CN105734662A - Preparation method of highly-ordered porous anodic alumina membrane - Google Patents
Preparation method of highly-ordered porous anodic alumina membrane Download PDFInfo
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- CN105734662A CN105734662A CN201610262587.2A CN201610262587A CN105734662A CN 105734662 A CN105734662 A CN 105734662A CN 201610262587 A CN201610262587 A CN 201610262587A CN 105734662 A CN105734662 A CN 105734662A
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- fine aluminium
- electrochemical polish
- pure aluminum
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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 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000012528 membrane Substances 0.000 title abstract description 6
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 47
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 47
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 18
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 16
- 230000003647 oxidation Effects 0.000 claims abstract description 15
- 239000004411 aluminium Substances 0.000 claims description 23
- 239000000243 solution Substances 0.000 claims description 18
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 claims description 11
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 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 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 3
- 239000011260 aqueous acid Substances 0.000 claims description 3
- 235000011194 food seasoning agent Nutrition 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
- 239000011574 phosphorus Substances 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000004140 cleaning Methods 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 2
- 238000005498 polishing Methods 0.000 abstract 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 18
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 229960000935 dehydrated alcohol Drugs 0.000 description 8
- 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
- 238000007743 anodising Methods 0.000 description 5
- 238000005868 electrolysis reaction Methods 0.000 description 4
- 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
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000010306 acid treatment Methods 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-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
- 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
- 238000007654 immersion Methods 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
- 230000000737 periodic effect Effects 0.000 description 1
- 235000011007 phosphoric acid Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/22—Light metals
-
- 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
Abstract
The invention discloses a preparation method of a highly-ordered porous anodic alumina membrane.The method comprises the following steps that 1, the surface of pure aluminum is preprocessed; 2, electrochemical polishing is performed on the preprocessed pure aluminum, and an electrochemical polishing solution is prepared from 1,2-propylene glycol and perchloric acid on the basis of the volume ratio being 9:1-2:1; 3, a nanoscale porous membrane layer on the surface of pure aluminum is removed; 4, anodic oxidation is performed for 1-5 h; 5, cleaning and drying are performed.By selecting the proper electrochemical polishing solution and proper electrochemical polishing conditions, the nanoscale porous membrane layer is formed on the surface of the pure aluminum by adopting electrochemical polishing, and the production cycle is greatly shortened.According to the preparation method, the highly-ordered porous anodic alumina membrane can be obtained finally.
Description
The application is Application No. 201310188114.9, filing date on May 17th, 2013, and invention and created name is the divisional application of the application for a patent for invention of " preparation method of porous anodic alumina films ".
Technical field
The invention belongs to field of metal surface treatment technology, be specifically related to the preparation method of a kind of porous anodic alumina films.
Background technology
Aluminum is the metal that comparison is active, in atmosphere can the oxide-film of the most hundreds of nanometer of self-assembling formation thick layer, this layer of oxide-film is amorphous, and thin porous, mechanical strength is low, it is impossible to meet the requirement of functionalized application.
In order to obtain the oxidation film layer of specific function, it is necessary to aluminum surface is processed, it is common that in the electrolytic solution, aluminum is carried out electrolysis process as anode, thus obtains oxide-film on aluminum surface.According to the difference of electrolyte, densification (or stop) anodic alumina films and porous anodic alumina films can be respectively obtained.Fine and close (or stop) anodic alumina films carries out anodic oxidation to aluminum in neutral electrolyte and obtains, it is a kind of densification, pellumina unformed, in uniform thickness, this pellumina has good dielectric properties, can be used as the anode foils of aluminium electrolutic capacitor.Porous anodic alumina films is then self to have in the acidic electrolysis bath of certain oxidability at oxalic acid, phosphoric acid, sulphuric acid etc. aluminum is carried out anodic oxidation to obtain, it is made up of one layer of barrier layer near metal and outer layer Woelm Alumina, in six side's solid matter periodic structures, porous anodic alumina films is mainly used in filter membrane and the template of preparation nano material.
At present, the preparation of porous anodic alumina films mainly uses two step anodizings (such as Chinese patent literature CN1609283A, CN101007645A, CN101139730A etc.), the most first aluminium is carried out pretreatment, then aoxidize first in acidic electrolysis bath, oxidization time is usually 1h～5h, then pass through chemical attack and remove the oxide-film aoxidizing generation first, finally in acidic electrolysis bath, carry out secondary oxidation 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, thus beneficially obtains size and the porous array film more uniformly spread after anodic oxidation.The solution that electrochemical polish uses all is made up of according to certain volume ratio dehydrated alcohol and perchloric acid.The shortcoming of the method is: (1) anodizing time is longer, thus causes the production cycle；(2) the oxide-film degree of order aoxidizing generation first is poor, thus affects the degree of order of the porous anodic alumina films finally given.
Summary of the invention
It is an object of the invention to solve the problems referred to above, it is provided that a kind of production cycle is shorter, the preparation method of the porous anodic alumina films of high-sequential.
The technical scheme realizing the object of the invention is: the preparation method of a kind of porous anodic alumina films, has steps of: 1. surface of pure aluminum is carried out pretreatment；2. using the most pretreated for step fine aluminium as anode and with put into together with the platinum electrode of negative electrode in electrochemical polish solution, and to make cathode and anode spacing be 50mm～70mm, the most at ambient temperature (0 DEG C～40 DEG C, lower with), at 80mA/cm2～160mA/cm2Electric current density under carry out electrochemical polish 10s～90s, thus form nanometer porous film layer at surface of pure aluminum；Described electrochemical polish solution is made up of according to the volume ratio of 9: 1～2: 1 1,2-propylene glycol and perchloric acid；Or using the most pretreated for step fine aluminium as anode and with put in electrochemical polish solution together with the graphite of negative electrode, under the voltage of 15V～50V, carry out electrochemical polish 10s～90s, thus form nanometer porous film layer at surface of pure aluminum；Described electrochemical polish solution is made up of according to the weight ratio of 10: 1～3: 1 dehydrated alcohol and perchloric acid；3. it is immersed in 0.5h～6h in the treatment fluid of 50 DEG C～90 DEG C after being washed by the fine aluminium after step 2. electrochemical polish, thus remove the nanometer porous film layer of surface of pure aluminum；4. put in electrolyte after the fine aluminium washing after 3. step being processed, at a temperature of the voltage of 60V～140V and-10 DEG C～20 DEG C, carry out anodic oxidation 1h～5h；5. the fine aluminium after step 4. anodic oxidation is carried out and dries.
Above-mentioned steps 3. described in treatment fluid be every liter containing the chromic acid of 10g～25g and the phosphorus aqueous acid of 10mL～35mL.
Above-mentioned steps 4. described in the phosphate aqueous solution that electrolyte is 0.2mol/L～0.6mol/L.
Above-mentioned steps 1. described in surface of pure aluminum is carried out pretreatment be by through oil removing and washing after fine aluminium be placed in 30s～60s in the aqueous slkali of 60 DEG C～80 DEG C, take out and wash, it is placed in dilute nitric acid solution dipping 30s～60s again, takes out and carry out ultrasonic cleaning 5min～10min.Described aqueous slkali is the aqueous solution of every liter of sodium hydroxide containing 15g～30g.The percent by volume of described dilute nitric acid solution is 10%～30%.
Above-mentioned steps 5. described in cleaning for deionized water ultrasonic cleaning 5min～10min；Described drying is hot-air seasoning.
The good effect that the present invention has: (1) present invention is by selecting suitable electrochemical polish solution and suitable electrochemical polish condition, electrochemical polish is used to form nanometer porous film layer at surface of pure aluminum, be equivalent to the oxidation first in two step anodizings, but the oxidization time first that the electrochemical polish time of 10s～90s is compared to 1h～5h, substantially reduces the production cycle.(2) the nanometer porous film layer that the electrochemical polish of the present invention obtains also has the advantages such as big, the high-sequential of scope, may finally obtain the porous anodic alumina films of high-sequential.(3) the method technique of the present invention is simple, and cost is relatively low.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph on the porous anodic alumina films surface that embodiment 1 prepares.
Fig. 2 is the graph of pore diameter distribution of the porous anodic alumina films that embodiment 1 prepares.
Fig. 3 is the scanning electron microscope (SEM) photograph on the porous anodic alumina films surface that embodiment 5 prepares.
Fig. 4 is the graph of pore diameter distribution of the porous anodic alumina films that embodiment 5 prepares.
Detailed description of the invention
(embodiment 1)
The preparation method of the porous anodic alumina films of the present embodiment has steps of:
1. surface of pure aluminum is carried out pretreatment:
First, fine aluminium is put into immersion 5min in dehydrated alcohol, thus removes greasy dirt when surface machines.Then, wash fine aluminium with clear water, thus remove dust and the dirt of surface of pure aluminum.Then, the fine aluminium after being washed by clear water is placed in 30s in the aqueous slkali of 60 DEG C, thus removes the thin oxide layer that surface of pure aluminum is natural, and described aqueous slkali is every liter of aqueous solution containing 20g sodium hydroxide.Followed by, fine aluminium is taken out and again washes with clear water, be placed in the dilute nitric acid solution that percent by volume is 25% impregnating 30s.Finally, fine aluminium taken out and use deionized water ultrasonic cleaning 5min.
2. using the most pretreated for step fine aluminium as anode and with put into together with the platinum electrode of negative electrode in electrochemical polish solution, and to make cathode and anode spacing be 60mm, the most at ambient temperature (the present embodiment is 10 DEG C), at 120mA/cm2Electric current density under carry out electrochemical polish 60s, thus form nanometer porous film layer at surface of pure aluminum；
Above-mentioned electrochemical polish solution is made up of according to the volume ratio of 4: 1 1,2-propylene glycol and perchloric acid.
3. it is immersed in 3h in the treatment fluid of 60 DEG C after being washed by the fine aluminium clear water after step 2. electrochemical polish, thus removes the nanometer porous film layer of surface of pure aluminum.
Above-mentioned treatment fluid is every liter of chromic acid containing 20g and the phosphorus aqueous acid of 30mL.
4. put in electrolyte after the fine aluminium clear water washing after 3. step being processed, at a temperature of the voltage of 110V and 5 DEG C, carry out anodic oxidation 1h.
Above-mentioned electrolyte is the phosphate aqueous solution of 0.4mol/L.
5. to the deionized water ultrasonic cleaning 10min of the fine aluminium after step 4. anodic oxidation, then hot-air seasoning.
The scanning electron microscope (SEM) photograph on the porous anodic alumina films surface that the present embodiment prepares is shown in Fig. 1, graph of pore diameter distribution is shown in Fig. 2, from Fig. 1 and Fig. 2: the pore-size distribution of the porous anodic alumina films that the present embodiment prepares is highly uniform, and average pore size is about 320nm, and porosity reaches 30%.
(embodiment 2～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 |
| Cathode and anode spacing | 60mm | 60mm | 60mm | 70mm |
| Electric 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 contains 20g chromic acid and 30mL phosphoric acid | Every liter contains 15g chromic acid and 25mL phosphoric acid | Every liter contains 25g chromic acid and 35mL phosphoric acid | Every liter contains 10g chromic acid and 30mL phosphoric acid |
| Treatment temperature | 60℃ | 60℃ | 70℃ | 80℃ |
| The process 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, difference is that step is 2.: using the most pretreated for step fine aluminium as anode and with put in electrochemical polish solution together with the graphite of negative electrode, under the voltage of 20V, carry out electrochemical polish 30s, thus form nanometer porous film layer at surface of pure aluminum.
Above-mentioned electrochemical polish solution is made up of according to the weight ratio of 4: 1 dehydrated alcohol and perchloric acid.
The scanning electron microscope (SEM) photograph on the porous anodic alumina films surface that the present embodiment prepares is shown in Fig. 3, graph of pore diameter distribution is shown in Fig. 4, from Fig. 3 and Fig. 4: the pore-size distribution of the porous anodic alumina films that the present embodiment prepares is a bit weaker, porosity also only has about 5%, and average pore size is 80nm.
(embodiment 6～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 | Dehydrated alcohol: perchloric acid 4: 1 | Dehydrated alcohol: perchloric acid 5: 1 | Dehydrated alcohol: perchloric acid 6: 1 | Dehydrated alcohol: perchloric acid 10: 1 |
| Electrochemical polish voltage | 20V | 20V | 25V | 25V |
| The electrochemical polish time | 30s | 20s | 10s | 30s |
| Treatment fluid | Every liter contains 20g chromic acid and 30mL phosphoric acid | Every liter contains 15g chromic acid and 25mL phosphoric acid | Every liter contains 25g chromic acid and 35mL phosphoric acid | Every liter contains 10g chromic acid and 30mL phosphoric acid |
| Treatment temperature | 60℃ | 60℃ | 70℃ | 80℃ |
| The process 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. the preparation method of the porous anodic alumina films of a high-sequential, it is characterised in that have steps of:
30s～60s in the aqueous solution of every liter of sodium hydroxide containing 15g～30g that 1. fine aluminium after oil removing and washing is placed in 60 DEG C～80 DEG C, take out and wash, it is placed in the dilute nitric acid solution that percent by volume is 10%～30% dipping 30s～60s again, takes out and carry out ultrasonic cleaning 5min～10min.
2. using the most pretreated for step fine aluminium as anode and with put into together with the platinum electrode of negative electrode in electrochemical polish solution, and to make cathode and anode spacing be 50mm～70mm, the most at ambient temperature, at 80mA/cm2～160mA/cm2Electric current density under carry out electrochemical polish 10s～90s, thus form nanometer porous film layer at surface of pure aluminum；Described electrochemical polish solution is made up of according to the volume ratio of 9: 1～2: 1 1,2-propylene glycol and perchloric acid；
3. it is immersed in 0.5h～6h in every liter of chromic acid containing 10g～25g of 50 DEG C～90 DEG C and the phosphorus aqueous acid of 10mL～35mL after being washed by the fine aluminium after step 2. electrochemical polish, thus removes the nanometer porous film layer of surface of pure aluminum；
4. put in 0.2mol/L～0.6mol/L phosphate aqueous solution after the fine aluminium washing after 3. step being processed, at a temperature of the voltage of 60V～140V and-10 DEG C～20 DEG C, carry out anodic oxidation 1h～5h；
5. to the fine aluminium after step 4. anodic oxidation first with deionized water ultrasonic cleaning 5min～10min, then hot-air seasoning.
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