CN109777358B - Graphene-based anti-icing/deicing integrated folded film and preparation method thereof - Google Patents
Graphene-based anti-icing/deicing integrated folded film and preparation method thereof Download PDFInfo
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Abstract
A graphene-based anti-icing/deicing integrated folded film and a preparation method thereof belong to the technical field of aerial real-time anti-icing/deicing. The invention aims to solve the technical problem of difficult ice prevention and deicing in extreme environments. The pleated film (FSGF) is prepared by transferring rGO to a biaxially oriented acrylic acid VHB 4910 substrate film by dry transfer, and retracting the substrate film to obtain the pleated rGO film; then pass through
Method, growing SiO on the surface of rGO2Nanoparticles, finally by FDTS modification of the surface. The folded film still keeps the anti-icing performance at the temperature of minus 20 ℃; meanwhile, when the temperature is-20 ℃, complete deicing and defrosting can be realized within 30s under low voltage, excellent anti-icing and deicing performances are shown, and the method has a huge application prospect in the field of aerial real-time anti-icing/deicing.
Description
Technical Field
The invention belongs to the technical field of aerial real-time ice prevention/removal; in particular to a preparation method of a novel graphene-based micro-nano hierarchical structure corrugated film with both super-hydrophobic property and electrothermal property.
Background
Large areas of ice accretion on the surface of an aircraft can lead to frequent flight delays; the ice accumulation of the wings can cause the increase of flight resistance, the weight of the two wings is unbalanced, and even the crash accident can happen; the view and judgment of the pilot are affected by the accumulated ice on the windshield of the cockpit. The ice accretion not only brings inconvenience to the travel of passengers on the airplane, but also threatens the lives of the passengers, and meanwhile, the falling airplane can cause casualties or damages to people or buildings on the land.
At present, the super-hydrophobic material is considered as the best choice in the field of ice prevention/removal, the solid-liquid contact area can be reduced by utilizing an air layer captured when water drops contact with a film through the super-hydrophobic characteristic of the super-hydrophobic material, and when the surface has a slight inclination angle, super-cooled liquid drops can bounce off the surface of the super-hydrophobic material before icing, so that the ice prevention performance at low temperature is realized. However, under extreme environments, such as low-temperature high-humidity or low-temperature condensation conditions, an anchoring effect can be formed between the liquid drops and the material, so that the adhesion force between the liquid drops and the material is increased, the anti-icing performance is lost, and meanwhile, the deicing work is difficult.
Disclosure of Invention
The invention aims to solve the technical problem of difficult anti-icing and deicing in extreme environments; and provides a graphene-based anti-icing/deicing integrated folded film and a preparation method thereof. In the invention, rGO is transferred to a stretched VHB 4910 substrate film by dry transfer, and a folded rGO film is obtained by retraction of the substrate film; by passing
According to the method, SiO2 nano particles grow on the surface of rGO, and finally FSGF is obtained by modifying the surface through FDTS. The FSGF is tested for anti-icing performance, electrothermal defrosting performance and electrothermal deicing performance, and excellent anti-icing and deicing characteristics are shown. The folded film is light, super-hydrophobic, high in electric heating and good in flexibility. The film is formed by FDTS modified SiO2The obtained product has good super-hydrophobic characteristic and excellent electric heating performance, and has important significance for aerial anti-icing and real-time deicing.
In order to solve the technical problems, the graphene-based anti-icing/deicing integrated folded film (FSGF) is prepared by transferring rGO to a biaxially oriented acrylic acid VHB 4910 substrate film by dry transfer, and retracting the substrate film to obtain the folded rGO film; then pass through
Method, growing SiO on the surface of rGO2Nano particles are prepared by modifying the surface by FDTS; the method is realized by the following steps:
step one, transferring an rGO (reduced graphene oxide) film to a biaxially oriented acrylic acid VHB 4910 substrate film by a dry method;
step two, releasing the substrate film along one uniaxial direction to enable the substrate film to retract, and then releasing the substrate film along the other uniaxial direction to enable the substrate film to retract to the original size to obtain the rGO corrugated film;
adding a cationic surfactant into the ammonia water mixed solution, uniformly mixing, then putting the mixture into the second step to obtain an rGO corrugated film, magnetically stirring the mixture for 5 to 7 hours under the heating of a water bath, dropwise adding ethyl orthosilicate, keeping the temperature and stirring the mixture after the dropwise adding is finished, and then taking out the mixture and drying the mixture;
step four, dripping FDTS diluted by n-hexane on the surface of the wrinkled film treated in the step three, and drying to obtain the graphene-based anti-icing/deicing integrated wrinkled film (FSGF);
wherein the ammonia water mixed solution is prepared from deionized water, absolute ethyl alcohol and ammonia water.
And diluting the FDTS with n-hexane to obtain an n-hexane solution of the FDTS.
Further, the first step of the rGO (reduced graphene oxide) thin film is performed by the following steps: diluting the graphene oxide aqueous solution to 0.1mg/mL, taking 3mL, carrying out vacuum filtration to a polytetrafluoroethylene film with the diameter of 50mm and the pore diameter of 0.45 mu m, drying at 50 ℃ to obtain a GO film, then putting the GO film into a HI solution, reducing in an oven at 90-100 ℃ for 1-1.5 h, taking out, putting in an oven at 120 ℃ for 6h, and removing redundant HI on the surface.
Further defined, the preparation method of the graphene oxide is as follows:
adding 23mL of 98% concentrated sulfuric acid into a 250mL beaker, cooling to-1 ℃ in an ice bath, adding 1g of natural graphite, stirring for 40-60 min, and adding 6g of KMnO in portions4Stirring for 2.5-3 h, then replacing the ice bath, placing in a constant-temperature water bath at 35-45 ℃, stirring for 40-50 min, then making the solution become viscous, then stabilizing the water at 40-50 ℃, transferring to a constant-temperature water bath kettle at 80 ℃, stirring, adding 80mL of distilled water in batches, stirring for 10-20 min, adding 60mL of distilled water for dilution, adding 10.81mL of a mixed solution consisting of 30% hydrogen peroxide and 60mL of deionized water, making the solution become golden yellow, and centrifugally washing with deionized water until the pH value of the solution is 5-6.
Further defined, the prestrain of the biaxially oriented acrylic base film in the step one is 300-400%.
Further limiting, in the third step, 30mg to 50mg of the cationic surfactant is added into the ammonia water mixed solution, wherein the ammonia water mixed solution is prepared from 40mL of deionized water, 10mL of anhydrous ethanol and 1mL to 2mL of ammonia water.
Further defined, the cationic surfactant in step three is cetyltrimethylammonium bromide (CTAB).
Further limiting, the dosage of the tetraethoxysilane in the step three is 1 mL-2 mL.
Further, it is defined that the concentration of the FDTS solution in step III is 1% by mass, and the amount of the FDTS n-hexane solution is 10. mu.L.
Further limiting, the temperature of the water bath in the third step is 40-45 ℃, and the magnetic stirring speed is 400-500 r/min.
Further limiting, drying at 40-60 ℃ in the third step.
The invention prepares rGO micron folds and SiO2The nanometer particles are combined to form a special micro-nano hierarchical structure, meanwhile, a low surface energy substance FDTS is used for modification to obtain an anti-icing/deicing surface FSGF, and a layer of air layer is captured when water drops are contacted with the wrinkled film by using the super-hydrophobic characteristic of the wrinkled film, so that the solid-liquid contact area is reduced, and when the surface has a slight inclination angle, the supercooled liquid drops can bounce off the surface of the material before icing, so that the anti-icing performance at low temperature is realized. Meanwhile, when a water drop is on the surface of the FSGF, the contact angle at low temperature is larger, so that the free energy barrier of the liquid drop nucleation is higher, the ice nucleation rate is lower, and the heterogeneous nucleation time at a solid-liquid interface is delayed; meanwhile, the air layer captured between solid and liquid effectively slows down the heat exchange between the surface and the liquid drops, thereby achieving the purpose of delaying the icing of the supercooled water drops. Meanwhile, the graphene material has excellent conductivity, and can melt an ice layer in contact with the folded film through the joule heat principle, so that the adhesion between ice and the material is reduced, and quick deicing can be realized under the action of external forces such as vibration, wind power, gravity and the like.
The graphene-based anti-icing/deicing integrated folded film (FSGF) still keeps the anti-icing performance when the surface inclination angle is more than or equal to 16.1 ℃ at the temperature of-20 ℃; when the temperature is-10 ℃, compared with the rGO planar membrane, the freezing time of water drops can be delayed by about 6.8 times; meanwhile, when the temperature is-20 ℃, complete deicing and defrosting can be realized within 30s under low voltage, excellent anti-icing and deicing performances are shown, and the method has a huge application prospect in the field of aerial real-time anti-icing/deicing.
Drawings
FIG. 1 SEM image of FSGF;
FIG. 2 shows contact and rolling angles of a water drop on FSGF at different temperatures;
FIG. 3 delays the process of freezing supercooled water droplets;
FIG. 4 is a graph of the temperature rise of FSGF with the application of DC voltage;
FIG. 5 electrothermal defrost process;
fig. 6 electrothermal deicing process.
Detailed Description
Example 1: in the embodiment, the graphene-based anti-icing/deicing integrated pleated membrane (FSGF) is realized by the following steps:
step one, transferring an rGO (reduced graphene oxide) film to a biaxially oriented acrylic acid substrate film with the pre-strain of 400% by a dry method;
step two, releasing the substrate film along one uniaxial direction to enable the substrate film to retract, and then releasing the substrate film along the other uniaxial direction to enable the substrate film to retract to the original size to obtain the rGO corrugated film;
step three, adding 30mg of Cetyl Trimethyl Ammonium Bromide (CTAB) into the ammonia water mixed solution, uniformly mixing, then putting the mixture into the step two to obtain an rGO corrugated film, magnetically stirring the mixture for 6 hours under the heating of a water bath at 40 ℃, then dropwise adding 1mL of tetraethoxysilane, keeping the temperature and stirring the mixture for 12 hours after the dropwise adding is finished, and then taking the mixture out and drying the mixture at 50 ℃;
step four, dripping 10 mu L of normal hexane solution of FDTS (1H,1H,2H, 2H-perfluorodecyl trichlorosilane) with the concentration of 1 percent (mass) on the surface of the folded film treated in the step three, putting the folded film into a vacuum oven, and drying for 3 hours at 50 ℃ to obtain the graphene-based anti-icing/deicing integrated folded film (FSGF);
wherein the ammonia water mixed solution is prepared from 40mL of deionized water, 10mL of anhydrous ethanol and 1-2 mL of ammonia water;
the preparation of the rGO film described in step one is as follows:
Adding 23mL of 98% concentrated sulfuric acid into a 250mL beaker, and cooling to-1 ℃ in an ice bath. Adding 1g of natural graphite, stirring for 40-60 min, and adding 6g of KMnO in portions4And stirring for 2.5-3 h. And (4) replacing the ice bath, placing the ice bath in a constant-temperature water bath at 35-45 ℃, stirring for 40-50 min, and stabilizing the solution in water at about 40-50 ℃. Transferring the mixture into a water bath kettle with the constant temperature of 80 ℃, stirring, adding 80mL of distilled water in batches, stirring for 10-20 min, and adding 60mL of distilled water for dilution. And adding 10.81mL of a mixed solution consisting of 30% hydrogen peroxide and 60mL of deionized water, wherein the solution turns into golden yellow, and centrifugally washing with deionized water until the pH value of the solution is about 5-6.
Diluting the graphene oxide aqueous solution prepared in the step 1 to 0.1mg/mL, vacuum-filtering 3mL of the graphene oxide aqueous solution to a polytetrafluoroethylene film with the diameter of 50mm and the pore diameter of 0.45 mu m, and drying at 50 ℃ to obtain a GO film; and (3) putting the GO thin film into the HI solution, reducing the GO thin film in an oven at 90-100 ℃ for 1-1.5 h, taking out the GO thin film, putting the GO thin film in an oven at 120 ℃ for 6h, and removing redundant HI on the surface.
The morphology picture of the FSGF prepared by the embodiment is shown in figure 1, and the inset in the upper right corner is an enlarged view of the structure. It can be seen from the figure that the FSGF prepared is a micro-nano hierarchical structure with nano-particles grown on the micro-pleat structure, wherein the width of the micro-pleat is about 22.0 μm, the distance between the pleats is about 36.4 μm, and the diameter of the surface nano-silica particles is about 100 nm.
The Water Contact Angle (WCA) and the rolling angle (SA) of FSGF under different low temperature conditions are shown in figure 2, and it can be seen that even when the temperature is-20 ℃, if the surface inclination angle is more than or equal to 16.1 degrees, the water drop can bounce off, and good anti-icing performance is maintained.
When the surface temperature of the material is-10 ℃, the icing process of 10 mu L of water drops on the surfaces of the planar rGO membrane and the FSGF is shown in figure 3, and the icing time of the water drops on the FSGF is delayed by about 6.8 times, so that the material shows good icing delaying performance.
The electrothermal performance of FSGF under low direct current voltage (5-15V) is shown in figure 4, the temperature can be raised to the maximum within 20s, and the characteristics of low energy consumption and rapid temperature rise are shown.
When the surface temperature of the material is-20 ℃ and the relative humidity is more than 90%, the electrothermal defrosting process when the voltage at two ends of the FSGF is 15V is shown in figure 5, and the FSGF can realize complete defrosting within 30 s.
When the surface temperature of the material is-20 ℃, the relative humidity is 35 +/-5 percent, and the voltage at two ends of the FSGF is 15V, the removal process of 10 mu L of frozen water drops is shown in figure 6, when the material is electrified for 23s, the contact layer of ice and the folded film is completely melted and forms a water layer, the adhesion force between the ice and the material is reduced, and when the inclination angle of the FSGF is 30 degrees, the ice drops slide under the action of gravity, so that the rapid deicing is realized.
Example 2: in the embodiment, the graphene-based anti-icing/deicing integrated pleated membrane (FSGF) is realized by the following steps:
step one, transferring an rGO (reduced graphene oxide) film to a biaxially oriented acrylic acid substrate film with the pre-strain of 400% by a dry method;
step two, releasing the substrate film along one uniaxial direction to enable the substrate film to retract, and then releasing the substrate film along the other uniaxial direction to enable the substrate film to retract to the original size to obtain the rGO corrugated film;
step three, adding 50mg of Cetyl Trimethyl Ammonium Bromide (CTAB) into the ammonia water mixed solution, uniformly mixing, then putting the mixture into the step two to obtain an rGO corrugated film, magnetically stirring the mixture for 6 hours under the heating of a water bath at the temperature of 45 ℃, then dropwise adding 2mL of tetraethoxysilane, keeping the temperature and stirring the mixture for 12 hours after the dropwise adding is finished, and then taking the mixture out and drying the mixture at the temperature of 50 ℃;
step four, dripping 10 mu L of normal hexane solution of FDTS (1H,1H,2H, 2H-perfluorodecyl trichlorosilane) with the concentration of 1 percent (mass) on the surface of the folded film treated in the step three, putting the folded film into a vacuum oven, and drying for 3 hours at 50 ℃ to obtain the graphene-based anti-icing/deicing integrated folded film (FSGF);
wherein the ammonia water mixed solution is prepared from 40mL of deionized water, 10mL of anhydrous ethanol and 1-2 mL of ammonia water;
the preparation method of the rGO film described in step one is the same as the steps and process parameters of example 1.
Claims (11)
1. The graphene-based anti-icing/deicing integrated wrinkled film is characterized in that the wrinkled film is obtained by transferring reduced graphene oxide onto a biaxially-oriented acrylic acid VHB 4910 substrate film through dry transfer and retracting the substrate film; then growing SiO on the surface of the reduced graphene oxide by a baby method2Nano particles are finally prepared by modifying the surface with 1H,1H,2H, 2H-perfluorodecyl trichlorosilane; the preparation method comprises the following steps:
transferring a reduced graphene oxide film to a biaxially oriented acrylic acid VHB 4910 substrate film by using a dry method;
step two, releasing the substrate film along one uniaxial direction to enable the substrate film to retract, and then releasing the substrate film along the other uniaxial direction to enable the substrate film to retract to the original size, so as to obtain a reduced graphene oxide wrinkled film;
adding a cationic surfactant into the ammonia water mixed solution, uniformly mixing, then putting the mixture into the reduced graphene oxide wrinkled film obtained in the step two, magnetically stirring the mixture for 5 to 7 hours under the heating of a water bath, then dropwise adding ethyl orthosilicate, keeping the temperature and stirring the mixture after the dropwise adding is finished, and then taking out the mixture and drying the mixture;
step four, dripping 1H,1H,2H, 2H-perfluorodecyl trichlorosilane diluted by n-hexane on the surface of the folded film treated in the step three, and drying to obtain the graphene-based anti-icing/deicing integrated folded film;
wherein the ammonia water mixed solution is prepared from deionized water, absolute ethyl alcohol and ammonia water.
2. The preparation method of the graphene-based integrated anti-icing/deicing pleated membrane as claimed in claim 1, characterized in that the preparation method is realized by the following steps:
transferring a reduced graphene oxide film to a biaxially oriented acrylic acid VHB 4910 substrate film by using a dry method;
step two, releasing the substrate film along one uniaxial direction to enable the substrate film to retract, and then releasing the substrate film along the other uniaxial direction to enable the substrate film to retract to the original size, so as to obtain a reduced graphene oxide wrinkled film;
adding a cationic surfactant into the ammonia water mixed solution, uniformly mixing, then putting the mixture into the reduced graphene oxide wrinkled film obtained in the step two, magnetically stirring the mixture for 5 to 7 hours under the heating of a water bath, then dropwise adding ethyl orthosilicate, keeping the temperature and stirring the mixture after the dropwise adding is finished, and then taking out the mixture and drying the mixture;
step four, dripping 1H,1H,2H, 2H-perfluorodecyl trichlorosilane diluted by n-hexane on the surface of the folded film treated in the step three, and drying to obtain the graphene-based anti-icing/deicing integrated folded film;
wherein the ammonia water mixed solution is prepared from deionized water, absolute ethyl alcohol and ammonia water.
3. The method according to claim 2, wherein the step of reducing the graphene oxide thin film is performed by: diluting the graphene oxide aqueous solution to 0.1mg/mL, vacuum-filtering 3mL of the graphene oxide aqueous solution to a polytetrafluoroethylene film with the diameter of 50mm and the pore diameter of 0.45 mu m, drying at 50 ℃ to obtain a graphene oxide film, putting the graphene oxide film into an HI solution, reducing in an oven at 90-100 ℃ for 1-1.5 h, taking out, putting in an oven at 120 ℃ for 6h, and removing redundant HI on the surface.
4. The method according to claim 3, wherein the graphene oxide is prepared by the following steps:
adding 23mL of 98% concentrated sulfuric acid into a 250mL beaker, cooling to-1 ℃ in an ice bath, adding 1g of natural graphite, stirring for 40-60 min, and adding 6g of KMnO in portions4Stirring for 2.5-3 h, then replacing the ice bath, placing in a constant-temperature water bath at 35-45 ℃, stirring for 40-50 minThe solution begins to become viscous, then the water is stabilized at 40-50 ℃, then the solution is transferred to a constant-temperature water bath kettle at 80 ℃ to be stirred, 80mL of distilled water is added in several times, after the solution is stirred for 10 min-20 min, 60mL of distilled water is added to be diluted, 10.81mL of mixed solution consisting of 30% hydrogen peroxide and 60mL of deionized water is added, the solution becomes golden yellow, and the solution is centrifugally washed by deionized water until the pH value of the solution is 5-6.
5. The method of claim 2, wherein the prestrain of the biaxially oriented acrylic base film of step one is from 300% to 400%.
6. The preparation method of claim 2, wherein 30mg to 50mg of the cationic surfactant is added to the ammonia water mixed solution in the third step, wherein the ammonia water mixed solution is prepared from 40mL of deionized water, 10mL of anhydrous ethanol and 1mL to 2mL of ammonia water.
7. The process according to claim 2 or 6, wherein the cationic surfactant in the third step is cetyltrimethylammonium bromide.
8. The preparation method according to claim 2, wherein the amount of tetraethoxysilane in the step three is 1 mL-2 mL.
9. The method according to claim 2, wherein in the step III, the 1H,1H,2H, 2H-perfluorodecyltrichlorosilane is diluted with n-hexane to a concentration of 1% by mass, and the amount of the 1H,1H,2H, 2H-perfluorodecyltrichlorosilane diluted with n-hexane is 10. mu.L.
10. The preparation method of claim 2, wherein the temperature of the water bath in the third step is 40 ℃ to 45 ℃, and the magnetic stirring speed is 400r/min to 500 r/min.
11. The method of claim 6, wherein the drying is carried out at 40-60 ℃ in the third step.
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| US11958748B2 (en) * | 2019-01-14 | 2024-04-16 | Khalifa University of Science and Technology | 3D reduced graphene oxide/sio2 composite for ice nucleation |
| CN110775962B (en) * | 2019-11-18 | 2022-03-15 | 哈尔滨工业大学 | Preparation method of super-hydrophobic graphene-based wrinkled film capable of controlling water drop resilience direction |
| CN111859663B (en) * | 2020-07-20 | 2022-05-03 | 哈尔滨工业大学 | Design method of anti-icing and deicing coating on large-area coating surface |
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