CN102492945B - Preparation method of ice coating prevention surface of bionic micro-nano composite structure - Google Patents

Preparation method of ice coating prevention surface of bionic micro-nano composite structure Download PDF

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CN102492945B
CN102492945B CN 201110407972 CN201110407972A CN102492945B CN 102492945 B CN102492945 B CN 102492945B CN 201110407972 CN201110407972 CN 201110407972 CN 201110407972 A CN201110407972 A CN 201110407972A CN 102492945 B CN102492945 B CN 102492945B
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surface
icing
anti
structure
surperficial
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CN 201110407972
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CN102492945A (en
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郑咏梅
郭鹏
江雷
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北京航空航天大学
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Abstract

The invention discloses an ice coating prevention surface of a bionic micro-nano composite structure and a preparation method thereof, and belongs to the technical fields of chemistry and materials. The preparation method comprises the steps of: processing a surface micro structure on the surface of a substrate, planting a nano structure on the surface micro structure and finishing the surface to obtain the ice coating prevention surface. The ice coating prevention surface has a micro-nano composite structure, thus the surface roughness of the material is greatly increased, the contact area between liquid drops and the surface of the substrate is reduced, and the surface of the substrate not only has hydrophobicity, but also has lower adhesion property; under the condition of -10 DEG C even -15 DEG C, the surface has hydrophobic and anti-icing effects, and the icing time is larger than 7200 seconds; and the ice coating prevention surface can be formed on multiple materials, thus the limit to low-temperature icing prevention of the materials is greatly widened.

Description

The preparation method on the anti-icing surface of a kind of bionical micro-nano compound structure

Technical field

The invention belongs to chemistry, material technology field, relate to anti-icing surface of a kind of bionical micro-nano compound structure and preparation method thereof.

Background technology

The icing phenomenon is very common, and facilities such as outdoor machinery, building, aircraft, steamer, cable, electric tower cover the phenomenon of ice sheet, and cause the equipment cisco unity malfunction even cause great disaster, be a global problem.The southern freezing disaster of China's winter in 2008, because successive snowfall and sleet cause the ice sheet accumulation, crush electric tower, transmission line, cable, communications tower have been interrupted electric power and communication; Simultaneously, local-style dwelling houses, land communications and aerial operation are all had a strong impact on, and have caused the loss of loss of life and personal injury and tremendous economic.In ice and snow disaster prone areas, set up particular study mechanism as Canadian and the U.S. and carried out special project research at anti-icing disaster, yet de-icing method in the past is confined to remove ice by methods such as mechanical deicing, sprinkling deicing agent, heating behind the icing more, these not environmental protection of de-icing method, and need special equipment more and caused the waste of resource, the energy.In recent years, some documents and patent are mentioned to the purpose that methods such as material surface coating, surface modification realize preventing that material surface from freezing.As, patent CN101358106 discloses a kind of anti-icing nano composite paint that comprises that organic fluorine silicon compound high-molecular material, nano material, solidifying agent, solvent, filler prepare in proportion, the anti-icing paint that is applied to transmitting line of this method preparation needs multiple complicated organism, and the multiple solvent toxicity that this method adopts is big, high volatility has the potential security threat to environment and workmen; Patent CN101705488A discloses a kind of preparation method who prepares super-hydrophobic low tackyness icing-resistant copper surface, and this method makes the copper surface possess coarse structure by etch earlier, and hydrophobic modification makes the super-hydrophobic ice-covering-proof surface then.Though this method at-5 ℃, decreases than untreatment surface icing layer thickness under 10 minutes conditions, still can not prevent preferably adhering to of ice sheet.

Summary of the invention

The present invention relates to a kind of brand-new anti-icing surface design method, purpose is to overcome the realistic situation of existing anti-icing poor effect, mechanical workout that utilization is simple and easy to realize and hydrothermal synthesis method are realized micron and nanometer composite structure, reach-10 ℃ of following material surface drops and surpass 1.5 hours non-icing anti-icing effects.

The present invention is subjected to butterfly in thick fog and the inspiration that still can fly in the rain, furthers investigate its structure, and imitated this structure is also used at low temperatures and got.Butterfly's wing makes it possess the super-hydrophobic ability of unidirectional drive because of possessing helical teeth shape scale structure and the scale surface has finer nanostructure, does not also get wet and drips even be in the situation of high humidity, keeps body quality not increase.Use for reference this micro-nano compound structure, the present invention prepares the micron-scale unsymmetrical structure on common base material, plant nanostructure on this structure, as nano wire, nanometer rod, nanocone etc.; Three one step process by finishing reduction material surface energy prepare the anti-icing surface that normal temperature is super-hydrophobic, low temperature is prevented the micro-nano compound structure of icing again.

The preparation method on the anti-icing surface of bionical micro-nano compound structure provided by the invention comprises the steps:

The first step is at substrate surface finished surface micrometer structure; Mechanical processing method, molding casting, laser ablation method, heating stamped method, photolithography, gas phase directional etching method, laser ablation method, directional etching method or moulding method etc. are adopted in the processing of surface micrometer structure.

Second step, on surperficial micrometer structure, plant nanostructure, concrete steps are:

(1) preparation seed-solution: get Zinc diacetate dihydrate, Monoethanolamine MEA BASF and ethylene glycol monomethyl ether, mix and firmly stirring, obtain the not seed-solution of molten material of transparent nothing, the volumetric molar concentration of Zinc diacetate dihydrate is 0.05 mole every liter in the seed-solution, the concentration of Monoethanolamine MEA BASF is 0.05 mole every liter, and solvent is an ethylene glycol monomethyl ether;

(2) preparation growth media: take by weighing zinc nitrate hexahydrate and hexamethylenetetramine, measure deionized water, mix and firmly stirring, make growth media, the volumetric molar concentration of zinc nitrate hexahydrate is every liter of 0.25 mmole in the growth media, the volumetric molar concentration of hexamethylenetetramine is every liter of 0.25 mmole, and solvent is a water;

(3) substrate surface with surperficial micrometer structure is cleaned;

(4) behind the substrate naturally cooling after cleaning, dip in the seed-solution of getting preparation in (1) step with substrate, make seed-solution form one deck liquid film at substrate surface, sole keeps flat in the retort furnace, 350~400 ℃ of sintering 5 minutes;

(5) substrate behind the sintering is taken out from retort furnace, put into the polytetrafluoroethylliner liner of high-temperature high-pressure reaction kettle behind the naturally cooling, need to guarantee to have the surface of surperficial micrometer structure downward, and the surface of surperficial micrometer structure can not contact with wall of inner container; In reactor, pour the growth media of preparation in (2) step into, assemble reactor, put into baking oven, it is 85 ℃ that temperature of reaction is set, and the reaction times is 15 hours, reaction finishes, take out reactor, treat to take out substrate behind its naturally cooling, rinse well with deionized water on the surface, dry stand-byly, promptly on surperficial micrometer structure, plant nanostructure.

In the 3rd step, finishing obtains anti-icing surface; It is fluorine cpd that modifier is adopted in finishing, modifying method is a vacuum vapour deposition, is specially: after will having the substrate cleaning of surperficial micrometer structure and nanostructure, put into vacuum vessel, drip 2~3 modifiers at substrate surface, be evacuated in the vacuum vessel-below the 0.1Mpa; Vacuum vessel is put into baking oven, keep 90 ℃ of reactions 3 hours, reaction finishes and has just gone out the anti-icing surface of bionical micro-nano compound structure in substrate surface preparation.

Described bionical micro-nano compound structure has surperficial micrometer structure and nanostructure on the anti-icing surface, become the anti-icing surface of micro-nano compound, wherein surperficial micrometer structure is bar shaped helical teeth, matrix helical teeth or conical insert, nanostructure is nano wire, nanotube, nanometer rod or nanometer pyramid, and described nanostructure is planted on the surperficial micrometer structure.

The invention has the advantages that:

1, the anti-icing surface of bionical micro-nano compound structure provided by the invention has micron-nanometer compound structure, increased the material surface roughness greatly, reduced the contact area of drop and substrate surface, made substrate surface not only possess ultra-hydrophobicity and have lower adhesivity;

2, the anti-icing surface of bionical micro-nano compound structure provided by the invention, under-10 ℃ even-15 ℃ of conditions, the surface possesses hydrophobic anti-icing effect, and the time of freezing was greater than 7200 seconds;

3, the anti-icing surface of bionical micro-nano compound structure provided by the invention can be realized on multiple material, has widened material is dredged ice to low temperature restriction greatly;

4, the preparation method on the anti-icing surface of bionical micro-nano compound structure provided by the present invention realizes that easily cost is low;

5, the anti-icing surface of the bionical micro-nano compound structure of the present invention preparation after the repeatedly circulation between low temperature-20 ℃ and the room temperature, does not influence result of use, and weather resistance is strong, even and damage lost efficacy and still can prepare once more, waste material not;

6, the anti-icing surface hydrophobicity of the bionical micro-nano compound structure of the present invention's acquisition is dredged ice, does not need outside energy and device;

Even 7, the anti-icing of the bionical micro-nano compound structure surface that obtains of the present invention is at low temperature lower surface deposition ice more, temperature is recovered on the freezing point rear surface, and residuary water or residuary water seldom do not have self-cleaning net energy power.

Description of drawings

Fig. 1 is the finish size synoptic diagram of bar shaped helical teeth structure among the embodiment 1;

Fig. 2 A and Fig. 2 B are the front view of bar shaped helical teeth structure among the embodiment 1 and the microtexture synoptic diagram of top view;

Fig. 3 A and Fig. 3 B are the sem photograph with top view faced of the anti-icing surface tissue of preparation among the embodiment 1;

Fig. 4 is the icing time comparison diagram on the anti-icing surface of embodiment 1 preparation;

Fig. 5 is the matrix helical teeth scantlings of the structure synoptic diagram among the embodiment 2;

Fig. 6 A and 6B are facing of matrix helical teeth structure and the main sem photograph of looking;

Fig. 7 A~7C is the sem photograph of nanostructure among the embodiment 2;

Fig. 8 is the anti-icing of the matrix helical teeth micro-nano compound structure anti-icing test process time of lag figure in surface.

Embodiment

Below in conjunction with drawings and Examples anti-icing surface of bionical micro-nano compound structure provided by the invention and preparation method thereof is elaborated.

The anti-icing surface of bionical micro-nano compound structure provided by the invention prepares by the following method:

The first step, at substrate surface finished surface micrometer structure:

Described surperficial micrometer structure is bar shaped helical teeth structure, matrix helical teeth structure or tilted conical structure etc.The cycle (space width) of surface micrometer structure is 200~1100 μ m, highly is 70~900 μ m, and the angle of inclination of surperficial micrometer structure is 25~45 °.The main effect of these surperficial micrometer structures is the contacts area that reduce liquid and substrate surface as much as possible, and realizes that the anisotropy of substrate surface is beneficial to the directed easily disengaging of the water of substrate surface, ice.

According to the material selection difference of substrate, the surperficial micrometer structure working method difference that is adopted, specific as follows:

1, the base material on anti-icing surface is metallic substance such as stainless steel, the pig iron, magnalium or aluminium, and surperficial micrometer structure can adopt mechanical processing method, the processing of molding casting.

2, the base material on anti-icing surface is the high materials of unreactiveness such as pottery, can make the shape base by the powder molding compacting, and then solid state sintering obtains surperficial micrometer structure; Also can adopt the laser ablation method to realize surperficial micrometer structure.

3, the base material on anti-icing surface is the material of non-refractory such as organic polymer, can adopt the heating stamped method to thermoplastic material, to thermosetting material can adopt mechanical processing method or solidify before earlier the preparation shape again the solidified method realize the processing and preparing of surperficial micrometer structure.

4, the surperficial base material of anti-icing is corrodible materials such as silicon, can adopt photolithography, gas phase directional etching method, laser ablation method etc. to realize surperficial micrometer structure.

5, the surperficial base material of anti-icing is a glass, can adopt directional etching method, moulding method to realize surperficial micrometer structure.

Not mentioned to other material can select the implementation method of surperficial micrometer structure according to the material intrinsic performance.

In second step, on surperficial micrometer structure, plant nanostructure:

Described nanostructure can be nano wire, nanometer rod, nanometer pyramid etc., and single nanostructure diameter is 70~100nm, and length is 1~3 μ m.Nano structural material can realize that complexity reaches and coupling, bonding force and other particular requirements of base material are selected according to existing preparation method's maturity, preparation complexity, scale production, and specific implementation method has hydrothermal synthesis method, vapour deposition process etc.As the nanostructure of, ZnO realize very ripe, can be many and easy for implementation method; And for example, also can select TiO for use 2Nano wire.

In the 3rd step, finishing reduces surface energy:

The method that reduces surface energy generally adopts the finishing method, and the modifier in the finishing method generally adopts fluorine cpd, and as tetrafluoroethylene, perfluor silane etc., wherein effect is perfluor silane preferably.Modifying method generally adopts vacuum vapour deposition, and this method uses less perfluor silane and effect splendid.

Above-mentioned through after the finishing, promptly form the anti-icing surface of bionical micro-nano compound structure of the present invention at substrate surface, bar shaped helical teeth with micrometer structure, matrix helical teeth or oblique cone structure, the nano wire that on the basis of surperficial micrometer structure, also has nanostructure, nanometer rod or nanometer pyramid, the anti-icing surface of this bionical micro-nano compound structure can be used for waterproof, anti-icing, not only at normal temperature, possesses super-hydrophobic performance under the low temperature, in the room temperature environment, the substrate that will have anti-icing surface is placed on the cold drawing, the cold drawing temperature is below freezing, as-10 ℃, can make the water droplet of about 7 μ L keep more than 1.5 hours icing.Temperature is reduced to-20 ℃, gos up to the freeze-thaw cycle test of room temperature again, and the anti-icing surface of this bionical micro-nano compound structure can be unaffected 20 circulation rear defence icing effects.

Come specifically described bionical micro-nano compound structure to be prevented that the preparation method on icing surface describes below by embodiment:

Embodiment 1:Adopt stainless steel as base material, surperficial micrometer structure is the bar shaped helical teeth, and nanostructure is the ZnO nano wire, and preparation process is as follows:

The first step, at substrate surface finished surface micrometer structure:

Adopt the method for mechanical workout, on stainless steel-based basal surface, process bar shaped helical teeth structure.As shown in Figure 1, wherein A is a front view, and B is a left view, and C is a vertical view, and the length of described substrate is 30.0mm, and width is 10.0mm, highly is 1.5mm; Mechanical workout bar shaped helical teeth micrometer structure is of a size of: bar shaped helical teeth parallelism structural is in the width edge direction, bar shaped helical teeth structure space width 200~400 μ m, highly be 70~80 μ m, bar shaped helical teeth angle of inclination is 25~30 °, scanning electron microscope picture such as Fig. 2 A, the 2B of surface micrometer structure, Fig. 2 A is a front view, Fig. 2 B is a top view, scale is 500 μ m, has formed surperficial micrometer structure at substrate surface.

Second step, the plantation nanostructure:

The comparatively ripe and convenient-to-running ZnO nano wire hydrothermal synthesis method realization nanostructure plantation of employing technology.

(1) preparation seed-solution: get Zinc diacetate dihydrate, Monoethanolamine MEA BASF and ethylene glycol monomethyl ether, mix and stir about 30 minutes firmly, obtain the not seed-solution of molten material of transparent nothing, the volumetric molar concentration of Zinc diacetate dihydrate is 0.05 mole every liter in the seed-solution, the concentration of Monoethanolamine MEA BASF is 0.05 mole every liter, and solvent is an ethylene glycol monomethyl ether.

(2) preparation growth media: take by weighing zinc nitrate hexahydrate and hexamethylenetetramine, measure deionized water, mix and stir about 30 minutes firmly, make growth media.The volumetric molar concentration of zinc nitrate hexahydrate is every liter of 0.25 mmole in the growth media, and the volumetric molar concentration of hexamethylenetetramine is every liter of 0.25 mmole, and solvent is a water.

Described Zinc diacetate dihydrate, ethylene glycol monomethyl ether, Monoethanolamine MEA BASF, zinc nitrate hexahydrate and hexamethylenetetramine are analytical pure, and the water of employing is deionized water.

(3) substrate surface with surperficial micrometer structure is cleaned: 0.1 mole every liter about 5 minutes of dilute hydrochloric acid solution ultrasonic cleaning is put at the stainless steel-based end after the processing in the first step, remove surperficial iron rust.Subsequently base material is used acetone, ethanol and deionized water ultrasonic cleaning 5 minutes respectively, in stink cupboard, dried.

(4) behind the substrate naturally cooling after cleaning, dip in the seed-solution of getting preparation in second step with substrate, make seed-solution form the very thin liquid film of one deck at substrate surface, sole keeps flat in the retort furnace, 350~400 ℃ of sintering 5 minutes.

(5) substrate behind the sintering is taken out from retort furnace, put into the polytetrafluoroethylliner liner of high-temperature high-pressure reaction kettle behind the naturally cooling, need to guarantee to have the surface of bar shaped helical teeth structure downward, and the surface of bar shaped helical teeth structure can not contact with wall of inner container; Pour the growth media of preparation in second step in reactor, assemble reactor, put into baking oven, it is 85 ℃ that temperature of reaction is set, and the reaction times is 15 hours.Reaction finishes, and takes out reactor, treats to take out substrate behind its naturally cooling, and rinse well with deionized water on the surface, dries stand-byly, promptly plants nanostructure on surperficial micrometer structure.

The 3rd step, finishing:

Use the high-grade power gear cleaning of Plsma cleaning machine after 10 minutes the substrate surface with nanostructure of oven dry, put into vacuum vessel, drip 2~3 perfluor silane (perfluoroalkyl organoalkoxysilane) at substrate surface, be evacuated in the vacuum vessel-below the 0.1Mpa.Vacuum vessel is put into baking oven, keep 90 ℃ of reactions 3 hours.Reaction finishes and has just gone out efficient anti-icing surface in substrate surface preparation.The anti-icing surface scan Electronic Speculum picture for preparing and synoptic diagram such as Fig. 3 A and the 3B of micro-nano compound structure, Fig. 3 A is the sem photograph of the front view of the anti-icing surface tissue for preparing, Fig. 3 B is the sem photograph of the top view of anti-icing surface tissue, Fig. 3 C is a bar shaped helical teeth surface plantation nanostructure synoptic diagram, as we know from the figure, nanostructure evenly is planted in the surface of bar shaped helical teeth structure, and wherein the diameter of ZnO nano wire is 70~100nm, and length is 1~3 μ m.Micrometer structure combines with nanostructure, forms the anti-icing surface of micro-nano compound.

Anti-icing performance to the anti-icing surface of above-mentioned preparation is tested as follows:

Test conditions: 25 ℃ of laboratory temperatures, relative humidity 70%, cooling table temperature-10 ℃ adopts Po Er to paste the type of cooling.

With the smooth stainless steel surface (S surface) that do not process, only prepare surperficial micrometer structure surface (M surface), anti-these four surfaces, icing surface (MN surface) of bionical micro-nano compound structure of only preparing nanostructured surface (N surface) and possess micron, nanostructure simultaneously are placed on the cooling table simultaneously, drip the common drinking mineral water of 7 μ L respectively, test its icing time, the results are shown in Figure 4.As shown in Figure 4, the time of coagulation of the anti-icing surface of bionical micro-nano compound structure provided by the invention under-10 ℃ temperature condition is 7220S, the icing time of remaining surface S face, M face, N face is respectively 1260S, 30.5S and 1740S, and the icing time of the anti-lip-deep water droplet of icing of bionical micro-nano compound structure of the present invention is much larger than the icing time on other three kinds of surfaces.

Embodiment 2:

The first step, the pattern processing of substrate surface:

In substrate surface processing matrix helical teeth structure, pig iron material substrate is adopted in described substrate, and as shown in Figure 5, base length is 21.5mm, and width is 11.5mm, highly is 3.0mm; The machining surface micrometer structure is a matrix helical teeth structure, helical teeth height 0.4~0.9mm, and the length direction helical teeth cycle is 0.4~1.1mm, 40~45 ° at angle of inclination; The width helical teeth cycle is 0.4~1.0mm, and the angle of inclination is 30~40 °.The optics picture of matrix helical teeth structure is shown in Fig. 6 A, 6B, and Fig. 6 A is a front view, and Fig. 6 B is a top view, and as seen from the figure, substrate surface forms the matrix helical teeth body structure surface of micrometer structure.

In second step, on surperficial micrometer structure, plant nanostructure:

Adopt the method identical to plant the ZnO nano wire on surperficial micrometer structure surface with embodiment 1, the scanning electron microscope picture of the synoptic diagram of micro-nano compound structure and plantation synoptic diagram are shown in Fig. 7 A~7C, formed uniform nano thread structure on the surface of matrix helical teeth, the diameter of nano wire is 70~90nm, and length is 1~3 μ m.

The 3rd step, finishing:

Adopt the method identical with embodiment 1 to carry out substrate surface and modify, selecting modifier for use is tetrafluoroethylene, and the vacuum evaporation condition prepares bionical micro-nano compound structure and prevents the icing surface with embodiment 1 in pig iron substrate.

The anti-icing performance test on the anti-icing surface of the bionical micro-nano compound structure of preparation is as follows:

Test conditions: 25 ℃ of laboratory temperatures, relative humidity 70%, cooling table temperature-10 ℃ adopts Po Er to paste the type of cooling.

The anti-icing surface of two matrix helical teeth that the helical teeth height is respectively 0.9mm and 0.4mm is placed on the cooling table, drip the one 7 common drinking mineral water of μ L respectively, the anti-icing test process on the anti-icing surface of observation matrix helical teeth micro-nano compound structure, occur freezing at 118min and 124min respectively, see Fig. 8.

According to the preparation method among embodiment 1 and the embodiment 2, can also select for use materials such as pottery, organic polymer, glass as base material, change surperficial micrometer structure shape and size, nanostructure, can also obtain having the anti-icing surface of processing condition preparation as shown in the table, as following table:

To the anti-icing surface of the above-mentioned bionical micro-nano compound structure that the prepares time test that freezes, test conditions is with embodiment 1, and the result shows, under-10 ℃ of conditions, icing time of water droplet of preventing the icing surface is all greater than 7200S.Carried out circulating between-20 ℃ and the room temperature in anti-icing surface, test the icing time of water droplet on it, circulate after 20 times, the effect on anti-icing surface is before identical with circulation, do not change, illustrate that anti-icing provided by the invention surface has good environmental compatibility, has good application prospects.Outdoor machinery, building, aircraft, steamer, cable, electric tower etc. may produce the facility that ice sheet covers phenomenon, and have and substrate identical materials of the present invention, can adopt preparation method provided by the invention on the anti-icing surface of the facility surface preparation micro-nano compound of the anti-icing of needs.

Claims (3)

1. a bionical micro-nano compound structure is prevented the preparation method on icing surface, it is characterized in that:
The first step is at substrate surface finished surface micrometer structure; Described surperficial micrometer structure is bar shaped helical teeth, matrix helical teeth or tilted conical structure; The cycle or the space width of surface micrometer structure are 200~1100 μ m, highly are 70~900 μ m, and the angle of inclination of surperficial micrometer structure is 25~45 °;
In second step, planting nanostructure on the surperficial micrometer structure: adopt hydrothermal synthesis method to plant zinc oxide nanowire on surperficial micrometer structure, the diameter of zinc oxide nanowire is 70~100nm, and length is 1~3 μ m; The concrete steps of plantation zinc oxide nanowire are on surperficial micrometer structure:
(1) preparation seed-solution: get Zinc diacetate dihydrate, Monoethanolamine MEA BASF and ethylene glycol monomethyl ether, mix and firmly stirring, obtain the not seed-solution of molten material of transparent nothing, the volumetric molar concentration of Zinc diacetate dihydrate is 0.05 mole every liter in the seed-solution, the concentration of Monoethanolamine MEA BASF is 0.05 mole every liter, and solvent is an ethylene glycol monomethyl ether;
(2) preparation growth media: take by weighing zinc nitrate hexahydrate and hexamethylenetetramine, measure deionized water, mix and firmly stirring, make growth media, the volumetric molar concentration of zinc nitrate hexahydrate is every liter of 0.25 mmole in the growth media, the volumetric molar concentration of hexamethylenetetramine is every liter of 0.25 mmole, and solvent is a water;
(3) substrate surface after the pattern processing in the first step is cleaned;
(4) behind the substrate naturally cooling after cleaning, dip in the seed-solution of getting preparation in (1) step with substrate, make seed-solution form one deck liquid film at substrate surface, sole keeps flat in the retort furnace, 350~400 ℃ of sintering 5 minutes;
(5) substrate behind the sintering is taken out from retort furnace, put into the polytetrafluoroethylliner liner of high-temperature high-pressure reaction kettle behind the naturally cooling, need to guarantee to have the surface of surperficial micrometer structure downward, and the surface of surperficial micrometer structure can not contact with wall of inner container; In reactor, pour the growth media of preparation in (2) step into, assemble reactor, put into baking oven, it is 85 ℃ that temperature of reaction is set, and the reaction times is 15 hours, reaction finishes, take out reactor, treat to take out substrate behind its naturally cooling, rinse well with deionized water on the surface, dry stand-byly, promptly on surperficial micrometer structure, plant nanostructure;
In the 3rd step, finishing obtains anti-icing surface; It is fluorine cpd that modifier is adopted in finishing, and modifying method is a vacuum vapour deposition, and described surface modification method is specially:
After will having the substrate cleaning of nanostructure, put into vacuum vessel, drip 2~3 modifiers at substrate surface, be evacuated in the vacuum vessel-below the 0.1MPa; Vacuum vessel is put into baking oven, keep 90 ℃ of reactions 3 hours, reaction finishes and has just gone out anti-icing surface in substrate surface preparation; Described anti-icing surface is under-10 ℃ of conditions, and the icing time of the water droplet on anti-icing surface is all greater than 7000s; Between-20 ℃ and room temperature, circulate, to the not influence of anti-icing effect on anti-icing surface.
2. the preparation method on the anti-icing surface of bionical micro-nano compound structure according to claim 1 is characterized in that: molding casting, laser ablation method, heating stamped method or gas phase directional etching method are adopted in the processing of surperficial micrometer structure.
3. the preparation method on the anti-icing surface of bionical micro-nano compound structure according to claim 1, it is characterized in that: described modifier is tetrafluoroethylene or perfluor silane.
CN 201110407972 2011-12-09 2011-12-09 Preparation method of ice coating prevention surface of bionic micro-nano composite structure CN102492945B (en)

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