CN103588164A - Copper-silver micro-nano multi-stage structure super-hydrophobic surface and production method thereof - Google Patents
Copper-silver micro-nano multi-stage structure super-hydrophobic surface and production method thereof Download PDFInfo
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Abstract
The invention discloses a copper-silver micro-nano multi-stage structure super-hydrophobic surface formed on a metal base surface. The copper-silver micro-nano multi-stage structure super-hydrophobic surface comprises a copper-sliver micro-nano multi-stage structure and a hydrophobic film. The hydrophobic film is self-fitted on the surface of the copper-sliver micro-nano multi-stage structure. The copper-sliver micro-nano multi-stage structure comprises a plurality of copper-sliver micro-nano cones which longitudinally grow perpendicular to a metal base and which are tightly arranged. The hydrophobic film is self-composed of low surface energy material. Compared with common self-assemblies, the copper-silver micro-nano multi-stage structure super-hydrophobic surface has the advantages that sulfydryl of hydrophobe long-chain mercaptan and outermost silver ions of the copper-sliver micro-nano multi-stage structure form a coordinate bond having a large stable constant, and accordingly, the copper-silver micro-nano multi-stage structure super-hydrophobic surface is well stable, resistant to acid, alkali, organic solutions, high temperature and low temperature.
Description
Technical field
The invention belongs to surface of solids preparation micron or/and nanostructured field is specifically related to micro-nano multilevel hierarchy super hydrophobic surface of a kind of metallic copper silver and preparation method thereof.
Background technology
At occurring in nature, lotus leaf effect has caused more and more researchers' concern.The formation of lotus leaf effect, mainly by two because usually controlling, one is surface topography, another is surperficial chemical state.Y T Cheng(Nanotechnology, 17 (5), research 1359-1362) shows, lotus leaf surface has secondary microstructure, be diameter 5-9 μ m, the micrometer structure of height 1-20 μ m, on micrometer structure, distribution diameter is about the nanoscale fluff structures of 124nm, and shows the wax that contains low-surface-energy.Research shows, the contact angle of the lotus leaf that contains multilevel hierarchy is 142 °, and the contact angle that only contains the lotus leaf of micrometer structure is 126 °, and the surface contact angle that only contains wax is 74 °.Illustrate that microstructure and surface chemistry form have determined superhydrophobic characteristic jointly.Super hydrophobic surface refers to that contact angle is greater than 150 °, the surface that roll angle is less than 10 °.Because it has the features such as waterproof, antifog, automatically cleaning, significant in basic research and commercial Application.
The practical application of super hydrophobic surface need to solve two key issues: the firstth, there is corrosion resistance, and possess acidproof, alkaline-resisting and organic solvent resistance, the secondth, possess enough interface bond strengths.
Preparation about super hydrophobic surface at present has relevant report, by being oxidized, the rear super hydrophobic surface great majority that form are not acidproof and quality is soft very easily comes off by metal for some of them, and other macromolecule super hydrophobic surfaces mobility due to molecule under hot conditions easily causes losing efficacy; In addition, also have some super-hydrophobicity materials there is no enough interface bond strengths, after use a period of time, hydrophobic film easily comes off and lost efficacy.These defects, have restricted the practical application of superhydrophobic surface material greatly above.Therefore the superhydrophobic surface material of, inventing a kind of corrosion resistance and having a higher stability is very important.
Summary of the invention
The present invention is directed to existing super-hydrophobicity material above shortcomings, provide a kind of metallic copper silver micro-nano multilevel hierarchy super hydrophobic surface.Micro-nano multistage the tying of metallic copper silver has one deck hydrophobic layer, and the hydrophobic performance acting in conjunction of its design feature and material surface itself, has produced excellent hydrophobic performance; Its preparation method is step chemical deposition process, at material surface, form the micro-nano multilevel hierarchy of similar lotus leaf structure, recycle Chemical self-assembly principle at micro-nano multilevel hierarchy surface-assembled one deck organic sulfur alcohols hydrophobic substance, thereby reach the hydrophobicity of whole material.
Technical scheme of the present invention is as follows:
The micro-nano multilevel hierarchy super hydrophobic surface of a kind of metallic copper silver, be formed at metallic substrate surface, it comprises the metallic copper micro-nano multilevel hierarchy of silver and hydrophobic film, wherein, hydrophobic film is self-assembled to the micro-nano multilevel hierarchy of described metallic copper silver surface, the micro-nano multilevel hierarchy of described metallic copper silver comprises a plurality of perpendicular to metal base longitudinal growth and arrange the micro-nano cone of copper silver closely, and described hydrophobic film is formed by the self assembly of low-surface-energy material.
In order to obtain higher contact angle, the micro-nano multilevel hierarchy super hydrophobic surface of above metallic copper silver is following structure more preferably: the micro-nano multilevel hierarchy of described metallic copper silver comprises the secondary structure that the primary structure that consists of copper micron cone and silver nano-grain form, described silver nano-grain grows on copper micron cone, the height of described primary structure is 0.8～8 μ m, base diameter is 0.5～5 μ m, and described silver nano-grain diameter is 50～500nm.
Preferably, described hydrophobic film is the organic matter film of thickness 4～20nm.This organic matter film can cover the described metallic copper micro-nano multilevel hierarchy of silver completely and keep the complete shape and appearance of this structure simultaneously.
A preparation method for the micro-nano multilevel hierarchy super hydrophobic surface of metallic copper silver, comprises the following steps:
The first step, choose metal base, metal base is carried out to surface degreasing processing and pickling processes; Surface degreasing is processed and pickling processes is carried out according to conventional method, and does not limit the sequencing of processing, but preferably carries out successively surface degreasing processing and pickling processes;
Wherein, described metal base can be any suitable sheet metal, for example sheet material of copper, aluminium, nickel or irony;
Described surface degreasing is processed the treatment process that refers to the organic substance removals such as greasy dirt that metallic substrate surface is adhered to;
Described pickling processes refers to the operation that the oxide skin(coating) of metallic substrate surface is removed by acid solution;
Second step, metal base after the first step is processed is immersed to electroless copper with activating in activating solution; Wherein, electroless copper can be a kind of disclosed or commercial conventional chemical copper facing activating solution with activating solution, as PdCl
2or SnCl
2solution, its concentration basis in the industry general knowledge is chosen;
With activating solution PdCl for example for electroless copper
2or SnCl
2the effect that solution activates is that first the copper ion in next step chemical sinking effusion is reduced on these active Metal Palladium particles or tin particle, and the metallic copper nucleus that these are reduced itself becomes the Catalytic Layer of copper ion, make the reduction reaction of copper continue to carry out on these new copper nucleating surfaces;
The 3rd step, the metal base after activation is put into the copper facing chemical sinking effusion configuring and carried out chemical deposition, the constituent of copper facing chemical sinking effusion and concentration are: copper sulphate and/or copper chloride 0.02～0.2mol/L, nickelous sulfate and/or nickel chloride 0.001～0.01mol/L, complexing agent 0.02～0.2mol/L, boric acid 0.2～2mol/L, inferior sodium phosphate 0.2～2mol/L and crystallization adjusting agent 5～50ppm, adjust PH to 8～9 of this copper facing chemical sinking effusion, wherein pH value can be adjusted with alkaline reagent; The time of this copper facing chemical deposition is 6～60min, 20～80 ℃ of temperature;
Described complexing agent is selected from one or more in citrate, malic acid, edetate, acetate, ethylenediamine;
Described crystallization adjusting agent is selected from one or more in polyethylene glycol, polypropylene glycol, polytetramethylene glycol;
The 4th step, will be after the metal substrate washes clean of carrying out in copper facing chemical sinking effusion after chemical deposition dry, wash available common solvent, such as deionized water etc., then put into the silver-plated chemical sinking effusion configuring and carry out chemical deposition again, the constituent of silver-plated chemical sinking effusion and concentration are: silver nitrate and/or silver acetate 0.01～0.1mol/L, sodium thiosulfate 0.02～0.2mol/L, potassium metabisulfite 0.002～0.02mol/L, ammonium acetate 0.05～0.2mol/L; Wherein, the time of this silver-plated chemical deposition is 5～50min, and 20～50 ℃ of temperature, obtain metal-plated sheet;
The 5th step, the metal-plated sheet washes clean that the 4th step chemical deposition is obtained are dried afterwards, wash available common solvent, such as deionized water etc., then immerse in the water-repelling agent that concentration is 0.01～0.05mol/L, and its heating is carried out to self-assembling reaction, reaction temperature is 30～120 ℃, and the reaction time is 15～120min, then obtains the micro-nano multilevel hierarchy super hydrophobic surface of metallic copper silver of the present invention.Preferably, can in baking oven, to being soaked with the water-repelling agent solution of metal-plated sheet, heat and carry out self-assembling reaction; Wherein preferred, water-repelling agent is selected from the chain alkyl mercaptan of C8-C22 and one or more in fluorine-containing mercaptan, more preferably, water-repelling agent is selected from one or more in positive lauryl mercaptan, positive tetradecanylthioalcohol, positive 16 mercaptan, positive stearylmercaptan or positive 20 mercaptan.
Compared with prior art, beneficial effect of the present invention is as follows:
First, compare with general self assembly, the sulfydryl of the water-repelling agent long-chain mercaptan of the micro-nano multilevel hierarchy super hydrophobic surface of metallic copper silver of the present invention and the outermost silver ion of the copper micro-nano multilevel hierarchy of silver have formed the large coordinate bond of stability constant, make this surface there is good stability, make it have acidproof, alkaline-resisting, resistance to organic solution, high temperature resistant and lower temperature resistance;
The second, the hydrophobic performance of the micro-nano multilevel hierarchy super hydrophobic surface of metallic copper of the present invention silver is good, and the contact angle of itself and water droplet can reach 166 °, and roll angle is less than 10 °;
The 3rd, the preparation method of the micro-nano multilevel hierarchy super hydrophobic surface of metallic copper of the present invention silver is simple, need to be by any template, without complex apparatus, simultaneously to the shape of metal base, material without specific (special) requirements.
Certainly, implement arbitrary product of the present invention and might not need to reach above-described all advantages simultaneously.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the micro-nano multilevel hierarchy super hydrophobic surface of tool metallic copper silver of the embodiment of the present invention 1 preparation.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be appreciated that, these embodiment are only for the present invention is described, and are not intended to limit the scope of the invention.Technical staff makes according to the present invention in actual applications improvement and adjustment, still belong to protection scope of the present invention.
Embodiment 1
Adopt following methods to prepare the micro-nano multilevel hierarchy super hydrophobic surface of tool metallic copper silver:
(1) select copper sheet as metal base, oil removing, pickling processes are carried out in its surface;
(2) the good metal base of (1) step process is placed in to the PdCl that concentration is 0.15g/L
2in solution, carry out activation processing;
(3) metal base after the activation of (2) step is placed in to plating chemical sinking effusion and carries out chemical deposition, the constituent of this chemical sinking effusion and concentration are: copper sulphate 0.05 mol/L, nickelous sulfate 0.008 mol/L, trisodium citrate 0.08mol/L, boric acid 0.5mol/L, inferior sodium phosphate 0.4 mol/L, and polyethylene glycol 15ppm, with NaOH, adjust PH to 9, the temperature of chemical deposition is 50 ℃, and the chemical deposition time is 25min;
(4) the metal substrate deionized water washes clean that copper chemical deposition obtains in (3) step, dry afterwards, then be placed in silver-plated chemical sinking effusion and carry out chemical deposition, the constituent of this silver-plated chemical sinking effusion and concentration are: silver nitrate 0.01mol/L, sodium thiosulfate 0.02mol/L, potassium metabisulfite 0.002mol/L, ammonium acetate 0.04mol/L, chemical deposition temperature is 25 ℃, the chemical deposition time is 20min, obtains metal-plated sheet;
(5) the metal-plated sheet deionized water washes clean that chemical deposition obtains in (4) step, dry afterwards, then be placed in positive 16 thiol solutions of 0.02mol/L, be placed in 50 ℃ of baking ovens and react 30min, obtain the micro-nano multilevel hierarchy super hydrophobic surface of metallic copper silver.
The micro-nano multilevel hierarchy super hydrophobic surface of metallic copper silver of above-mentioned preparation is carried out to SEM observation, result is referring to Fig. 1, in figure, the micro-nano multilevel hierarchy super hydrophobic surface of visible this metallic copper silver comprises primary structure and secondary structure, wherein primary structure consists of copper micron cone, the height of copper micron cone is 0.8～8 μ m, and base diameter is 0.5～5 μ m, and secondary structure is silver nano-grain, it is upper that it grows in copper micron cone, and silver nano-grain diameter is 50～500nm.
With Germany, produce contact angle instrument, the micro-nano multilevel hierarchy super hydrophobic surface of metallic copper silver that 4 μ L water droplets obtain the present embodiment carries out hydrophobic experiment, and result shows that its contact angle is 166 °, and roll angle is less than 10 °.
That the micro-nano multilevel hierarchy super hydrophobic surface of metallic copper silver that the present embodiment is obtained carries out is acidproof, alkaline-resisting, the test of organic solvent-resistant and high-low temperature resistant, and result is as follows:
Under acid condition, 25 ℃, in the hydrochloric acid solution of PH1-PH6 (GB1763-79), contact angle and roll angle have no significant change;
Under alkali condition, 25 ℃, in the sodium hydroxide solution of PH8-PH13 (GB1763-79), contact angle and roll angle have no significant change;
Under organic solvent condition, in acetone, ethanolic solution, contact angle and roll angle have no significant change.
In the refrigerator-freezer of 0 ℃, place 24h., contact angle and roll angle have no significant change.
At the boiling water of 100 ℃, place 24h., contact angle and roll angle have no significant change.
Embodiment 2
According to the method for embodiment 1, change the concentration of positive 16 thiol solutions into 0.03mol/L, the micro-nano multilevel hierarchy super hydrophobic surface of the metallic copper for preparing silver, the contact angle of itself and water is 165 °, roll angle is less than 10 °.
Embodiment 3
Adopt following methods to prepare the micro-nano multilevel hierarchy super hydrophobic surface of metallic copper silver:
(1) select aluminium flake as metal base, oil removing, pickling processes are carried out in its surface;
(2) the good metal base of (1) step process is placed in to the PdCl of 0.35g/L
2in solution, carry out activation processing;
(3) metal base after the activation of (2) step is placed in to copper facing chemical sinking effusion and carries out chemical deposition, the constituent of this copper facing chemical sinking effusion and concentration are: copper chloride 0.02 mol/L, nickel chloride 0.01mol/L, malic acid 0.08mol/L, boric acid 0.2mol/L, inferior sodium phosphate 0.2mol/L, and polypropylene glycol 5ppm, with potassium hydroxide, adjust PH to 8, the temperature of chemical deposition is 20 ℃, and the chemical deposition time is 60min;
(4) the metal substrate deionized water washes clean that copper chemical deposition obtains in (3) step, dry afterwards, then be placed in silver-plated chemical sinking effusion and carry out chemical deposition, the constituent of this silver-plated chemical sinking effusion and concentration are: silver nitrate 0.02mol/L, sodium thiosulfate 0.04mol/L, potassium metabisulfite 0.01mol/L, ammonium acetate 0.1mol/L, chemical deposition temperature is 30 ℃, the chemical deposition time is 25min, obtains metal-plated sheet;
(5) the metal-plated sheet deionized water washes clean that chemical deposition obtains in (4) step, dry afterwards, then be placed in the positive stearylmercaptan solution of 0.01mol/L, be placed in 30 ℃ of baking ovens and react 120 min, then obtain the micro-nano multilevel hierarchy super hydrophobic surface of metallic copper silver.
The micro-nano multilevel hierarchy super hydrophobic surface of metallic copper silver of above-mentioned preparation is carried out to SEM observation, find that the micro-nano multilevel hierarchy super hydrophobic surface of this metallic copper silver comprises primary structure and secondary structure, wherein primary structure consists of copper micron cone, the height of copper micron cone is 0.8～8 μ m, base diameter is 0.5～5 μ m, secondary structure is silver nano-grain, and it is upper that it grows in copper micron cone, and silver nano-grain diameter is 50～500nm.With Germany, produce contact angle instrument, the micro-nano multilevel hierarchy super hydrophobic surface of metallic copper silver that 4 μ L water droplets are prepared the present embodiment carries out hydrophobic experiment, and result shows greatly 164 ° of its contact angles, and roll angle is less than 10 °.
Each raw material and method that the present invention is cited can realize the present invention, and the bound value of each raw material and technique, interval value can realize the present invention, at this, do not enumerate embodiment.
Claims (8)
1. the micro-nano multilevel hierarchy super hydrophobic surface of metallic copper silver, be formed at metallic substrate surface, it is characterized in that, it comprises the copper micro-nano multilevel hierarchy of silver and hydrophobic film, wherein, hydrophobic film is self-assembled to the micro-nano multilevel hierarchy of described copper silver surface, and the micro-nano multilevel hierarchy of described copper silver comprises a plurality of perpendicular to metal base longitudinal growth and arrange the micro-nano cone of copper silver closely.
2. the micro-nano multilevel hierarchy super hydrophobic surface of a kind of metallic copper silver according to claim 1, it is characterized in that, the micro-nano multilevel hierarchy of described metallic copper silver comprises the secondary structure that the primary structure that consists of copper micron cone and silver nano-grain form, described silver nano-grain grows on copper micron cone, the height of described primary structure is 0.8～8 μ m, base diameter is 0.5～5 μ m, and described silver nano-grain diameter is 50～500nm.
3. the micro-nano multilevel hierarchy super hydrophobic surface of a kind of metallic copper silver according to claim 1, is characterized in that, described hydrophobic film is the organic matter film of thickness 4～20nm.
4. the preparation method of the micro-nano multilevel hierarchy super hydrophobic surface of arbitrary described metallic copper silver in claim 1-3, is characterized in that, comprises the following steps:
The first step, choose metal base, metal base is carried out to surface degreasing processing and pickling processes;
Second step, metal base after the first step is processed is immersed to electroless copper with activating in activating solution;
The 3rd step, the metal base after activation is put into the copper facing chemical sinking effusion configuring and carried out chemical deposition, the constituent of described copper facing chemical sinking effusion and concentration are: copper sulphate and/or copper chloride 0.02～0.2mol/L, nickelous sulfate and/or nickel chloride 0.001～0.01mol/L, complexing agent 0.02～0.2mol/L, boric acid 0.2～2mol/L, inferior sodium phosphate 0.2～2mol/L and crystallization adjusting agent 5～50ppm, and adjust its PH to 8～9; The time of this chemical deposition is 6～60min, 20～80 ℃ of temperature;
The 4th step, will be after the metal substrate washes clean of carrying out in copper facing chemical sinking effusion after chemical deposition dry, then put into the silver-plated chemical sinking effusion configuring and carry out chemical deposition, the constituent of described silver-plated chemical sinking effusion and concentration are: silver nitrate and/or silver acetate 0.01～0.1mol/L, sodium thiosulfate 0.02～0.2mol/L, potassium metabisulfite 0.002～0.02mol/L, ammonium acetate 0.05～0.2mol/L; The time of this chemical deposition is 5～50min, and 20～50 ℃ of temperature, obtain metal-plated sheet;
The 5th step, the metal-plated sheet washes clean that chemical deposition in the 4th step is obtained are dried afterwards, then immerse in the water-repelling agent that concentration is 0.01～0.05mol/L, and its heating is carried out to self-assembling reaction, reaction temperature is 30～120 ℃, reaction time is 15～120min, then obtains the micro-nano multilevel hierarchy super hydrophobic surface of metallic copper silver.
5. the preparation method of the micro-nano multilevel hierarchy super hydrophobic surface of metallic copper silver according to claim 4, is characterized in that, described complexing agent is selected from one or more in citrate, malic acid, edetate, acetate, ethylenediamine.
6. the preparation method of the micro-nano multilevel hierarchy super hydrophobic surface of metallic copper silver according to claim 4, is characterized in that, described crystallization adjusting agent is selected from one or more in polyethylene glycol, polypropylene glycol, polytetramethylene glycol.
7. the preparation method of the micro-nano multilevel hierarchy super hydrophobic surface of metallic copper according to claim 4 silver, is characterized in that, described water-repelling agent is selected from the chain alkyl mercaptan of C8-C22 and one or more in fluorine-containing mercaptan.
8. the micro-nano multilevel hierarchy super hydrophobic surface of a kind of metallic copper silver according to claim 7, it is characterized in that, described water-repelling agent is selected from one or more in positive lauryl mercaptan, positive tetradecanylthioalcohol, positive 16 mercaptan, positive stearylmercaptan or positive 20 mercaptan.
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