CN114232051A - Preparation method of nano-pore metal structure - Google Patents
Preparation method of nano-pore metal structure Download PDFInfo
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- CN114232051A CN114232051A CN202111546784.4A CN202111546784A CN114232051A CN 114232051 A CN114232051 A CN 114232051A CN 202111546784 A CN202111546784 A CN 202111546784A CN 114232051 A CN114232051 A CN 114232051A
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 57
- 239000002184 metal Substances 0.000 title claims abstract description 57
- 239000011148 porous material Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 67
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 58
- 238000000034 method Methods 0.000 claims abstract description 44
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000007769 metal material Substances 0.000 claims abstract description 26
- 238000004070 electrodeposition Methods 0.000 claims abstract description 15
- 238000001179 sorption measurement Methods 0.000 claims abstract description 14
- 238000000151 deposition Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000010408 film Substances 0.000 claims description 83
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 28
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 25
- 229910052802 copper Inorganic materials 0.000 claims description 25
- 239000010949 copper Substances 0.000 claims description 25
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
- 239000011521 glass Substances 0.000 claims description 14
- 238000005530 etching Methods 0.000 claims description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- 239000010409 thin film Substances 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 239000011651 chromium Substances 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 3
- 239000007864 aqueous solution Substances 0.000 claims 1
- 239000012528 membrane Substances 0.000 abstract description 7
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 239000002070 nanowire Substances 0.000 description 9
- 239000002073 nanorod Substances 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
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- 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
- C25D11/18—After-treatment, e.g. pore-sealing
-
- 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
- C25D11/18—After-treatment, e.g. pore-sealing
- C25D11/20—Electrolytic after-treatment
-
- 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
- C25D11/18—After-treatment, e.g. pore-sealing
- C25D11/24—Chemical after-treatment
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Laminated Bodies (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
The invention discloses a preparation method of a nano-pore metal structure, which relates to the technical field of nano-material preparation and comprises the following steps: s1, carrying out hydrophilic treatment on the ultrathin anodic aluminum oxide film with the double-through-hole structure and the conductive substrate; s2, transferring the ultrathin anodic aluminum oxide film to the surface of a target substrate, wherein the aluminum oxide film and the target substrate form tight adsorption; s3, transferring the multi-layer ultrathin anodic aluminum oxide film by adopting the transferring method of the step S2, thereby forming a double-through-hole ultrathin anodic aluminum oxide film laminated structure; s4, depositing a metal material by using an electrochemical deposition method until the metal completely fills the gap part of the laminated structure; s5, dissolving the anodic alumina template by using corrosive liquid to obtain a nano-pore metal structure on the target substrate, wherein the pore period, the pore diameter and the membrane thickness of the alumina membrane can be independently regulated and controlled each time, so that the internal pore structure of the obtained metal membrane can be changed in a great number and is easy to regulate and control.
Description
Technical Field
The invention relates to the technical field of nano material preparation, in particular to a preparation method of a nano-pore metal structure.
Background
Due to its high electrical conductivity, metal materials have wide application as the main component of electrode materials in the fields of lithium batteries, supercapacitors, fuel cells, electro-catalytic sewage treatment, gas sensors, and the like. In these applications, the performance of the device is directly related to the structure of the metal, and when the specific surface area of the metal is increased, the effective metal surface per unit volume is increased, thereby improving the main electrical performance of the device. Therefore, increasing the specific surface area of metals is one of the major development directions of electrode materials. The metal material with the nano-scale microstructure has a high specific surface area, and the metal microstructures most used in the scientific research and industry are metal nano-rods and nanowire structures. When the ratio of the length to the diameter is smaller, the nano-rod is generally called as a nano-rod, and when the ratio is larger, the nano-rod is a nano-wire. In order to facilitate the conduction of the directional current, one end of the metal nanowire is required to be connected to a metal plate or a metal film to form a metal nanowire array structure. Such nanowire array structures are typically obtained using anodic aluminum oxide with a double-pass nanopore structure in combination with electrochemical deposition.
However, the metal nanowires inevitably have an agglomeration phenomenon due to a large aspect ratio, that is, a large number of nanowires are agglomerated together to form a bundle of nanowire bundles, thereby seriously reducing the specific surface area of the structure. An important method for solving this problem is to prepare a metal thin film having a nanoporous structure. Because the inside of the nano-pore metal film is of a porous structure and the main body framework is connected together, the problem of agglomeration like the nano-wires does not exist. The nano-porous metal film with a regular pore diameter structure is difficult to obtain by a direct processing method, and usually needs to be prepared by combining a non-conductive template with a nano structure with electrochemical deposition, although a small amount of literature reports [ adv. mater.2014,26, 7654-.
Disclosure of Invention
The present invention is directed to a method for preparing a nanoporous metal structure, so as to solve the problems mentioned in the background art.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for preparing a nanoporous metal structure, comprising the steps of:
s1, carrying out hydrophilic treatment on the ultrathin anodic aluminum oxide film with the double-through-hole structure and the conductive substrate;
s2, transferring the ultrathin anodic aluminum oxide film to the surface of a target substrate, wherein the aluminum oxide film and the target substrate form tight adsorption;
s3, transferring the multi-layer ultrathin anodic aluminum oxide film by adopting the transferring method of the step S2, thereby forming a double-through-hole ultrathin anodic aluminum oxide film laminated structure;
s4, depositing a metal material by using an electrochemical deposition method until the metal completely fills the gap part of the laminated structure;
and S5, dissolving the anodic alumina template by using corrosive liquid, and further obtaining the nano-pore metal structure on the target substrate.
Preferably, in step S1, the conductive substrate includes a metal material, ITO conductive glass, and FTO conductive glass.
Preferably, in step S1, during the hydrophilic treatment, the copper substrate is subjected to hydrophilic treatment by ultraviolet light irradiation.
Preferably, in step S1, the ultra-thin anodized aluminum template used has a hole center-to-center distance of 50nm to 3 μm, a hole diameter of 30nm to 2 μm, and a template thickness of 50nm to 1 μm.
Preferably, in step S2, the ultra-thin anodized aluminum oxide film is transferred to the surface of the copper substrate in acetone, and after the acetone is completely volatilized, the aluminum oxide film and the copper substrate form a close adsorption.
Preferably, in step S3, the number of the alumina thin film layers is 2 to 20.
Preferably, in step S4, the metal material is one or more of copper, nickel, chromium, gold and silver.
Preferably, in step S5, the etching solution used for dissolving the alumina film is an aqueous NaOH solution, the concentration of the NaOH is 5 wt%, and the temperature is room temperature.
Preferably, in step S5, the etching solution used for dissolving the alumina film is phosphoric acid, the concentration of the phosphoric acid is 6 wt%, and the temperature of the solution is 60 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1) because the period of the pores, the diameter of the pores and the thickness of the membrane of the alumina membrane can be independently regulated and controlled each time, the internal pore structure of the metal membrane obtained by the invention can be changed in a great way and is easy to regulate and control;
2) the prepared nano-pore metal film is directly connected with the conductive substrate, the conductive substrate is used as a carrier, the mechanical strength of the metal film is increased, the nano-pore metal film is prevented from cracking, and the yield is improved;
3) the invention uses the laminated staggered ultrathin alumina film, the staggered structure between the alumina pore walls between layers and the staggered communicated structure between pores, thereby greatly improving the specific surface area of the nano-pore metal film.
Drawings
Fig. 1 is a schematic flow structure diagram of a method for preparing a nanoporous metal structure.
Fig. 2 is a flow chart of a method of fabricating a nanoporous metal structure.
Detailed Description
The technical solution of the present invention will be described in further detail with reference to specific embodiments.
Example 1
Referring to fig. 1-2, a method for fabricating a nanopore metal structure includes the following steps:
s1, carrying out hydrophilic treatment on the ultrathin anodic aluminum oxide film with the double-through-hole structure and the conductive substrate;
in step S1, the conductive substrate includes a metal material, ITO conductive glass, and FTO conductive glass, and in the hydrophilic treatment process, the copper substrate is subjected to hydrophilic treatment by ultraviolet light irradiation, the center-to-center distance of the holes of the ultrathin anodized aluminum template is 50nm, the diameter of the holes is 30nm, and the thickness of the template is 50 nm;
specifically, a plurality of layers of superposed ultrathin anodic aluminum oxide films with a double-through-hole structure are used as templates, the ultrathin anodic aluminum oxide films are transferred to the surface of a conductive substrate, then metal filling materials are deposited in holes from the surface of the conductive substrate by an electrochemical deposition method, and finally the aluminum oxide films are dissolved and removed by a corrosive solution to obtain the metal films with the nano-hole structure;
s2, transferring the ultrathin anodic aluminum oxide film to the surface of a target substrate, wherein the aluminum oxide film and the target substrate form tight adsorption;
in step S2, transferring the ultra-thin anodized aluminum oxide film to the surface of the copper substrate in acetone, and after the acetone is completely volatilized, the aluminum oxide film and the copper substrate form a tight adsorption;
specifically, before the alumina film is transferred, hydrophilic treatment is required to be carried out on the alumina film and the substrate so as to improve the adhesion between the alumina films and between the alumina film and the conductive substrate, if the hydrophilic treatment is not carried out, the adhesion between the alumina films and the conductive substrate is poor, and the alumina films and the conductive substrate are separated and disintegrated in the electrochemical deposition process;
s3, transferring the multi-layer ultrathin anodic aluminum oxide film by adopting the transferring method of the step S2, thereby forming a double-through-hole ultrathin anodic aluminum oxide film laminated structure;
in step S3, the number of the alumina thin film layers is 2;
specifically, after the multiple layers of aluminum oxide films are stacked, the holes of the films are staggered, so that a communicated nano-scale cavity structure is formed in the whole volume range of the multiple layers of films;
s4, depositing a metal material by using an electrochemical deposition method until the metal completely fills the gap part of the laminated structure;
in step S4, the metal material is copper;
specifically, in the electrochemical deposition process, the cavity is filled with electrochemical deposition and dissolution and is filled with a metal material formed in the electrodeposition process, and the space occupied by the hole wall of the alumina porous membrane is not filled with the metal material;
s5, dissolving the anodic alumina template by using corrosive liquid, and further obtaining a nano-pore metal structure on the target substrate to obtain a nano-pore metal film;
in step S5, the etching solution used to dissolve the alumina film is an aqueous NaOH solution, the concentration of the NaOH is 5 wt%, and the temperature is room temperature.
Example 2
A method for preparing a nanoporous metal structure, comprising the steps of:
s1, carrying out hydrophilic treatment on the ultrathin anodic aluminum oxide film with the double-through-hole structure and the conductive substrate;
in step S1, the conductive substrate includes a metal material, ITO conductive glass, and FTO conductive glass, and in the hydrophilic treatment process, the copper substrate is subjected to hydrophilic treatment by ultraviolet light irradiation, the center-to-center distance of the holes of the ultrathin anodized aluminum template is 200nm, the diameter of the holes is 100nm, and the thickness of the template is 400 nm;
s2, transferring the ultrathin anodic aluminum oxide film to the surface of a target substrate, wherein the aluminum oxide film and the target substrate form tight adsorption;
in step S2, transferring the ultra-thin anodized aluminum oxide film to the surface of the copper substrate in acetone, and after the acetone is completely volatilized, the aluminum oxide film and the copper substrate form a tight adsorption;
s3, transferring the multi-layer ultrathin anodic aluminum oxide film by adopting the transferring method of the step S2, thereby forming a double-through-hole ultrathin anodic aluminum oxide film laminated structure;
in step S3, the number of the alumina thin film layers is 5;
s4, depositing a metal material by using an electrochemical deposition method until the metal completely fills the gap part of the laminated structure;
in step S4, the metal material is copper;
s5, dissolving the anodic alumina template by using corrosive liquid, and further obtaining a nano-pore metal structure on the target substrate to obtain a nano-pore metal film;
in step S5, the etching solution used to dissolve the alumina film is phosphoric acid, the concentration of the phosphoric acid is 6 wt%, and the temperature of the solution is 60 ℃.
Example 3
A method for preparing a nanoporous metal structure, comprising the steps of:
s1, carrying out hydrophilic treatment on the ultrathin anodic aluminum oxide film with the double-through-hole structure and the conductive substrate;
in step S1, the conductive substrate includes a metal material, ITO conductive glass, and FTO conductive glass, and in the hydrophilic treatment process, the copper substrate is subjected to hydrophilic treatment by ultraviolet light irradiation, the center-to-center distance of the holes of the ultrathin anodized aluminum template is 450nm, the diameter of the holes is 300nm, and the thickness of the template is 500 nm;
s2, transferring the ultrathin anodic aluminum oxide film to the surface of a target substrate, wherein the aluminum oxide film and the target substrate form tight adsorption;
in step S2, transferring the ultra-thin anodized aluminum oxide film to the surface of the copper substrate in acetone, and after the acetone is completely volatilized, the aluminum oxide film and the copper substrate form a tight adsorption;
s3, transferring the multi-layer ultrathin anodic aluminum oxide film by adopting the transferring method of the step S2, thereby forming a double-through-hole ultrathin anodic aluminum oxide film laminated structure;
in step S3, the number of the alumina thin film layers is 8;
s4, depositing a metal material by using an electrochemical deposition method until the metal completely fills the gap part of the laminated structure;
in step S4, the metal material is chromium;
s5, dissolving the anodic alumina template by using corrosive liquid, and further obtaining a nano-pore metal structure on the target substrate to obtain a nano-pore metal film;
in step S5, the etching solution used to dissolve the alumina film is an aqueous NaOH solution, the concentration of the NaOH is 5 wt%, and the temperature is room temperature.
Example 4
A method for preparing a nanoporous metal structure, comprising the steps of:
s1, carrying out hydrophilic treatment on the ultrathin anodic aluminum oxide film with the double-through-hole structure and the conductive substrate;
in step S1, the conductive substrate includes a metal material, ITO conductive glass, and FTO conductive glass, and in the hydrophilic treatment process, the copper substrate is subjected to hydrophilic treatment by ultraviolet light irradiation, the center-to-center distance of the holes of the ultrathin anodized aluminum template is 800nm, the diameter of the holes is 900nm, and the thickness of the template is 700 nm;
s2, transferring the ultrathin anodic aluminum oxide film to the surface of a target substrate, wherein the aluminum oxide film and the target substrate form tight adsorption;
in step S2, transferring the ultra-thin anodized aluminum oxide film to the surface of the copper substrate in acetone, and after the acetone is completely volatilized, the aluminum oxide film and the copper substrate form a tight adsorption;
s3, transferring the multi-layer ultrathin anodic aluminum oxide film by adopting the transferring method of the step S2, thereby forming a double-through-hole ultrathin anodic aluminum oxide film laminated structure;
in step S3, the number of the alumina thin film layers is 12;
s4, depositing a metal material by using an electrochemical deposition method until the metal completely fills the gap part of the laminated structure;
in step S4, the metal material is gold;
s5, dissolving the anodic alumina template by using corrosive liquid, and further obtaining a nano-pore metal structure on the target substrate to obtain a nano-pore metal film;
in step S5, the etching solution used to dissolve the alumina film is phosphoric acid, the concentration of the phosphoric acid is 6 wt%, and the temperature of the solution is 60 ℃.
Example 5
A method for preparing a nanoporous metal structure, comprising the steps of:
in step S1, the conductive substrate includes a metal material, ITO conductive glass, and FTO conductive glass, and in the hydrophilic treatment process, the copper substrate is subjected to hydrophilic treatment by ultraviolet light irradiation, the center-to-center distance of the holes of the ultrathin anodized aluminum template is 3 μm, the diameter of the holes is 2 μm, and the thickness of the template is 1 μm;
s2, transferring the ultrathin anodic aluminum oxide film to the surface of a target substrate, wherein the aluminum oxide film and the target substrate form tight adsorption;
in step S2, transferring the ultra-thin anodized aluminum oxide film to the surface of the copper substrate in acetone, and after the acetone is completely volatilized, the aluminum oxide film and the copper substrate form a tight adsorption;
s3, transferring the multi-layer ultrathin anodic aluminum oxide film by adopting the transferring method of the step S2, thereby forming a double-through-hole ultrathin anodic aluminum oxide film laminated structure;
in step S3, the number of the alumina thin film layers is 20;
s4, depositing a metal material by using an electrochemical deposition method until the metal completely fills the gap part of the laminated structure;
in step S4, the metal material is silver;
s5, dissolving the anodic alumina template by using corrosive liquid, and further obtaining a nano-pore metal structure on the target substrate to obtain a nano-pore metal film;
in step S5, the etching solution used to dissolve the alumina film is an aqueous NaOH solution, the concentration of the NaOH is 5 wt%, and the temperature is room temperature.
While the preferred embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (9)
1. A method for preparing a nano-pore metal structure is characterized by comprising the following steps:
s1, carrying out hydrophilic treatment on the ultrathin anodic aluminum oxide film with the double-through-hole structure and the conductive substrate;
s2, transferring the ultrathin anodic aluminum oxide film to the surface of a target substrate, wherein the aluminum oxide film and the target substrate form tight adsorption;
s3, transferring the multi-layer ultrathin anodic aluminum oxide film by adopting the transferring method of the step S2, thereby forming a double-through-hole ultrathin anodic aluminum oxide film laminated structure;
s4, depositing a metal material by using an electrochemical deposition method until the metal completely fills the gap part of the laminated structure;
and S5, dissolving the anodic alumina template by using corrosive liquid, and further obtaining the nano-pore metal structure on the target substrate.
2. The method as claimed in claim 1, wherein the conductive substrate comprises a metal material, ITO conductive glass and FTO conductive glass in step S1.
3. The method of claim 2, wherein in step S1, the copper substrate is hydrophilically treated by ultraviolet irradiation during the hydrophilization process.
4. The method of claim 3, wherein in step S1, the ultra-thin anodized aluminum template has a hole center-to-center distance of 50nm to 3 μm, a hole diameter of 30nm to 2 μm, and a template thickness of 50nm to 1 μm.
5. The method as claimed in claim 4, wherein the ultra-thin anodic aluminum oxide film is transferred to the surface of the copper substrate in acetone in step S2, and the aluminum oxide film and the copper substrate are tightly adsorbed after the acetone is completely volatilized.
6. The method as claimed in claim 5, wherein the number of the alumina thin film layers is 2 to 20 in step S3.
7. The method as claimed in claim 6, wherein in step S4, the metal material is one or more of copper, nickel, chromium, gold and silver.
8. The method of claim 7, wherein in step S5, the etching solution used for dissolving the alumina film is NaOH aqueous solution, the concentration of NaOH is 5 wt%, and the temperature is room temperature.
9. The method of claim 8, wherein in step S5, the etching solution used for dissolving the alumina film is phosphoric acid, the concentration of phosphoric acid is 6 wt%, and the temperature of the solution is 60 ℃.
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| CN109437095A (en) * | 2018-11-21 | 2019-03-08 | 广东工业大学 | A kind of silicon nano hole construction manufacturing method that etching direction is controllable |
| CN109778249A (en) * | 2019-02-22 | 2019-05-21 | 浙江交通科技股份有限公司 | A kind of preparation method preparing metal nucleocapsid nano wire |
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