CN104499024A - Anodization method for construction of corrosion resistant superhydrophobic aluminium surface - Google Patents
Anodization method for construction of corrosion resistant superhydrophobic aluminium surface Download PDFInfo
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- CN104499024A CN104499024A CN201410668488.5A CN201410668488A CN104499024A CN 104499024 A CN104499024 A CN 104499024A CN 201410668488 A CN201410668488 A CN 201410668488A CN 104499024 A CN104499024 A CN 104499024A
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- aluminium
- aluminium flake
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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
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
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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
- C25D11/16—Pretreatment, e.g. desmutting
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Abstract
An anodization method for construction of a corrosion resistant superhydrophobic aluminium surface. The method is as below: carrying out ultrasonic cleaning on an aluminum sheet with acetone and ethanol at room temperature, then rinsing with deionized water, then putting the aluminum sheet in sodium hydroxide solution for alkali corrosion, then rinsing with deionized water, and placing the aluminum sheet in a nitrate solution for acid etching; using the pretreated aluminum sheet as anode and a lead plate as cathode for electrolysis in a phosphoric acid solution, and keeping the electrolyte at a constant temperature to generate an alumina film on the surface; immersing the treated aluminum sheet in ammonia water, and corroding the aluminum sheet with ammonia water; immersing the treated aluminum sheet into a hexamethyl-disilazane solution, then taking out the aluminum sheet, sealing in a closed container, placing the container in an oven at a constant temperature between 100-140 DEG C for 15-30 h, and taking out the container to obtain the superhydrophobic aluminum sheet. The prepared superhydrophobic film and aluminum substrate surface are combined by chemical bond, thus the superhydrophobic character is easy to control and stable.
Description
Technical field
The invention belongs to materialogy field, particularly relate to a kind of super hydrophobic material, a kind of anonizing builds the method on non-corrosibility Super-hydrophobic aluminium surface specifically.
Background technology
Super-hydrophobic have self-cleaning performance as lotus leaf surface, thus can be applicable to, on the actual articles for use such as shield glass, concrete formation rear surface, ceramic surface, high-class timber, rainwash can be utilized to realize automatically cleaning; Be applied to inner-walls of duct or submarine, boats and ships shell time, the frictional force between its appearance and current or other liquid can be reduced thus improve dynamic performance; Super hydrophobic surface is applied on textiles, can play the effect of good automatically cleaning, antifouling, waterproof; Be applied in effect high-tension cable effectively can playing passive deicing, prevent the overweight snow and ice cover caused due to ice and snow weather on cable, cause the situation of power system " paralysis " to a certain extent.
Aluminium is the profuse metallic element of content on the earth, and its standing stock occupy the 2nd in a metal.But the metallic surface that conventional aluminium alloy surface treatment method obtains does not have self-cleaning property, easily contaminated, and the digital preservation performance in the caustic soln environment such as acid, alkali, salt is also short of very much.Therefore, the aluminium alloy guard method that the more stable stronger and long lasting protective of research can better be novel is needed.Super-hydrophobic process is carried out on metallic aluminum material surface, can be anticorrosive, and can automatic cleaning action be played; Be applied in some microfluidic devices, can effectively control the resistance between fluid and device, leakage loss situation, in miniature high-tech test products, application prospect is vast.
Through years development, the at present preparation method of existing multiple Al and Alalloy super hydrophobic surface, but adhesive power between prepared based superhydrophobic thin films and substrate surface is inadequate, mechanical property and weather resistance poor, in actual use, based superhydrophobic thin films is easy to be destroyed.For a long time, the adhesion strength between super hydrophobic surface and substrate and its own mechanical performance always are that researchist is in research with prepare the problem that super hydrophobic surface process difficult overcomes.
Summary of the invention
For technical problem of the prior art, the invention provides a kind of anonizing and build the method on non-corrosibility Super-hydrophobic aluminium surface, the method that described this anonizing builds non-corrosibility Super-hydrophobic aluminium surface solves that aluminium flake surface low-surface energy substance in prior art easily comes off, super-hydrophobic poor stability and the technical problem that is easily corroded.
Anonizing of the present invention builds the method on non-corrosibility Super-hydrophobic aluminium surface, comprises the steps:
(1) one by pretreated for aluminium flake step, at ambient temperature successively with acetone and EtOH Sonicate cleaning aluminium flake, then use deionized water rinsing, then aluminium flake is placed on alkaline etching in sodium hydroxide solution, use deionized water rinsing again, finally aluminium flake is placed in salpeter solution acid etching; Thus reach the object of aluminium surface finish.
The step of aluminium flake surface oxidation using above-mentioned pretreated aluminium flake as anode, is negative electrode with stereotype by (2) one, and electrolysis in phosphoric acid solution, electrolytic solution constant temperature, makes its Surface Creation aluminum oxide film.
(3) one by the step of aluminium flake surface roughening, the aluminium flake after step (2) being processed immerses in ammonia soln, and aluminium flake is corroded by ammoniacal liquor.Thus the surface topography of structure micro-nano structure, and aluminum oxide and ammoniacal liquor are reacted, produce hydroxyl.
(4) one by the step of aluminium flake finishing, aluminium flake after step (3) being processed immerses in hexamethyldisilazane solution, then take out and put into encloses container, and place 15 ~ 30h in the constant temperature oven of 100 ~ 140 DEG C, can obtain after taking-up and there is super-hydrophobic aluminium flake.
Further, in step (1), the concentration of sodium hydroxide is 0.5 ~ 2 mol/L, and preferably concentration is 1mol/L, and the time of sodium hydroxide corrosion is 0.5 ~ 2min, and preferably etching time is 1min; The concentration of nitric acid is massfraction 5 ~ 15%, and preferably concentration is massfraction 10%, and the time of nitric acid corrosion is 1-1.5min, and preferably the time is 1.5min.
Further, in step (2), the concentration of phosphoric acid solution is 2.5-4mol/L; Temperature of reaction is-0.5 ~ 2 DEG C; The best is 0 DEG C; Reaction times is 5min-2h, and voltage is 30-60V.
Further, in step (3), the soak time of ammoniacal liquor is 2-5h, the massfraction 25 ~ 40% of ammonia concn.
Further, in step (4), the best constant temperature Heating temperature of aluminium flake is 120 DEG C, and best constant temperature time is 24h.
Further, described aluminium flake is metallic aluminium or aluminium alloy.
The present invention adopts anonizing to make aluminium flake Surface Creation aluminum oxide film, improves the Corrosion Protection of aluminium flake significantly.The form of aluminium flake film with chemical bond between low-surface energy substance is combined, the super hydrophobic material making its bonding force be better than physics to stick formation, thus strengthens the mechanical property of super-hydrophobic aluminium flake and extends its work-ing life.The super-hydrophobic aluminium flake prepared by method of the present invention and the static contact angle of water are all greater than 150o, and Structure deformation angle is less than 5o, to place after three months this aluminium flake static contact angle without considerable change, stable performance.
The present invention compares with prior art, and its technical progress is significant.The present invention makes aluminum substrate be combined with the form of chemical bonding with surface film, substantially increases mechanical property and the anti-corrosion capability of super hydrophobic surface, and long-time its super-hydrophobicity of preserving is without noticeable change, quality is easy to control, and its technique is simple, materials are cheap, are suitable for suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph on super-hydrophobic aluminium flake surface in embodiment 1.
Fig. 2 is the contact angle figure of super-hydrophobic aluminium flake surface and water droplet in embodiment 1.
Embodiment
Also by reference to the accompanying drawings the present invention is set forth further below by specific embodiment, but do not limit the present invention.
embodiment 1
First, by aluminium flake (aluminium element content is 99,99%) successively with acetone, EtOH Sonicate cleaning, and dry up with deionized water rinsing.Immerse subsequently in the aqueous sodium hydroxide solution of 1mol/L and process, the time is 1min, takes out rear deionized water rinsing, and dries up, next immerse 1min in the salpeter solution of massfraction 10% again, takes out rear deionized water rinsing, dries up.The phosphoric acid solution of preparation 2.7mol/L is as electrolytic solution, and be then anode with aluminium sheet, stereotype is that cathodal closing reacts.Controlling temperature of reaction is 0 DEG C, and constant voltage 50V, the reaction times is 15min.Reacted aluminium flake washed with de-ionized water is dried up; In the ammoniacal liquor of massfraction 35%, soak 3h, dry up with deionized water rinsing after taking-up; Finally aluminium flake is immersed in hexamethyldisilazane solution, after taking-up, put into encloses container, and place 24h in the constant temperature oven of 120 DEG C, the aluminium flake with super-hydrophobicity can be prepared.Test this aluminium flake wettability of the surface with contact angle tester, it is 154o that result shows with the contact angle of water.
embodiment 2
First, by aluminium flake (aluminium element content is 99,99%) successively with acetone, EtOH Sonicate cleaning, and dry up with deionized water rinsing.Immerse subsequently in the aqueous sodium hydroxide solution of 1mol/L and process, the time is 1min, takes out rear deionized water rinsing, and dries up, next immerse 1min in the salpeter solution of massfraction 10% again, takes out rear deionized water rinsing, dries up.The phosphoric acid solution of preparation 3.0mol/L is as electrolytic solution, and be then anode with aluminium sheet, stereotype is that cathodal closing reacts.Controlling temperature of reaction is 0 DEG C, and constant voltage 45V, the reaction times is 15min.Reacted aluminium flake washed with de-ionized water is dried up; In the ammoniacal liquor of massfraction 35%, soak 3.5h, dry up with deionized water rinsing after taking-up; Finally aluminium flake is immersed in hexamethyldisilazane solution, after taking-up, put into encloses container, and place 24h in the constant temperature oven of 120 DEG C, the aluminium flake with super-hydrophobicity can be prepared.Test this aluminium flake wettability of the surface with contact angle tester, it is 152o that result shows with the contact angle of water.
embodiment 3
First, by aluminium flake (aluminium element content is 99,99%) successively with acetone, EtOH Sonicate cleaning, and dry up with deionized water rinsing.Immerse subsequently in the aqueous sodium hydroxide solution of 1mol/L and process, the time is 1min, takes out rear deionized water rinsing, and dries up, next immerse 1min in the salpeter solution of massfraction 10% again, takes out rear deionized water rinsing, dries up.The phosphoric acid solution of preparation 2.9mol/L is as electrolytic solution, and be then anode with aluminium sheet, stereotype is that cathodal closing reacts.Controlling temperature of reaction is 0 DEG C, and constant voltage 50V, the reaction times is 20min.Reacted aluminium flake washed with de-ionized water is dried up; In the ammoniacal liquor of massfraction 35%, soak 4h, dry up with deionized water rinsing after taking-up; Finally aluminium flake is immersed in hexamethyldisilazane solution, after taking-up, put into encloses container, and place 26h in the constant temperature oven of 120 DEG C, the aluminium flake with super-hydrophobicity can be prepared.Test this aluminium flake wettability of the surface with contact angle tester, it is 155o that result shows with the contact angle of water.
Claims (6)
1. anonizing builds the method on non-corrosibility Super-hydrophobic aluminium surface, comprises the steps:
One by pretreated for aluminium flake step, at ambient temperature successively with acetone and EtOH Sonicate cleaning aluminium flake, then use deionized water rinsing, then aluminium flake is placed on alkaline etching in sodium hydroxide solution, use deionized water rinsing again, finally aluminium flake is placed in salpeter solution acid etching;
The step of aluminium flake surface oxidation using above-mentioned pretreated aluminium flake as anode, take stereotype as negative electrode by one, electrolysis in phosphoric acid solution, and electrolytic solution constant temperature, makes its Surface Creation aluminum oxide film;
One by the step of aluminium flake surface roughening, the aluminium flake after step (2) being processed immerses in ammonia soln, and aluminium flake is corroded by ammoniacal liquor;
One by the step of aluminium flake finishing, aluminium flake after step (3) being processed immerses in hexamethyldisilazane solution, then take out and put into encloses container, and place 15 ~ 30h in the constant temperature oven of 100 ~ 140 DEG C, can obtain after taking-up and there is super-hydrophobic aluminium flake.
2. a kind of anonizing according to claim 1 builds the method on non-corrosibility Super-hydrophobic aluminium surface, it is characterized in that: in step (1), the concentration of sodium hydroxide is 0.5 ~ 2 mol/L, and the time of sodium hydroxide corrosion is 0.5 ~ 2min; The concentration of nitric acid is massfraction 5 ~ 15%, and the time of nitric acid corrosion is 1-1.5min.
3. a kind of anonizing according to claim 1 builds the method on non-corrosibility Super-hydrophobic aluminium surface, it is characterized in that: in step (2), the concentration of phosphoric acid solution is 2.5-4mol/L; Temperature of reaction is-0.5 ~ 2 DEG C; The best is 0 DEG C; Reaction times is 5min-2h, and voltage is 30-60V.
4. a kind of anonizing according to claim 1 builds the method on non-corrosibility Super-hydrophobic aluminium surface, it is characterized in that: in step (3), the soak time of ammoniacal liquor is 2-5h.
5. a kind of anonizing according to claim 1 builds the method on non-corrosibility Super-hydrophobic aluminium surface, it is characterized in that: in step (4), the best constant temperature Heating temperature of aluminium flake is 120 DEG C, and best constant temperature time is 24h.
6. a kind of anonizing according to claim 1 builds the method on non-corrosibility Super-hydrophobic aluminium surface, it is characterized in that: described aluminium flake is metallic aluminium or aluminium alloy.
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| CN201410668488.5A CN104499024A (en) | 2014-11-20 | 2014-11-20 | Anodization method for construction of corrosion resistant superhydrophobic aluminium surface |
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| CN201410668488.5A CN104499024A (en) | 2014-11-20 | 2014-11-20 | Anodization method for construction of corrosion resistant superhydrophobic aluminium surface |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109267135A (en) * | 2018-11-29 | 2019-01-25 | 上海交通大学 | A kind of three-dimensional network interpenetrating organic/inorganic hydrophobic coating and preparation method thereof |
| CN109468648A (en) * | 2018-12-29 | 2019-03-15 | 哈尔滨工业大学 | The large-scale producing method on aluminum or aluminum alloy antifrost surface |
| CN112871606A (en) * | 2021-01-08 | 2021-06-01 | 同曦集团有限公司 | Preparation method of super-hydrophobic antibacterial antiviral stainless steel based on electrochemical etching |
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| CN1695049A (en) * | 2001-12-21 | 2005-11-09 | 恩德莱斯和豪瑟尔两合公司 | Hydrophobically coated pressure sensor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109267135A (en) * | 2018-11-29 | 2019-01-25 | 上海交通大学 | A kind of three-dimensional network interpenetrating organic/inorganic hydrophobic coating and preparation method thereof |
| CN109468648A (en) * | 2018-12-29 | 2019-03-15 | 哈尔滨工业大学 | The large-scale producing method on aluminum or aluminum alloy antifrost surface |
| CN112871606A (en) * | 2021-01-08 | 2021-06-01 | 同曦集团有限公司 | Preparation method of super-hydrophobic antibacterial antiviral stainless steel based on electrochemical etching |
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Application publication date: 20150408 |