CN106400079A - Preparation method of multiple super-hydrophobic composite film layers on aluminium alloy surface - Google Patents
Preparation method of multiple super-hydrophobic composite film layers on aluminium alloy surface Download PDFInfo
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- CN106400079A CN106400079A CN201611010176.0A CN201611010176A CN106400079A CN 106400079 A CN106400079 A CN 106400079A CN 201611010176 A CN201611010176 A CN 201611010176A CN 106400079 A CN106400079 A CN 106400079A
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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
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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
- C25D11/024—Anodisation under pulsed or modulated current or potential
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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
- C25D11/24—Chemical after-treatment
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Abstract
The invention discloses a preparation method of multiple super-hydrophobic composite film layers on an aluminium alloy surface. According to the method, firstly, micro-arc oxidation treatment is performed on a pretreated aluminium alloy sample, and a porous micro-arc oxidation ceramic layer with the micron-scale surface roughness is obtained; the obtained ceramic layer is arranged in a mixed solution to have a hydrothermal reaction, hydrotalcite films are generated on the surface and inner walls of holes of the ceramic layer, and composite film layers adopting micron/nano binary coarse structures are constructed; low-surface-energy modification is performed on the composite film layers with stearic acid, and the multiple super-hydrophobic composite film layers are formed on the aluminium alloy surface finally. With the preparation method, the problems that the construction cost of the micron/nano binary coarse structures is high and the environment is polluted can be solved, and a novel technical means for constructing the micron/nano binary coarse structures on the aluminium alloy surface is provided, so that the multiple super-hydrophobic composite film layers are prepared.
Description
Technical field
The present invention relates to technical field of aluminum alloy technology, more particularly, to a kind of system of aluminum alloy surface multilamellar super-hydrophobic composite film layer
Preparation Method.
Background technology
At present, the density of aluminium alloy is low, specific strength and specific stiffness are high, be widely used in Aero-Space, transportation and
The fields such as electrical equipment furniture, but because its anti-corrosion sex chromosome mosaicism is also subject to a definite limitation in application, so table need to be carried out to aluminium alloy
Face is processed to improve its surface property.Super hydrophobic material is widely used in daily life, commercial production and military affairs, super-hydrophobic material
Material can reduce frictional force, such as in shipping industry, if ship hull surface has super-hydrophobicity, can reduce boat trip
Resistance, thus improving its headway and reducing fuel consumption.In addition prepare superhydrophobic film in metal surface can carry
The resistance to corrosion on highly metallic material surface, if the metal framework of outer surface of building has a super-hydrophobicity, rainy day or
Under wet environment, water droplet would not rest on metal surface, also just reduces the corrosivity to metal surface, so super-hydrophobicity
Material possesses the prospect of being widely applied.
In prior art, the preparation method of based superhydrophobic thin films has a lot, but will consider two factors：One is that surface will have
Have micro-/receive binary coarse structure, two is that surface mass has low-surface-energy.Build micro-/receive binary coarse structure method general
There are etching method, such as chemical etching method and plasma etching method.But a kind of etching liquid generally corresponds to one kind or minority matrix, and
Prepare rough surface versatility in this way bad；In addition also useful template build micro-/receive binary coarse structure, but this
Method needs to make the template with specific microstructure, is then assigned specific microstructure by modes such as extruding, cast
Give target material, process is more complicated.
Content of the invention
It is an object of the invention to provide a kind of preparation method of aluminum alloy surface multilamellar super-hydrophobic composite film layer, using this system
Preparation Method can solve the problem that building micro-/binary coarse structure of receiving involves great expense, pollutes the problem of environment, provides a kind of new closing in aluminum
Gold surface build micro-/receive the technological means of binary coarse structure, thus preparing multilamellar super-hydrophobic composite film layer.
A kind of preparation method of aluminum alloy surface multilamellar super-hydrophobic composite film layer, described preparation method includes：
Step 1, first differential arc oxidation process is carried out to pretreated aluminum alloy specimen, obtaining surface roughness is micron
The porous arc differential oxide ceramic layer of level；
Step 2, obtained pottery be placed in mixed solution carry out hydro-thermal reaction, on the surface of described ceramic layer and
Generate hydrotalcite film at hole inwall, construct have micro-/receive the composite film of binary coarse structure；
Step 3, using stearic acid, low-surface-energy modification is carried out to described composite film, finally formed in aluminum alloy surface many
Layer super-hydrophobic composite film layer.
In described step 1：Described differential arc oxidation processes used electrolyte and includes：The sodium silicate of 5-20g/L, 1-
The potassium hydroxide of 10g/L and the glycerol of 1-10ml/L；And the temperature of described electrolyte is 20-25 DEG C；
It is 300-500V that described differential arc oxidation processes used DC pulse voltage；
The surface roughness of obtained porous arc differential oxide ceramic layer is 1-3 μm.
In described step 2：Described mixed solution be sulphuric acid slaine and anhydrous sodium sulfate according to material amount ratio for 1:5
It is formulated；The pH value of this mixed solution is 5-7, and the concentration of wherein said sulphuric acid slaine is 0.05-0.3mol/L；
The temperature of described hydro-thermal reaction is 50-100 DEG C, and the response time is 2-48h；
The surface roughness of obtained composite film is 500-900nm.
In described step 3：The stearic acid being adopted is to comprise the stearic ethanol solution of 0.01-0.1mol/L, and molten
Liquid temp is 20-25 DEG C；
The response time that described low-surface-energy is modified controls in 4-7h；Composite film after low-surface-energy moditied processing
150 ° of contact angle ＞.
As seen from the above technical solution provided by the invention, using above-mentioned preparation method can solve the problem that structure micro-/receive
Binary coarse structure involves great expense, pollutes the problem of environment, provides that a kind of new to build micro-/binary of receiving in aluminum alloy surface coarse
The technological means of structure, thus prepare multilamellar super-hydrophobic composite film layer.
Brief description
In order to be illustrated more clearly that the technical scheme of the embodiment of the present invention, below will be to required use in embodiment description
Accompanying drawing be briefly described it should be apparent that, drawings in the following description are only some embodiments of the present invention, for this
For the those of ordinary skill in field, on the premise of not paying creative work, other can also be obtained according to these accompanying drawings
Accompanying drawing.
Fig. 1 illustrates by the preparation method flow process of the embodiment of the present invention provided aluminum alloy surface multilamellar super-hydrophobic composite film layer
Figure.
Specific embodiment
With reference to the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Ground description is it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.Based on this
Inventive embodiment, the every other enforcement that those of ordinary skill in the art are obtained under the premise of not making creative work
Example, broadly falls into protection scope of the present invention.
Below in conjunction with accompanying drawing, the embodiment of the present invention is described in further detail, is illustrated in figure 1 the present invention and implements
The preparation method schematic flow sheet of the provided aluminum alloy surface multilamellar super-hydrophobic composite film layer of example, described preparation method includes：
Step 1, first differential arc oxidation process is carried out to pretreated aluminum alloy specimen, obtaining surface roughness is micron
The porous arc differential oxide ceramic layer of level；
In this step 1, described differential arc oxidation processes used electrolyte and includes：The sodium silicate of 5-20g/L, 1-10g/
The potassium hydroxide of L and the glycerol of 1-10ml/L；
And the temperature of described electrolyte is 20-25 DEG C；
It is 300-500V that described differential arc oxidation processes used DC pulse voltage；
The surface roughness of obtained porous arc differential oxide ceramic layer is 1-3 μm.
Step 2, obtained pottery be placed in mixed solution carry out hydro-thermal reaction, on the surface of described ceramic layer and
Generate hydrotalcite film at hole inwall, construct have micro-/receive the composite film of binary coarse structure；
In described step 2, described mixed solution is sulphuric acid slaine (as magnesium sulfate, zinc sulfate etc.) and anhydrous sodium sulfate
According to material amount than for 1:5 are formulated；The pH value of this mixed solution is 5-7, and the concentration of wherein said sulphuric acid slaine is
0.05-0.3mol/L；
The temperature of described hydro-thermal reaction is 50-100 DEG C, and the response time is 2-48h；
The surface roughness of obtained composite film is 500-900nm.
Step 3, using stearic acid, low-surface-energy modification is carried out to described composite film, finally formed in aluminum alloy surface many
Layer super-hydrophobic composite film layer.
In described step 3, the stearic acid being adopted is to comprise the stearic ethanol solution of 0.01-0.1mol/L, and molten
Liquid temp is 20-25 DEG C；
The response time that described low-surface-energy is modified controls in 4-7h；Composite film after low-surface-energy moditied processing
150 ° of contact angle ＞, shows ultra-hydrophobicity, and composite film is good with basal body binding force.
With specific example, above-mentioned preparation method is described in detail below：
Prepare arc differential oxide ceramic layer first, first aluminum alloy specimen is positioned in the NaOH alkali wash water of 50g/L, is heated to
60 DEG C, until taking out after the complete blackening of specimen surface；Then be positioned over after sample being cleaned in 20% nitric acid light-emitting solution until
Sample recovers alloy gloss itself；Repeat above-mentioned two steps until specimen surface puts into blackening immediately in alkali wash water；Again by aluminum
Alloy surface is through 200#, 600#, 1000#, 2000# sand papering, after polishing, ultrasonic with acetone, ethanol and deionization solution
Dry up standby after cleaning；The consisting of of micro-arc oxidation electrolyte：18g/L sodium silicate, 9g/L potassium hydroxide, 3ml/L glycerol；Micro-
Arc aoxidizes pulse power voltage：36 0V；The temperature control of electrolyte is for 20～25 DEG C；Arc differential oxide ceramic layer rough surface
Spend for 2.4 μm.Connected entering the aluminum alloy specimen processing by aluminium wire, one end is fixed on anode copper rod, has the one of sample
End submergence in the electrolytic solution, carries out differential arc oxidation process.After being disposed, sample taking-up is cleaned with ethanol solution and dry up again.
Then build compound hydrotalcite film, specifically first prepare mixed solution：Magnesium sulfate concentration be 0.05mol/L,
Anhydrous slufuric acid na concn is 0.3mol/L, and adjusting mixed solution pH value using sodium hydroxide solution is 6.5；Then by above-mentioned steps
Prepared sample is disposed vertically in mixed solution, and carries out closed processes；After reaction 24h at 70 DEG C, take out sample and use
Ethanol solution cleaning dries up again.
Finally carry out low-surface energy substance modification, specifically first prepare the stearic ethanol solution of 0.05mol/L, then will
The sample that second step obtains is disposed vertically in solution, takes out sample at room temperature and cleaned with ethanol solution again after reaction 5h
Dry, finally give aluminum alloy surface multilamellar super-hydrophobic composite film layer.
In sum, embodiment of the present invention methods described is by carrying out differential arc oxidation process and in the differential of the arc in aluminum alloy surface
Oxidation ceramic layer surface recombination hydrotalcite film, construct have micro-/receive the film layer of binary coarse structure, using stearic acid pair
Composite film carries out low-surface-energy modification, reduces its surface energy, constructs based superhydrophobic thin films in aluminum alloy surface.Due to differential of the arc oxygen
Changing ceramic layer with hydrotalcite film is all growth in situ, so with basal body binding force preferably, difficult for drop-off；And differential arc oxidation
Process low with compound the used material toxicity of hydrotalcite film, environment is not polluted, the cost of material being used
Cheaply, beneficial to large-scale industrial production.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art in the technical scope of present disclosure, the change or replacement that can readily occur in,
All should be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Enclose and be defined.
Claims (4)
1. a kind of preparation method of aluminum alloy surface multilamellar super-hydrophobic composite film layer is it is characterised in that described preparation method includes：
Step 1, first differential arc oxidation process is carried out to pretreated aluminum alloy specimen, it is micron-sized for obtaining surface roughness
Porous arc differential oxide ceramic layer；
Step 2, obtained pottery is placed in mixed solution carries out hydro-thermal reaction, in surface and the hole of described ceramic layer
Generate hydrotalcite film at inwall, construct have micro-/receive the composite film of binary coarse structure；
Step 3, using stearic acid, low-surface-energy modification is carried out to described composite film, finally form multilamellar in aluminum alloy surface and surpass
Hydrophobic composite membrane layer.
2. according to claim 1 the preparation method of aluminum alloy surface multilamellar super-hydrophobic composite film layer it is characterised in that in institute
State in step 1：
Described differential arc oxidation processes used electrolyte and includes：The sodium silicate of 5-20g/L, the potassium hydroxide of 1-10g/L and 1-
The glycerol of 10ml/L；And the temperature of described electrolyte is 20-25 DEG C；
It is 300-500V that described differential arc oxidation processes used DC pulse voltage；
The surface roughness of obtained porous arc differential oxide ceramic layer is 1-3 μm.
3. according to claim 1 the preparation method of aluminum alloy surface multilamellar super-hydrophobic composite film layer it is characterised in that in institute
State in step 2：
Described mixed solution be sulphuric acid slaine and anhydrous sodium sulfate according to material amount ratio for 1:5 are formulated；This mixing is molten
The pH value of liquid is 5-7, and the concentration of wherein said sulphuric acid slaine is 0.05-0.3mol/L；
The temperature of described hydro-thermal reaction is 50-100 DEG C, and the response time is 2-48h；
The surface roughness of obtained composite film is 500-900nm.
4. according to claim 1 the preparation method of aluminum alloy surface multilamellar super-hydrophobic composite film layer it is characterised in that in institute
State in step 3：
The stearic acid being adopted is to comprise the stearic ethanol solution of 0.01-0.1mol/L, and solution temperature is 20-25 DEG C；
The response time that described low-surface-energy is modified controls in 4-7h；The contact of the composite film after low-surface-energy moditied processing
150 ° of angle ＞.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107287640A (en) * | 2017-06-29 | 2017-10-24 | 北京石油化工学院 | A kind of preparation method of arc differential oxide ceramic layer nano surface graphite super-hydrophobic coat |
| CN108930042A (en) * | 2018-07-13 | 2018-12-04 | 西安理工大学 | A kind of preparation method of Mg alloy surface super-hydrophobic film |
| CN108977865A (en) * | 2018-07-19 | 2018-12-11 | 中国人民解放军92228部队 | A kind of preparation method of 5XXX aluminium and the high anti-corrosion single fine and close differential arc oxidation film layer of aluminum alloy surface |
| CN109338451A (en) * | 2018-12-03 | 2019-02-15 | 中国科学院海洋研究所 | A kind of aluminium base is anticorrosive, antimicrobial attachment super-hydrophobic film and preparation method thereof |
| CN109853022A (en) * | 2019-03-21 | 2019-06-07 | 福州大学 | A kind of preparation method of the anti-corrosion Mg-Al LDH/MAO composite coating of aluminium alloy |
| CN111945157A (en) * | 2020-07-30 | 2020-11-17 | 江苏中新瑞光学材料有限公司 | Preparation method of environment-friendly hydrophobic material |
| CN112226771A (en) * | 2020-09-28 | 2021-01-15 | 长安大学 | Super-hydrophobic composite film layer of titanium alloy and preparation method thereof |
| CN113046689A (en) * | 2021-03-05 | 2021-06-29 | 漆雷廷 | Super-hydrophobic corrosion-resistant aluminum alloy for biomedical treatment and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107287640A (en) * | 2017-06-29 | 2017-10-24 | 北京石油化工学院 | A kind of preparation method of arc differential oxide ceramic layer nano surface graphite super-hydrophobic coat |
| CN108930042A (en) * | 2018-07-13 | 2018-12-04 | 西安理工大学 | A kind of preparation method of Mg alloy surface super-hydrophobic film |
| CN108977865A (en) * | 2018-07-19 | 2018-12-11 | 中国人民解放军92228部队 | A kind of preparation method of 5XXX aluminium and the high anti-corrosion single fine and close differential arc oxidation film layer of aluminum alloy surface |
| CN108977865B (en) * | 2018-07-19 | 2021-01-05 | 中国人民解放军92228部队 | Preparation method of 5XXX aluminum and aluminum alloy surface high-corrosion-resistance single-compact micro-arc oxidation film layer |
| CN109338451A (en) * | 2018-12-03 | 2019-02-15 | 中国科学院海洋研究所 | A kind of aluminium base is anticorrosive, antimicrobial attachment super-hydrophobic film and preparation method thereof |
| CN109853022A (en) * | 2019-03-21 | 2019-06-07 | 福州大学 | A kind of preparation method of the anti-corrosion Mg-Al LDH/MAO composite coating of aluminium alloy |
| CN111945157A (en) * | 2020-07-30 | 2020-11-17 | 江苏中新瑞光学材料有限公司 | Preparation method of environment-friendly hydrophobic material |
| CN112226771A (en) * | 2020-09-28 | 2021-01-15 | 长安大学 | Super-hydrophobic composite film layer of titanium alloy and preparation method thereof |
| CN113046689A (en) * | 2021-03-05 | 2021-06-29 | 漆雷廷 | Super-hydrophobic corrosion-resistant aluminum alloy for biomedical treatment and preparation method thereof |
| CN114836724A (en) * | 2021-03-05 | 2022-08-02 | 漆雷廷 | Preparation method of super-hydrophobic corrosion-resistant aluminum alloy for biomedical use |
| CN113046689B (en) * | 2021-03-05 | 2022-12-06 | 苏州鱼得水电气科技有限公司 | Super-hydrophobic corrosion-resistant aluminum alloy for biomedical treatment and preparation method thereof |
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