CN114702863B - Preparation method of photo-thermal super-hydrophobic deicing coating - Google Patents

Preparation method of photo-thermal super-hydrophobic deicing coating Download PDF

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CN114702863B
CN114702863B CN202210231547.7A CN202210231547A CN114702863B CN 114702863 B CN114702863 B CN 114702863B CN 202210231547 A CN202210231547 A CN 202210231547A CN 114702863 B CN114702863 B CN 114702863B
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amyl acetate
hydrophobic
polytetrafluoroethylene suspension
aluminum sheet
coating
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CN114702863A (en
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欧军飞
张红亮
雷胜
房新佐
王法军
李文
阿里达·阿米法兹力
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Jiangsu University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
    • C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
    • C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C09D127/18—Homopolymers or copolymers of tetrafluoroethene
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/12—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by mechanical means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/18—Materials not provided for elsewhere for application to surfaces to minimize adherence of ice, mist or water thereto; Thawing or antifreeze materials for application to surfaces

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Combustion & Propulsion (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Laminated Bodies (AREA)

Abstract

The invention discloses a preparation method of a photo-thermal super-hydrophobic deicing coating, which comprises the following steps of: polishing with sand paper to remove uneven oxide layer on the surface of the aluminum sheet; secondly, dripping polytetrafluoroethylene suspension into a beaker containing amyl acetate solvent, and carrying out ultrasonic treatment for 5-10min to uniformly mix the polytetrafluoroethylene suspension; the mass ratio of the polytetrafluoroethylene suspension to amyl acetate is 1:1-2; thirdly, prussian blue and hydrophobic silica are sequentially added into the beaker, and stirring is carried out for 6-24 hours, so that precursor solution preparation is completed; the content of Prussian blue and hydrophobic silicon dioxide is 1-5% of the total mass of polytetrafluoroethylene suspension and amyl acetate respectively; and fourthly, spraying the precursor solution on the surface of the pretreated aluminum sheet, drying for 1h at 100-150 ℃, wherein the extremely small dynamic rolling angle of the surface of the coating reduces the adhesion force between water drops or wet snow and ice coating and the surface, so that the water drops or ice coating are easy to fall off under the action of external forces such as self gravity or wind force, and the accumulation of rain, snow and ice on the surface is delayed and even prevented.

Description

Preparation method of photo-thermal super-hydrophobic deicing coating
Technical Field
The invention relates to the technical field of coating materials, in particular to a preparation method of a photo-thermal super-hydrophobic deicing coating.
Background
Ice formation is an unavoidable phenomenon in nature. Ice accumulation can cause serious interference to the operation of high-voltage transmission lines, airplanes and wind turbines, resulting in serious economic loss and even life loss. To prevent ice accumulation, conventional techniques mainly use electrical heating or mechanical force to remove ice from the substrate, or spray chemicals to retard the freezing point of water, making ice growth slower. However, the main problems of these techniques are low efficiency and high energy consumption, and may cause damage to the environment.
As a passive anti-icing coating, the super-hydrophobic surface has good anti-icing effect. On the one hand, the excellent hydrophobicity increases the energy barrier between solid and liquid, prevents heat exchange, delays the formation of ice, enables water drops to leave the surface of the material before freezing, and prevents the formation of ice coating. On the other hand, the extremely small dynamic rolling angle of the super-hydrophobic surface reduces the adhesion force between water drops or wet snow and ice coating and the surface, so that the water drops or ice coating are easy to fall off under the action of external forces such as self gravity or wind force, and the accumulation of rain, snow and ice on the surface is delayed and even prevented, thereby achieving the effect of ice coating prevention. In microcosmic, icing needs to be processed by the processes of formation, growth, accumulation and the like of ice crystal nucleus, and the probability of nucleation is reduced by the small contact area of the superhydrophobic surface and the dynamic behavior of water drops, so that the probability of icing on the surface is reduced.
The condensation occurs in the rough structure gaps of the superhydrophobic surface under the extreme conditions of ultralow temperature, high humidity and the like, and micro liquid drops nucleate and grow in the gaps with relatively large rough size, so that the surface is in a Wenzel state, the adhesion is increased, and the liquid drops are more difficult to remove once frozen. Compared with the traditional electrothermal ice-proof technology, the composite technology has better ice-proof effect and lower energy consumption. Unlike electrothermal coatings, photothermal coatings do not require complex circuit control fittings and are easier to implement. Therefore, photothermal superhydrophobic anti-icing coatings are becoming a new research hotspot.
Disclosure of Invention
The invention aims at providing a preparation method of a photo-thermal super-hydrophobic deicing coating aiming at the defects of the prior art.
The technical scheme for solving the problems is as follows: a preparation method of a photo-thermal super-hydrophobic deicing coating mainly comprises the following steps:
firstly, pretreating an aluminum sheet: polishing with sand paper to remove uneven oxide layer on the surface of the aluminum sheet;
secondly, dripping polytetrafluoroethylene suspension into a beaker containing amyl acetate solvent, and carrying out ultrasonic treatment for 5-10min to uniformly mix the polytetrafluoroethylene suspension; the mass ratio of the polytetrafluoroethylene suspension to amyl acetate is 1:1-2;
thirdly, prussian blue and hydrophobic silica are sequentially added into the beaker, and stirring is carried out for 6-24 hours, so that precursor solution preparation is completed; the content of Prussian blue and hydrophobic silicon dioxide is 1-5% of the total mass of polytetrafluoroethylene suspension and amyl acetate respectively;
fourthly, spraying the precursor solution on the surface of the pretreated aluminum sheet, and baking for 1h at 100-150 ℃.
Further, polishing to remove uneven oxide layers on the surface of the aluminum sheet in the first step, ultrasonically cleaning the aluminum sheet for 5-10min by using ethanol, and then drying for later use.
Further, the mass ratio of polytetrafluoroethylene suspension to amyl acetate is 1:1.
further, prussian blue content is 3% of the total mass of the polytetrafluoroethylene suspension and amyl acetate, and the content of hydrophobic silica is 3% of the total mass of the polytetrafluoroethylene suspension and amyl acetate.
The invention has the beneficial effects that:
the invention provides a preparation method of a photo-thermal super-hydrophobic deicing coating, wherein the extremely small dynamic rolling angle of the surface of the coating reduces the adhesion force between water drops or wet snow and ice coating and the surface, so that the water drops or ice coating are easy to fall off under the action of external forces such as self gravity or wind force, and the accumulation of rain, snow and ice on the surface is delayed and even prevented, and meanwhile, the coating can absorb sunlight or infrared laser to quickly heat up, so that accumulated frost is quickly separated; polishing with sand paper to remove uneven oxide layer on the surface of the aluminum sheet, and increasing surface roughness; prussian blue has a good photo-thermal effect, because Prussian blue nano particles have strong absorption in a near infrared region, can convert absorbed near infrared light into heat, and have good photo-thermal conversion effect and high photo-thermal stability; prussian blue, a large amount of particles of silicon dioxide and polytetrafluoroethylene form a micro-nano structure, air is entrained between fibers and particles, the contact area with water is remarkably reduced, the super-hydrophobicity is displayed, when the surface temperature is reduced, an air layer in the micro-nano structure plays a role of a heat insulation layer, water drops can be well delayed to freeze, and good ice coating resistance is displayed; when icing occurs, the coating can absorb infrared laser to quickly heat up, so that the effect of quick deicing is achieved.
Drawings
FIG. 1 is a schematic illustration of the results of a wettability test of a sample surface;
FIG. 2 is a microscopic topography of a sample surface;
FIG. 3 is a graph showing the variation of surface wettability of a high and low temperature resistant test sample;
FIG. 4 is a graph showing the change in surface wettability of a UV accelerated aging test sample;
FIG. 5 is an infrared thermogram of a sample over time;
fig. 6 is a comparative graph of anti-icing and photo-thermal de-icing tests for bare aluminum flakes and superhydrophobic coated aluminum flakes.
Detailed Description
In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art in a specific case.
A preparation method of a photo-thermal super-hydrophobic deicing coating mainly comprises the following steps:
firstly, pretreating an aluminum sheet: polishing with sand paper to remove uneven oxide layer on the surface of aluminum sheet, ultrasonic cleaning with ethanol for 5-10min, and oven drying.
Secondly, dripping polytetrafluoroethylene suspension into a beaker containing amyl acetate solvent, and carrying out ultrasonic treatment for 5-10min to uniformly mix the polytetrafluoroethylene suspension; the mass ratio of the polytetrafluoroethylene suspension to amyl acetate is 1:1-2.
Thirdly, prussian blue and hydrophobic silica are sequentially added into the beaker, and stirring is carried out for 6-24 hours, so that precursor solution preparation is completed; the content of Prussian blue and hydrophobic silica is 1-5% of the total mass of polytetrafluoroethylene suspension and amyl acetate respectively.
Fourthly, spraying the precursor solution on the surface of the pretreated aluminum sheet, and baking for 1h at 100-150 ℃.
Spraying the solution prepared in the second step on the surface of the pretreated aluminum sheet, and performing four groups of comparison tests:
the mass ratio of polytetrafluoroethylene suspension to amyl acetate in the first group is 2:0, the contact angle of the water drop is 102.6+/-0.8 degrees.
The second group, polytetrafluoroethylene suspension to amyl acetate mass ratio is 2:2, the contact angle of the water drop is 102.5+/-1.1 degrees.
The third group, polytetrafluoroethylene suspension to amyl acetate mass ratio of 2:3, the contact angle of the water drop is 102.9+/-1.1 degrees.
The fourth group, polytetrafluoroethylene suspension to amyl acetate mass ratio of 2:4, the contact angle of the water drop is 97.6+/-1.2 degrees.
The smaller the contact angle of the water drop on the surface of the aluminum sheet, the better, and the second group of prepared solutions are taken for preparing the precursor solution.
Example 1
In this example, in the third step, the Prussian blue content was 3% of the total mass of the polytetrafluoroethylene suspension and amyl acetate, the hydrophobic silica content was 1% of the total mass of the polytetrafluoroethylene suspension and amyl acetate, and the prepared precursor solution was sprayed onto the surface of the pretreated aluminum sheet, and the contact angle of water drops was 163.6.+ -. 1.5 °, and the roll angle was 8.+ -. 0.4 °.
Example 2
In this example, in the third step, the Prussian blue content was 3% of the total mass of the polytetrafluoroethylene suspension and amyl acetate, the hydrophobic silica content was 2% of the total mass of the polytetrafluoroethylene suspension and amyl acetate, and the prepared precursor solution was sprayed onto the surface of the pretreated aluminum sheet, and the contact angle of the water drop was 164.5.+ -. 1.2 °, and the roll angle was 6.+ -. 0.5 °.
Example 3
In this example, in the third step, the Prussian blue content was 3% of the total mass of the polytetrafluoroethylene suspension and amyl acetate, the hydrophobic silica content was 3% of the total mass of the polytetrafluoroethylene suspension and amyl acetate, and the prepared precursor solution was sprayed onto the surface of the pretreated aluminum sheet, and the contact angle of water drops was 167.6.+ -. 1.2 °, and the roll angle was 5.+ -. 0.3 °.
Example 4
In this example, in the third step, the Prussian blue content was 3% of the total mass of the polytetrafluoroethylene suspension and amyl acetate, the hydrophobic silica content was 4% of the total mass of the polytetrafluoroethylene suspension and amyl acetate, and the prepared precursor solution was sprayed onto the surface of the pretreated aluminum sheet, and the contact angle of the water drop was 165.3.+ -. 1.0 °, and the roll angle was 6.+ -. 0.4 °.
The smaller the rolling angle, the smaller the adhesion between water drops or wet snow and ice coating and the surface, the precursor solution prepared in example 3 was sprayed onto the surface of the pretreated aluminum sheet, and test experiments were performed.
The wettability of the sample surface was measured by a contact angle measuring instrument (KRUSS, DSA 30) measuring 10 μl of the droplet, and the contact angle was 167.6 ° ± 1.2 °, as shown in fig. 1, with a roll angle of 5 ° ± 0.3 °.
Microscopic morphology of the sample surface was observed using an optical electron microscope (FE-SEM, novananom, FEI, USA), and a microscopic morphology map is shown in fig. 2.
And testing the high and low temperature resistance of the sample by adopting a high and low temperature oven. The method comprises the following specific steps: the highest temperature of the oven was set at 80℃and the lowest temperature at-20 ℃. The temperature rising rate (cooling rate) is 3 ℃/min. The sample was placed in a high and low temperature oven. The oven is firstly raised to the highest temperature from the room temperature at a rising rate, and is kept for 1h; then the temperature is reduced to the lowest temperature at the speed reduction rate, and the temperature is kept for 1h; the high and low temperature cycles are repeated in this way. Thus simulating outdoor temperature changes. The change curve of the surface wettability was taken out every 5 days, and as shown in fig. 3, CA is the contact angle and SA is the roll angle.
The samples were tested for their UV resistance by means of a UV accelerated ageing test box (LUV-iii). The temperature of the test chamber was set at 35 ℃. And putting the sample in, clicking a light switch, and then clicking for operation. The change curve of the surface wettability was taken out every 3 days, and as shown in fig. 4, CA is the contact angle and SA is the roll angle.
In a sun (1 kw/m) 2 ) Respectively observing infrared thermal imaging diagrams of the aluminum sheet with the superhydrophobic coating on the surface of the exposed aluminum sheet along with time by using an infrared thermal imager (FLUKE, tiS 45), wherein as shown in fig. 5, when the illumination time reaches 1min, the surface temperature of the exposed aluminum sheet is 38.0 ℃ and the surface temperature of a superhydrophobic coating sample is 99.4 ℃; when the illumination time reaches 3min, the surface temperature of the exposed aluminum sheet is 42.2 ℃ and the surface temperature of the super-hydrophobic coating sample is 148.4 ℃; the Prussian blue has a good photo-thermal effect, and the Prussian blue nano particles have strong absorption in a near infrared region, can convert absorbed near infrared light into heat, and have good photo-thermal conversion effect and high photo-thermal stability.
As shown in fig. 6, the anti-icing and photo-thermal deicing tests of the bare aluminum sheet and the super-hydrophobic coated aluminum sheet are shown in fig. 6, a1 and a2 are the anti-icing test of the bare aluminum sheet, b1 and b2 are the anti-icing test of the super-hydrophobic coated aluminum sheet, c1-c3 are the photo-thermal deicing test of the bare aluminum sheet, and d1-d3 are the photo-thermal deicing test of the super-hydrophobic coated aluminum sheet; the radiation light source for the photo-thermal deicing test is 808nm laser, and the power is 2000mW.
The test content of the anti-icing test is as follows: the sample is placed in a sealed box with 35% relative humidity, cooled by water cooling equipment, and the contact angle measuring instrument monitors the temperature. When the surface temperature of the substrate is minus 10 ℃, a drop of water drop with the volume of 10 mu L is dropped on the surface of the substrate, the icing process of the water drop is observed, the time is recorded, the a1, the a2, the b1 and the b2 are compared, the aluminum sheet sprayed with the super-hydrophobic coating is frozen at 35s, and compared with the exposed aluminum sheet, the super-hydrophobic coating has better capability of delaying icing, namely, the anti-icing capability is better; this is due to: the Prussian blue, a large amount of particles of silicon dioxide and polytetrafluoroethylene form a micro-nano structure, air is entrained between fibers and particles, the contact area with water is obviously reduced, the super-hydrophobicity is displayed, when the surface temperature is reduced, an air layer in the micro-nano structure plays a role of a heat insulation layer, water drops can be well delayed to freeze, and good ice coating resistance is displayed.
The test contents of the photo-thermal deicing test are as follows: and (3) placing the sample on a ceramic plate for cooling and icing, and deicing by using laser, wherein the thickness of an ice layer is about 3mm before deicing. The deicing process was recorded with a camera to detect the photo-thermal deicing performance of the fabric with superhydrophobic coating. As shown in d1-d3, the ice accumulation on the surface begins to melt after the coating absorbs heat energy at 12s, and the coating achieves a complete deicing function when the time reaches 599 s. And the ice layer on the exposed aluminum sheet is not melted after 1500 seconds.
The present invention is not limited to the above-mentioned embodiments, and any equivalent embodiments which can be changed or modified by the technical content disclosed above can be applied to other fields, but any simple modification, equivalent changes and modification made to the above-mentioned embodiments according to the technical substance of the present invention without departing from the technical content of the present invention still belong to the protection scope of the technical solution of the present invention.

Claims (2)

1. A preparation method of a photo-thermal super-hydrophobic deicing coating is characterized by comprising the following steps of: mainly comprises the following steps:
firstly, pretreating an aluminum sheet: polishing with sand paper to remove uneven oxide layer on the surface of the aluminum sheet;
secondly, dripping polytetrafluoroethylene suspension into a beaker containing amyl acetate solvent, wherein the mass ratio of the polytetrafluoroethylene suspension to the amyl acetate is 1:1, a step of; ultrasonic treatment for 5-10min to mix them uniformly; the mass ratio of the polytetrafluoroethylene suspension to amyl acetate is 1:1-2;
thirdly, prussian blue and hydrophobic silica are sequentially added into the beaker, and stirring is carried out for 6-24 hours, so that precursor solution preparation is completed; the content of Prussian blue and hydrophobic silicon dioxide is 1-5% of the total mass of polytetrafluoroethylene suspension and amyl acetate respectively; prussian blue content is 3% of the total mass of polytetrafluoroethylene suspension and amyl acetate, and hydrophobic silica content is 3% of the total mass of polytetrafluoroethylene suspension and amyl acetate;
fourthly, spraying the precursor solution on the surface of the pretreated aluminum sheet, and baking for 1h at 100-150 ℃.
2. The method for preparing the photothermal super-hydrophobic deicing coating as set forth in claim 1, wherein the method comprises the following steps: polishing to remove uneven oxide layer on the surface of the aluminum sheet, ultrasonically cleaning with ethanol for 5-10min, and drying for later use.
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