L | 0.3mol/L | 0.6mol/L | 0.4mol/L |
| Anodic oxidation voltage | 110V | 90V | 80V | 100V |
| Anodizing temperature | 5℃ | 10℃ | 10℃ | 5℃ |
（Embodiment 5）
The preparation method of the present embodiment is substantially the same manner as Example 1, the difference is that step is 2.：1. step is pre-processed
Fine aluminium afterwards is put into togerther as anode and with the graphite as cathode in electrochemical polish solution, is carried out under the voltage of 20V
Electrochemical polish 30s, to form nanometer porous film layer in surface of pure aluminum.
Above-mentioned electrochemical polish solution is made of absolute ethyl alcohol and perchloric acid according to 4: 1 weight ratio.
The scanning electron microscope (SEM) photograph on porous anodic alumina films surface made from the present embodiment is shown in that Fig. 3, graph of pore diameter distribution are shown in Fig. 4,
As can be seen from figs. 3 and 4：The pore-size distribution of porous anodic alumina films made from the present embodiment is a bit weaker, and porosity also only has
5% or so, average pore size 80nm.
（6~embodiment of embodiment 8）
The preparation method of each embodiment is substantially the same manner as Example 5, and difference is shown in Table 2.
Table 2
| Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 | |
| Electrochemical polish solution | Absolute ethyl alcohol: perchloric acid 4: 1 | Absolute ethyl alcohol: perchloric acid 5: 1 | Absolute ethyl alcohol: perchloric acid 6: 1 | Absolute ethyl alcohol: perchloric acid 10: 1 |
| Electrochemical polish voltage | 20V | 20V | 25V | 25V |
| The electrochemical polish time | 30s | 20s | 10s | 30s |
| Treatment fluid | Every liter of chromium trioxide containing 20g and 30mL phosphoric acid | Every liter of chromium trioxide containing 15g and 25mL phosphoric acid | Every liter of chromium trioxide containing 25g and 35mL phosphoric acid | Every liter of chromium trioxide containing 10g and 30mL phosphoric acid |
| Treatment temperature | 60℃ | 60℃ | 70℃ | 80℃ |
| Processing time | 3h | 2h | 5h | 4h |
| Electrolyte | 0.4mol/L | 0.2mol/L | 0.3mol/L | 0.5mol/L |
| Anodic oxidation voltage | 110V | 90V | 80V | 100V |
| Anodizing temperature | 5℃ | 10℃ | 10℃ | 5℃ |
Claims (1)
1. a kind of preparation method of the porous anodic alumina films of high-sequential, it is characterised in that have steps of：
1. being pre-processed to surface of pure aluminum；
2. using step, 1. to be put into togerther electrochemical polish as anode and with the platinum electrode as cathode molten for pretreated fine aluminium
In liquid, and anode and cathode spacing is made to be 50mm~70mm, then at a temperature of 0 DEG C~40 DEG C, in 80mA/cm2~160mA/cm2
Current density under carry out electrochemical polish 10s~90s, in surface of pure aluminum form nanometer porous film layer；The electricity
Chemical polishing soln is made of 1,2- propylene glycol and perchloric acid according to 9: 1~2: 1 volume ratio；
Or 1. to be put into togerther electrochemical polish as anode and with the graphite as cathode molten for pretreated fine aluminium using step
In liquid, electrochemical polish 10s~90s is carried out under the voltage of 15V~50V, to form nanometer porous film in surface of pure aluminum
Layer；The electrochemical polish solution is made of absolute ethyl alcohol and perchloric acid according to 10: 1~3: 1 weight ratio；
3. by every liter of 50 DEG C~90 DEG C three containing 10g~25g are immersed in after the fine aluminium washing after step 2. electrochemical polish
0.5h~6h in the aqueous solution of the phosphoric acid of chromium oxide and 10mL~35mL, to remove the nanometer porous film of surface of pure aluminum
Layer；
4. by being put into 0.2mol/L~0.6mol/L phosphate aqueous solutions after step 3. treated fine aluminium washing, 60V~
Anodic oxidation 1h~5h is carried out at a temperature of the voltage of 140V and -10 DEG C~20 DEG C；
5. being first cleaned by ultrasonic 5min~10min with deionized water to the fine aluminium after step 4. anodic oxidation, then hot-air seasoning.
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| CN104294344A (en) * | 2014-09-19 | 2015-01-21 | 华南理工大学 | Method for preparing nano/submicron/micron multi-stage anode alumina template |
| CN106400021B (en) * | 2016-08-30 | 2019-06-11 | 成都凯赛尔电子有限公司 | A kind of electrical pure iron and its oxidation resistant processing method of piece surface |
| CN108251877A (en) * | 2016-12-29 | 2018-07-06 | 北京有色金属研究总院 | A kind of Woelm Alumina film layer and preparation method thereof |
| CN107236985A (en) * | 2017-07-26 | 2017-10-10 | 江苏苏丰机械科技有限公司 | A kind of method of almag casting electrochemical deoiling |
| TWI733963B (en) * | 2017-12-12 | 2021-07-21 | 國立成功大學 | Method of pretreatment for metal-plating with thick-film aluminum electrode |
| CN109989085B (en) * | 2019-03-27 | 2021-04-13 | 江苏理工学院 | Preparation method of porous anodic aluminum oxide film |
| CN109972183A (en) * | 2019-03-27 | 2019-07-05 | 江苏理工学院 | The preparation method of deposit cobalt on a kind of anodic oxidation aluminium formwork |
| CN111088503A (en) * | 2019-12-31 | 2020-05-01 | 中山市皓祥模具五金有限公司 | Surface treatment process for aluminum product |
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| JPS6428397A (en) * | 1987-07-23 | 1989-01-30 | Mitsubishi Aluminium | Production of wheel rim |
| CN1880516B (en) * | 2006-04-30 | 2010-06-23 | 浙江工业大学 | Template for preparing nano materials and its preparation and application |
| CN1974873A (en) * | 2006-11-23 | 2007-06-06 | 上海交通大学 | Fast stable growth process of alumina film with nanometer pore array in relatively great pore distance |
| CN101240440B (en) * | 2007-11-16 | 2011-02-16 | 苏州有色金属研究院有限公司 | Technique for preparing high-hardness large-aperture thick film by mixed acid anode oxidation |
| CN101603192A (en) * | 2009-07-14 | 2009-12-16 | 桂林理工大学 | A kind of method of utilizing commercial-purity aluminium to prepare porous anodic alumina films |
| CN102162115B (en) * | 2011-01-20 | 2012-05-02 | 浙江大学 | Color regulation and control method based on porous alumina and single atom deposition technology |
| CN102277607B (en) * | 2011-08-17 | 2013-07-10 | 中国科学院金属研究所 | Method for preparing through hole anode alumina film with controllable aperture and thickness |
| CN102776542A (en) * | 2012-07-25 | 2012-11-14 | 华南理工大学 | Preparation method of anodized aluminum film of through hole |
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2013
- 2013-05-17 CN CN201610261245.9A patent/CN105887156B/en active Active
- 2013-05-17 CN CN201310188114.9A patent/CN103225096B/en active Active
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| CN103225096A (en) | 2013-07-31 |
| CN105887156A (en) | 2016-08-24 |
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