CN110775962A - Preparation method of super-hydrophobic graphene-based wrinkled film capable of controlling water drop resilience direction - Google Patents
Preparation method of super-hydrophobic graphene-based wrinkled film capable of controlling water drop resilience direction Download PDFInfo
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Abstract
A preparation method of a super-hydrophobic graphene-based wrinkled film capable of controlling the rebound direction of water drops belongs to the field of anti-icing. The invention realizes that the bounce direction of cold water drops can deviate from the surface after the cold water drops are impacted, and greatly improves the anti-icing efficiency. According to the invention, the rGO film is transferred onto a biaxially stretched base film through dry transfer, and forces in four directions of the base film are retracted in sequence to obtain an irregular-fold film; by passing
Method, growing SiO on the surface of rGO
2Nano particles and obtaining SiO with micro-nano hierarchical structure by FDTS modification
2a/rGO pleated membrane. The film of the invention has a water contact angle still larger than 150 degrees at minus 20 ℃, a rolling angle smaller than 4 degrees, and shows excellent low-temperature super-hydrophobic characteristics. Meanwhile, at the temperature of minus 10 ℃, supercooled water drops impact the surface of the film, and the viscous force between the solid and the liquid is asymmetrically distributed due to the irregular microstructure of the supercooled water drops, so that the water drops are asymmetrically retracted, and the rebound direction deviates in the fixed direction.
Description
Technical Field
The invention belongs to the field of anti-icing; in particular to a preparation method of a super-hydrophobic graphite alkenyl corrugated film capable of controlling the rebound direction of water drops. The invention provides a preparation method of a graphene-based irregular folded film with a super-hydrophobic characteristic under a low-temperature condensation condition, and the film can be used for controlling the rebound direction of supercooled water drops after impact.
Background
Ice accretion presents a series of safety, efficiency and economic problems for aircraft, wind turbine blades, solar panels and heat exchangers, etc. Superhydrophobic surfaces are considered one of the ideal strategies in the field of anti-icing because of their good hydrophobicity. At present, research on the application of super-hydrophobic surfaces in the field of ice prevention has made certain progress, and mainly focuses on accelerating resilience of supercooled water droplets, delaying freezing of supercooled water droplets, and reducing solid-liquid ice adhesion. However, the direction of rebound after impingement of supercooled water droplets was less studied. If the water drops bounce along the vertical direction after impacting the super-hydrophobic surface and move repeatedly until the kinetic energy of the water drops is consumed, the water drops finally still stand on the cold super-hydrophobic surface and freeze.
Disclosure of Invention
The rebound direction of supercooled water drops after impacting the superhydrophobic surface has potential significance in the field of ice protection. However, under low temperature condensation conditions, it is still a challenge how to control the rebound direction of impinging water droplets while maintaining the superhydrophobic character of the film surface. The invention realizes that the bounce direction of cold water drops can deviate from the surface after the cold water drops are impacted, and greatly improves the anti-icing efficiency.
The method is prepared by adopting an improved Hummers method, a lamella of natural graphite is opened by using concentrated sulfuric acid as an intercalating agent, potassium permanganate as a strong oxidant and hydrogen peroxide are used for reducing unreacted oxidants to obtain graphene oxide, and hydroiodic acid is used as a reducing agent for reducing the graphene oxide film obtained by suction filtration to obtain the rGO film.
Then transferring the rGO thin film to a biaxially stretched VHB 4910 substrate thin film through dry transfer, and applying a compression force to the graphene thin film through sequential retraction of the substrate thin film in four directions to obtain an irregular rGO corrugated thin film; by passing
Method, growing SiO on the surface of rGO
2Nanoparticles to obtain SiO in micro-nano hierarchical structure
2a/rGO pleated membrane; and finally, modifying the wrinkled film by using low surface energy 1H,1H,2H, 2H-perfluorodecyl trichlorosilane (FDTS) to obtain the ISGF. And characterizing contact angles and rolling angles of the ISGF at room temperature (20 ℃) and different low temperature conditions, and characterizing the dynamic impact process of the supercooled water drops.
The specific scheme is as follows: the preparation method of the super-hydrophobic graphene-based wrinkled film capable of controlling the rebound direction of water drops comprises the following steps:
transferring a reduced graphene oxide (rGO) film to a biaxially stretched acrylic acid base film with the pre-strain of 400% by a dry method, and then sequentially releasing the forces in four directions of the base film to enable the base film to retract so as to obtain an rGO irregular-folded film;
step two, passing
The method comprises the step of growing SiO on the surface of the rGO irregularly-folded film obtained in the step one
2Nanoparticles.
And step three, modifying by using FDTS to obtain the super-hydrophobic graphene-based wrinkled film.
Further defined, the step one of reducing the graphene oxide (rGO) thin film is realized by the following steps:
step 1.1: cooling 23mL of concentrated sulfuric acid with the mass concentration of 98% by using an ice water bath, adding 1g of natural graphite, stirring at 400-600 r/min for 40-60 min, and slowly stirring for several times6g of KMnO were added
4Then stirring for 2.5-3.5 h;
step 1.2: then transferring the mixture into a water bath with the temperature of 35-45 ℃, and mechanically stirring the mixture for 40-50 min at the speed of 600-800 r/min until the solution becomes viscous.
Step 1.3: transferring the solution to a constant-temperature water bath at 70-90 ℃ for mechanical stirring, adding 80mL of distilled water in a small amount and a large amount of distilled water in a plurality of times, 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, changing the solution into golden yellow, centrifugally washing the solution by using deionized water until the pH value of the solution is 5-6, and performing ultrasonic treatment for 30 min to obtain a graphene oxide aqueous solution;
step 1.4: diluting the graphene oxide aqueous solution prepared in the step 1.3 to the concentration of 0.2mg/mL by using deionized water, carrying out vacuum filtration on 5-6 mL of the graphene oxide aqueous solution to a polytetrafluoroethylene film with the diameter of 50mm and the aperture of 0.45 mu m, and drying the polytetrafluoroethylene film in an oven at the temperature of 50-60 ℃ to obtain a GO film; and putting the GO film into HI atmosphere, putting the GO film into an oven at 90-110 ℃ for 2h, taking out the GO film, and putting the GO film into an oven at 120 ℃ to remove redundant HI on the GO film.
To be further limited, KMnO is added in 6 equal portions in step 1.1
4The time interval is 5 min.
Further limiting, adding distilled water for 6 times in the step 1.3, wherein the adding amount of the distilled water for the first 4 times is 5 mL/time to 10 mL/time, and the time interval is 5min to 7 min; the dosage of the last two times is 20 mL/time to 30 mL/time, and the time interval is 1min to 2 min.
And further limiting, in the second step, uniformly mixing 40mL of deionized water, 10mL of anhydrous ethanol and 1 mL-2 mL of ammonia water, adding 80 mg-120 mg of hexadecyl trimethyl ammonium bromide to obtain a mixed solution A, then placing the mixed solution A into an oil bath at 35-45 ℃, placing the irregular folded rGO film obtained in the first step into the mixed solution A, magnetically stirring for 4-6 h, then dropwise adding 1 mL-2 mL of ethyl orthosilicate, continuously stirring for 10-14 h after dropwise adding is finished, taking out, washing with an ethanol water solution, and drying at 50-60 ℃.
Further limiting, the step three of modifying with FDTS is to soak the rGO irregular folded film treated in the step two with a normal hexane solution of FDTS, and then vacuum-drying; wherein the mass concentration of the normal hexane solution of FDTS is 0.8-1.1%; further limiting, the soaking time is 30-50 s; further limiting, vacuum drying for 10-12 h at 50-60 ℃.
The invention provides a super-hydrophobic graphene-based micro-nano hierarchical irregular folded film, which is prepared by modifying silicon dioxide (SiO) by 1H,1H,2H, 2H-perfluorodecyl trichlorosilane (FDTS)
2) The water drop control method is characterized by comprising the following steps of (1) reducing a graphene oxide (rGO) wrinkled film (ISGF), and adjusting the adhesion distribution between a water drop and the film through the irregularity of wrinkles on the surface of the film so as to control the retraction and bounce directions of the water drop. The film has good super-hydrophobic performance and controllable rebound direction of impact liquid drops under the condition of low-temperature condensation, and has important significance in the field of deicing.
The method comprises the steps of sequentially applying compressive force to four edges of the graphene film to obtain the irregular graphene wrinkled film, and recycling
According to the method, a low-surface-energy substance FDTS is used for modification, so that the graphene-based irregular folded film with the super-hydrophobic micro-nano hierarchical structure is obtained, and the super-hydrophobic characteristic of the film is kept at a low temperature by utilizing the synergistic effect of micro graphene folds and nano silicon dioxide particles; meanwhile, due to the structural asymmetry, the super-cooled water drops are asymmetric in adhesion force between solid and liquid after being impacted at low temperature, so that the impacting water drops are not retracted uniformly, the bouncing direction of the impacting water drops is deviated, the deviation direction of the water drops can be controlled by rotating the angle of the film, and the bouncing direction of the water drops is controllable.
The film prepared by the method has a water contact angle of more than 150 degrees and a rolling angle of less than 4 degrees even at the temperature of-20 ℃, and shows excellent super-hydrophobic characteristics. Meanwhile, at the temperature of minus 10 ℃, supercooled water drops impact the surface of the film, and the viscous force between the solid and the liquid is asymmetrically distributed due to the irregular microstructure of the supercooled water drops, so that the water drops are asymmetrically retracted, and the rebound direction deviates in the fixed direction.
Drawings
FIG. 1 SEM image of ISGF;
FIG. 2 shows contact and rolling angles of a water drop on ISGF at different temperatures;
fig. 3 shows the dynamic process of super-cooled water droplets impacting the surface of the ISGF.
Detailed Description
Example 1: the preparation method of the super-hydrophobic graphene-based wrinkled film capable of controlling the rebound direction of water drops comprises the following steps:
1. preparation of graphene oxide
The preparation is divided into three stages: and (3) a low-temperature reaction stage: 23mL of concentrated sulfuric acid having a mass concentration of 98% was added to a 250mL beaker, and cooled in an ice-water bath. Then adding 1g of natural graphite, stirring at 500r/min for 60min, slowly adding 6g of KMnO in 6 times with equal amount (5 min time interval)
4And stirring for 3.0 h. A medium-temperature reaction stage: the beaker was transferred to 40 ℃ and the solution started to thicken after mechanical stirring at 600r/min for 40min, finally the temperature in water stabilized at 40 ℃. A high-temperature reaction stage: transferring the graphene oxide solution to a 80-DEG C constant-temperature water bath pot, mechanically stirring, adding distilled water for 6 times, adding 8 mL/time of the first 4 times of the distilled water, stirring for 15min, adding 60mL of distilled water for dilution, adding 10.81mL of a mixed solution consisting of 30% hydrogen peroxide and 60mL of deionized water, centrifuging and washing the solution until the pH value of the solution is 5-6, and performing ultrasonic treatment for 30 min to obtain the graphene oxide aqueous solution, wherein the time interval is 6min, the dosage of the second two times of the distilled water is 20 mL/time, and the time interval is 2 min.
2. Preparation of reduced graphene oxide (rGO) thin films
Diluting the graphene oxide aqueous solution prepared in the step 1 until the concentration of the graphene oxide is 0.2mg/mL, vacuum-filtering 5mL of the aqueous solution onto a polytetrafluoroethylene film with the diameter of 50mm and the aperture of 0.45 mu m, and drying in an oven at 50-60 ℃ to obtain a GO film; and putting the GO film into HI atmosphere, putting the GO film into an oven at 90-110 ℃ for 2h, taking out the GO film, and putting the GO film into an oven at 120 ℃ to remove redundant HI on the GO film.
Preparation of ISGF
Preparing an rGO irregular pleated film: transferring the rGO film to a biaxially stretched acrylic base film with the pre-strain of 400% by a dry method, and sequentially releasing the forces in four directions of the base film to enable the base film to retract to the original size to obtain the irregular-folded rGO film.
SiO
2Preparation of/rGO micro-nano graded irregular-folded film: weighing 40mL of deionized water, 10mL of anhydrous ethanol and 1mL of ammonia water, uniformly mixing, weighing 100mg of hexadecyl trimethyl bromide, adding into the mixed solution, putting into an oil bath at 35-45 ℃, putting the rGO irregular folded film into the mixed solution, magnetically stirring for 5 hours, then dropwise adding 1mL of ethyl orthosilicate, continuously stirring for 12 hours after dropwise adding, taking out, cleaning with 20mL of mixed solution of ethanol and aqueous solution with the volume ratio of 1:1, and drying at 50 ℃.
Preparing an ISGF irregular-pleated film: mixing FDTS with n-hexane, preparing 1.0% FDTS n-hexane solution, and mixing with SiO
2And soaking the rGO irregular pleated film in the mixed solution for 30s, taking out the rGO irregular pleated film, and putting the rGO irregular pleated film into a vacuum oven at 50 ℃ for 12h to obtain the ISGF irregular pleated film.
The shape of the ISGF irregular pleated film prepared in this example is shown in the scanning electron microscope picture of fig. 1, and the inset in the lower left corner is an enlarged view of this structure. The white particles in the figure are SiO
2Nanoparticles, and meanwhile, the folds are irregular structures and the size is in a micron level, so that the prepared ISGF is a graphene-based irregular fold film with a micro-nano hierarchical structure.
The relative humidity is 50 +/-5%, and the Water Contact Angle (WCA) and the rolling angle (SA) of the ISGF surface under different temperatures (-20 ℃) are shown in figure 2, and it can be seen that when the temperature is reduced to-20 ℃, the contact angle is still larger than 150 ℃ and the rolling angle is smaller than 4 ℃, which indicates that the film keeps good super-hydrophobic property at low temperature.
When the surface temperature of the film is-10 ℃ and the relative humidity of air is 50 +/-5%, the dynamic impact process of 4.2 mu L of water drops falling freely from a height of 50mm to impact the super-hydrophobic surface is shown in figure 3, a green dotted line is a falling symmetry axis of the water drops, and as can be known from the figure, the retraction of the water drops is not uniform along the symmetry axis, the retraction speed of the water drops on the left side of the symmetry axis is higher than that on the right side, so that the phenomenon of deviation towards the right side occurs (figure 3 a). Meanwhile, the film is marked with a marker pen, and when the film is rotated by 90 ° clockwise, the water drop bounces off and is deviated to the marking direction (fig. 3b), so that the water drop bouncing direction can be controlled by rotating the film direction.
Claims (9)
1. A preparation method of a super-hydrophobic graphene-based wrinkled film capable of controlling the rebound direction of water drops is characterized by comprising the following steps:
transferring a reduced graphene oxide (rGO) film to a biaxially stretched acrylic acid base film with the pre-strain of 400% by a dry method, and then sequentially releasing the forces in four directions of the base film to enable the base film to retract so as to obtain an rGO irregular-folded film;
step two, passing
The method comprises the step of growing SiO on the surface of the rGO irregularly-folded film obtained in the step one
2Nanoparticles.
And step three, modifying by using FDTS to obtain the super-hydrophobic graphene-based wrinkled film.
2. The method for preparing the superhydrophobic graphene-based wrinkled film capable of controlling the water drop rebound direction of the water drops as claimed in claim 1, wherein the step of reducing the graphene oxide (rGO) film is realized by the following steps:
step 1.1: cooling 23mL of concentrated sulfuric acid with the mass concentration of 98% in an ice water bath, adding 1g of natural graphite, stirring at 400-600 r/min for 40-60 min, and slowly adding 6g of KMnO in batches
4Then stirring for 2.5-3.5 h;
step 1.2: then transferring the mixture into a water bath with the temperature of 35-45 ℃, and mechanically stirring the mixture for 40-50 min at the speed of 600-800 r/min until the solution becomes viscous.
Step 1.3: transferring the solution to a constant-temperature water bath at 70-90 ℃ for mechanical stirring, adding 80mL of distilled water in a small amount and a large amount of distilled water in a plurality of times, 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, changing the solution into golden yellow, centrifugally washing the solution by using deionized water until the pH value of the solution is 5-6, and performing ultrasonic treatment for 30 min to obtain a graphene oxide aqueous solution;
step 1.4: diluting the graphene oxide aqueous solution prepared in the step 1.3 to the concentration of 0.2mg/mL by using deionized water, carrying out vacuum filtration on 5-6 mL of the graphene oxide aqueous solution to a polytetrafluoroethylene film with the diameter of 50mm and the aperture of 0.45 mu m, and drying the polytetrafluoroethylene film in a 50-DEG C oven to obtain a GO film; and putting the GO film into HI atmosphere, putting the GO film into an oven at 90-110 ℃ for 2h, taking out the GO film, and putting the GO film into an oven at 120 ℃ to remove redundant HI on the GO film.
3. The method for preparing the superhydrophobic graphene-based wrinkled film capable of controlling the water drop rebound direction as claimed in claim 2, wherein KMnO is added in 6 times in step 1.1
4The time interval is 5 min.
4. The method for preparing the superhydrophobic graphene-based pleated membrane capable of controlling the water drop rebound direction according to claim 2, characterized in that distilled water is added in 6 times in step 1.3; the adding amount of the first 4 times is 5 mL/time to 10 mL/time, the time interval is 5min to 7min, and the using amount of the last two times is 20 mL/time to 30 mL/time each time; the time interval is 1 min-2 min.
5. The preparation method of the superhydrophobic graphene-based wrinkled film with the controllable water drop resilience direction according to claim 1, wherein in the second step, 40mL of deionized water, 10mL of anhydrous ethanol and 1 mL-2 mL of ammonia water are uniformly mixed, 80 mg-120 mg of hexadecyl trimethyl ammonium bromide is added to obtain a mixed solution A, then the mixed solution A is placed in an oil bath at the temperature of 35 ℃ to 45 ℃, the irregular wrinkled film obtained in the first step is placed in the mixed solution A to be magnetically stirred for 4 h-6 h, then 1 mL-2 mL of ethyl orthosilicate is dropwise added, stirring is continued for 10 h-14 h after the dropwise addition is finished, the irregular wrinkled film is taken out and washed by an ethanol water solution, and the wrinkled film is dried at the temperature of 50 ℃ to 60 ℃.
6. The method for preparing the superhydrophobic graphene-based wrinkled film with the controllable water drop rebound direction according to the claim 1, wherein the step three of modifying with FDTS is that the rGO irregular wrinkled film treated in the step two is soaked in a normal hexane solution of FDTS for 30s and then dried in vacuum.
7. The method for preparing the superhydrophobic graphene-based wrinkled film capable of controlling the rebounding direction of water drops as claimed in claim 6, wherein the mass concentration of the n-hexane solution of FDTS is 0.8% -1.1%.
8. The method for preparing the superhydrophobic graphene-based wrinkled film capable of controlling the rebounding direction of water drops as claimed in claim 6, wherein the soaking time is 30-50 s.
9. The method for preparing the superhydrophobic graphene-based wrinkled film capable of controlling the rebounding direction of water drops as claimed in claim 6, wherein the superhydrophobic graphene-based wrinkled film is vacuum dried at 50-60 ℃ for 10-12 h.
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| CN114323852A (en) * | 2021-12-27 | 2022-04-12 | 山东大学 | Preparation method and application of laser-induced graphene without pinning effect |
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| CN111807356B (en) * | 2020-06-24 | 2023-02-10 | 哈尔滨工业大学 | Preparation method of graphene-based wrinkled film with anti-icing and sensing characteristics |
| CN114323852A (en) * | 2021-12-27 | 2022-04-12 | 山东大学 | Preparation method and application of laser-induced graphene without pinning effect |
| CN114323852B (en) * | 2021-12-27 | 2023-08-29 | 山东大学 | Preparation method and application of laser-induced graphene without pinning effect |
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