CN101705488A - Surface processing method of super-hydrophobic ice-covering-proof aluminum and steel with rough surface - Google Patents
Surface processing method of super-hydrophobic ice-covering-proof aluminum and steel with rough surface Download PDFInfo
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Abstract
The invention relates to a surface processing method of super-hydrophobic ice-covering-proof aluminum and steel with rough surfaces. The method comprises the following steps: performing ultrasonic cleaning to aluminum and steel plates with acetone and deionized water, drying, suspending the aluminum and steel plates in a sealed container with 20vol.%-80vol.% of hydrochloric acid solution, then etching aluminum and steel plates with volatile hydrochloric acid for 15min-1h in a water bath under the temperature of boiling water, namely 100 DEG C; after the etching, placing the aluminum and steel plates in the normal hexane solution of fluorosilane to performing evaporation and modification of fluorosilane at 200-300 DEG C for 1-2h, and finally taking out the samples to keep temperature in the air at 180-300 DEG C for 1-2h; and in the fluorosilane solution, the weight ratio of fluorosilane to normal hexane is 1-5%, and the pH value of the added acetic acid aqueous solution is 3 and the content is 2-4% of the normal hexane solution of fluorosilane.
Description
Technical field
The present invention relates to a kind of the have super-hydrophobic ice-covering-proof aluminum of uneven surface and the surface treatment method of steel.
Background technology
The frosting phenomenon extensively is present in the metallic element of refrigeration and cold operation equipment, and for example the wing of the air-coil of heat pump set, aerospacecraft and surface, air-conditioning, refrigerator internal surface etc. have brought harm in various degree for the steady operation of equipment.
The anti-freeze technology in traditional engineering materials surface is utilized machinery or heating technique deicing, ice-melt more, as thermal ice-melting, excess current de-icing, short circuit ice-melt, on-load ice-melt etc.More existing invention technology also are based on the thinking of " ice-melt ", as: adopt high-frequency pulse current to add thermal oscillation the anti-icing of electric line is removed ice-melt, the conductor that the lead of employing and power transmission and distribution together lays generates heat to prevent icing.But these methods can not tackle the problem at its root, and need arrestment when deicing, and are equipped with special ice removal system and equipment.This has brought inconvenience to production undoubtedly, has also consumed a large amount of energy simultaneously, has increased cost.For this reason, part Study personnel are starting point to suppress icing, have explored some and have suppressed icing method.As being coated with at cold surface with wetting ability dope of restraining frost [Okoroafor EU, J Phy.D-App.Phy., 1999,32 (18): 2454-2461; Okoroafor EU, Newborough M, App.Thermal Eng., 2000,20 (8): 737-758], the thickness that can reduce frost reaches 10-30%, but this coating is thicker, about 0.77mm, have influence on the cold surface airiness, and the organic composition in the coating is volatile, makes that its work-ing life is lower; The good grade developed a kind of strongly hydrophilic dope of restraining frost among Liu of Beijing University of Technology, this coating contains absorbent resin, can absorb large quantity of moisture, and the freezing point that sodium-chlor that adds or potassium chloride particle can effectively reduce water, make the moisture in the absorbing coating keep for a long time not freezing, thereby suppress the appearance of initial hoar crystal, play the effect that presses down frost, but the moisture that this strongly hydrophilic surface absorbs is difficult for volatilization fast, owing to just reduce the freezing point of water, so when temperature is lower, can promote the formation of hoar crystal on the contrary, the frosting on aggravation surface.
Copy to have " lotus leaf effect (Lotus Effect) " special surface microstructure of organism, can construct similar special construction, the metallic surface that obtains having superhydrophobic characteristic in the metallic surface.There are extremely huge application potential and wide application prospect in this super-hydrophobic metallic surface in fields such as self-cleaning, drag reduction, corrosion-resistant, freezings.As inspiration, some hydrophobicity anti-icing coating and coating technique are developed in succession.As with organosilane and/or fluorine silicon resin, the quick-drying solvent, after the main body solvent stirring at room, add polyoxyethylene in succession, silane coupling agent promotor, silicon oxide and/or alumina particle stir, be coated in specimen surface curing at last and obtain anti-icing coatings, can make frosting degree reduce 40%, but this technology is difficult for applying to some positions of complex-shaped equipment and part, make that protection is inhomogeneous, and the organic solvent in the coating is volatile, work-ing life is lower, the frosting layer also needs to remove under mechanical vibration, and some are needed precision instrument anti-freeze but that can not vibrate, equipment and part have certain limitation; By the vacuum evaporation mode, coating n-hexatriacontane hydrophobic layer also can postpone the formation of initial hoar crystal on the feeder cable surface, and the hoar crystal short texture of formation is more easily removed, but be it is pointed out that this film coating method need be in vacuum tightness less than 1.3 * 10
-5Vacuum condition under carry out, obviously be difficult for carrying out scale operation.
Studies show that [Byeongchul N, Ralph LW, Int.J Heat﹠amp; Mass Transfer, 2003,46,3797-3808], the roughness of solid surface can reduce the degree of supersaturation of water vapour, thereby reduce the nucleation rate and the nucleation rate of the globule, delay the formation of initial hoar crystal, play the effect that presses down frost. simultaneously, the potential barrier that water repellent surface forms the globule is bigger than hydrophilic surface, therefore the quantity that condenses into liquid nuclear on the water repellent surface is little than hydrophilic surface. therefore, at solid surface, the surface of especially widely used aluminium and steel is constructed roughness and hydrophobicity simultaneously, will more effectively delay the appearance of initial hoar crystal, significantly improve the freezing performance on aluminium and steel surface. but based on this thinking, and do not see as yet that at the hydrophobicity anti-icing technology on aluminium and steel surface report is arranged.
Summary of the invention
The invention provides the treatment process on coarse aluminium of a kind of super-hydrophobic ice-covering-proof and steel surface.
The present invention adopts following technical scheme:
The treatment process on coarse aluminium of a kind of super-hydrophobic ice-covering-proof and steel surface, the step of processing is as follows:
(1) pre-treatment: aluminium flake and steel disc are also dried with acetone, deionized water ultrasonic cleaning successively;
(2) wet-chemical chamber: aluminium flake or steel disc are hung in the closed unit that fills hydrochloric acid soln, then closed unit is placed constant temperature water bath, make the hydrochloric acid volatilization under 100 ℃ of boiled water temperatures, and, also dry with flushing with clean water behind taking-up aluminium flake or the steel disc with evaporable salt acid etch aluminium flake or steel disc; The volume fraction of described hydrochloric acid is 20%-80%, and etching time is 15min-1h;
(3) fluoridation: aluminium flake after the etching and steel disc are put into the encloses container that fills the silicon fluoride hexane solution, and together put into cabinet-type electric furnace 200-300 ℃ of insulation 1-2h down, realize that the silicon fluoride on aluminium flake and steel disc surface is modified; Take out sample subsequently, under 180-300 ℃, in air, be incubated 1-2h, can obtain possessing the aluminium and the steel surface of superhydrophobic characteristic; The aluminium of preparation and the frosting on steel surface experiment show that there is good anti-icing performance on this surface; The process for preparation of described silicon fluoride solution is: silicon fluoride is dissolved in the normal hexane solvent, the weight percent of silicon fluoride and normal hexane solvent is 1-5%, the 2-4%, the pH value that add silicon fluoride hexane solution weight again are 3 aqueous acetic acid, can use after fully stirring.
The present invention has prepared the super-hydrophobic ice-covering-proof aluminum with uneven surface and the surface of steel.At first, the roughness on aluminium and steel surface can reduce the degree of supersaturation of water vapour, thereby reduces the nucleation rate and the nucleation rate of water droplet, delays the formation of initial hoar crystal, plays the effect that presses down frost.Secondly, there are good ultra-hydrophobicity and very low viscous force in this surface to glassware for drinking water, when contacting with water droplet, has very high contact angle (＞150 °) and extremely low roll angle (1 °).Super hydrophobic surface not only can increase the potential barrier that forms the globule, reduce the quantity that surperficial water droplet condenses into liquid nuclear, simultaneously can be when contacting with water droplet, form " air cushion " at the contact interface entrapped air, significantly reduce the real contact area (＜10%) of the globule and solid surface, thereby when low temperature, effectively reduce the thermal exchange between surface and water droplet, increase the globule required energy that condenses, finally make water droplet be difficult to condense into karyomorphism and become initial hoar crystal, and be suppressed at the formation and the growth of the frost layer of growing on the initial hoar crystal basis.It is to be noted, because the aluminium and the steel surface of preparation are lower to the viscosity of water droplet, water droplet very easily tumbles on this surface, slight vibration, or even wind might make that all water droplet tumbles, thereby be difficult for absorption and freeze to form hoar crystal, even form, also very easily landing because viscosity is lower, thus not only played the icing effect that suppresses, also play the effect of deicing, really realized the anti-icing on aluminium and steel surface.Therefore, the super-hydrophobic ice-covering-proof surface that has certain roughness in widely used aluminium and steel surface preparation, not only can more effectively delay the appearance of initial hoar crystal, significantly improve the freezing performance on aluminium and steel surface, can also utilize the low viscosity on surface to come deicing, realize the anti-icing in real aluminium and steel surface.As this super-hydrophobic ice-covering-proof of preparation surface on the shell on submarine or naval vessel, automatically cleaning, raising route speed and the resistance to corrosion seawater that not only can keep the surface, also can make shell under cold condition, not have icing, thereby be that they are under cold condition, as in the South Pole, the navigation of the arctic or other extremely frigid zones, provide safeguard.
Preparation technology provided by the invention is based on the wet-chemical chamber method, required starting material are acetone, hydrochloric acid, silicon fluoride, normal hexane, common solvent such as acetic acid, required equipment is a Ultrasonic Cleaners, constant temperature water bath, encloses container, common devices such as cabinet-type electric furnace, processing step and operation of equipment are very simple, and according to production-scale demand, can meet the demands by suitable adjustment, the efficient height, cost is low. in addition, the treatment process of the anti-icing of this aluminium and steel surface super hydrophobic, aluminium and steel itself there is not particular requirement, and the position that some of complex product is difficult for coating also can effectively be handled. therefore, the surface treatment method suitability of super-hydrophobic ice-covering-proof aluminum with uneven surface provided by the invention and steel is wider, easily industrial applications.
Description of drawings:
Fig. 1 is the sem photograph and the surperficial globule form of the super-hydrophobic ice-covering-proof roughened aluminum surfaces of preparation.
Fig. 2 is the frosting form (binary conversion treatment after) of undressed aluminium surface under the frosting experiment condition.
Fig. 3 is the frosting form (binary conversion treatment after) of super-hydrophobic ice-covering-proof roughened aluminum surfaces under the frosting experiment condition of preparation.
The sem photograph and the surperficial globule form on the coarse steel of the super-hydrophobic ice-covering-proof surface of Fig. 4 preparation.
Fig. 5 is the frosting form (binary conversion treatment after) of undressed steel surface under the frosting experiment condition.
Fig. 6 is the frosting form (binary conversion treatment after) of the coarse steel of super-hydrophobic ice-covering-proof surface under the frosting experiment condition of preparation.
Embodiment
The treatment process on coarse aluminium of a kind of super-hydrophobic ice-covering-proof and steel surface:
(1) pre-treatment: aluminium flake and steel disc are also dried with acetone, deionized water ultrasonic cleaning successively;
(2) wet-chemical chamber: aluminium flake or steel disc are hung in the closed unit that fills hydrochloric acid soln, then closed unit is placed constant temperature water bath, make the hydrochloric acid volatilization under 100 ℃ of boiled water temperatures, and, also dry with flushing with clean water behind taking-up aluminium flake or the steel disc with evaporable salt acid etch aluminium flake or steel disc; The volume fraction of described hydrochloric acid is 20%-80%, and etching time is 15min-1h; In the present embodiment, the volume fraction of hydrochloric acid selects 20%, 80% or 68% for use, etching time 15min, 1h or 37min;
(3) fluoridation: aluminium flake after the etching or steel disc are put into the encloses container that fills the silicon fluoride hexane solution, and together put into cabinet-type electric furnace 200-300 ℃ of insulation 1-2h down, realize that the silicon fluoride on aluminium flake and steel disc surface is modified; Take out sample subsequently, under 180-300 ℃, in air, be incubated 1-2h, can obtain possessing the aluminium and the steel surface of superhydrophobic characteristic; The aluminium of preparation and the frosting on steel surface experiment show that there is good anti-icing performance on this surface; The process for preparation of described silicon fluoride solution is: silicon fluoride is dissolved in the normal hexane solvent, the weight percent of silicon fluoride and normal hexane solvent is 1-5%, the 2-4%, the pH value that add silicon fluoride hexane solution weight again are 3 aqueous acetic acid, can use after fully stirring; In the present embodiment, fluoridize in the silicon fluoride hexane solution of usefulness, the weight percent of silicon fluoride and normal hexane solvent is 1%, 5% or 3.2%, the aqueous acetic acid that adds is 2%, 4% or 3.3% of a silicon fluoride hexane solution weight, encloses container is put into cabinet-type electric furnace and is heated to 200 ℃, 300 ℃ or 148 ℃, and insulation 1h, 2h or 1.4h, aluminium flake or steel disc sample are incubated 1h, 2h or 1.7h in the air under 180 ℃, 300 ℃ or 247 ℃ at last.
Example 1
At first with acetone, deionized water ultrasonic cleaning aluminium flake and oven dry; Be 40% aqueous hydrochloric acid subsequently with concentration, in the encloses container in the boiling water groove, steaming process etching aluminium flake 1h takes out back flushing with clean water and oven dry; With the pH value is that 3 aqueous acetic acid is regulated silicon fluoride normal hexane solvent, and wherein the weight percent of silicon fluoride and normal hexane is 2%, and the weight percent of aqueous acetic acid and silicon fluoride hexane solution also is 2%; Aluminium flake after the etching is hung on above-mentioned silicon fluoride hexane solution top, together put into 250 ℃ of cabinet-type electric furnaces insulation 2h down after airtight, realize that the silicon fluoride on aluminium flake surface is modified; Take out sample subsequently, continue at 250 ℃ of insulation 0.5h down, the pattern of the roughened aluminum surfaces that possesses superhydrophobic characteristic that obtains and surperficial water droplet form are as shown in Figure 1, corresponding data is as shown in table 1. as seen from Table 1, compare with untreated aluminium flake surface, the aluminum surface super hydrophobic better performances for preparing, and water droplet very easily tumbles.
Sample frosting experimental conditions is as follows: 5 ℃ of envrionment temperatures, cold surface temperature-5 ℃, relative humidity 77%, adopt the semiconductor refrigerating mode to freeze, every 2min gathers the process of frosting in real time by image capturing system, and the image of gathering carried out binary conversion treatment, from binary image, obtain relevant informations such as white layer height at last, and weigh the freezing performance of sample with this.
For undressed aluminium flake surface, its frosting experimental result as shown in Figure 2, when 2min was carried out in frosting test, undressed aluminium flake surface had formed the frost layer, and be evenly distributed (1 indication among Fig. 2); Along with the carrying out of frosting test, the constantly growth of lip-deep frost layer, white layer height constantly increases, frosting serious (5 indications among Fig. 2) during 10min, frost level reaches 0.1542mm, demonstrates relatively poor deicing properties.For the super-hydrophobic ice-covering-proof roughened aluminum surfaces of preparation, its frosting experimental result as shown in Figure 3.The frosting speed on this surface obviously reduces, in initial 4min, almost there is not hoar crystal to form (1 and 2 indications among Fig. 3), though there is a small amount of initial hoar crystal to form (3 and 4 indications among Fig. 3) subsequently, but speed is lower, during to 10min, a small amount of initial hoar crystal is also only arranged, do not form frost layer (5 indications among Fig. 3) yet, the center line average of hoar crystal only is 0.0354mm.
The aluminium flake surface of table 1 preparation and contact angle, roll angle and the anti-icing performance of water
| Sample | Contact angle | Roll angle | Icing layer height (mm) during 10min |
| The super-hydrophobic ice-covering-proof roughened aluminum surfaces | ??155° | ??1° | ??0.0354 |
| The aluminium surface of being untreated | ??75° | ??- | ??0.1542 |
Example 2
Steel disc is also dried with acetone, deionized water ultrasonic cleaning successively; With concentration is that 75% hydrochloric acid soln and the encloses container that is hung with steel disc place 30min in the boiling water groove, takes out flushing with clean water and oven dry subsequently; With the pH value is that 3 aqueous acetic acid is regulated silicon fluoride normal hexane solvent, and wherein the weight percent of silicon fluoride and normal hexane is 2%, and the weight percent of aqueous acetic acid and silicon fluoride hexane solution also is 2%; Steel disc after the etching is put into the encloses container that fills above-mentioned silicon fluoride hexane solution, and together put into 250 ℃ of following insulation 2h of cabinet-type electric furnace, realize that the silicon fluoride on steel disc surface is modified; Take out sample subsequently, continue at 250 ℃ of down insulation 0.5h, the pattern on the coarse steel surface that possesses superhydrophobic characteristic that obtains and surperficial water droplet form as shown in Figure 4, corresponding data is as shown in table 2.As seen from Table 2, compare with untreated steel disc surface, the steel surface super hydrophobic performance for preparing is better, and water droplet very easily tumbles.
The steel disc surface of table 2 preparation and contact angle, roll angle and the anti-icing performance of water
| Sample | Contact angle | Roll angle | Icing layer height (mm) during 10min |
| The coarse steel of super-hydrophobic ice-covering-proof surface | ??161° | ??1° | ??0.0108 |
| The steel surface of being untreated | ??72° | ??- | ??0.1400 |
Steel disc surface frosting experiment condition is identical with the frosting experiment of aluminium flake surface, and corresponding results as shown in Figure 5 and Figure 6.The frosting situation and the undressed aluminium flake on undressed steel disc surface are similar, frosting experiment 2min just begins to occur hoar crystal, but it is sparse to distribute, white layer has appearred during 4min, and along with the carrying out of frosting test, the frost layer constantly increases, as shown in Figure 5, reached 0.14mm during 10min, the phenomenon of freezing is serious.Super-hydrophobic ice-covering-proof roughened aluminum surfaces with preparation is similar, very sparse hoar crystal only appears in the coarse steel of the super-hydrophobic ice-covering-proof surface of preparation in the 10min of frosting experiment, do not form the frost layer always, as shown in Figure 6, and the average hoar crystal height during 10min has only 0.0108mm, demonstrates excellent anti-icing effect.
Claims (1)
1. the preparation method of a super-hydrophobic low tackiness icing-resistant copper surface is characterized in that described preparation method comprises the following steps:
(1) pre-treatment: aluminium flake and steel disc are also dried with acetone, deionized water ultrasonic cleaning successively;
(2) wet-chemical chamber: aluminium flake or steel disc are hung in the closed unit that fills hydrochloric acid soln, then closed unit is placed constant temperature water bath, make the hydrochloric acid volatilization under 100 ℃ of boiled water temperatures, and, also dry with flushing with clean water behind taking-up aluminium flake or the steel disc with evaporable salt acid etch aluminium flake or steel disc; The volume fraction of described hydrochloric acid is 20%-80%, and etching time is 15min-1h;
(3) fluoridation: aluminium flake after the etching and steel disc are put into the encloses container that fills the silicon fluoride hexane solution, and together put into cabinet-type electric furnace 200-300 ℃ of insulation 1-2h down, realize that the silicon fluoride on aluminium flake and steel disc surface is modified; Take out sample subsequently, under 180-300 ℃, in air, be incubated 1-2h, can obtain possessing the aluminium and the steel surface of superhydrophobic characteristic; The aluminium of preparation and the frosting on steel surface experiment show that there is good anti-icing performance on this surface; The process for preparation of described silicon fluoride solution is: silicon fluoride is dissolved in the normal hexane solvent, the weight percent of silicon fluoride and normal hexane solvent is 1-5%, the 2-4%, the pH value that add silicon fluoride hexane solution weight again are 3 aqueous acetic acid, can use after fully stirring.
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| CN111849329B (en) * | 2020-07-10 | 2021-11-02 | 东南大学 | In-situ-regulated water-based super-amphiphobic coating and preparation method thereof |
| CN115029767A (en) * | 2022-05-31 | 2022-09-09 | 珠海市湖大科技有限公司 | Preparation method of inorganic super-hydrophobic surface of aluminum alloy |
| CN115029767B (en) * | 2022-05-31 | 2023-12-29 | 湖北大学 | Preparation method of inorganic superhydrophobic surface of aluminum alloy |
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