CN106319588A - Electrochemical deposition based method for preparing metal material surface super-hydrophobic film - Google Patents
Electrochemical deposition based method for preparing metal material surface super-hydrophobic film Download PDFInfo
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- CN106319588A CN106319588A CN201610928122.6A CN201610928122A CN106319588A CN 106319588 A CN106319588 A CN 106319588A CN 201610928122 A CN201610928122 A CN 201610928122A CN 106319588 A CN106319588 A CN 106319588A
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- electrochemical deposition
- metal material
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- material surface
- drying
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Classifications
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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
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/54—Electroplating of non-metallic surfaces
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
Abstract
The invention discloses an electrochemical deposition based method for preparing a metal material surface super-hydrophobic film. The method comprises the following steps of conductive substrate preparing, wherein a conductive film adheres to a cleaned-up hard substrate, and washing, blow-drying and drying are carried out; electroforming solution preparation; electrochemical deposition, wherein a prepared conductive substrate serves as a cathode, a phosphor copper plate serves as an anode, the power type is direct-current power supply, an electroforming solution is not stirred, the electrodeposition temperature and the current density are controlled, and a plating layer is obtained after electroforming is carried out for 5 min to 10 min; plating layer cleaning, wherein the plating layer obtained after electrochemical deposition is fully cleaned up with deionized water, blow-drying is carried out, and drying is achieved through a drying table; and low surface energy gas treatment, wherein the dried plating layer is subjected to low surface energy gas treatment, the coarse microstructure surface of the plating layer is covered with a low surface energy film, and therefore the plating layer can become the metal super-hydrophobic film. The method has the main beneficial effects that the process is simple, and the cost is low; no complex chemical solvent is needed for electroforming solution preparation; and environmental pollution is low.
Description
Technical field
The present invention relates to metal surface properties modification and metal micro-fabrication technology field, particularly relate to a kind of based on electrification
Learn the metal material surface based superhydrophobic thin films preparation method of deposition.
Background technology
Nature exists a lot of wonderful super-hydrophobic phenomenon, the such as lower limb of Folium Nelumbinis, ephydrid, the shell of insecticide, butterfly
The wing of butterfly.Potential value in the basic research of super hydrophobic surface and actual application causes concern greatly.
Especially for occupying the metal material of critical role in national life, super hydrophobic surface has great meaning
Justice.Due to metal material during life-time service, there will be erosion corrosion, the phenomenon such as surface is stained, thereby result in huge damage
Lose, and will play a great role in fields such as anticorrosion, Drag Reduction, automatically cleanings in the metal surface with super hydrophobic functional,
Cause the great interest of people.
Common metal super-hydrophobic structure is passed through solution soaking method, chemical etching method, template, self-assembly method, is separated
Method, plasma technique can successfully be prepared, but said method exists equipment complexity, cost intensive, severe reaction conditions
And Part Methods shortcoming disagreeableness to environment.
Have the following characteristics that preparation process is simple, easily controllable compared to the method for said method electrochemical deposition, react
Mild condition.Therefore electrochemical deposition method greatly reduces the cost of preparation, weakens reaction condition, for the most super-hydrophobic
Metallic film preparation provides probability.Application number 201210462398.1 discloses an a kind of step electro-deposition and prepares super-hydrophobic table
The method in face, utilization carries out electrochemical deposition containing chain alkyl siloxanes hydrolyzed solution and prepares coarse Silan-based Thin Films, reaches super
Hydrophobic state;Application No. 201310398379.1 discloses the preparation method of a kind of super-hydrophobic biomimetic surface on copper substrate, profit
The electroforming solution formed with cerium chloride, myristic acid and dehydrated alcohol deposits one layer of metallic film with low-surface-energy, this thin film
There is micro-nano classification double-decker;Application number 201410145166.2 discloses a kind of metal super-hydrophobic surface and preparation side thereof
Method, utilizes tradition nickel plating Watts bath deposition layer of metal nickel, then is heated in the ethanol solution containing silicon fluoride by coating, thus
Prepare metal super-hydrophobic thin film.
At present research utilize electrochemical deposition to prepare in the method for metal super-hydrophobic thin film generally to there is problems in that electricity
Casting liquid complicated component, adds other more chemical reagent, improves cost in electroforming solution;Portion of reagent is unfriendly to environment;
Part Methods has the post processing links such as heating, thus increases the complexity of operation.
Summary of the invention
It is super-hydrophobic that the technical problem that present invention mainly solves is to provide a kind of metal material surface based on electrochemical deposition
Method for manufacturing thin film, only by changing the simple of conventional electroforming solution composition and the reasonable adjusting of electric current density, then through too low table
Super-hydrophobic metallic film gas treatment can just be prepared in face, and method is simple, reduce cost, it is not necessary to use complicated chemical solvent
Carrying out electroforming solution preparation, environmental pollution is little.
For solving above-mentioned technical problem, the technical scheme that the present invention uses is: provide a kind of based on electrochemical deposition
Metal material surface based superhydrophobic thin films preparation method, comprise the following steps:
(1) preparation of conductive substrates: adhere to conductive film in the hard substrate cleaned up, clean, dry up, dry;
(2) preparation of electroforming solution: main salt is copper sulfate, conducting electrolyte is sulphuric acid, and solvent is deionized water, according to proportioning by three
Person is sufficiently mixed;
(3) electrochemical deposition: negative electrode is conductive substrates prepared by step (1), anode is phosphorus copper plate, and power supply type is unidirectional current
Source, electroforming solution does not stirs, and controls electrodeposition temperature and electric current density, obtains coating after electroforming;
(4) coating cleans: is fully cleaned up by the coating deionized water after electrochemical deposition, dries up, and dries platform and dries;
(5) low-surface-energy gas treatment: the coating after drying carries out low-surface-energy gas treatment, makes the micro structure that coating is coarse
Surface covers a layered low-surface energy thin film, so that coating becomes metal super-hydrophobic thin film.
In a preferred embodiment of the present invention, the hard substrate described in step (1) is microscope slide, described conductive thin
Film is conductive copper adhesive tape.
In a preferred embodiment of the present invention, concretely comprising the following steps of the preparation of described step (1) conductive substrates: glass will be carried
Sheet deionized water ultrasonic cleaning, after nitrogen dries up, dries on platform drying;Paste conductive copper adhesive tape on the microscope slide that will dry to make
For the conductive seed layer of electrochemical deposition, use detergent, acetone, ethanol that conductive substrates is carried out ultrasonic cleaning successively, clean
After completing, nitrogen dries up, dries platform heating, drying.
In a preferred embodiment of the present invention, the sulphuric acid in step (2) be mass fraction be 98% concentrated sulphuric acid.
In a preferred embodiment of the present invention, concretely comprising the following steps of the preparation of described step (2) electroforming solution: will
CuSO4·5H2O reagent obtains CuSO after being sufficiently stirred for dissolving in beaker4Solution;It is that 98% concentrated sulphuric acid slowly falls by mass fraction
Enter the CuSO prepared4In solution and constantly stir, after concentrated sulfuric acid solution is all poured in beaker, beaker is placed on magnetic force
It is sufficiently mixed on agitator, set aside for use.
In a preferred embodiment of the present invention, the electrodeposition temperature in step (3) is 20 ~ 30 DEG C.
In a preferred embodiment of the present invention, the electric current density in step (3) is 4 ~ 5A/dm2。
In a preferred embodiment of the present invention, the low-surface-energy gas described in step (5) is C4F8。
The invention has the beneficial effects as follows: the present invention is only close by changing the composition of conventional acid copper electroforming solution and electric current
Degree changes the coarse structure of coating surface, and the coating after electro-deposition surpasses by having obtained metal after the process of low-surface-energy gas
Hydrophobic film, contact angle test is more than 150 °;Main advantages of the present invention are that technique is simple, easily controllable, reaction condition is gentle,
Low cost, it is not necessary to using complicated chemical solvent to carry out electroforming solution preparation, environmental pollution is little, has a good application prospect.
Accompanying drawing explanation
For the technical scheme being illustrated more clearly that in the embodiment of the present invention, in embodiment being described below required for make
Accompanying drawing be briefly described, it should be apparent that, below describe in accompanying drawing be only some embodiments of the present invention, for
From the point of view of those of ordinary skill in the art, on the premise of not paying creative work, it is also possible to obtain other according to these accompanying drawings
Accompanying drawing, wherein:
Fig. 1 is the metal material surface based superhydrophobic thin films flow chart of electrochemical deposition;
Fig. 2 is the contact angle test result processed without low-surface-energy;
Fig. 3 is the contact angle test result processed through low-surface-energy;
Fig. 4 is to amplify 1000 times of deposited metal surface pattern SEM figures;
Fig. 5 is to amplify 10000 times of deposited metal surface pattern SEM figures;
Fig. 6 is that contact angle tests pictorial diagram.
Detailed description of the invention
Technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described enforcement
Example is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, this area is common
All other embodiments that technical staff is obtained under not making creative work premise, broadly fall into the model of present invention protection
Enclose.
As it is shown in figure 1, a kind of metal material surface based superhydrophobic thin films preparation method based on electrochemical deposition, including following
Step:
(1) preparation of conductive substrates: by microscope slide detergent, deionized water each ultrasonic cleaning 10min, after nitrogen dries up,
Dry and dry on platform, temperature 120 DEG C, time 30 ~ 60min are set;Conductive copper adhesive tape is pasted as electrification on the microscope slide that will dry
Learn the conductive seed layer of deposition, thickness 200 ~ 300 μm;Use successively detergent, acetone, ethanol conductive substrates is carried out ultrasonic clearly
Washing, three process each ultrasonic cleaning 10 minutes, every procedure re-uses deionized water and carries out ultrasonic cleaning after having cleaned
5min, has cleaned rear nitrogen and has dried up, dries platform heating, arrange temperature be 100 DEG C, the time be 60 ~ 90min;
(2) preparation of electroforming solution: weigh 250g CuSO4·5H2O reagent is put in beaker, adds deionized water and is stirred continuously also
Constant volume 1L, obtains the CuSO of 1mol/L after fully dissolving4Solution;Weighing 60 ~ 70g mass fraction is 98% dense H2SO4, slowly fall
Enter the CuSO prepared4In solution and constantly stir, after concentrated sulphuric acid is all poured in beaker, beaker is placed on magnetic force and stirs
Mix and be sufficiently mixed on device, rotating speed 500 ~ 800r/min, incorporation time 1 ~ 2h, after having mixed, set aside for use;
(3) electrochemical deposition: negative electrode is conductive substrates prepared by step (1), anode be phosphorous mass percent be the phosphorus of 0.02%
Copper coin, the power supply type used is DC source, and electrodeposition process is not stirred, and electrodeposition temperature is 20 ~ 30 DEG C, does not contains
The copper electroforming surface of additive and chloride ion can become coarse, and in the case of being somebody's turn to do, the current density value scope allowed is narrower, in reality
4A/dm is reached when electric current density in testing2During left and right, a little red powder occurs, when more than 5A/dm2There will be substantial amounts of
Red powder, electric current density controls at 4 ~ 5A/dm2;After calculating conductive area, cathode and anode is put in electroforming solution, it is ensured that cloudy,
Distance between anode is 10 ~ 15cm, switches on power, and regulation electric current makes electric current density maintain 4 ~ 5A/dm2, electroforming 5 ~ 10min
After obtain coating;
(4) coating cleans: the coating that step (3) obtains, and removes, its surface redness copper powder with the abundant ultrasonic cleaning of deionized water
Coating 10 ~ 15min, dries up with nitrogen after cleaning up, and places and dries platform 100 DEG C heating 60 ~ 90min, delays and be down to room temperature;
(5) low-surface-energy gas treatment: the coating after drying uses dry etching machine one layer of C of deposition4F8Thin film, thickness is about
30 ~ 50nm, the micro-structure surface making coating coarse covers one layer of low surface energy film containing fluorin radical, so that coating becomes
Metal super-hydrophobic thin film.
As in figure 2 it is shown, be the contact angle test result processed without low-surface-energy, static contact angle reaches
135.5°;As it is shown on figure 3, be the contact angle test result processed through low-surface-energy, static contact angle reaches 151.4 °;As
Shown in Fig. 4, being to amplify 1000 times of deposited metal surface pattern SEM figures, as can be seen from the figure coating surface occurs cylindric prominent
Rise;As it is shown in figure 5, be to amplify 10000 times of deposited metal surface pattern SEM figures, the as can be seen from the figure cylinder of coating surface
The diameter of shape projection is about 2 ~ 4 μm;As shown in Figure 6, be we by coating through C4F8Gas treatment, obtains super-hydrophobic state
Pictorial diagram, it can be seen that metallic film has good ultra-hydrophobicity.
The foregoing is only embodiments of the invention, not thereby limit the scope of the claims of the present invention, every utilize this
Equivalent structure or equivalence flow process that bright description is made convert, or are directly or indirectly used in other relevant technology neck
Territory, is the most in like manner included in the scope of patent protection of the present invention.
Claims (8)
1. a metal material surface based superhydrophobic thin films preparation method based on electrochemical deposition, it is characterised in that include following
Step:
(1) preparation of conductive substrates: adhere to conductive film in the hard substrate cleaned up, clean, dry up, dry;
(2) preparation of electroforming solution: main salt is copper sulfate, conducting electrolyte is sulphuric acid, and solvent is deionized water, according to proportioning by three
Person is sufficiently mixed;
(3) electrochemical deposition: negative electrode is conductive substrates prepared by step (1), anode is phosphorus copper plate, and power supply type is unidirectional current
Source, electroforming solution does not stirs, and controls electrodeposition temperature and electric current density, obtains coating after electroforming 5 ~ 10min;
(4) coating cleans: is fully cleaned up by the coating deionized water after electrochemical deposition, dries up, and dries platform and dries;
(5) low-surface-energy gas treatment: the coating after drying carries out low-surface-energy gas treatment, makes the micro structure that coating is coarse
Surface covers a layered low-surface energy thin film, so that coating becomes metal super-hydrophobic thin film.
Metal material surface based superhydrophobic thin films preparation method based on electrochemical deposition the most according to claim 1, it is special
Levying and be, the hard substrate described in step (1) is microscope slide, and described conductive film is conductive copper adhesive tape.
Metal material surface based superhydrophobic thin films preparation method based on electrochemical deposition the most according to claim 2, it is special
Levy and be, concretely comprising the following steps of the preparation of described step (1) conductive substrates: by microscope slide deionized water ultrasonic cleaning, nitrogen
After drying up, dry on platform drying;The conductive copper adhesive tape conductive seed layer as electrochemical deposition is pasted on the microscope slide that will dry,
Use detergent, acetone, ethanol that conductive substrates is carried out ultrasonic cleaning successively, cleaned rear nitrogen and dried up, dry platform and add baking the affected part after applying some drugs
Dry.
Metal material surface based superhydrophobic thin films preparation method based on electrochemical deposition the most according to claim 1, it is special
Levy and be, the sulphuric acid in step (2) be mass fraction be 98% concentrated sulphuric acid.
Metal material surface based superhydrophobic thin films preparation method based on electrochemical deposition the most according to claim 4, it is special
Levy and be, concretely comprising the following steps of the preparation of described step (2) electroforming solution: by CuSO4·5H2O reagent is sufficiently stirred in beaker
CuSO is obtained after dissolving4Solution;It is that 98% concentrated sulphuric acid is poured slowly into the CuSO prepared by mass fraction4In solution and constantly stir
Mix, after concentrated sulfuric acid solution is all poured in beaker, beaker is placed on magnetic stirring apparatus and is sufficiently mixed, set aside for use.
Metal material surface based superhydrophobic thin films preparation method based on electrochemical deposition the most according to claim 1, it is special
Levying and be, the electrodeposition temperature in step (3) is 20 ~ 30 DEG C.
Metal material surface based superhydrophobic thin films preparation method based on electrochemical deposition the most according to claim 1, it is special
Levying and be, the electric current density in step (3) is 4 ~ 5A/dm2。
Metal material surface based superhydrophobic thin films preparation method based on electrochemical deposition the most according to claim 1, it is special
Levying and be, the low-surface-energy gas described in step (5) is C4F8。
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106987872A (en) * | 2017-02-27 | 2017-07-28 | 东北大学 | A kind of preparation method of metal material surface super-hydrophobic film |
CN107191796A (en) * | 2017-06-15 | 2017-09-22 | 华南理工大学 | A kind of great power LED cooling lamp and a kind of preparation method of non-homogeneous wetability patterned surface |
CN110075570A (en) * | 2019-05-05 | 2019-08-02 | 四川农业大学 | One-step method prepares super hydrophilic/underwater superoleophobic oil-water separation mesh film and method |
CN112795963A (en) * | 2020-12-28 | 2021-05-14 | 青岛大学 | Method for simply and rapidly preparing ultramicro electrode array |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106987872A (en) * | 2017-02-27 | 2017-07-28 | 东北大学 | A kind of preparation method of metal material surface super-hydrophobic film |
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CN107191796A (en) * | 2017-06-15 | 2017-09-22 | 华南理工大学 | A kind of great power LED cooling lamp and a kind of preparation method of non-homogeneous wetability patterned surface |
CN107191796B (en) * | 2017-06-15 | 2023-09-19 | 华南理工大学 | High-power LED heat dissipation lamp and preparation method of non-uniform wettability patterned surface |
CN110075570A (en) * | 2019-05-05 | 2019-08-02 | 四川农业大学 | One-step method prepares super hydrophilic/underwater superoleophobic oil-water separation mesh film and method |
CN112795963A (en) * | 2020-12-28 | 2021-05-14 | 青岛大学 | Method for simply and rapidly preparing ultramicro electrode array |
CN112795963B (en) * | 2020-12-28 | 2022-05-27 | 青岛大学 | Method for simply and rapidly preparing ultramicro electrode array |
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