CN112226807B - Method for producing micropores in commercial aluminum foil - Google Patents

Method for producing micropores in commercial aluminum foil Download PDF

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CN112226807B
CN112226807B CN202011083839.8A CN202011083839A CN112226807B CN 112226807 B CN112226807 B CN 112226807B CN 202011083839 A CN202011083839 A CN 202011083839A CN 112226807 B CN112226807 B CN 112226807B
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aluminum foil
electrode
solution
ionic liquid
mol
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CN112226807A (en
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丁克强
赵棉
陈家晟
张冬月
石赋娟
李博霞
曲润玲
周兰俊
王庆飞
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Hebei Normal University
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    • 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
    • C25F3/02—Etching
    • C25F3/04—Etching of light metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • H01M4/661—Metal or alloys, e.g. alloy coatings
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/64—Carriers or collectors
    • H01M4/70—Carriers or collectors characterised by shape or form
    • H01M4/80—Porous plates, e.g. sintered carriers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
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  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)
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Abstract

The invention discloses a method for making aluminum foil generate micropores, which comprises the following steps: is prepared from2SO4、Na2SO4And aniline, adding ionic liquid 1-butyl-3-methylimidazole tetrafluoroborate into the solution to form an electrolyte solution containing the ionic liquid, adopting a CHI660E electrochemical workstation and a three-electrode system, controlling the potential scanning speed to be 20-100 mV/s by using a cyclic voltammetry method, setting a potential window in a range of-0.8-1.1V, and taking out the aluminum foil to dry at room temperature to obtain the aluminum foil with micropores of which the surface has the pore diameter of 30-500 mu m. The diameter of the aluminum foil micropores can be effectively regulated and controlled according to different parameters such as a potential window, the amount of ionic liquid, the number of circulating scanning circles and the like, and the method is simple and easy to implement and suitable for large-scale production. The microporous aluminum foil prepared by the invention has potential application value in the fields of microelectronic devices and the like.

Description

Method for producing micropores in commercial aluminum foil
Technical Field
The invention relates to a method for generating micropores in an aluminum foil, in particular to a method for generating micropores in a commercial aluminum foil by adopting a cyclic voltammetry method in an electrolyte in the presence of an ionic liquid, belonging to the technical field of energy materials.
Background
The aluminum foil has good flexibility, high conductivity and low price, and is widely applied to the fields of various electric appliances, electronics and the like. In electrochemical energy storage devices, aluminum foil generally serves as a current collector, serving the dual function of carrying electroactive materials and transporting electrons. In the technical field of mesoporous materials, the aluminum foil with micropores can be used for realizing the effective separation and collection of oil and water mixtures. The current methods for making the commercial aluminum foil micro-porous are mainly physical methods and chemical methods. Physical methods, i.e. the etching of micropores in the surface of the aluminum foil by means of highly precise instruments and equipment, obviously make it difficult to achieve the dimensions of nanometer and micrometer. Meanwhile, the method has high equipment cost, complex operation and high cost, and is not suitable for large-scale production. The chemical method generally comprises the steps of carrying out chemical reaction on aluminum foil and acid or alkali, generating micropores through chemical corrosion, strictly controlling the conditions such as acid dosage, soaking time and the like in the preparation process, and being difficult to operate, and meanwhile, if the diameter of the pores is required to reach the nanometer or micrometer scale, the pores can be realized only by means of a nanometer or micrometer template. In addition, it is difficult to generate scattered micropores on the surface of the aluminum foil due to the uniformity of the surface properties of the aluminum foil.
Disclosure of Invention
The invention aims to provide a method for producing micropores in a commercial aluminum foil, which has the characteristics of simplicity and convenience.
Specifically, the invention provides a method for producing micropores in a commercial aluminum foil, which comprises the following steps:
(1) preparation of the Material
A sulfuric acid solution; a sodium sulfate solution; aniline; an ionic liquid; commercial aluminum foil;
(2) preparation of instruments and materials for electrochemical preparation
CHI660E electrochemical workstation; a salt bridge; a saturated calomel electrode; a platinum sheet electrode;
(3) preparation of samples
First, 100mL of a solution containing H was prepared with distilled water2SO4、Na2SO4 and aniline in solution, H in this solution2Concentration of SO4In the range of 0.5 to 1.0 mol/L, Na2The concentration of SO4 is 0.1-0.8 mol/L, the concentration of aniline is 0.4 mol/L, and then 0.5-2 g of 1-butyl-3-methylimidazolium tetrafluoroborate is added into the solution to form an electrolyte solution containing ionic liquid;
(4) micropore preparation
The method comprises the steps of adopting a CHI660E electrochemical workstation and a three-electrode system, wherein the three-electrode system is formed by taking a commercial aluminum foil as a working electrode, taking a saturated calomel electrode as a reference electrode and taking a platinum sheet electrode as a counter electrode, adopting cyclic voltammetry, controlling the potential scanning speed to be 20-100 mV/s, setting a potential window in a range of-0.8-1.1V, and taking out the aluminum foil for drying at room temperature to obtain the microporous aluminum foil with the surface aperture of 30-500 mu m, wherein the number of cyclic scanning turns is 10-100.
The invention has the following beneficial effects: the invention can generate micropores on the surface of the aluminum foil, and the diameter of the micropores can be adjusted according to the potential window, the number of cycles of cyclic scanning and the amount of ionic liquid, thereby realizing the effective regulation and control of the aperture. The method is simple and easy to implement, has low cost, opens up a new idea for the application of the aluminum foil in the micro device, and has potential commercial value.
Drawings
Fig. 1 is a photograph of a pure commercial aluminum foil and an aluminum foil with micro-holes produced. Where photo a is a pure commercial aluminum foil with a smooth surface showing an off-white natural color of aluminum. Photograph B is a microporous aluminum foil after cyclic voltammetry treatment. Therefore, after cyclic voltammetry scanning, a green film is produced on the surface of the aluminum foil, micropores are formed, and black spots in the figure are the generated micropores.
Fig. 2 is a photograph of the aluminum foil magnified 5 times under a microscope. Wherein A is1A photograph of a pure commercial aluminum foil, magnified 5 times. It can be seen that a uniform off-white color was shown on the surface of the aluminum foil. B is1The photograph of the pure aluminum foil after cyclic voltammetry scanning in the electrolyte containing the ionic liquid shows that besides the appearance of a gray green film, obvious micropores (black spots in the figure are the generated micropores) are also formed on the surface of the aluminum foil, and the diameter of the micropores is about 180 micrometers.
Detailed Description
The following examples serve to illustrate the invention.
Example 1
Make up 100mL of distilled water containing H2SO4、Na2SO4 and aniline in solution, H in this solution2The concentration of SO4 was 0.8 mol/L, Na2The concentration of SO4 was 0.6 mol/L and the concentration of aniline was 0.4 mol/L. 1 g of 1-butyl-3-methylimidazolium tetrafluoroborate is then added to the solution to form an ionic liquid-containing electrolyte solution. The microwell was prepared using the CHI660E electrochemical workstation and a three-electrode system. The three-electrode system is formed by using a commercial aluminum foil as a working electrode, a saturated calomel electrode as a reference electrode and a platinum sheet electrode as a counter electrode. And then, controlling the potential scanning speed to be 50 mV/s by adopting a cyclic voltammetry, setting a potential window in a range of-0.8-1.1V, wherein the number of cycles of cyclic scanning is 50, and then taking out the aluminum foil and drying at room temperature to obtain the microporous aluminum foil with the surface pore diameter of about 200 mu m.
Example 2
Make up 100mL of distilled water containing H2SO4、Na2SO4 and aniline in solution, H in this solution2The concentration of SO4 was 0.6 mol/L, Na2The concentration of SO4 was 0.5 mol/L and the concentration of aniline was 0.4 mol/L. 0.75 g of 1-butyl-3-methylimidazolium tetrafluoroborate was then added to the solution to form an ionic liquid-containing electrolyte solution. The microwell was prepared using the CHI660E electrochemical workstation and a three-electrode system. The three-electrode system is formed by using a commercial aluminum foil as a working electrode, a saturated calomel electrode as a reference electrode and a platinum sheet electrode as a counter electrode. And then, controlling the potential scanning speed to be 80 mV/s by adopting a cyclic voltammetry, setting a potential window in a range of-0.8-1.1V, wherein the number of the cyclic scanning circles is 60, and then taking out the aluminum foil and drying at room temperature to obtain the microporous aluminum foil with the surface pore diameter of about 250 microns.
Example 3
Make up 100mL of distilled water containing H2SO4、Na2Solution of SO4 and anilineH in this solution2The concentration of SO4 was 0.5 mol/L, Na2The concentration of SO4 was 0.3 mol/L and the concentration of aniline was 0.4 mol/L. 0.8 g of 1-butyl-3-methylimidazolium tetrafluoroborate was then added to the solution to form an ionic liquid-containing electrolyte solution. The microwell was prepared using the CHI660E electrochemical workstation and a three-electrode system. The three-electrode system is formed by using a commercial aluminum foil as a working electrode, a saturated calomel electrode as a reference electrode and a platinum sheet electrode as a counter electrode. And then, controlling the potential scanning speed to be 60 mV/s by adopting a cyclic voltammetry, setting a potential window in a range of-0.8-1.1V, wherein the number of cycles of cyclic scanning is 70, and then taking out the aluminum foil and drying at room temperature to obtain the microporous aluminum foil with the surface pore diameter of about 350 mu m.
Example 4
Make up 100mL of distilled water containing H2SO4、Na2SO4 and aniline in solution, H in this solution2The concentration of SO4 was 0.7 mol/L, Na2The concentration of SO4 was 0.75 mol/L and the concentration of aniline was 0.4 mol/L. 0.75 g of 1-butyl-3-methylimidazolium tetrafluoroborate was then added to the solution to form an ionic liquid-containing electrolyte solution. The microwell was prepared using the CHI660E electrochemical workstation and a three-electrode system. The three-electrode system is formed by using a commercial aluminum foil as a working electrode, a saturated calomel electrode as a reference electrode and a platinum sheet electrode as a counter electrode. And then, controlling the potential scanning speed to be 80 mV/s by adopting a cyclic voltammetry, setting a potential window in a range of-0.8-1.1V, wherein the number of cycles of cyclic scanning is 40, and then taking out the aluminum foil and drying at room temperature to obtain the microporous aluminum foil with the surface pore diameter of about 400 mu m.
Example 5
Make up 100mL of distilled water containing H2SO4、Na2SO4 and aniline in solution, H in this solution2The concentration of SO4 was 0.9 mol/L, Na2The concentration of SO4 was 0.65 mol/L and the concentration of aniline was 0.4 mol/L. 1.5 g of 1-butyl-3-methylimidazolium tetrafluoroborate was then added to the solution to form an ionic liquid-containing electrolyte solution. CHI660E electrochemical method is adopted in preparation of microporesA chemical workstation and a three-electrode system. The three-electrode system is formed by using a commercial aluminum foil as a working electrode, a saturated calomel electrode as a reference electrode and a platinum sheet electrode as a counter electrode. And then, controlling the potential scanning speed to be 80 mV/s by adopting a cyclic voltammetry, setting a potential window in a range of-0.8-1.1V, wherein the number of cycles of cyclic scanning is 70, and then taking out the aluminum foil and drying at room temperature to obtain the microporous aluminum foil with the surface pore diameter of about 400 microns.
Example 6
Make up 100mL of distilled water containing H2SO4、Na2SO4 and aniline in solution, H in this solution2The concentration of SO4 was 0.8 mol/L, Na2The concentration of SO4 was 0.35 mol/L and the concentration of aniline was 0.4 mol/L. 1.3 g of 1-butyl-3-methylimidazolium tetrafluoroborate was then added to the solution to form an ionic liquid-containing electrolyte solution. The microwell was prepared using the CHI660E electrochemical workstation and a three-electrode system. The three-electrode system is formed by using a commercial aluminum foil as a working electrode, a saturated calomel electrode as a reference electrode and a platinum sheet electrode as a counter electrode. And then, controlling the potential scanning speed to be 80 mV/s by adopting a cyclic voltammetry, setting a potential window in a range of-0.8-1.1V, wherein the number of cycles of cyclic scanning is 50, and then taking out the aluminum foil and drying at room temperature to obtain the microporous aluminum foil with the surface pore diameter of about 440 mu m.

Claims (1)

1. A method of making micro-holes in a commercial aluminum foil, comprising the steps of:
(1) material preparation
A sulfuric acid solution; a sodium sulfate solution; aniline; an ionic liquid; commercial aluminum foil;
(2) apparatus and material preparation for electrochemical preparation
CHI660E electrochemical workstation; a salt bridge; a saturated calomel electrode; a platinum sheet electrode;
(3) sample preparation
First, 100mL of a solution containing H was prepared with distilled water2SO4、Na2SO4 and aniline in solution, H in this solution2Of SO4The concentration is 0.5 to 1.0 mol/L, Na2The concentration of SO4 is 0.1-0.8 mol/L, the concentration of aniline is 0.4 mol/L, and then 0.5-2 g of 1-butyl-3-methylimidazolium tetrafluoroborate is added into the mixed solution to form an electrolyte solution containing ionic liquid;
(4) micropore preparation
The method comprises the steps of adopting a CHI660E electrochemical workstation and a three-electrode system, wherein the three-electrode system is formed by taking a commercial aluminum foil as a working electrode, taking a saturated calomel electrode as a reference electrode and taking a platinum sheet electrode as a counter electrode, adopting cyclic voltammetry, controlling the potential scanning speed to be 20-100 mV/s, setting a potential window in a range of-0.8-1.1V, and taking out the aluminum foil for drying at room temperature to obtain the microporous aluminum foil with the surface aperture of 30-500 mu m, wherein the number of cyclic scanning turns is 10-100.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101285208A (en) * 2007-04-12 2008-10-15 深圳市比克电池有限公司 Coursing and hole-distributing method at aluminum foil surface for lithium ion secondary battery
CN109860514A (en) * 2019-03-25 2019-06-07 河北师范大学 A method of changing lithium battery copper foil of affluxion body surface topography
CN110048126A (en) * 2019-03-24 2019-07-23 荆门市亿美工业设计有限公司 A kind of manufacture craft and plus plate current-collecting body of aluminium foil
CN110257893A (en) * 2019-05-29 2019-09-20 安徽省临泉县康悦电子科技有限公司 A kind of aluminum foil corrosion technique
CN111074258A (en) * 2019-12-30 2020-04-28 河北师范大学 Method for blackening copper foil and recovering primary color at room temperature

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101285208A (en) * 2007-04-12 2008-10-15 深圳市比克电池有限公司 Coursing and hole-distributing method at aluminum foil surface for lithium ion secondary battery
CN110048126A (en) * 2019-03-24 2019-07-23 荆门市亿美工业设计有限公司 A kind of manufacture craft and plus plate current-collecting body of aluminium foil
CN109860514A (en) * 2019-03-25 2019-06-07 河北师范大学 A method of changing lithium battery copper foil of affluxion body surface topography
CN110257893A (en) * 2019-05-29 2019-09-20 安徽省临泉县康悦电子科技有限公司 A kind of aluminum foil corrosion technique
CN111074258A (en) * 2019-12-30 2020-04-28 河北师范大学 Method for blackening copper foil and recovering primary color at room temperature

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Corrosion and electrochemical behaviors of pure aluminum in novel KOH-ionic liquid-water solutions;J. M. Wang et.al.;《Materials and Corrosion》;20091231;第60卷(第12期);第977-981页 *

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