CN100527300C - Method for modifying surface of aluminum electrode foil - Google Patents
Method for modifying surface of aluminum electrode foil Download PDFInfo
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- CN100527300C CN100527300C CNB200710009215XA CN200710009215A CN100527300C CN 100527300 C CN100527300 C CN 100527300C CN B200710009215X A CNB200710009215X A CN B200710009215XA CN 200710009215 A CN200710009215 A CN 200710009215A CN 100527300 C CN100527300 C CN 100527300C
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Abstract
The invention is related to method for modifying surface of porous Al2O3 substrate of aluminum foil for electrode. The method includes steps: using organic solvent to clean out, and air-dry the aluminum foil for electrode; preparing water solution of negative matter; preparing alcohol solution of silane coupler, or mixed liquor of alcohol and water; immersing the aluminum foil into the water solution of negative matter for dipping, cleaning and drying it; then, dipping it into prepared solution, and cleaning and drying it; preparing monomeric organic solutions of pyrrole, surface active agent, and dopant as well as water solution of oxidant; mixing monomeric organic solutions with water solution of oxidant to form polyreaction liquid; dipping the aluminum foil for electrode into the polyreaction liquid, and cleaning and drying it so as to obtain aluminum electrode foil with surface covered by well electric, consecutive, compact pyrrole film.
Description
Technical field
The present invention relates to a kind of aluminum electric pole foil, especially relate to a kind of employing negative substance and silane coupler aluminum electric pole foil porousness Al
2O
3The method of modification is carried out on the surface of substrate.
Background technology
Electric polypyrrole (Polypyrrole is called for short PPY) film is a kind of novel conductive polymer functional material. the PPY film that will conduct electricity is deposited on the deielectric-coating Al of aluminum electric pole foil
2O
3The surface is as negative electrode, replace the higher Working electrolyte negative electrode of original resistivity, can reduce the equivalent series resistance of capacitor effectively, make capacitor have good impedance frequency characteristic, high reliability and be easy to characteristics such as chip type (forestry is clear, Hong Xuebao. the aluminium electrolytic capacitor engineering. Xiamen: publishing house of Xiamen University, 2007).But Al
2O
3Belong to ionic crystals, after surface ion loses outer ion, destroyed electrostatic equilibrium, because polarization can produce " electric double layer effect " (Zhu Lvbing on its surface, wrap emerging. surface and surface physics. Tianjin: publishing house of University Of Tianjin, 1992), make the crystal film surface have negative potential, thereby in the less acid solution of pH value, Al
2O
3H in the film surface meeting adsorbent solution
+, form Al-OH
2(Zhang Lide, Mu Jimei. nano material and nanostructure. Beijing: Science Press, 2001), cause Al
2O
3The film surface has positive potential, and especially after technologies such as surface clean, its hydrophily increases greatly.This makes in polymerization process, positively charged and have fine oil loving pyrrole monomer and basilar memebrane surface produces repulsion, increased it in the suprabasil difficulty of adhering to of porousness, to the coverage rate of polypyrrole film forming and continuously, problems such as even compact and tack produce very big influence.So in the research of this novel electrolytic capacitor, difficult point that faces and most critical point are how at surface irregularity and be cavernous aluminum electric pole foil deielectric-coating Al
2O
3Form on the surface evenly continuously, adhere to favorable conductive PPY film.
Summary of the invention
The objective of the invention is to overcome and solve above-mentioned difficult point problem, a kind of method of modifying of surface of aluminum electrode foil is provided.
Technical scheme of the present invention be adopt negative substance and silane coupler to the surface modification of aluminum electric pole foil and in the substrate after the modification chemistry form conducting polymer thin film.
The present invention includes following steps:
1) aluminum electric pole foil is dried with the organic solvent cleaning;
2) the preparation mass fraction is the aqueous solution of 1%～8% negative substance;
3) the preparation mass fraction is the ethanolic solution of 0.5%～100% silane coupler or the mixed solution of ethanol and water;
4) aluminum electric pole foil cleaned in the step 1) is immersed step 2) in the mass fraction for preparing be the aqueous solution of 1%～8% negative substance, impregnation process is cleaned oven dry with deionized water and absolute ethyl alcohol;
5) aluminum electric pole foil after will drying immerses in the solution that step 3) prepares, and cleans drying with deionized water and absolute ethyl alcohol again;
6) the monomer organic solution of preparation pyrroles, surfactant and dopant, and the aqueous solution of oxidant;
7) aqueous solution with monomer organic solution and oxidant forms polymerization liquid;
8) under-25～0 ℃ of temperature with step 4) or 5) aluminum electric pole foil of gained immerses in the polymerization liquid of step 7) and reacts, clean with deionized water and absolute ethyl alcohol, drying can obtain the surface and be coated with continuous densification, adheres to the aluminum electric pole foil of favorable conductive polypyrrole film.
In step 1), organic solvent can adopt absolute ethyl alcohol, acetone, methyl alcohol, carrene, ethyl acetate etc.
Negative substance can adopt a kind of in stearic acid, enanthic acid, neopelex, naphthalene sulfonic acids, dodecyl sodium sulfonate, the camphorsulfonic acid etc.
Silane coupler can adopt a kind of in vinyl three TMOSs, γ-aminopropyltriethoxywerene werene, γ-methacrylate propyl group three TMOSs, vinyl three (β-methoxyethoxy) silane, the γ-glycidoxy trimethoxy silane etc.
In step 4), the time of impregnation process is preferably 10～60min.
In step 5), the time that aluminum electric pole foil is immersed in the solution that step 3) prepares is preferably 10～120min.
Surfactant can adopt neopelex, paratoluenesulfonic acid sodium salt, sodium naphthalene sulfonate or dodecyl sodium sulfate.Dopant can adopt p-nitrophenol.In molar ratio, pyrroles: oxidant: surfactant: dopant=1: (0.20～0.35): (0.02～0.05): (0.08～0.27).Organic solvent in the monomer organic solution is selected from methyl alcohol, ethanol, ethylene glycol, glycerol, acetonitrile or oxolane.Oxidant is selected from least a in ammonium persulfate, ferric sulfate, iron chloride, p-methyl benzenesulfonic acid iron, the hydrogen peroxide etc.
In step 8), the time of reaction is preferably 0.5～12h.
React 0.5～12h again in the polymerization liquid of the aluminum electric pole foil immersion step 7) that step 8) can be obtained, clean with deionized water and absolute ethyl alcohol, can obtain the continuous compactness and the better aluminum electric pole foil of adhesive force of the electric polypyrrole film of surperficial coating after the drying.But this step repetitive operation 1～3 time, the repetitive operation number of times is many more, and the quality of resulting surface of aluminum electrode foil coating is good more.
Advantage of the present invention is: by negative substance and silane coupler aluminum electric pole foil cellular dielectric layer is carried out surface modification, the conducting polymer thin film that the cellular dielectric layer surface of the aluminum electric pole foil after the modification forms, have evenly, continuously, fine and close, adhere to good characteristics, improved film of poly pyrrole in suprabasil coverage rate and uniformity, obtain the surface and be coated with continuous densification, adhered to the aluminum electric pole foil of favorable conductive polypyrrole film.
Description of drawings
Fig. 1 is the SEM photo of the embodiment of the invention 1.
Fig. 2 is the SEM photo of the embodiment of the invention 2.
Fig. 3 is the SEM photo of the embodiment of the invention 3.
Fig. 4 is the SEM photo of the embodiment of the invention 4.
Fig. 5 is the SEM photo of the embodiment of the invention 5.
Fig. 6 is the SEM photo of comparative example's (aluminum electric pole foil of long time without surface modification treatment reaction polypyrrole).
Embodiment
Embodiment 1
With size is the aluminum electric pole foil acetone ultrasonic waves for cleaning 5min of 0.5cm * 4.5cm, the immersion mass fraction was γ-aminopropyltriethoxywerene werene solution of 100% after room temperature was dried, at room temperature surface modification treatment 10min cleans drying earlier again with ethanolic solution with washed with de-ionized water.Immerse under-15 ℃ of temperature and contain the molar ratio pyrroles: ammonium persulfate: neopelex: p-nitrophenol is 1: 0.35: 0.02: react 4h in 0.08 the polymerization liquid, clean drying with deionized water and absolute ethyl alcohol respectively then; Repeat the step twice of aluminum electric pole foil dipping polymerization liquid reaction, obtain the surface be coated with the electric polypyrrole film aluminum electric pole foil the SEM photo as shown in Figure 1.
Embodiment 2
With size is the aluminum electric pole foil methyl alcohol ultrasonic waves for cleaning 5min of 0.5cm * 4.5cm, the immersion mass fraction was 100% vinyl three TMOS solution after room temperature was dried, at room temperature surface modification treatment 120min cleans drying earlier again with ethanolic solution with washed with de-ionized water.Immerse under-15 ℃ of temperature and contain the molar ratio pyrroles: ammonium persulfate: neopelex: p-nitrophenol is 1: 0.20: 0.04: react 4h in 0.08 the polymerization liquid, clean drying with deionized water and absolute ethyl alcohol respectively then.Obtain the surface be coated with the electric polypyrrole film aluminum electric pole foil the SEM photo as shown in Figure 2.
Embodiment 3
With size is the aluminum electric pole foil ethanol ultrasonic waves for cleaning 5min of 0.5cm * 4.5cm, it is 0.5% γ-aminopropyltriethoxywerene werene solution that room temperature is dried back immersion mass fraction, at room temperature surface modification treatment 120min cleans drying earlier again with ethanolic solution with washed with de-ionized water.Immerse under-15 ℃ of temperature and contain the molar ratio pyrroles: ammonium persulfate: neopelex: p-nitrophenol is 1: 0.25: 0.04: react 4h in 0.10 the polymerization liquid, clean drying with deionized water and absolute ethyl alcohol respectively then.Obtain the surface be coated with the electric polypyrrole film aluminum electric pole foil the SEM photo as shown in Figure 3.
Embodiment 4
The aluminum electric pole foil that with size is 0.5cm * 4.5cm is with ethyl acetate ultrasonic waves for cleaning 5min, and room temperature is dried the back, and to immerse mass fraction be surface modification treatment 30min in 4% the sodium dodecyl benzene sulfonate aqueous solution, cleans oven dry respectively with deionized water and ethanol; Immerse mass fraction again and be γ-aminopropyltriethoxywerene werene solution solution of 100%, at room temperature surface modification treatment 120min cleans drying earlier again with ethanolic solution with washed with de-ionized water; Immerse under-15 ℃ of temperature and contain the molar ratio pyrroles: ammonium persulfate: neopelex: p-nitrophenol is 1: 0.35: 0.05: react 4h in 0.15 the polymerization liquid, clean drying with deionized water and absolute ethyl alcohol respectively then.Obtain the surface be coated with the electric polypyrrole film aluminum electric pole foil the SEM photo as shown in Figure 4.
Embodiment 5
The aluminum electric pole foil that with size is 0.5cm * 4.5cm is with carrene ultrasonic waves for cleaning 5min, and room temperature is dried the back, and to immerse mass fraction be surface modification treatment 30min in 8% the sodium dodecyl benzene sulfonate aqueous solution, cleans oven dry respectively with deionized water and ethanol; Immerse pure γ-aminopropyltriethoxywerene werene solution solution again, at room temperature surface modification treatment 120min cleans drying earlier again with ethanolic solution with washed with de-ionized water; Immerse under-15 ℃ of temperature and contain the molar ratio pyrroles: ammonium persulfate: neopelex: p-nitrophenol is 1: 0.35: 0.04: react 4h in 0.27 the polymerization liquid, clean drying with deionized water and absolute ethyl alcohol respectively then; Repeat the step twice of aluminum electric pole foil dipping polymerization liquid reaction.Obtain the surface be coated with the electric polypyrrole film aluminum electric pole foil the SEM photo as shown in Figure 5.
Embodiment 6
The aluminum electric pole foil that with size is 0.5cm * 4.5cm is with acetone ultrasonic waves for cleaning 5min, and room temperature is dried the back, and to immerse mass fraction be surface modification treatment 10min in 1% the dodecyl sodium sulfonate aqueous solution, cleans oven dry respectively with deionized water and ethanol; Immerse mass fraction again and be γ-glycidoxy trimethoxy silane solution of 0.5%, at room temperature surface modification treatment 30min cleans drying earlier again with ethanolic solution with washed with de-ionized water; Immerse under-25 ℃ of temperature and contain the molar ratio pyrroles: ferric sulfate: dodecyl sodium sulfate: p-nitrophenol is 1: 0.30: 0.04: react 12h in 0.08 the polymerization liquid, clean drying with deionized water and absolute ethyl alcohol respectively then; Repeat the step twice of aluminum electric pole foil dipping polymerization liquid reaction.Can obtain the aluminum electric pole foil that the surface is coated with the electric polypyrrole film of even compact.
Embodiment 7
The aluminum electric pole foil that with size is 0.5cm * 4.5cm is with ethyl acetate ultrasonic waves for cleaning 5min, and room temperature is dried the back, and to immerse mass fraction be surface modification treatment 40min in 4% the enanthic acid aqueous solution, cleans oven dry respectively with deionized water and ethanol; Immerse mass fraction again and be 10% vinyl three (β-methoxyethoxy) solution of silane, at room temperature surface modification treatment 60min cleans drying earlier again with ethanolic solution with washed with de-ionized water; Immerse under-20 ℃ of temperature and contain the molar ratio pyrroles: p-methyl benzenesulfonic acid iron: dodecyl sodium sulfate: p-nitrophenol is 1: 0.35: 0.03: react 8h in 0.12 the polymerization liquid, clean drying with deionized water and absolute ethyl alcohol respectively then; Repeat the step 3 time of aluminum electric pole foil dipping polymerization liquid reaction.Can obtain the aluminum electric pole foil that the surface is coated with the electric polypyrrole film of even compact.
Embodiment 8
The aluminum electric pole foil that with size is 0.5cm * 4.5cm is with carrene ultrasonic waves for cleaning 5min, and room temperature is dried the back, and to immerse mass fraction be surface modification treatment 60min in 6% the naphthalene sulfonic acids aqueous solution, cleans oven dry respectively with deionized water and ethanol; Immerse mass fraction again and be γ-methacrylate propyl group three TMOS solution of 10%, at room temperature surface modification treatment 60min cleans drying earlier again with ethanolic solution with washed with de-ionized water; Immerse under-10 ℃ of temperature and contain the molar ratio pyrroles: iron chloride: sodium naphthalene sulfonate: p-nitrophenol is 1: 0.35: 0.05: react 2.5h in 0.20 the polymerization liquid, clean drying with deionized water and absolute ethyl alcohol respectively then; Repeat the step 1 time of aluminum electric pole foil dipping polymerization liquid reaction.Can obtain the aluminum electric pole foil that the surface is coated with the electric polypyrrole film of even compact.
Embodiment 9
The aluminum electric pole foil that with size is 0.5cm * 4.5cm is with acetone ultrasonic waves for cleaning 5min, and room temperature is dried the back, and to immerse mass fraction be surface modification treatment 60min in 1% the stearic acid aqueous solution, cleans oven dry respectively with deionized water and ethanol; Immerse mass fraction again and be γ-methacrylate propyl group three TMOS solution of 75%, at room temperature surface modification treatment 60min cleans drying earlier again with ethanolic solution with washed with de-ionized water; Immerse under-5 ℃ of temperature and contain the molar ratio pyrroles: hydrogen peroxide: paratoluenesulfonic acid sodium salt: p-nitrophenol is 1: 0.25: 0.04: react 1.5h in 0.10 the polymerization liquid, clean drying with deionized water and absolute ethyl alcohol respectively then; Repeat the step twice of aluminum electric pole foil dipping polymerization liquid reaction.Can obtain the aluminum electric pole foil that the surface is coated with the electric polypyrrole film of even compact.
Embodiment 10
The aluminum electric pole foil that with size is 0.5cm * 4.5cm is with acetone ultrasonic waves for cleaning 5min, and room temperature is dried the back, and to immerse mass fraction be surface modification treatment 30min in 4% the camphorsulfonic acid aqueous solution, cleans oven dry respectively with deionized water and ethanol; Immerse mass fraction again and be 100% vinyl three TMOS solution, at room temperature surface modification treatment 90min cleans drying earlier again with ethanolic solution with washed with de-ionized water; Immerse under 0 ℃ of temperature and contain the molar ratio pyrroles: ammonium persulfate+p-methyl benzenesulfonic acid iron (etc. mol ratio): neopelex: p-nitrophenol is 1: 0.30: 0.04: react 0.5h in 0.08 the polymerization liquid, clean drying with deionized water and absolute ethyl alcohol respectively then; Repeat the step twice of aluminum electric pole foil dipping polymerization liquid reaction.Can obtain the aluminum electric pole foil that the surface is coated with the electric polypyrrole film of even compact.
The comparative example
With size is the aluminum electric pole foil acetone ultrasonic waves for cleaning 5min of 0.5cm * 4.5cm, room temperature is dried back immersion under-15 ℃ of temperature and contained the molar ratio pyrroles: ammonium persulfate: neopelex: p-nitrophenol is 1: 0.35: 0.02: react 4h in 0.08 the polymerization liquid, clean drying with deionized water and absolute ethyl alcohol respectively then; Repeat the step twice of aluminum electric pole foil dipping polymerization liquid reaction.Obtain SEM photo such as Fig. 6 that the surface is coated with the aluminum electric pole foil of electric polypyrrole film.As seen from Figure 6, the electric polypyrrole film continuity and the compactness of coating is bad on the aluminum electric pole foil of long time without surface modification.
Claims (9)
1. the method for modifying of surface of aluminum electrode foil is characterized in that may further comprise the steps:
1) aluminum electric pole foil is dried with the organic solvent cleaning;
2) the preparation mass fraction is the aqueous solution of 1%～8% negative substance;
3) the preparation mass fraction is the ethanolic solution of 0.5%～100% silane coupler or the mixed solution of ethanol and water;
4) aluminum electric pole foil cleaned in the step 1) is immersed step 2) in the mass fraction for preparing be the aqueous solution of 1%～8% negative substance, impregnation process is cleaned oven dry with deionized water and absolute ethyl alcohol;
5) aluminum electric pole foil after will drying immerses in the solution that step 3) prepares, and cleans drying with deionized water and absolute ethyl alcohol again;
6) the monomer organic solution of preparation pyrroles, surfactant and dopant, and the aqueous solution of oxidant;
7) aqueous solution with monomer organic solution and oxidant forms polymerization liquid;
8) under-25～0 ℃ of temperature with step 4) or 5) aluminum electric pole foil of gained immerses in the polymerization liquid of step 7) and reacts, clean with deionized water and absolute ethyl alcohol, drying can obtain the surface and be coated with continuous densification, adheres to the aluminum electric pole foil of favorable conductive polypyrrole film;
Described negative substance is a kind of in stearic acid, enanthic acid, neopelex, naphthalene sulfonic acids, dodecyl sodium sulfonate, the camphorsulfonic acid.
2. the method for modifying of surface of aluminum electrode foil as claimed in claim 1 is characterized in that in step 1), and organic solvent is absolute ethyl alcohol, acetone, methyl alcohol, carrene or ethyl acetate.
3. the method for modifying of surface of aluminum electrode foil as claimed in claim 1 is characterized in that silane coupler is a kind of in vinyl three TMOSs, γ-aminopropyltriethoxywerene werene, γ-methacrylate propyl group three TMOSs, vinyl three (β-methoxyethoxy) silane, the γ-glycidoxy trimethoxy silane.
4. the method for modifying of surface of aluminum electrode foil as claimed in claim 1 is characterized in that in step 4), and the time of impregnation process is 10～60min.
5. the method for modifying of surface of aluminum electrode foil as claimed in claim 1 is characterized in that in step 5), and the time that aluminum electric pole foil is immersed in the solution that step 3) prepares is 10～120min.
6. the method for modifying of surface of aluminum electrode foil as claimed in claim 1 is characterized in that surfactant is neopelex, paratoluenesulfonic acid sodium salt, sodium naphthalene sulfonate or dodecyl sodium sulfate; Dopant is a p-nitrophenol.
7. the method for modifying of surface of aluminum electrode foil as claimed in claim 1 is characterized in that in the polymerization liquid in molar ratio pyrroles: oxidant: surfactant: dopant=1: 0.20～0.35: 0.02～0.05: 0.08～0.27.
8. the method for modifying of surface of aluminum electrode foil as claimed in claim 1 is characterized in that the organic solvent in the monomer organic solution is selected from methyl alcohol, ethanol, ethylene glycol, glycerol, acetonitrile or oxolane; Oxidant is selected from least a in ammonium persulfate, ferric sulfate, iron chloride, p-methyl benzenesulfonic acid iron, the hydrogen peroxide.
9. the method for modifying of surface of aluminum electrode foil as claimed in claim 1 is characterized in that in step 8), and the time of reaction is 0.5～12h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200710009215XA CN100527300C (en) | 2007-07-13 | 2007-07-13 | Method for modifying surface of aluminum electrode foil |
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|---|---|---|---|
| CNB200710009215XA CN100527300C (en) | 2007-07-13 | 2007-07-13 | Method for modifying surface of aluminum electrode foil |
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| CN100527300C true CN100527300C (en) | 2009-08-12 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101901694A (en) * | 2010-06-23 | 2010-12-01 | 万星光电子(东莞)有限公司 | Super capacitor electrode slice |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101609748B (en) * | 2008-06-16 | 2011-02-02 | 吴昊 | Modified liquid of anode aluminum foil of electrolytic capacitor and preparation method and application thereof |
| CN104577039B (en) * | 2014-12-13 | 2016-11-16 | 山东精工电子科技有限公司 | The preparation method of lithium titanate anode collector |
| CN105061731A (en) * | 2015-07-31 | 2015-11-18 | 天津大学 | Method for constructing multistage morphology polypyrrole membrane based on in situ wrinkling and thermal expansion |
| CN107731531A (en) * | 2017-11-22 | 2018-02-23 | 贵州振华电子信息产业技术研究有限公司 | Mixed polymerization solution, chip-type solid aluminium electrolutic capacitor and its hybrid polymerization technique |
| CN111223678A (en) * | 2020-01-08 | 2020-06-02 | 重庆电子工程职业学院 | Method for preparing PPy flexible capacitor film conductor with porous structure |
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| US6440288B1 (en) * | 2000-01-13 | 2002-08-27 | Korea Advanced Institute Of Science And Technology | Method for preparing anode electrode for high voltage electrolytic capacitor |
| CN1484259A (en) * | 2003-07-10 | 2004-03-24 | 深圳市东阳光化成箔股份有限公司 | Method for mfg of anode foil of aluminium electrolytic capacitor |
| CN1598985A (en) * | 2004-08-20 | 2005-03-23 | 厦门大学 | Nano holing method on surface of low-voltage anode foil for aluminium electrolytic capacitor |
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2007
- 2007-07-13 CN CNB200710009215XA patent/CN100527300C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6440288B1 (en) * | 2000-01-13 | 2002-08-27 | Korea Advanced Institute Of Science And Technology | Method for preparing anode electrode for high voltage electrolytic capacitor |
| CN1484259A (en) * | 2003-07-10 | 2004-03-24 | 深圳市东阳光化成箔股份有限公司 | Method for mfg of anode foil of aluminium electrolytic capacitor |
| CN1598985A (en) * | 2004-08-20 | 2005-03-23 | 厦门大学 | Nano holing method on surface of low-voltage anode foil for aluminium electrolytic capacitor |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101901694A (en) * | 2010-06-23 | 2010-12-01 | 万星光电子(东莞)有限公司 | Super capacitor electrode slice |
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