CN103952732B - Metal super-hydrophobic surface and preparation method thereof - Google Patents
Metal super-hydrophobic surface and preparation method thereof Download PDFInfo
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- CN103952732B CN103952732B CN201410145166.2A CN201410145166A CN103952732B CN 103952732 B CN103952732 B CN 103952732B CN 201410145166 A CN201410145166 A CN 201410145166A CN 103952732 B CN103952732 B CN 103952732B
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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 present invention relates to the method for obtaining super hydrophobic surface in different shape metallic substrate surface, the super-hydrophobic table for being obtained
Face not only has extraordinary super-hydrophobic and self-cleaning function, and with excellent wear-resisting and corrosion proof function.
Background technology
Super hydrophobic surface refers to the surface with water contact angle more than 150 °.Because super hydrophobic surface has special moistening special
Property so as to waterproof, the automatically cleaning of antifog, antifouling, anti-freeze, commercial plant and building, high voltage electric equipment automatically cleaning
With anti-flashover, biomedicine and biomimetic material application, pipeline waterproof and anticorrosive, fluid drag-reduction energy-conservation, power transmission pylon and
In the winter time many aspects such as Anti-ice-and-snow have potential application foreground to cable.When water droplet is less than 10 ° in the roll angle of super hydrophobic surface
When, the super hydrophobic surface also has self-cleaning function, the mistake that the super hydrophobic surface with self-cleaning function can be rolled in drop
Adsorb pollutant in journey and taken away surface, so as to reach the purpose of cleaning.
Under normal circumstances, proof gold metal surface is hydrophilic, and in metal base surface the surface with super hydrophobic functional is prepared
Cause the concern of vast researcher.At present, the method such as chemical etching, thermal spraying, vapour deposition and plating can be used in metal
Matrix surface prepares the surface with super hydrophobic functional.Application No. 201110152051.2 discloses a kind of galvanoplastic and prepares and surpasses
The method of hydrophobic cobalt coating, electroplate liquid used using choline chloride ionic liquid as solvent, with NiCl2Or NiCl2·6H2O is
Solute, under uniform temperature and electroplating voltage, plating is prepared for super-hydrophobic cobalt coating.The disclosure of Application No. 201210114736.2
A kind of magnesium alloy preparation method with super-hydrophobic coating, prepares the micro-nano coarse structure of binary first on magnesium alloy, then
Ultra-hydrophobicity is obtained Jing after the long linear alkanoic acid modification of low-surface-energy.Application No. 201210483659.8 discloses a kind of gold
Metal surface Super-hydrophobic aluminium surface preparation method, builds micro-nano compound structure, so in active metal base Magnetron Sputtered Al coating surface
Afterwards immersion a period of time in tetradecylic acid, obtain Super-hydrophobic aluminium surface.Regrettably, these publications are not directed to obtained super
The crocking resistance of hydrophobic surface.Past method for preparing super-hydrophobic surface, the super hydrophobic surface crocking resistance of preparation is weaker,
And the weak super hydrophobic surface of crocking resistance is difficult industrially have using value in actual.
The present invention, can be in conducting metals such as the aluminum of complicated shape, copper and rustless steels using simple plating and heat treatment method
Prepared by surface there is contact angle to be more than 155 °, and the super-hydrophobic automatic cleaning surface that roll angle is less than 10 °, the surface has resistance to well
Corrosion and rub resistance, the super hydrophobic surface and metal base for illustrating present invention preparation has very high adhesion.
The content of the invention
Patent of the present invention provides a kind of super hydrophobic surface and preparation method thereof, using simple plating and heat treatment method,
Can prepare in the metal surface of complicated shape and there is contact angle more than 155 °, super-hydrophobic automatic cleaning surface of the roll angle less than 10 °,
The surface also has excellent corrosion-resistant and crocking resistance.The method for preparing super-hydrophobic surface of the present invention is simple, is easy to industry
Change, it is with low cost, it is with a wide range of applications in electric utility, ship and automobile industry and building trade.
The purpose of the present invention is realized by following technical proposal：A kind of super hydrophobic surface and preparation method thereof, including under
Row step：
1）Surface of the work electroplates nickel coating：By surface of the work sand papering, clean and dry up, as negative electrode, with copper sheet
Used as anode, in basic bath, plating prepares nickel coating, the workpiece after being electroplated；
2）Heat treatment is modified：Workpiece after plating and the ethanol solution containing silicon fluoride are put in heating furnace, heat treatment
Clean afterwards and dry up, obtain metal super-hydrophobic surface.
Preferentially, step 1）Described in workpiece include rustless steel, copper, aluminium alloy or magnalium；The workpiece is conduction
Metal.
Preferentially, in step 1）Described in sand papering be by workpiece 400 mesh and 800 mesh sand paperings, it is described to clean
It is to be cleaned with pure water.
Preferentially, step 1）Described in basic electroplate liquid be Watts electroplate liquids, its component includes the g l of nickel sulfate 320-1,
The g l of Nickel dichloride hexahydrate 50-1With the g l of boric acid 45-1。
Preferentially, step 1) described in electroplate in electroplating temperature be 20-80 DEG C, electric current density be 0.1 ~ 0.5 A cm-2, electricity
The plating time is 30-120 min.
Preferentially, the silicon fluoride include 17 fluorine decyl triethoxysilanes, 17 fluorine decyl trimethoxy silanes, ten
Trifluoro octyl group trimethoxy silane or tridecafluoro-n-octyltriethoxysilane more than one.
Preferentially, silicon fluoride volumn concentration is 0.5%-10 % in the ethanol solution of the silicon fluoride.
Preferentially, the heat treatment temperature of the heat treatment is 100-200 DEG C, and heat treatment time is 10-120 min.
The present invention has the advantage that compared with prior art：
1st, preparation method of the invention can prepare super hydrophobic surface on the conductive metallic material surface of all complicated shapes.
2nd, the process equipment that preparation method of the present invention need not be complicated, preparation process is simple, with good using value.
3rd, present invention plating electroplating bath components used are simple, and market can sell, environmentally friendly.Electroplating technology is simply controllable,
Without corrosive substance, electroplating process is without discharge of steam.
4th, heat treatment method of the present invention is simple, and chemical reagent composition used is simple, with low cost.
5th, the present invention is smooth, uniform in super hydrophobic surface prepared by metal surface, and with superhydrophobic characteristic, contact angle exists
155 ~ 165 ° of scopes, roll angle is less than 10 °, and has excellent rub resistance and decay resistance.Prepared by the present invention super-hydrophobic
Surface can be applicable to various industrial part outer surfaces and metal pipe internal wall etc. to be needed automatically cleaning, corrosion-resistant, freezing and subtracts
The various occasions such as little water resistance.
Description of the drawings
Fig. 1 prepares super hydrophobic surface contact angle photo for embodiment 1；
Fig. 2 prepares super hydrophobic surface contact angle photo for embodiment 2；
Fig. 3 prepares super hydrophobic surface contact angle photo for embodiment 3；
Fig. 4 prepares super hydrophobic surface contact angle photo for embodiment 4；
Fig. 5 prepares super hydrophobic surface contact angle photo for embodiment 5；
Fig. 6 prepares super hydrophobic surface contact angle photo for embodiment 6.
Instantiation mode
Further detailed description is done to the present invention with reference to example, but the scope of protection of present invention is not limited to
This.
Embodiment 1
Latten(-tin) is rinsed with after 400 mesh and 800 mesh sand paperings with pure water, is dried up, as negative electrode, with same size
Latten(-tin) is containing 320 g l as anode-1Nickel sulfate, 50g l-1Nickel dichloride hexahydrate and 45g l-1The Watts of boric acid is electric
Electroplated in plating solution, electroplating current density is 0.5A cm-2, electroplating temperature is 50 DEG C, and electroplating time is plating after 60 min
After the completion of take out workpiece, cleaned with water, dry up.
To put together with 17 fluorine decyl triethoxysilane ethanol solution that electroplating parts and concentration of volume percent are 5%
In being placed in baking oven, in 100 DEG C of min of heat treatment 60, sample is taken out after heat treatment, test its hydrophobic, corrosion-resistant and rub resistance
Can, as a result as shown in table 1, its contact angle figure is as shown in Fig. 1.
Embodiment 2
Latten(-tin) is rinsed with after 400 mesh and 800 mesh sand paperings with pure water, is dried up, as negative electrode, with same size
Latten(-tin) is containing 320 g l as anode-1Nickel sulfate, 50g l-1Nickel dichloride hexahydrate and 45g l-1The Watts of boric acid is electric
Electroplated in plating solution, electroplating current density is 0.3A cm-2, electroplating temperature is 30 DEG C, and electroplating time is plating after 30 min
After the completion of take out workpiece, cleaned with water, dry up.
To put together with 17 fluorine decyl triethoxysilane ethanol solution that electroplating parts and concentration of volume percent are 1%
In being placed in baking oven, in 120 DEG C of min of heat treatment 30, sample is taken out after heat treatment, test its hydrophobic, corrosion-resistant and rub resistance
Can, as a result as shown in table 1, its contact angle figure is as shown in Fig. 2.
Embodiment 3
Aluminium flake is rinsed with after 400 mesh and 800 mesh sand paperings with pure water, is dried up, it is yellow with same size as negative electrode
Copper sheet is containing 320 g l as anode-1Nickel sulfate, 50g l-1Nickel dichloride hexahydrate and 45g l-1The Watts plating of boric acid
Electroplated in liquid, electroplating current density is 0.4 A cm-2, electroplating temperature is 50 DEG C, and electroplating time is after 40 min, to have electroplated
Into rear taking-up workpiece, cleaned with water, dried up.
To put together with 17 fluorine decyl triethoxysilane ethanol solution that electroplating parts and concentration of volume percent are 10%
In being placed in baking oven, in 150 DEG C of min of heat treatment 10, sample is taken out after heat treatment, test its hydrophobic, corrosion-resistant and rub resistance
Can, as a result as shown in table 1, its contact angle figure is as shown in Fig. 3.
Embodiment 4
Magnalium piece is rinsed with after 400 mesh and 800 mesh sand paperings with pure water, is dried up, as negative electrode, with same
Size latten(-tin) is containing 320 g l as anode-1Nickel sulfate, 50g l-1Nickel dichloride hexahydrate and 45g l-1Boric acid
Electroplated in Watts electroplate liquids, electroplating current density is 0.5A cm-2, electroplating temperature is 50 DEG C, and electroplating time is 30 min
Afterwards, workpiece is taken out after the completion of plating, is cleaned with water, dried up.
To put together with 17 fluorine decyl trimethoxy silane ethanol solution that electroplating parts and concentration of volume percent are 5%
In being placed in baking oven, in 100 DEG C of min of heat treatment 70, sample is taken out after heat treatment, test its hydrophobic, corrosion-resistant and rub resistance
Can, as a result as shown in table 1, its contact angle figure is as shown in Fig. 4.
Embodiment 5
Copper sheet is rinsed with after 400 mesh and 800 mesh sand paperings with pure water, is dried up, it is yellow with same size as negative electrode
Copper sheet is containing 320 g l as anode-1Nickel sulfate, 50g l-1Nickel dichloride hexahydrate and 45g l-1The Watts plating of boric acid
Electroplated in liquid, electroplating current density is 0.3 A cm-2, electroplating temperature is 50 DEG C, and electroplating time is after 50 min, to have electroplated
Into rear taking-up workpiece, cleaned with water, dried up.
To put together with ten trifluoro octyl group trimethoxy silane ethanol solution that electroplating parts and concentration of volume percent are 10%
In being placed in baking oven, in 120 DEG C of min of heat treatment 20, sample is taken out after heat treatment, test its hydrophobic, corrosion-resistant and rub resistance
Can, as a result as shown in table 1, its contact angle figure is as shown in Fig. 5.
Embodiment 6
Aluminium flake is rinsed with after 400 mesh and 800 mesh sand paperings with pure water, is dried up, it is yellow with same size as negative electrode
Copper sheet is containing 320 g l as anode-1Nickel sulfate, 50g l-1Nickel dichloride hexahydrate and 45g l-1The Watts plating of boric acid
Electroplated in liquid, electroplating current density is 0.5 A cm-2, electroplating temperature is 50 DEG C, and electroplating time is after 60 min, to have electroplated
Into rear taking-up workpiece, cleaned with water, dried up.
To put together with tridecafluoro-n-octyltriethoxysilane ethanol solution that electroplating parts and concentration of volume percent are 8%
In being placed in baking oven, in 110 DEG C of min of heat treatment 40, sample is taken out after heat treatment, test its hydrophobic, corrosion-resistant and rub resistance
Can, as a result as shown in table 1, 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 the patient maximum of super-hydrophobicity institute is still kept after 2 meters of 800 mesh Sandpapering of super hydrophobic surface
Pressure；Corrosion resistance refers to the electrochemical corrosion rate tested in 3.5wt%NaCl aqueous solutions）
| Example number | Contact angle/o | Roll angle/o | Rub resistance pressure/kPa | Rate of corrosion/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 adapted to large-scale production, can be in the various metallic substrate surface systems of complicated shape
Standby super-hydrophobic and corrosion-resistant surface.Meanwhile, by accompanying drawing 1-6 and table 1 it can be seen that the rub resistance of prepared super hydrophobic surface
Preferably there can be higher application.
The above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not to the present invention
Embodiment restriction.For those of ordinary skill in the field, can also make on the basis of the above description
The change or variation of other multi-forms.There is no need to be exhaustive to all of embodiment.It is all the present invention
Any modification, equivalent and improvement made within spirit and principle etc., should be included in the protection of the claims in the present invention
Within the scope of.
Claims (1)
1. a kind of preparation method of metal super-hydrophobic surface, it is characterised in that comprise the following steps：
1）Surface of the work electroplates nickel coating：By surface of the work sand papering, clean and dry up, as negative electrode, using copper sheet as
Anode, in basic bath, plating prepares nickel coating, the workpiece after being electroplated；
2）Heat treatment is modified：Workpiece after plating and the ethanol solution containing silicon fluoride are put in heating furnace, are washed after heat treatment
Only dry up, obtain metal super-hydrophobic surface；
Step 1）Described in workpiece include rustless steel, copper, aluminium alloy or magnalium；
Step 1）Described in basic electroplate liquid be Watts electroplate liquids, its component includes the g L of nickel sulfate 320-1, six chloride hydrates
The g L of nickel 50-1With the g L of boric acid 45-1；
Step 1) described in electroplate in electroplating temperature be 20-80 DEG C, electric current density be 0.1 ~ 0.5 A cm-2, electroplating time is 30-
120 min；
The silicon fluoride includes 17 fluorine decyl triethoxysilanes, 17 fluorine decyl trimethoxy silanes, ten trifluoro octyl groups three
Methoxy silane or tridecafluoro-n-octyltriethoxysilane more than one；
Silicon fluoride volumn concentration is 0.5%-10 % in the ethanol solution of the silicon fluoride；
The heat treatment temperature of the heat treatment is 100-200 DEG C, and heat treatment time is 10-120 min.
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| CN104746118B (en) * | 2015-04-20 | 2017-06-20 | 中国矿业大学 | A kind of method that nano combined Brush Plating of Fe bases prepares super-hydrophobic coating in steel base |
| CN106987872B (en) * | 2017-02-27 | 2019-05-21 | 东北大学 | A kind of preparation method of metal material surface super-hydrophobic film |
| CN107164746A (en) * | 2017-04-27 | 2017-09-15 | 武汉科技大学 | The preparation method on drag reduction copper surface |
| CN110685003B (en) * | 2018-07-05 | 2023-05-05 | 南京农业大学 | Preparation of super-hydrophobic Ni-P-Al on 45 steel surface 2 O 3 Electrochemical method of nano composite coating |
| CN109023439A (en) * | 2018-08-22 | 2018-12-18 | 中国科学院海洋研究所 | A kind of copper substrate superhydrophobic surface preparation method for characteristic of bouncing certainly with condensing droplet |
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| CN110714212B (en) * | 2019-10-12 | 2021-04-30 | 常州大学 | Method for preparing super-hydrophobic nickel film in aqueous solution system by nickel chloride one-step method |
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| CN111228858B (en) * | 2020-02-17 | 2021-06-08 | 大连理工大学 | Preparation method of super-hydrophobic super-oleophylic nickel-plated carbon fiber |
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| CN113005489B (en) * | 2021-02-20 | 2022-03-29 | 浙江泰仑电力集团有限责任公司 | Super-hydrophobic aluminum alloy surface preparation method |
| CN113318948B (en) * | 2021-05-21 | 2022-07-08 | 南京航空航天大学 | Preparation method of extremely wear-resistant functional texture capable of accurately regulating and controlling surface super-hydrophobic characteristics |
| CN115110128B (en) * | 2022-06-21 | 2023-10-27 | 华南理工大学 | Method for preparing high-stability nickel myristate super-hydrophobic coating on metal surface |
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