CN103952732A - Metal super-hydrophobic surface and preparation method thereof - Google Patents
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Abstract
The invention relates to a metal super-hydrophobic surface and a preparation method thereof. The preparation method comprises following two steps: firstly, electroplating method is adopted, traditional Watts electroplate liquid is taken as a base electroplate liquid, conductive metal base materials such as stainless steel, copper, aluminium alloy, and magnesium aluminum alloy, are taken as a negative electrode, and copper sheets are taken as a positive electrode so as to prepare a nickel coating layer; and secondly, an obtained electroplated surface and an ethanol solution containing fluorosilane are delivered into a heating furnace for heat treatment, and an obtained sample is subjected to washing and blow drying so as to obtain the surface with super-hydrophobicity on metal workpieces. The preparation method of the metal super-hydrophobic surface is simple; cost is low; and the preparation method is convenient for industrialized application. Contact angle of the obtained metal super-hydrophobic surface is more than 155 DEG, and rolling angel is less than 10 DEG; the metal super-hydrophobic surface possesses excellent super hydrophobicity, self-cleaning performance, wear resistance, and corrosion resistance; the preparation method is suitable for obtaining the metal super-hydrophobic surfaces with super hydrophobicity, self-cleaning performance, wear resistance, and corrosion resistance on the surfaces of a plurality of metal base materials with complex shapes and large area.
Description
Technical field
The method that the present invention relates to obtain in different shapes metallic substrate surface super hydrophobic surface, the super hydrophobic surface obtaining not only has extraordinary super-hydrophobic and self-cleaning function, and has excellent wear-resisting and corrosion proof function.
Background technology
Super hydrophobic surface refers to the surface that is greater than 150 ° with water contact angle.Because super hydrophobic surface has special wetting property, make it at waterproof, antifog, antifouling, anti-freeze, full scale plant and the automatically cleaning of buildings, the automatically cleaning of high voltage electric equipment and anti-flashover, biomedicine and biomimetic material application, pipeline waterproof and anticorrosive, fluid drag-reduction is energy-conservation, power transmission pylon and cable in the winter time Anti-ice-and-snow etc. have potential application foreground aspect many.When water droplet is when the roll angle of super hydrophobic surface is less than 10 °, this super hydrophobic surface also has self-cleaning function, have the super hydrophobic surface of self-cleaning function can be in the process that drop rolls absorb polluted matter taken away surface, thereby reach clean object.
Generally, pure metal surface is wetting ability, and the surface in metal base surface preparation with super hydrophobic functional has caused numerous investigators' concern.At present, the method such as chemical etching, thermospray, vapour deposition and plating is used in the surface that metal base surface preparation has super hydrophobic functional.Application number is 201110152051.2 to disclose a kind of method that electrochemical plating are prepared super-hydrophobic cobalt coating, and electroplate liquid used is usingd choline chloride 60 ionic liquid as solvent, with NiCl
2or NiCl
26H
2o is solute, under certain temperature and electroplating voltage, electroplates and has prepared super-hydrophobic cobalt coating.Application number is 201210114736.2 to disclose a kind of magnesium alloy preparation method with super-hydrophobic coating, first on magnesium alloy, prepares the micro-nano coarse structure of binary, then obtains ultra-hydrophobicity after the long linear alkanoic acid of low surface energy is modified.Application number is 201210483659.8 to disclose a kind of metal surface superhydrophobic aluminium surface preparation method, at active metal base Magnetron Sputtered Al coating surface, builds micro-nano compound structure, then in TETRADECONIC ACID, soaks for some time, obtains super-hydrophobic aluminium surface.Regrettably, these publications do not relate to the crocking resistance of obtained super hydrophobic surface.The method for preparing super-hydrophobic surface in past, the super hydrophobic surface crocking resistance of preparation a little less than, and the weak super hydrophobic surface of crocking resistance is difficult to have using value in reality industrial.
The present invention adopts simple plating and heat treating method, can there is contact angle in the electrically-conducting metal surface preparations such as aluminium, copper and stainless steel of complicated shape and be greater than 155 °, the super-hydrophobic automatic cleaning surface that roll angle is less than 10 °, this surface has well corrosion-resistant and rub resistance, illustrates that super hydrophobic surface and metal base prepared by the present invention have very high bonding force.
Summary of the invention
Patent of the present invention provides a kind of super hydrophobic surface and preparation method thereof, adopt simple plating and heat treating method, can there is contact angle in the preparation of the metallic surface of complicated shape and be greater than 155 °, the super-hydrophobic automatic cleaning surface that roll angle is less than 10 °, this surface also has excellent corrosion-resistant and crocking resistance.Method for preparing super-hydrophobic surface of the present invention is simple, is convenient to industrialization, with low cost, in electric utility, boats and ships and automobile industry and building trade, is with a wide range of applications.
Object of the present invention realizes by following technical proposal: a kind of super hydrophobic surface and preparation method thereof, comprises the following steps:
1) workpiece surface electronickelling coating: by sand papering for workpiece surface, clean and dry up, as negative electrode, using copper sheet as anode, in basic plating solution, electroplate and prepare nickel coating, the workpiece after being electroplated;
2) thermal treatment modification: the workpiece after electroplating and the ethanolic soln that contains silicon fluoride are put into process furnace, and thermal treatment afterwash dries up, and obtains metal super-hydrophobic surface.
Preferentially, workpiece described in step 1) comprises stainless steel, copper, aluminium alloy or magnalium; Described workpiece is conducting metal.
Preferentially, in sand papering described in step 1), be by 400 orders and 800 order sand paperings for workpiece, described cleaning is to clean with pure water.
Preferentially, basic electroplate liquid described in step 1) is Watts electroplate liquid, and its component comprises single nickel salt 320 g l
-1, Nickel dichloride hexahydrate 50 g l
-1with boric acid 45 g l
-1.
Preferentially, step 1) in electroplating described in, electroplating temperature is 20-80 ℃, and current density is 0.1 ~ 0.5 A cm
-2, electroplating time is 30-120 min.
Preferentially, described silicon fluoride comprises more than one of 17 fluorine decyl triethoxyl silanes, 17 fluorine decyl Trimethoxy silanes, ten trifluoro octyl group Trimethoxy silanes or ten trifluoro octyltri-ethoxysilane.
Preferentially, in the ethanolic soln of described silicon fluoride, silicon fluoride volumn concentration is 0.5%-10 %.
Preferentially, described heat treated thermal treatment temp is 100-200 ℃, and heat treatment time is 10-120 min.
The present invention compared with prior art tool has the following advantages:
1, preparation method of the present invention can prepare super hydrophobic surface on the conductive metallic material surface of all complicated shapes.
2, preparation method of the present invention does not need complicated processing units, and preparation process is simple, has good using value.
3, to electroplate electroplating bath components used simple in the present invention, and market can be sold, environmentally friendly.Electroplating technology is simply controlled, and or not containing corrosives, electroplating process is not without discharge of steam.
4, heat treating method of the present invention is simple, and chemical reagent composition used is simple, with low cost.
5, the super hydrophobic surface that the present invention is prepared in metallic surface is smooth, even, has superhydrophobic characteristic, and contact angle is 155 ~ 165 ° of scopes, and roll angle is less than 10 °, and has excellent rub resistance and corrosion resistance nature.Super hydrophobic surface prepared by the present invention can be applicable to multiple industrial part outside surface and metal pipe internal wall etc. to be needed automatically cleaning, corrosion-resistant, freezing and reduces the various occasions such as water resistance.
Accompanying drawing explanation
Fig. 1 is that embodiment 1 prepares super hydrophobic surface contact angle photo;
Fig. 2 is that embodiment 2 prepares super hydrophobic surface contact angle photo;
Fig. 3 is that embodiment 3 prepares super hydrophobic surface contact angle photo;
Fig. 4 is that embodiment 4 prepares super hydrophobic surface contact angle photo;
Fig. 5 is that embodiment 5 prepares super hydrophobic surface contact angle photo;
Fig. 6 is that embodiment 6 prepares super hydrophobic surface contact angle photo.
specific examples mode
Below in conjunction with example, the present invention is done to further detailed description, but the scope of protection of present invention is not limited to this.
embodiment 1
Latten(-tin), with using purified rinse water after 400 orders and 800 order sand paperings, is dried up, as negative electrode, using same size latten(-tin) as anode, containing 320 g l
-1single nickel salt, 50g l
-1nickel dichloride hexahydrate and 45g l
-1in the Watts electroplate liquid of boric acid, electroplate, electroplating current density is 0.5A cm
-2, electroplating temperature is 50 ℃, after electroplating time is 60 min, has electroplated rear taking-up workpiece, water cleans, and dries up.
Together with the 17 fluorine decyl triethoxyl silane ethanolic solns that are 5% with concentration of volume percent by electroplating parts, be positioned in baking oven, at 100 ℃ of thermal treatment 60 min, after thermal treatment, take out sample, test its hydrophobic, corrosion-resistant and crocking resistance, result is as shown in table 1, and its contact angle figure is as shown in Fig. 1.
embodiment 2
Latten(-tin), with using purified rinse water after 400 orders and 800 order sand paperings, is dried up, as negative electrode, using same size latten(-tin) as anode, containing 320 g l
-1single nickel salt, 50g l
-1nickel dichloride hexahydrate and 45g l
-1in the Watts electroplate liquid of boric acid, electroplate, electroplating current density is 0.3A cm
-2, electroplating temperature is 30 ℃, after electroplating time is 30 min, has electroplated rear taking-up workpiece, water cleans, and dries up.
Together with the 17 fluorine decyl triethoxyl silane ethanolic solns that are 1% with concentration of volume percent by electroplating parts, be positioned in baking oven, at 120 ℃ of thermal treatment 30 min, after thermal treatment, take out sample, test its hydrophobic, corrosion-resistant and crocking resistance, result is as shown in table 1, and its contact angle figure is as shown in Fig. 2.
embodiment 3
Aluminium flake, with using purified rinse water after 400 orders and 800 order sand paperings, is dried up, as negative electrode, using same size latten(-tin) as anode, containing 320 g l
-1single nickel salt, 50g l
-1nickel dichloride hexahydrate and 45g l
-1in the Watts electroplate liquid of boric acid, electroplate, electroplating current density is 0.4 A cm
-2, electroplating temperature is 50 ℃, after electroplating time is 40 min, has electroplated rear taking-up workpiece, water cleans, and dries up.
Together with the 17 fluorine decyl triethoxyl silane ethanolic solns that are 10% with concentration of volume percent by electroplating parts, be positioned in baking oven, at 150 ℃ of thermal treatment 10 min, after thermal treatment, take out sample, test its hydrophobic, corrosion-resistant and crocking resistance, result is as shown in table 1, and its contact angle figure is as shown in Fig. 3.
embodiment 4
Magnalium sheet, with using purified rinse water after 400 orders and 800 order sand paperings, is dried up, as negative electrode, using same size latten(-tin) as anode, containing 320 g l
-1single nickel salt, 50g l
-1nickel dichloride hexahydrate and 45g l
-1in the Watts electroplate liquid of boric acid, electroplate, electroplating current density is 0.5A cm
-2, electroplating temperature is 50 ℃, after electroplating time is 30 min, has electroplated rear taking-up workpiece, water cleans, and dries up.
Together with the 17 fluorine decyl Trimethoxy silane ethanolic solns that are 5% with concentration of volume percent by electroplating parts, be positioned in baking oven, at 100 ℃ of thermal treatment 70 min, after thermal treatment, take out sample, test its hydrophobic, corrosion-resistant and crocking resistance, result is as shown in table 1, and its contact angle figure is as shown in Fig. 4.
embodiment 5
Copper sheet, with using purified rinse water after 400 orders and 800 order sand paperings, is dried up, as negative electrode, using same size latten(-tin) as anode, containing 320 g l
-1single nickel salt, 50g l
-1nickel dichloride hexahydrate and 45g l
-1in the Watts electroplate liquid of boric acid, electroplate, electroplating current density is 0.3 A cm
-2, electroplating temperature is 50 ℃, after electroplating time is 50 min, has electroplated rear taking-up workpiece, water cleans, and dries up.
Together with the ten trifluoro octyl group Trimethoxy silane ethanolic solns that are 10% with concentration of volume percent by electroplating parts, be positioned in baking oven, at 120 ℃ of thermal treatment 20 min, after thermal treatment, take out sample, test its hydrophobic, corrosion-resistant and crocking resistance, result is as shown in table 1, and its contact angle figure is as shown in Fig. 5.
embodiment 6
Aluminium flake, with using purified rinse water after 400 orders and 800 order sand paperings, is dried up, as negative electrode, using same size latten(-tin) as anode, containing 320 g l
-1single nickel salt, 50g l
-1nickel dichloride hexahydrate and 45g l
-1in the Watts electroplate liquid of boric acid, electroplate, electroplating current density is 0.5 A cm
-2, electroplating temperature is 50 ℃, after electroplating time is 60 min, has electroplated rear taking-up workpiece, water cleans, and dries up.
Together with the ten trifluoro octyltri-ethoxysilane ethanolic solns that are 8% with concentration of volume percent by electroplating parts, be positioned in baking oven, at 110 ℃ of thermal treatment 40 min, after thermal treatment, take out sample, test its hydrophobic, corrosion-resistant and crocking resistance, result is as shown in table 1, and its contact angle figure is as shown in Fig. 6.
Super hydrophobic surface performance prepared by the various examples of table 1
(rub resistance refers to that super hydrophobic surface still keeps the patient peak pressure of super-hydrophobicity with after 2 meters of 800 order Sandpaperings; Erosion resistance refers to the galvanic corrosion rate of testing in the 3.5wt%NaCl aqueous solution)
| Example number | Contact angle/ o | Roll angle/ o | Rub resistance pressure/kPa | Corrosion rate/mm a -1 |
| Embodiment 1 | 162 | 3 | 5.5 | 4.51×10 -3 |
| Embodiment 2 | 157 | 6 | 4.2 | 3.70×10 -3 |
| Embodiment 3 | 160 | 3 | 5.0 | 4.25×10 -3 |
| Embodiment 4 | 155 | 10 | 3.7 | 3.20×10 -3 |
| Embodiment 5 | 156 | 7 | 4.0 | 3.65×10 -3 |
| Embodiment 6 | 159 | 4 | 5.0 | 4.30×10 -3 |
The present invention program is simple to operation, is applicable to scale operation, can prepare super-hydrophobic and corrosion-resistant surface in the various metallic substrate surface of complicated shape.Meanwhile, by accompanying drawing 1-6 and table 1, can find out that the crocking resistance of prepared super hydrophobic surface is better, have stronger applicability.
The above embodiment of the present invention is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without also giving all embodiments.All any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in the protection domain of the claims in the present invention.
Claims (8)
1. a preparation method for metal super-hydrophobic surface, is characterized in that, comprises the following steps:
1) workpiece surface electronickelling coating: by sand papering for workpiece surface, clean and dry up, as negative electrode, using copper sheet as anode, in basic plating solution, electroplate and prepare nickel coating, the workpiece after being electroplated;
2) thermal treatment modification: the workpiece after electroplating and the ethanolic soln that contains silicon fluoride are put into process furnace, and thermal treatment afterwash dries up, and obtains metal super-hydrophobic surface.
2. according to the preparation method of metal super-hydrophobic surface described in right 1, it is characterized in that, workpiece described in step 1) comprises stainless steel, copper, aluminium alloy or magnalium; Described workpiece is conducting metal.
3. according to the preparation method of metal super-hydrophobic surface described in right 1, it is characterized in that, basic electroplate liquid described in step 1) is Watts electroplate liquid, and its component comprises single nickel salt 320 g l
-1, Nickel dichloride hexahydrate 50 g l
-1with boric acid 45 g l
-1.
4. according to the preparation method of metal super-hydrophobic surface described in right 1, it is characterized in that step 1) described in electroplate in electroplating temperature be 20-80 ℃, current density is 0.1 ~ 0.5 A cm
-2, electroplating time is 30-120 min.
5. according to the preparation method of metal super-hydrophobic surface described in right 1, it is characterized in that, described silicon fluoride comprises more than one of 17 fluorine decyl triethoxyl silanes, 17 fluorine decyl Trimethoxy silanes, ten trifluoro octyl group Trimethoxy silanes or ten trifluoro octyltri-ethoxysilane.
6. according to the preparation method of metal super-hydrophobic surface described in right 1, it is characterized in that, in the ethanolic soln of described silicon fluoride, silicon fluoride volumn concentration is 0.5%-10 %.
7. according to the preparation method of metal super-hydrophobic surface described in right 1, it is characterized in that, described heat treated thermal treatment temp is 100-200 ℃, and heat treatment time is 10-120 min.
8. the preparation method by the arbitrary described metal super-hydrophobic surface of claim 1-7 prepares a kind of metal super-hydrophobic surface.
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