CN1325698C - Preparation method of ordered porous anodic alumina template - Google Patents
Preparation method of ordered porous anodic alumina template Download PDFInfo
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- CN1325698C CN1325698C CNB2003101118341A CN200310111834A CN1325698C CN 1325698 C CN1325698 C CN 1325698C CN B2003101118341 A CNB2003101118341 A CN B2003101118341A CN 200310111834 A CN200310111834 A CN 200310111834A CN 1325698 C CN1325698 C CN 1325698C
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- acid
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- aluminium flake
- porous anodic
- ordered porous
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 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 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 29
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 24
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 12
- 230000003647 oxidation Effects 0.000 claims description 10
- 238000007254 oxidation reaction Methods 0.000 claims description 10
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 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 5
- 239000006210 lotion Substances 0.000 claims description 5
- 239000011159 matrix material Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 235000006408 oxalic acid Nutrition 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 102000004160 Phosphoric Monoester Hydrolases Human genes 0.000 claims description 2
- 108090000608 Phosphoric Monoester Hydrolases Proteins 0.000 claims description 2
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 2
- 235000011150 stannous chloride Nutrition 0.000 claims description 2
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims description 2
- 239000011148 porous material Substances 0.000 abstract description 3
- 239000012528 membrane Substances 0.000 abstract 1
- 239000011800 void material Substances 0.000 abstract 1
- 239000002086 nanomaterial Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000002071 nanotube Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- -1 nano thread Substances 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000000609 electron-beam lithography Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229910021426 porous silicon Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005287 template synthesis Methods 0.000 description 1
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Abstract
The invention discloses a preparation method of an ordered porous anodic alumina membrane. Compared with the prior art, the preparation method has the advantages that: large-area highly ordered nano-templates can be prepared; the success rate of template preparation is improved; the quality of the template is greatly improved, such as the arrangement sequence of nano holes, the uniformity of pore diameter, the consistency of depth and the improvement of void ratio (which can reach 10)11One cm-2)。
Description
Technical field
The present invention relates to a kind of preparation method of ordered porous anodic alumina template.
Background technology
Nano material is meant the material that has only nanoscale size in the material structure, and nano material is because its special electronic structure and physicals make it more and more be subjected to people's attention as functional material.In recent years, a large amount of work concentrates in the research of nano materials such as nano thread, nanotube, nanometer rod, nano belt and Nanoalloy, the monodimension nanometer material that wherein with the nanotube is representative becomes the focus in the nano material because it is had outstanding performance in nature in sound, light, electricity, magnetic, power and heat etc.The preparation nanotube generally adopts the template synthesis method, and the template of nano materials commonly used has porous silicon, polycarbonate, anodised aluminium templates such as (AAO).
Existing press mold technology, photoetching and electron beam lithography technology can obtain large-area nano sequential holes template, but can not obtain the long uniform nano aperture of diameter, and directly anonizing can only obtain small area ordered nano hole template.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of ordered porous anodic alumina template, that the relative other materials of anodised aluminium (AAO) template for preparing with this method has is high temperature resistant, stable in properties, pore distribution are uniform sequential, and since between the hole size and the thickness in density, hole adjustable within the specific limits.
Technical scheme of the present invention is as follows:
A kind of preparation method of ordered porous anodic alumina template may further comprise the steps:
(1) aluminium flake was polished 5～10 minutes down at 0～5 ℃ with 70% perchloric acid and dehydrated alcohol mixed solution (volume ratio 1: 4) earlier, voltage is 15～22V;
(2) (sulfuric acid 18～22V, oxalic acid 30～50V, phosphatase 11 00～130V) oxidation first 1～2 hour were done counter electrode with stainless steel plate with each self-corresponding voltage at polyprotonic acid (0.5～1.5mol/L sulfuric acid, 0.1～0.5mol/L oxalic acid or 0.3～1.0mol/L phosphoric acid) after aluminium flake cleaned with secondary water;
(3) under 60 ℃, mix washing lotion again and clean aluminium flake half an hour, remove oxide film with the chromic acid of 6% phosphoric acid and 1.8%;
(4) after aluminium flake cleans with secondary water, use with step (2) in same voltage carried out anodic oxidation 5～10 hours;
(5) peel off aluminum matrix with the muriate saturated aqueous solution, the phosphoric acid reaming with 5% 5～20 minutes is kept in the secondary water at last.
If the template that all open on the aluminium flake two sides need increase about 30 minutes reaming time.
As improvement of the technical scheme, used muriate is the tin protochloride saturated aqueous solution in the step 5 among the above-mentioned preparation method.
Beneficial effect of the present invention is: method of the present invention has improved the area scale and the success ratio of template preparation, has improved the quality of template greatly, as the nanoporous order of arranging, and the aperture homogeneity, the consistence of the degree of depth and the raising of voidage (can reach 10
11Individual cm
-2).
In addition, the anodised aluminium that method of the present invention makes (AAO) template with respect to other template have high temperature resistant, stable in properties, pore distribution is uniform sequential, and because the size in density, hole and thickness are adjustable in the certain limit again between the hole, this just makes with AAO to be that the nano material that template prepares has more use value.Utilize the AAO template can prepare a series of nano materials such as metal nano material (nano magnetic material, ultra micro pencil electrode materials, nanocomposite optical material and nanometer optical-thermal conversion material), semiconductor nano material, carbon nanomaterial and carbon nano-composite material with strange characteristic and function.
Description of drawings
Fig. 1 observes for the sample that adopts SEM (HITACHI S-5200) that embodiment 1 is made and obtains figure;
Fig. 2 observes for the sample that adopts SEM (HITACHI S-5200) that embodiment 1 is made and obtains figure;
Fig. 3 carries out the figure of surface observation gained for the sample that adopts AFM (DI-D3000) that embodiment 1 is made;
Fig. 4 carries out the rotation diagram of the figure that surface observation gets for the sample that adopts AFM (DI-D3000) that embodiment 1 is made;
Fig. 5 utilizes TME that the sample that embodiment 1 makes is carried out observable figure;
Fig. 6 utilizes SEM that the sample that embodiment 2 makes is carried out observable figure.
Embodiment
Following embodiment will help those of ordinary skill in the art further to understand the present invention, but not limit the present invention in any form.
Embodiment 1
1, aluminium flake was polished 10 minutes down at 5 ℃ with 70% perchloric acid and dehydrated alcohol mixed solution (volume ratio 1: 4) earlier, voltage is 20V;
2, aluminium flake with secondary water clean the back in the sulfuric acid of 1.0mol/L with the voltage oxidation first of 20V 2 hours, do counter electrode with stainless steel plate;
3, under 60 ℃, mix washing lotion again and clean aluminium flake half an hour, remove oxide film with the chromic acid of 6% phosphoric acid and 1.8%;
4, after aluminium flake cleans with secondary water, use with step 2 in identical voltage carried out anodic oxidation 5 hours;
5, peel off aluminum matrix with saturated tin protoxide, the phosphoric acid reaming with 5% 15 minutes is kept in the secondary water at last.
Embodiment 2
1, aluminium flake was polished 10 minutes down at 0 ℃ with 70% perchloric acid and dehydrated alcohol mixed solution (volume ratio 1: 4) earlier, voltage is 20V;
2, aluminium flake with secondary water clean the back in the oxalic acid of 0.3mol/L with the voltage oxidation first of 40V 2 hours, do counter electrode with stainless steel plate;
3, under 60 ℃, mix washing lotion again and clean aluminium flake half an hour, remove oxide film with the chromic acid of 6% phosphoric acid and 1.8%;
4, after aluminium flake cleans with secondary water, use with step 2 in identical voltage carried out anodic oxidation 8 hours;
5, peel off aluminum matrix with saturated tin protoxide, the phosphoric acid reaming with 5% 20 minutes is kept in the secondary water at last.
Embodiment 3
1, aluminium flake was polished 10 minutes down at 3 ℃ with 70% perchloric acid and dehydrated alcohol mixed solution (volume ratio 1: 4) earlier, voltage is 20V;
2, aluminium flake with secondary water clean the back in the phosphoric acid of 0.6mol/L with the voltage oxidation first of 110V 1.5 hours, do counter electrode with stainless steel plate;
3, under 60 ℃, mix washing lotion again and clean aluminium flake half an hour, remove oxide film with the chromic acid of 6% phosphoric acid and 1.8%;
4, after aluminium flake cleans with secondary water, use with step 2 in same voltage carry out anodic oxidation 8 hours;
5, peel off aluminum matrix with saturated tin protoxide, the sulfuric acid reaming with 5% 10 minutes is kept in the secondary water at last.
Embodiment 4 effect Experimental Characterization
The sample that adopts SEM (HITACHI S-5200) that embodiment 1 is made is observed and is obtained Fig. 1 and Fig. 2, and hole integral body is arranged uniform sequential as seen from Figure 1; Fig. 2 illustrates the big or small almost equal of hole; The aperture is between 25～35nm, and hole density is about 4.8 * 10
10Cm
-2
The sample that adopts AFM (DI-D3000) that embodiment 1 is made carries out surface observation and gets Fig. 3 and Fig. 4, and Fig. 4 is the rotation diagram on surface, can be clearly seen that the surface appearance of template from Fig. 4.
Utilize TEM (JEM-100SX) that the sample that embodiment 1 makes is observed, obtain Fig. 5, from the cut-plane slices of Fig. 5 sample as can be seen the aperture be parallel to each other and with the plane be strict vertical straight hole.
Utilize SEM that the sample that embodiment 2 makes is observed, obtain Fig. 6, hole integral body is arranged uniform sequential as seen from Figure 6; Fig. 6 illustrates the big or small almost equal of hole; The aperture is between 60～75nm, and hole density is about 1.0 * 10
10Cm
-2
Claims (3)
1, a kind of preparation method of ordered porous anodic alumina template may further comprise the steps:
(1) aluminium flake was polished 5～10 minutes down at 0～5 ℃ with 1: 4 70% perchloric acid of volume ratio and dehydrated alcohol mixed solution earlier, voltage is 15～22V;
(2) aluminium flake with secondary water clean the back in polyprotonic acid with the voltage oxidation first of correspondence 1～2 hour, do counter electrode with stainless steel plate;
(3) under 60 ℃, mix washing lotion again and clean aluminium flake half an hour, remove oxide film with the chromic acid of 6% phosphoric acid and 1.8%;
(4) after aluminium flake cleans with secondary water, use with step (2) in same voltage carried out anodic oxidation 5～10 hours;
(5) peel off aluminum matrix with the muriate saturated aqueous solution, the phosphoric acid reaming with 5% 5～20 minutes is kept in the secondary water at last.
2, the preparation method of ordered porous anodic alumina template according to claim 1, it is characterized in that polyprotonic acid used in the step (2) is 0.5～1.5mol/L sulfuric acid, 0.1～0.5mol/L oxalic acid or 0.3～1.0mol/L phosphoric acid, corresponding voltage is sulfuric acid 18～22V, oxalic acid 30～50V, phosphatase 11 00～130V.
3, the preparation method of ordered porous anodic alumina template according to claim 1 is characterized in that muriate used in the step (5) is the tin protochloride saturated aqueous solution.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101118341A CN1325698C (en) | 2003-10-21 | 2003-10-21 | Preparation method of ordered porous anodic alumina template |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101118341A CN1325698C (en) | 2003-10-21 | 2003-10-21 | Preparation method of ordered porous anodic alumina template |
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| Publication Number | Publication Date |
|---|---|
| CN1609283A CN1609283A (en) | 2005-04-27 |
| CN1325698C true CN1325698C (en) | 2007-07-11 |
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| CNB2003101118341A Expired - Fee Related CN1325698C (en) | 2003-10-21 | 2003-10-21 | Preparation method of ordered porous anodic alumina template |
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| KR101190657B1 (en) * | 2003-04-21 | 2012-10-15 | 삼성전자주식회사 | Manufacturing method of self-ordered nanochannel-array and manufacturing method of nano dot using the nanochannel-array |
| CN100378254C (en) * | 2005-05-19 | 2008-04-02 | 上海交通大学 | Production of free superthin porous alumina template with controllable thickness |
| CN100381613C (en) * | 2005-06-08 | 2008-04-16 | 武汉大学 | Method for preparing aluminium oxide nano-form photon crystal |
| CN101148245B (en) * | 2006-09-22 | 2011-08-24 | 清华大学 | Nanometer level microporous mould |
| CN101148246B (en) * | 2006-09-22 | 2011-01-26 | 鸿富锦精密工业（深圳）有限公司 | Method for manufacturing nanometer level microporous mould |
| CN101210337B (en) * | 2006-12-29 | 2010-08-25 | 新疆众和股份有限公司 | Method for stripping oxide film of nano aluminum anode |
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| CN101798701A (en) * | 2010-03-30 | 2010-08-11 | 西安理工大学 | Method for preparing alumina template by guidance of etching pattern |
| CN102776542A (en) * | 2012-07-25 | 2012-11-14 | 华南理工大学 | Preparation method of anodized aluminum film of through hole |
| CN105200510B (en) * | 2013-05-17 | 2017-11-21 | 江苏理工学院 | Method for forming nano-scale porous film layer on pure aluminum surface through electrochemical polishing |
| CN103526204A (en) * | 2013-10-15 | 2014-01-22 | 云南大学 | Preparation of heat shock-resisting functional oxide layer on surface of alloy by anodic oxidation |
| CN106048688B (en) * | 2014-05-22 | 2017-11-21 | 江苏理工学院 | Preparation method of highly ordered porous anodic oxide film |
| CN104003354B (en) * | 2014-06-18 | 2015-06-03 | 中山大学 | Aluminum nanometer particle size regulation method and application of aluminum nanometer particle size regulation method |
| CN105040065B (en) * | 2015-06-16 | 2019-01-01 | 天津工业大学 | A kind of preparation method of regular porous anodic alumina films |
| CN107964676A (en) * | 2016-10-20 | 2018-04-27 | 苏州汉力新材料有限公司 | A kind of preparation method of aluminium oxide super hydrophobic surface |
| CN108360036A (en) * | 2018-03-07 | 2018-08-03 | 大连理工大学 | A kind of method that high-purity aluminium surface obtains regular three-dimensional micro-nano structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5729595A (en) * | 1980-07-28 | 1982-02-17 | Mitsubishi Alum Co Ltd | Formation of colored film of aluminum |
| JPS5956594A (en) * | 1982-09-24 | 1984-04-02 | Nippon Light Metal Co Ltd | Method for coloring aluminum |
| US5486283A (en) * | 1993-08-02 | 1996-01-23 | Rohr, Inc. | Method for anodizing aluminum and product produced |
| CN1278024A (en) * | 2000-07-04 | 2000-12-27 | 南京大学 | Method for preparing template with macro nanometer sequential holes |
-
2003
- 2003-10-21 CN CNB2003101118341A patent/CN1325698C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5729595A (en) * | 1980-07-28 | 1982-02-17 | Mitsubishi Alum Co Ltd | Formation of colored film of aluminum |
| JPS5956594A (en) * | 1982-09-24 | 1984-04-02 | Nippon Light Metal Co Ltd | Method for coloring aluminum |
| US5486283A (en) * | 1993-08-02 | 1996-01-23 | Rohr, Inc. | Method for anodizing aluminum and product produced |
| CN1278024A (en) * | 2000-07-04 | 2000-12-27 | 南京大学 | Method for preparing template with macro nanometer sequential holes |
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Assignee: TAIAO ALUMINIUM (TAISHAN) CO., LTD. Assignor: Dongguan University of technology Contract record no.: 2010440000742 Denomination of invention: Process for producing ordered porous anodic alumina form Granted publication date: 20070711 License type: Exclusive License Open date: 20050427 Record date: 20100611 |
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