CN101096771B - Process for producing aluminum surface super hydrophobic thin film - Google Patents
Process for producing aluminum surface super hydrophobic thin film Download PDFInfo
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- CN101096771B CN101096771B CN2007100286723A CN200710028672A CN101096771B CN 101096771 B CN101096771 B CN 101096771B CN 2007100286723 A CN2007100286723 A CN 2007100286723A CN 200710028672 A CN200710028672 A CN 200710028672A CN 101096771 B CN101096771 B CN 101096771B
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Abstract
The invention discloses a super dewatering film preparing method on the Al surface, which comprises the following steps: formulating the organic coating film with the electrolysis solution by selecting 0.5-5mmol/l water-soluble triazoxide organic compound salt and 0.25-5mol/l basic supporting electrolysis salt; regarding the roughening and cleaning aluminium surface as the working electrode and putting in the electrolysis solution; proceeding with the organic coating with tri electrode method (the coating temperature is 5-25Deg. C, the current density is 0.5-10A/m2, the coating time is 30s-50min); preparing a layer dense super dewatering film with super dewatering function characteristic and binding the organic film with aluminium basis surface tightly by the conjugated linkage. The invention can be used for the large-area super dewatering modifying property on the aluminum surface, in particular to the specially-shaped and complicated parts. The method is provided with the simple operation, the easy industrialization characteristic.
Description
Technical field
The present invention relates to aluminium surface treatment and modification technology field, be meant a kind of method that has super hydrophobic functional characteristic organic nano film in the aluminium surface preparation especially.
Background technology
Nano material is with its special physics, chemistry, electricity, magnetic and optical property, and obtained using widely.In the middle of the research of material surface engineering, utilizing the organic nano film material that material surface is carried out modification is one of main direction of research.
With regard to the material surface performance, wellability is the key character of solid surface, is all to play an important role in daily life or in industrial and agricultural production.Along with the maturation gradually of and hydrophilicity research hydrophobic to material and the continuous development of bionics techniques, people have the surperficial preparation aspect of lotus leaf automatically cleaning effect to having focused on of research.The contact angle of this surface with lotus leaf effect and water droplet is greater than 150 °; And have important feature such as waterproof, antifog, anti-oxidant, automatically cleaning; Therefore can be applied to snow defence, anti-pollution, anti-oxidant and prevent aspect such as conduction of current, people are referred to as super hydrophobic surface.
At present, super hydrophobic surface prepares the aspect and has obtained very big progress, and people have also had new understanding for the formation mechanism of super hydrophobic surface.Jiang Lei is published in AdvancedMaterials; 2002; 14 (24): the super-hydrophobicity that the article of 1857-1860 has disclosed natural lotus leaf surface is by its surface microstructure and chemical constitution decision, and thinks and can obtain surface super hydrophobic material through roughness that increases the hydrophobic material surface or the surface free energy that reduces the surface irregularity material.
The existing report of the preparation method of many super hydrophobic surfaces comprises that fusing-solidification method, plasma processing method, microwave plasma strengthen chemical Vapor deposition process, phase separation method, template extrusion process, ion plating, electrochemical method, sol-gel processing.Yet the preparation method of the super hydrophobic surface of existing report needs special plant and instrument, and complicated operation; Secondly, because the low surface free energy material only is mode and the matrix bond that relies on Van der Waals force or physical adsorption, be restricted the work-ing life of super hydrophobic surface.For this reason, people explore method for preparing super-hydrophobic surface easy, easy handling.For example, Qian Baitai utilizes the method for chemical etching and surface fluorination to prepare super hydrophobic surface (QianBT, Shen ZQ.Langmuir; 2005; 21 (20): 9007-9009), yet the process of surface fluorination is comparatively complicated and consuming time, need test button be immersed in the methanol solution of 1.0wt.% ten trifluoro octyltri-ethoxysilane of hydrolysis in advance; Take out after soaking 1h under the room temperature, in baking oven, heat 1h again under 130 ℃.The Chinese invention patent application number is that 200310119322.X discloses a kind of simple super-hydrophobicity method for manufacturing thin film; It is to be that feedstock production obtains with the polymkeric substance and the longer chain fatty acid that are prone to be adsorbed in solid surface and contain the amido reaction active groups; Therefore; Combining between super-hydrophobicity film and the solid surface only is to combine through Van der Waals force, and the mass-producing that is not suitable for industrial circle is used.
Summary of the invention
The objective of the invention is in order to overcome the deficiency of super hydrophobic surface technology of preparing; A kind of preparation method of aluminum surface super hydrophobic thin film is proposed; It not only can simplify the preparation process of super hydrophobic surface, and combines with covalent linkage between organic film and the aluminum substrate surface of preparation, in conjunction with tight.
The preparation method of this aluminum surface super hydrophobic thin film of the present invention, it mainly may further comprise the steps and processing condition:
Step 1: preparation electrolyte solution
Choose water-soluble triazine organic compound organic cpds salt 0.5～5mmol/l, alkalescence support electrolytic salt 0.25～5mol/l, be mixed with organic film plating and use electrolyte solution;
Step 2: make working electrode
The fine aluminium surface of before preparation super-hydrophobicity film, carrying out roughening and clean is as substrate, and this substrate is working electrode;
Step 3: the preparation of fine and close organic nano film
Place the electrolyte solution for preparing to carry out handling with the organic film plating of three electrode mode work the work utmost point of making, the organic film plating processing condition are: 5～25 ℃ of coating temperatures, current density are 0.5～10A/m
2, the plated film time is 30s～5min, prepares one deck in the metallic surface and has the super hydrophobic functional characteristic, fine and close organic nano film is based superhydrophobic thin films.
What electrolyte solution was used is the triazine organic compound organic cpds monomer of functional fluoropolymer group, and its concrete structure is following:
R in the structure
1Be one of following functional group:
Perfluor aryl class:
CF
3C
6H
4-，C
4F
9C
6H
4-，C
6F
13C
6H
4-，C
8F
17C
6H
4-，C
10F
21C
6H
4-；
The perfluoroalkyl class:
C
4F
9CH
2-，C
6F
13CH
2-，C
8F
17CH
2-，C
10F
21CH
2-，C
4F
9CH
2CH
2-，
C
6F
13CH
2CH
2-，C
8F
17CH
2CH
2-，C
8F
17CH
2CH
2CH
2-，C
8F
17CH
2CH
2CH
2CH
2-，
C
8F
17C
5H
10-，C
10F
21CH
2CH
2-，C
10F
21CH
2CH
2CH
2-；
The perfluor class:
C
4F
9CH
2＝CHCH
2-，C
6F
13CH
2＝CHCH
2-，C
8F
17CH
2＝CHCH
2-，
C
10F
21CH
2＝CHCH
2-；
Perfluor alcoholic extract hydroxyl group class:
C
4F
9CH
2CH(OH)CH
2-，C
6F
13CH
2CH(OH)CH
2-，C
8F
17CH
2CH(OH)CH
2-，
C
6F
13CH
2CH(OH)CH
2-，C
8F
17CH
2CH(OH)CH
2-，C
10F
21CH
2CH(OH)CH
2；
Perfluor ether class:
C
9F
17OC
6H
4-，C
6F
11OC
6H
4-；
R in the structure
2Be one of following functional group:
Perfluor aryl class:
CF
3C
6H
4-，C
4F
9C
6H
4-，C
6F
13C
6H
4-，C
8F
17C
6H
4-，C
10F
21C
6H
4-；
The perfluoroalkyl class:
C
4F
9CH
2-，C
6F
13CH
2-，C
8F
17CH
2-，C
10F
21CH
2-，C
4F
9CH
2CH
2-，
C
6F
13CH
2CH
2-，C
8F
17CH
2CH
2-，C
8F
17CH
2CH
2CH
2-，C
8F
17CH
2CH
2CH
2CH
2-，
C
8F
17C
5H
10-，C
10F
21CH
2CH
2-，C
10F
21CH
2CH
2CH
2-；
The perfluor class:
C
4F
9CH
2＝CHCH
2-，C
6F
13CH
2＝CHCH
2-，C
8F
17CH
2＝CHCH
2-，
C
10F
21CH
2＝CHCH
2-；
Perfluor alcoholic extract hydroxyl group class:
C
4F
9CH
2CH(OH)CH
2-，C
6F
13CH
2CH(OH)CH
2-，C
8F
17CH
2CH(OH)CH
2-，
C
6F
13CH
2CH(OH)CH
2-，C
8F
17CH
2CH(OH)CH
2-，C
10F
21CH
2CH(OH)CH
2；
Rare base class: CH
2=CHCH
2-, CH
2=CH (CH
2)
8-, CH
2=CH (CH
2)
9-;
M in the structure
1, M
2Be one of following atom: lithium, sodium, potassium, hydrogen.
Used alkalescence is supported wherein one or both mixture of the preferred yellow soda ash of electrolytic salt, Pottasium Hydroxide, sodium hydroxide, Sodium Nitrite, borons acid sodium, Lithium Hydroxide MonoHydrate in the electrolyte solution.
The present invention compared with prior art has following outstanding advantage and effect:
1, the super hydrophobic functional film for preparing among the present invention and the static contact angle of zero(ppm) water be greater than 150 °, and roll angle is less than 1 °, antifouling applicable to the aluminium surface, the use field of widening aluminum.
2, the super hydrophobic functional film of the present invention's preparation is to obtain through functional group contained in the triazine organic compound organic cpds and the growth of aluminium surface atom electrochemical reaction; Functional group combines with covalent linkage with the aluminium surface atom; Compare with film with by the prior art that combines with Van der Waals force between the modification solid surface; Combine tightr between film and the aluminium surface; And this organic film growth is fine and close, thereby can effectively protect aluminum for a long time, and a kind of anti-corrosion method that can be used as aluminium uses.
3, film coating method easy, be convenient to operation, can be used for modifying super hydrophobicity with big area aluminium surface, be specially adapted to the special or complicated component of shape, be easy to industriallization.
4, the plating bath that the present invention relates to does not contain the characteristics to environment and the healthy poisonous and harmful element of human body, and nontoxic non-environmental-pollution belongs to the environment-friendly type prescription.
Description of drawings
Fig. 1 drops in the lip-deep static contact angle photo of aluminium behind the organic film plating for the zero(ppm) water of the embodiment of the invention one.
Fig. 2 drops in the lip-deep static contact angle photo of aluminium behind the organic film plating for the zero(ppm) water of the embodiment of the invention two.
Fig. 3 drops in the lip-deep static contact angle photo of aluminium behind the organic film plating for the zero(ppm) water of the embodiment of the invention three.
Fig. 4 drops in the lip-deep static contact angle photo of aluminium behind the organic film plating for the zero(ppm) water of the embodiment of the invention four.
Fig. 5 drops in the lip-deep static contact angle photo of aluminium behind the organic film plating for the zero(ppm) water of the embodiment of the invention five.
Embodiment
Through embodiment and accompanying drawing the present invention is described further below.
Embodiment one:
The substrate metal that is used for organic film plating is that the trade mark is 1200 fine aluminium, is of a size of 50 * 30 * 0.4 (mm).
After carrying out the dislocation etching processing, the aluminium sample with micro-rough structure carries out organic film plating to be handled, and its concrete steps and processing condition are following:
Step 1: preparation electrolyte solution
Choose contain above-mentioned shown in water-soluble triazine organic compound organic cpds salt 0.5mmol/l, the 1mol/l borons acid sodium of functional group, all the other are zero(ppm) water, are mixed with organic film plating and use electrolyte solution;
Step 2: make working electrode
The fine aluminium surface of before preparation super-hydrophobicity film, carrying out roughening and clean is as substrate, and this substrate is working electrode;
Step 3: the preparation of fine and close organic nano film
Place the electrolyte solution for preparing to carry out handling with the organic film plating of three electrode mode work the working electrode of making, organic film plating adopts three electrode mode of operation, and wherein supporting electrode is the stainless steel thin slice, and reference electrode is SCE (SCE); Prepare one deck in the metallic surface and have the super hydrophobic functional characteristic, fine and close organic nano film is based superhydrophobic thin films.
The organic film plating condition is following:
The organic film plating temperature is 5 ℃, and current density is 0.5A/m
2, the plated film time is 30s.
The performance test of zero(ppm) water contact angle is carried out on aluminium surface to after handling.Test result shows that aluminium surface after treatment has the super hydrophobic functional characteristic, and it is 1 ° that the contact angle that zero(ppm) water drops in aluminium surface reaches 154.7 ± 2 ° of roll angles.Fig. 1 drops in the lip-deep static contact angle photo of aluminium behind the organic film plating for the zero(ppm) water of the embodiment of the invention one.
Embodiment two:
The substrate metal that is used for organic film plating is that the trade mark is 1235 fine aluminium, is of a size of 50 * 30 * 0.4 (mm).
After carrying out the dislocation etching processing, the aluminium sample with micro-rough structure carries out organic film plating to be handled, and its concrete steps and processing condition are following:
Step 1: preparation electrolyte solution
Choose contain above-mentioned shown in the water-soluble triazine organic compound organic cpds salt 1.2mmol/l of functional group, 1.5mol/l yellow soda ash, the 0.3mol/l Lithium Hydroxide MonoHydrate, all the other are zero(ppm) water, are mixed with organic film plating and use electrolyte solution;
Step 2: make working electrode
The fine aluminium surface of before preparation super-hydrophobicity film, carrying out roughening and clean is as substrate, and this substrate is working electrode;
Step 3: the preparation of fine and close organic nano film
Place the electrolyte solution for preparing to carry out handling with the organic film plating of three electrode mode work the working electrode of making, organic film plating adopts three electrode mode of operation, and wherein supporting electrode is the stainless steel thin slice, and reference electrode is SCE (SCE); Prepare one deck in the metallic surface and have the super hydrophobic functional characteristic, fine and close organic nano film is based superhydrophobic thin films.
The organic film plating condition is following:
The organic film plating temperature is 10 ℃, and current density is 5A/m
2, the plated film time is 1min.
The performance test of zero(ppm) water contact angle is carried out on aluminium surface to after handling.Test result shows that aluminium surface after treatment has the super hydrophobic functional characteristic, and the contact angle that zero(ppm) water drops in the aluminium surface reaches 156.4 ± 2 °, and roll angle is 0.8 °.Fig. 2 drops in the lip-deep static contact angle photo of aluminium behind the organic film plating for the zero(ppm) water of the embodiment of the invention two.
Embodiment three:
The substrate metal that is used for organic film plating is that the trade mark is 1350 fine aluminium, is of a size of 50 * 30 * 0.4 (mm).
After carrying out the dislocation etching processing, the aluminium sample with micro-rough structure carries out organic film plating to be handled, and its concrete steps and processing condition are following:
Step 1: preparation electrolyte solution
Choose contain above-mentioned shown in the water-soluble triazine organic compound organic cpds salt 2mmol/l of functional group, 2mol/l Pottasium Hydroxide, all the other are zero(ppm) water, are mixed with organic film plating and use electrolyte solution;
Step 2: make working electrode
The fine aluminium surface of before preparation super-hydrophobicity film, carrying out roughening and clean is as substrate, and this substrate is working electrode;
Step 3: the preparation of fine and close organic nano film
Place the electrolyte solution for preparing to carry out handling with the organic film plating of three electrode mode work the working electrode of making, organic film plating adopts three electrode mode of operation, and wherein supporting electrode is the stainless steel thin slice, and reference electrode is SCE (SCE); Prepare one deck in the metallic surface and have the super hydrophobic functional characteristic, fine and close organic nano film is based superhydrophobic thin films.
The organic film plating condition is following:
The organic film plating temperature is 15 ℃, and current density is 10A/m
2, the plated film time is 2min.
Aluminium surface patch to after handling carries out the performance test of zero(ppm) water contact angle.Test result shows that aluminium surface after treatment has the super hydrophobic functional characteristic, and the contact angle that zero(ppm) water drops in the aluminium surface reaches 164.9 ± 2 °, and roll angle is 0.6 °.Fig. 3 drops in the lip-deep static contact angle photo of aluminium behind the organic film plating for the zero(ppm) water of the embodiment of the invention three.
Embodiment four:
The substrate metal that is used for organic film plating is that the trade mark is 1100 fine aluminium, is of a size of 50 * 30 * 0.4 (mm).
After carrying out the dislocation etching processing, the aluminium sample with micro-rough structure carries out organic film plating to be handled, and its concrete steps and processing condition are following:
Step 1: preparation electrolyte solution
Choose contain above-mentioned shown in the water-soluble triazine organic compound organic cpds salt 3.5mmol/l of functional group, the 4.2mol/l Sodium Nitrite, all the other are zero(ppm) water, are mixed with organic film plating and use electrolyte solution;
Step 2: make working electrode
The fine aluminium surface of before preparation super-hydrophobicity film, carrying out roughening and clean is as substrate, and this substrate is working electrode;
Step 3: the preparation of fine and close organic nano film
Place the electrolyte solution for preparing to carry out handling with the organic film plating of three electrode mode work the working electrode of making, organic film plating adopts three electrode mode of operation, and wherein supporting electrode is the stainless steel thin slice, and reference electrode is SCE (SCE); Prepare one deck in the metallic surface and have the super hydrophobic functional characteristic, fine and close organic nano film is based superhydrophobic thin films.
The organic film plating condition is following:
The organic film plating temperature is 20 ℃, and current density is 2A/m
2, the plated film time is 3min.
The performance test of zero(ppm) water contact angle is carried out on aluminium surface to after handling.Test result shows that aluminium surface after treatment has the super hydrophobic functional characteristic, and the contact angle that zero(ppm) water drops in the aluminium surface reaches 168.1 ± 2 °, and roll angle is 0.5 °.Fig. 4 drops in the lip-deep static contact angle photo of aluminium behind the organic film plating for the zero(ppm) water of the embodiment of the invention four.
Embodiment five:
The substrate metal that is used for organic film plating is that the trade mark is 1145 fine aluminium, is of a size of 50 * 30 * 0.4 (mm).
After carrying out the dislocation etching processing, the aluminium sample with micro-rough structure carries out organic film plating to be handled, and its concrete steps and processing condition are following:
Step 1: preparation electrolyte solution
Choose contain above-mentioned shown in the water-soluble triazine organic compound organic cpds salt 4mmol/l of functional group, 1.4mol/l sodium hydroxide, all the other are zero(ppm) water, are mixed with organic film plating and use electrolyte solution;
Step 2: make working electrode
The fine aluminium surface of before preparation super-hydrophobicity film, carrying out roughening and clean is as substrate, and this substrate is working electrode;
Step 3: the preparation of fine and close organic nano film
Place the electrolyte solution for preparing to carry out handling with the organic film plating of three electrode mode work the working electrode of making, organic film plating adopts three electrode mode of operation, and wherein supporting electrode is the stainless steel thin slice, and reference electrode is SCE (SCE); Prepare one deck in the metallic surface and have the super hydrophobic functional characteristic, fine and close organic nano film is based superhydrophobic thin films.
The organic film plating condition is following:
The organic film plating temperature is 25 ℃, and current density is 1A/m
2, the plated film time is 5min.
The performance test of zero(ppm) water contact angle is carried out on aluminium surface to after handling.Test result shows that aluminium surface after treatment has the super hydrophobic functional characteristic, and the contact angle that zero(ppm) water drops in the aluminium surface reaches 158.3 ± 2 °, and roll angle is 0.8 °.Fig. 5 drops in the lip-deep static contact angle photo of aluminium behind the organic film plating for the zero(ppm) water of the embodiment of the invention five.
Claims (3)
1. the preparation method of an aluminum surface super hydrophobic thin film, it is characterized in that: its step and processing condition are following:
Step 1: preparation electrolyte solution
Choose water-soluble fluorine-containing triazine organic compound organic cpds salt 0.5-5mmol/L, alkalescence support electrolytic salt 0.25-5mol/L, be mixed with organic film plating and use electrolyte solution;
Step 2: make working electrode
The fine aluminium surface of before preparation super-hydrophobicity film, carrying out roughening and clean is as substrate, and this substrate is working electrode;
Step 3: the preparation of fine and close organic nano film
Place the electrolyte solution for preparing to carry out handling with the organic film plating of three electrode mode work working electrode, the organic film plating processing condition are: coating temperature is 5-25 ℃, and current density is 0.5-10A/m
2, the plated film time is 30s-5min, prepares one deck in the metallic surface and has the super hydrophobic functional characteristic, fine and close organic nano film is based superhydrophobic thin films.
2. the preparation method of a kind of aluminum surface super hydrophobic thin film according to claim 1 is characterized in that: the triazine organic compound organic cpds monomer of the functional fluoropolymer group that electrolyte solution is used, and its concrete structure is following:
R in the structure
1Be one of following functional group:
C
4F
9C
6H
4-，C
8F
17CH
2CH
2-，C
6F
13CH＝CHCH
2-，C
9F
17OC
6H
4-，C
8F
17CH
2CH(OH)CH
2-；
R in the structure
2Be one of following functional group:
C
4F
9CH＝CHCH
2-，C
6F
13CH
2-，C
8F
17C
6H
4-，CH
2＝CHCH
2-，C
8F
17CH
2CH(OH)CH
2-；
M in the structure
1, M
2Be one of following atom: lithium, sodium, potassium, hydrogen.
3. the preparation method of a kind of aluminum surface super hydrophobic thin film according to claim 2 is characterized in that: described triazine organic compound organic cpds monomer supports electrolytic salt that following concrete matching relationship is arranged with alkalescence:
1. R in the triazine organic compound organic cpds monomer structure that ought select for use
1Be C
4F
9C
6H
4-, R
2Be C
4F
9CH=CHCH
2In-time, the alkalescence that is complementary with it supports that electrolytic salt is a borons acid sodium;
2. R in the triazine organic compound organic cpds monomer structure that ought select for use
1Be C
8F
17CH
2CH (OH) CH
2-, R
2Be C
6F
13CH
2In-time, the alkalescence that is complementary with it supports that electrolytic salt is the mixture of Lithium Hydroxide MonoHydrate and yellow soda ash;
3. R in the triazine organic compound organic cpds monomer structure that ought select for use
1Be C
9F
17OC
6H
4-, R
2Be C
8F
17C
6H
4In-time, the alkalescence that is complementary with it supports that electrolytic salt is a Lithium Hydroxide MonoHydrate;
4. R in the triazine organic compound organic cpds monomer structure that ought select for use
1Be C
8F
17CH
2CH
2-, R
2Be CH
2=CHCH
2In-time, the alkalescence that is complementary with it supports that electrolytic salt is a Sodium Nitrite;
5. R in the triazine organic compound organic cpds monomer structure that ought select for use
1Be C
6F
13CH=CHCH
2-, R
2Be C
8F
17CH
2CH (OH) CH
2In-time, the alkalescence that is complementary with it supports that electrolytic salt is a sodium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100286723A CN101096771B (en) | 2007-06-19 | 2007-06-19 | Process for producing aluminum surface super hydrophobic thin film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100286723A CN101096771B (en) | 2007-06-19 | 2007-06-19 | Process for producing aluminum surface super hydrophobic thin film |
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| Publication Number | Publication Date |
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| CN101096771B true CN101096771B (en) | 2012-08-08 |
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| CN102953105B (en) * | 2012-11-16 | 2015-01-14 | 浙江大学 | Method for preparing superhydrophobic surface through one-step electro-deposition way |
| CN104005066A (en) * | 2014-05-16 | 2014-08-27 | 华南理工大学 | Magnesium alloy surface super hydrophobic membrane layer and preparation method and application thereof |
| CN104630775B (en) * | 2015-02-15 | 2017-06-09 | 东南大学 | A kind of large-scale preparation method of heat exchanger aluminium foil fins set super hydrophobic surface |
-
2007
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Non-Patent Citations (5)
| Title |
|---|
| Baitai Qian等.Fabrication of superhydrophobic surfaces by dislocation-selective chemical etching on aluminum, copper, and zinc substrates.《Langmuir》.2005,第21卷(第20期),9007-9009. * |
| Fang Wang等."Electrochemical Polymerization of6-(N-Allyl-1,1,2,2-tetrahydroperfluorodecyl)amino-1,3,5-triazine-2,4-dithiol Monosodium on Aluminum".Polymer Journal第38卷 第5期.2006,第38卷(第5期),484-489. |
| Fang Wang等."Electrochemical Polymerization of6-(N-Allyl-1,1,2,2-tetrahydroperfluorodecyl)amino-1,3,5-triazine-2,4-dithiol Monosodium on Aluminum".Polymer Journal第38卷 第5期.2006,第38卷(第5期),484-489. * |
| JP特开平11-140626A 1999.05.25 |
| JP特开平11-291259A 1999.10.26 |
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