CN109627905B - Multifunctional coating with self-cleaning, anti-icing and microwave absorbing functions and preparation method thereof - Google Patents
Multifunctional coating with self-cleaning, anti-icing and microwave absorbing functions and preparation method thereof Download PDFInfo
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Abstract
A multi-functional coating with self-cleaning, anti-icing and microwave absorption belongs to the technical field of coatings, and can solve the problems that the existing microwave absorption coating has low wave-absorbing performance and cannot realize self-cleaning and anti-icing, and the invention comprises the following steps: respectively synthesizing nano particle oily dispersion liquid with low surface energy and Fe3O4the/rGO/PANI/resin composite coating is sprayed on a substrate by Fe3O4the/rGO/PANI/resin composite coating and the low-surface-energy nano particle oily dispersion liquid obtain the self-cleaning and anti-icing microwave absorption coating, compared with the traditional microwave absorption coating, the self-cleaning and anti-icing coating has more excellent absorption performance, excellent self-cleaning and anti-icing performance, can be prepared in a large-scale controllable manner, and has wide application prospects in the two fields of military and civilian.
Description
Technical Field
The invention belongs to the technical field of coatings, and particularly relates to a multifunctional coating with self-cleaning, anti-icing and microwave absorption functions and a preparation method thereof.
Background
With stealth technology and microwave weapons, radar and electronic countermeasures have increased in military battles, and research and application of microwave absorbing materials have become more and more important. In modern battlefields, airplanes and missiles of different models use microwave absorbing materials, so that the effective reflecting surface of the airplanes and the missiles can be reduced by 90%, and the radar power is greatly reduced. Ground weapons such as tanks, armored vehicles and artillery use wave-absorbing materials to hide, so that electronic reconnaissance of enemies, including satellite reconnaissance and ground electronic reconnaissance, can not effectively play a role. The development of a broadband high-performance and light thin-layer microwave absorbing material and the close combination of the material and the performance improvement of military weaponry have great influence on the improvement of the battle of troops; the high-power absorption material with good electromagnetic parameter temperature stability and absorption characteristics is developed and applied to the design and manufacture of microwave terminals and microwave weapon power detection systems, and is of great significance to the improvement of the performance of the existing industry float industry equipment.
In recent years, many reports have been made on nano microwave absorbing materials, and a nano microwave absorbing powder material having high performance in a wide frequency band has also been obtained, but the application thereof is very few. The main source is that the existing microwave absorption coating based on the nanometer microwave absorption powder also has the problem that the bandwidth and the thickness are difficult to simultaneously optimize. In addition, the existing microwave absorbing coating is easy to freeze and fall dust on the surface, which can reduce the performance of the microwave absorbing coating. These problems greatly limit the engineered application of nano-microwave absorbing coatings and increase the maintenance costs of the coatings.
The super-hydrophobic coating is in water, a gasification film is easily formed on the interface of the super-hydrophobic coating and an aqueous medium, dust can be prevented from entering the coating due to irregular movement of molecules after falling on the surface of the coating to influence the microwave absorption performance of the coating, the excellent super-hydrophobic performance enables the coating to have self-cleaning performance, and the dust falls on the surface of the coating and is still as before after being blown by wind and washed by rainwater, so that the super-hydrophobic coating and the microwave absorption coating are compounded, and the multifunctional coating with self-cleaning, anti-icing and microwave absorption is expected to be prepared. However, it is only reported that the multifunctional coating with self-cleaning, anti-icing and microwave absorption functions has a key technology in the preparation of the bifunctional coating, which is how to endow the microwave absorption coating with super-hydrophobic characteristics, and simultaneously, the microwave absorption performance is not influenced. The construction of micro-nano structures on the surface of a coating is the most effective way to realize super-hydrophobicity, such as the construction of porous or array structures on the surface of metal by adopting an aqueous solution chemical method, a chemical or laser etching method, a hydrothermal method, an anodic treatment method, an electrochemical deposition method, a sol-gel method, a nano composite coating method, a template method and the like. The porous or array structure is found to have excellent super-hydrophobic characteristics, but because the porous or array structure has large roughness and low mechanical strength, the porous or array structure is easily damaged when being acted by the outside, and the hydrophobic property of the porous or array structure is reduced. In addition, the preparation method of the super-hydrophobic coating or the microwave absorbing coating in the earlier stage mostly has the defects of expensive equipment, poor repeatability, complex process and the like, and is only suitable for experimental research and cannot be used for large-scale preparation. Therefore, how to develop a preparation method of the multifunctional coating which is simple to operate, can be applied in a large scale, has stable performance, and has self-cleaning, anti-icing and microwave absorption functions has important value and significance.
Disclosure of Invention
The invention provides a multifunctional coating with self-cleaning, anti-icing and microwave absorption functions and a preparation method thereof, aiming at the problems of complex preparation method and unstable performance of the existing composite coating with microwave absorption performance, self-cleaning function and anti-icing function.
The invention adopts the following technical scheme:
a multifunctional coating with self-cleaning, anti-icing and microwave absorption functions comprises an outer coating and an inner coating which are sequentially sprayed on a metal substrate from outside to inside, wherein the outer coating is a nano particle assembled film with low surface energy, and the inner coating is Fe3O4the/rGO/PANI/resin doped composite membrane.
A preparation method of a multifunctional coating with self-cleaning, anti-icing and microwave absorption functions comprises the following steps:
first, preparation of a nanoparticle oil dispersion with low surface energy
a. Weighing 4-6 g of NaOH and dissolving in 92.5mL of deionized water to prepare NaOH solution for later use, and weighing 2.86-4.29 g of FeCl2·4H2O and 4.864-7.296 g of FeCl3·6H2Dissolving O in 70-110 mL of deionized water, ultrasonically dispersing into a uniform solution, transferring the solution into a flask for heating, when the temperature is raised to 40-60 ℃, dropwise adding NaOH solution into the flask at the rate of 1 drop/second, continuing to react for 1.5 hours at the temperature of 40-60 ℃ after dropwise adding is finished, cooling to 25 ℃ after the reaction is finished, ultrasonically washing the solution for a plurality of times by using deionized water to obtain magnetic particles, ultrasonically dispersing the magnetic particles into 250-350 mL of water/ethanol solution with the volume ratio of 1:4 to obtain stable Fe3O4A dispersion liquid;
b. 250mL of Fe was taken3O4Adding 10ml ammonia water into the dispersion, stirring and dispersing for 1h, dropwise adding 4ml ethyl silicate in the stirring process, then stirring for 6h at 25 ℃, precipitating by magnetic adsorption, washing with ethanol and distilled water to obtain Fe3O4@SiO2Core-shell structured composite nanoparticles of Fe3O4@SiO2Ultrasonically dispersing the core-shell structure composite nano particles in 150ml of deionized water to obtain Fe3O4@SiO2A core-shell structure composite nanoparticle dispersion;
c. 120mL of Fe was taken3O4@SiO2Adding 1-4 g of urea, 2-6 g of cationic surfactant, 4-10 mL of 1-pentanol, 100-150 mL of cyclohexane and 10g of ethyl silicate in turn into core-shell structure composite nanoparticle dispersion liquid, stirring for 0.5-6h at 25 ℃ to obtain a mixed solution, transferring the mixed solution into a reaction kettle, reacting for 5h at 110-150 ℃, cooling to 25 ℃, performing magnetic adsorption precipitation, washing with water and ethanol, and drying to obtain Fe3O4@SiO2/organic composite nanoparticles of Fe3O4@SiO2Dispersing organic composite nano particles in 150ml of toluene solution to obtainFe3O4@SiO2Organic composite nano particle toluene dispersion;
d. 100mL of Fe was weighed3O4@SiO2Adding 30-50 mL of l-octyl trimethoxy siloxane into organic composite nanoparticle toluene dispersion, performing reflux reaction at 120 ℃ for 20-48 h, performing magnetic adsorption precipitation, and washing with toluene and xylene to obtain Fe3O4@H-SiO2/organic composite nanoparticles of Fe3O4@H-SiO2Performing ultrasonic dispersion on organic composite nanoparticles in a solvent to obtain a low-surface-energy nanoparticle oily dispersion liquid with the solid content of 10.0-25.0 wt%;
second step, Fe3O4Preparation of/rGO/PANI/resin composite coating
a. Dissolving 0.01M aniline in 10mL hydrochloric acid solution with the concentration of 1M, performing ultrasonic dispersion for 15min to obtain mixed solution A, dissolving 0.01M ammonium persulfate in 10mL hydrochloric acid solution with the concentration of 1M, performing ultrasonic dispersion for 15min to obtain mixed solution B, pouring the mixed solution B into the mixed solution A, stirring for 2h at 20 ℃, obtaining a dark green solution after the reaction is finished, filtering the dark green solution to obtain a filtrate, washing for several times with water and methanol until the washing liquid is colorless, and dissolving the washed filtrate in deionized water to obtain PANI solution with the mass fraction of 1wt% -3 wt%;
b. measuring 10mL of 80% hydrazine hydrate and 20mL of absolute ethanol, and uniformly mixing to obtain a hydrazine hydrate mixed solution for later use; respectively measuring 400mL of 2.5mg/mL graphene oxide aqueous solution and 0.5g of polyvinylpyrrolidone, adding the graphene oxide aqueous solution and the polyvinylpyrrolidone into a beaker, uniformly dispersing by ultrasound, transferring the mixture into the flask, starting heating, starting dropwise adding a hydrazine hydrate mixed solution into the flask when the temperature reaches 80 ℃, reacting for 3 hours after the dropwise adding is finished, and cooling to 25 ℃ after the reaction is finished to obtain an rGO dispersion liquid; respectively adding 20-40 ml of Fe into 100-150 ml of rGO dispersion liquid3O4Adding a surface modifier into the dispersion liquid and 30-60 ml of PANI solution at the temperature of 50-85 ℃, and reacting for 2-6 h to obtain Fe3O4An aqueous solution of/rGO/PANI composite magnetic particles;
c. adsorbing Fe by magnet3O4Aqueous solution of/rGO/PANI composite magnetic particles to make Fe3O4precipitating/rGO/PANI composite magnetic particles, and then washing with absolute ethyl alcohol for 3-5 times to obtain Fe3O4(rGO/PANI) magnetic particle slurry, mixing Fe3O4adding/rGO/PANI magnetic particle slurry into resin, and dispersing for 1.0h under stirring at the rotating speed of 1000-1500 rpm to obtain Fe with the concentration of 5-35 wt%3O4a/rGO/PANI/resin composite coating;
thirdly, preparing the multifunctional coating with self-cleaning, anti-icing and microwave absorbing functions
Mixing Fe3O4the/rGO/PANI/resin composite coating is uniformly sprayed on the surface of a metal substrate to serve as an inner coating, the metal substrate is placed in a 60 ℃ oven for 30-120 min, when the surface of the inner coating is not completely cured, the nano particle oil dispersion liquid with low surface energy is uniformly sprayed on the outer coating, and after further curing, the multifunctional coating with self-cleaning, anti-icing and microwave absorption functions is obtained.
In the first step, the cationic surfactant in step c is any one of cetyltrimethylammonium bromide, dodecyltrimethylammonium bromide, tetradecyltrimethylammonium bromide, octadecyltrimethylammonium bromide and cetylpyridinium bromide.
In the first step, step d, the solvent is ethyl acetate or xylene.
In the second step, the surface modifier in step b is any one of KH550, KH560, KH570, sodium dodecyl sulfonate, sodium dodecyl benzene sulfonate and cetyltrimethylammonium bromide.
In the step c of the second step, the resin is any one of 30.0 to 45.0wt% of epoxy resin, polyurethane resin and tetrafluoroethylene resin.
In the third step, the spraying pressure of the inner coating is 0.1 MPa-0.25 MPa, and the spraying pressure of the outer coating is 0.25 MPa-0.35 MPa.
In the third step, the further curing mode is curing in an oven at 60.0 ℃ for 4.0 to 8.0 hours or curing at 25 ℃ for 20.0 hours.
In the invention, the key technology for preparing the low-surface-energy nanoparticle oily dispersion liquid is to obtain the low-surface-energy nanoparticles with good structural stability, and simultaneously have good stability and dispersibility in a non-polar solvent. In view of the above requirements, the present application makes some corresponding innovations and improvements in several aspects, compared to the conventional low surface energy nanoparticle preparation process: in the preparation process of the particles, the particle size, the structure and the dosage of the surfactant and the dispersion concentration are controlled to improve the stability and the dispersibility of the particles in a non-polar solvent; secondly, in the whole preparation process, a wet transfer method is adopted to purify and disperse the particles, so that the particles are prevented from forming secondary agglomeration in the drying process, the stability and the dispersibility of the particles in a non-polar solvent are influenced, and the particles are not beneficial to re-modification; in addition, the synthesis process is controlled, proper low-surface-energy organic molecules are selected, and the organic molecules are modified on the surfaces of the nanoparticles by adopting a general chemical grafting method, so that the stable nanoparticles with low surface energy are obtained.
Fe3O4The key technology for preparing the/rGO/PANI/resin composite coating lies in how to obtain Fe with good dispersibility3O4the/rGO/PANI magnetic particles avoid secondary agglomeration of the magnetic particles in the drying process. In view of the above requirements, in the present application, Fe3O4Magnetic nanoparticles and rodlike PANI are loaded on the surface of the modified reduced graphene oxide sheet layer, and Fe3O4And PANI loading avoids the formation of agglomerates between graphene sheets and is difficult to re-disperse.
The key technology for preparing the multifunctional coating with self-cleaning, anti-icing and microwave absorption is to obtain a super-hydrophobic surface with stable structure and simultaneously prepare the coating stably in a large area. According to the traditional nano doping method, super-hydrophobicity is realized by utilizing the high thickness constructed on the surface of the coating by the high-concentration nano particles, although the method can be used for large-area preparation by adopting a spraying method, the repeated preparation stability is poor, the adhesive force between the coating and a substrate is poor, the coarse structure is easy to damage, the super-hydrophobicity is lost, and the application of the super-hydrophobicity is greatly limited. In order to solve the problems, the patent develops a super-hydrophobic coating with a novel structure, which not only has excellent super-hydrophobicity, mechanics and stable repeated preparation, but also can be prepared in a large area by adopting a spraying method.
The invention has the following beneficial effects:
1. the invention designs a composite coating with self-cleaning, anti-icing and microwave absorbing functions, which has more excellent super-hydrophobic characteristics, wherein the contact angle is more than 169 degrees, and the rolling angle is less than 2 degrees.
2. The composite coating with the functions of self-cleaning, anti-icing and microwave absorption is designed and prepared by the invention, the composite coating can be prepared in a large area by adopting a spraying method, the super-hydrophobicity mainly comes from the low surface energy of surface nano particles, the dependence on the surface roughness is small, and the repeated preparation stability of the coating is good.
3. The composite coating with the functions of self-cleaning, anti-icing and microwave absorption is prepared, the curing condition of the coating is easy to control, the coating can be cured under the heating condition or the room temperature (25 ℃), and the composite coating is more suitable for large-scale preparation in the outdoor real environment.
4. The composite coating with the functions of self cleaning, anti-icing and microwave absorption is prepared, the nano particles are directly sprayed on the surface of the coating which is not completely cured, the particles are stably embedded on the surface of the coating along with the further curing of the coating, the nano particles are bonded by the microwave absorption coating, the surface particle structure is stable, a 100g weight is loaded, the parallel movement is carried out for 10cm, the cycle is carried out for 100 times, the contact angle is still larger than 165 degrees, and the composite coating has excellent mechanical stability.
5. When the thickness of the coating is 2mm, the minimum reflection loss of the composite coating reaches-32.5 dB at the frequency of 9.47 GHz. The effective wave-absorbing bandwidth of [ RL < -10 dB ] is 13.93GHz [4.07-18 ].
Drawings
FIG. 1 shows highly dispersed Fe prepared in example 1 of the present invention3O4And Fe3O4@H-SiO2XRD pattern of/CTAB nano particle, a is high dispersion Fe3O4XRD pattern of (b) is Fe3O4@H-SiO2CTAB nanoparticlesXRD pattern of (a);
FIG. 2 is a diagram of a coated object prepared in example 2 of the present invention;
FIG. 3 shows Fe prepared according to an example of the present invention3O4@H-SiO2SEM image of/CTAB nanoparticles, wherein A is Fe of the silane-modified fibrous core-shell structure of example 13O4@H-SiO2SEM image of/CTAB nanoparticles, B being Fe of the silane-modified, fibrous core-shell structure of example 23O4@H-SiO2SEM image of/CTAB nanoparticles;
FIG. 4 is a graph of the microwave absorption energy of the coating prepared in example 3 of the present invention;
FIG. 5 is a graph representing the mechanical stability of a coating prepared in example 3 of the present invention;
FIG. 6 is a self-cleaning performance characterization of the coating prepared in example 4 of the present invention;
FIG. 7 is a graph representing the anti-icing performance of a coating prepared in example 4 of the present invention;
FIG. 8 is a schematic structural view of the self-cleaning and microwave absorbing dual-function coating of the present invention, wherein: 1-a metal substrate; 2-a resin; 3-Fe3O4a/rGO/PANI composite particle; 4-low surface energy nanoparticles.
Detailed Description
Example 1
A preparation method of a multifunctional coating with self-cleaning, anti-icing and microwave absorption functions comprises the following steps:
first, preparation of a nanoparticle oil dispersion with low surface energy
a. 5g of NaOH is weighed and dissolved in 92.5mL of deionized water to prepare a uniform solution for later use. 3.5g of ferrous chloride tetrahydrate (FeCl) was weighed2·4H2O) and 6.5g of iron chloride hexahydrate (FeCl)3·6H2O), dissolving in deionized water, transferring to a flask after ultrasonic dispersion to a uniform solution, starting to dropwise add NaOH solution when the temperature reaches 65 ℃, the dropwise adding rate is 1 drop/second, reacting for 1.5h after the dropwise addition is finished, cooling to room temperature after the reaction is finished, ultrasonically washing with deionized water for multiple times, and finally ultrasonically dispersing magnetic particles in water/ethylene glycolAlcohol solution (V)Water (W)/VEthanolIn =1:4), stable Fe is prepared3O4Dispersion (8.0 mg/ml);
b. at 250.0ml Fe3O4Adding 10ml of ammonia water into the dispersion, stirring and dispersing for 1h, dropwise adding 4ml of ethyl silicate in the stirring process, stirring and reacting for 6h at room temperature, removing the reaction solution through magnetic adsorption precipitation, and washing with ethanol and distilled water. To obtain Fe3O4@SiO2Core-shell structured composite nanoparticles of Fe3O4@SiO2Ultrasonically dispersing the core-shell structure composite nano particles in an aqueous solution to obtain Fe3O4@SiO2Core-shell structure composite nanoparticle dispersion (16.7 mg/ml);
c. at 120ml Fe3O4@SiO2Sequentially adding the core-shell structure composite nanoparticle dispersion liquid: 2.5g urea, 4g hexadecyl trimethyl ammonium bromide, 7ml 1-pentanol, 100ml cyclohexane and 10g ethyl silicate, stirring and dispersing for 2h at 25 ℃, then transferring the mixed solution into a reaction kettle for reaction for 5h at 130 ℃, cooling to room temperature, fully washing the precipitate by magnetic adsorption with water and ethanol, and drying Fe3O4@SiO2Dispersing organic composite nano particles in a toluene solution to prepare Fe3O4@SiO2Organic composite nano particle toluene dispersion (0.2 g/ml);
d. in 100ml Fe3O4@SiO2Adding 35ml of n-octyl trimethoxy siloxane into the organic composite nanoparticle toluene dispersion, then carrying out reflux reaction for 30 hours at 120 ℃, using magnetic adsorption to precipitate, and fully washing with toluene and xylene. Mixing Fe3O4@H-SiO2The organic composite nano particles are ultrasonically dispersed in dimethylbenzene to obtain nano particle oily dispersion liquid with low surface energy, and the solid content is 15.0 wt%;
second step, Fe3O4Preparation of/rGO/PANI/resin composite coating
a. Dissolving 0.01M (931 mg) aniline in 10ml 1M hydrochloric acid solution, and ultrasonically dispersing for 15min to form a uniform mixed solution (marked as A); 0.01M (2.282 g) ammonium persulfate was also dissolved in 10ml of 1M hydrochloric acid solution and dispersed by sonication to form a homogeneous mixed solution (denoted as B). The solution B is poured into the solution A and stirred vigorously by magnetic force for 2h at 20 ℃. After completion of the reaction, the resulting dark green solution was filtered and washed with water and methanol until the filtrate became colorless to remove excess ammonium persulfate and aniline oligomers. Then dissolving the washed sample in deionized water to obtain a PANI solution with the mass fraction of 1.62 wt%;
b. 400mL of 2.5mg/mL GO (graphene oxide) aqueous solution is weighed, 0.5g of PVP (polyvinylpyrrolidone) is weighed and added into a clean 500mL beaker, the mixture is transferred into a three-neck flask after being uniformly dispersed by ultrasound, and the mixture is heated in a water bath and stirred. 10mL of hydrazine hydrate (80%) is weighed and mixed evenly with 20mL of absolute ethyl alcohol for later use. And (3) dropwise adding the hydrazine hydrate mixed solution when the water bath temperature reaches 80 ℃, reacting for 3 hours after the dropwise adding is finished, cooling to 25 ℃ after the reaction is finished, and transferring to a bottle for storage. Adding 25ml of self-made Fe into 150ml of rGO dispersion liquid3O4The dispersion (8.0 mg/ml) and 30ml of the stable PANI rod-like dispersion prepared by the above method were reacted at 50 ℃ for 3 hours with a surface modifier to obtain Fe3O4An aqueous solution of/rGO/PANI composite magnetic particles;
c. mixing Fe3O4Fe adsorbed by magnet in aqueous solution of/rGO/PANI composite magnetic particles3O4precipitating/rGO/PANI magnetic particles, and washing with anhydrous ethanol for 3-5 times to obtain Fe3O4Adding the slurry into epoxy resin (30 wt%), and dispersing for 1.0h under high-speed electric stirring (1000 rpm) to obtain Fe3O4a/rGO/PANI/resin (15 wt%) composite coating;
thirdly, preparing the multifunctional composite coating with self-cleaning, anti-icing and microwave absorbing functions and a double-layer inclusion structure
Mixing the prepared Fe3O4the/rGO/PANI/resin coating is evenly sprayed on the surface of the metal substrate (the spraying pressure is 0.1 MPa), and the coating is put in an oven at 60.0 ℃ for solidificationDissolving for 1.0h, when the surface of the coating is not completely cured, uniformly spraying the prepared low-surface-energy nano particle coating on the surface of the coating (the spraying pressure is 0.25 MPa), putting the coating into a 60.0 ℃ oven, and continuously curing for 5h or naturally curing for 20.0h at room temperature to obtain the multifunctional composite coating with a double-layer inclusion structure and self-cleaning, anti-icing and microwave absorbing functions.
As can be seen from a in FIG. 1, the characteristic diffraction peak of XRD appears at 2θ=18.2 °, 29.9 °, 35.4 °, 37.1 °, 43.0 °, 53.3 °, 56.9 °, 62.6 °, and 74.1 ° for Fe3O4The (111), (220), (311), (400), (422), (511), (440), and (533) crystal planes of (c). (b) In 2θOccurrence of SiO =21.5 °2The amorphous diffraction peak well indicates the successful preparation of the core-shell structure Fe3O4@ H-SiO2/CTAB nano particle.
Example 2
The first step in example 1, 3.5g of ferrous chloride tetrahydrate (FeCl 2 & 4H 2O) was changed to 4.0g of ferrous chloride tetrahydrate (FeCl 2 & 4H 2O). 3g of urea and 5g of cetyltrimethylammonium bromide were changed to 2g of urea and 4g of tetradecyltrimethylammonium bromide and 35ml of n-octyltrimethoxysilane were changed to 45ml of n-octyltrimethoxysilane.
The remaining steps were the same as in example 1.
From FIG. 3, it can be seen that the size of the core-shell structure Fe3O4/H-SiO2/CTAB nanoparticles is reduced.
Example 3
The second step in example 1 of Fe3O4/rGO/PANI magnetic particle/resin composite coating preparation was changed from 150ml rGO dispersion to 200ml rGO dispersion and 30ml rod-like stable PANI dispersion to 20ml rod-like stable PANI dispersion. The content of the Fe3O4/rGO/PANI composite magnetic particles is changed from 15.0wt% to 20.0 wt%. The remaining steps were the same as in example 1.
As can be seen from fig. 4, the coating layer of the double inclusion structure has excellent microwave absorption performance.
FIG. 5 shows that the contact angle of the coating is still 168 degrees after a coating is pulled by a weight loaded with 100g on sandpaper, the coating moves 10cm each time and is circulated for 10 times to have a total length of 100cm, and the performance of the coating is not changed after the coating is subjected to cyclic friction, which indicates that the coating has good mechanical resistance. As can be seen from fig. 5, the composite coating with the double-layer inclusion structure exhibits very good mechanical stability and still has very high superhydrophobic performance after friction.
Example 4
In the third step of example 1, the solid content of the resin epoxy resin is changed to 40wt%, the spraying pressure of Fe3O 4/rGO/PANI/organic composite coating is changed to 0.2 MPa from 0.1MPa, the spraying pressure of the low-surface-energy nano particles is changed to 0.35MPa, and the curing at 60 ℃ is changed to the curing at room temperature (25 ℃).
FIG. 6 shows the process of loading dust on the coating and washing with water, wherein the surface of the coating is clean and free of any dust and impurities in the initial coating in the graph A, and the surface of the coating is loaded with dust in the graph B, and the surface of the coating is restored as before in the graph F after C, D, E water drops roll off and take away the dust. This procedure shows that the coating has excellent self-cleaning properties. As can be seen from fig. 6, the composite coating of the double-layer inclusion structure has excellent self-cleaning performance.
Spraying the surface of the coating with the double-layer inclusion structure and the EP/CMP coating prepared in the embodiment respectively, spraying the coating for 1 minute every 10 minutes, and after 15 minutes, seeing that the surface of the composite coating with the double-layer inclusion structure is not loaded with small water drops from A in figure 7, and the surface of the EP/CMP coating of B is uniformly loaded with a layer of small water drops; under the freezing condition, the coating surface of the double-layer inclusion structure is free from ice as seen from C in figure 7, and the EP/CMP coating surface of D is uniformly loaded with a layer of small ice beads, so that the composite coating of the double-layer inclusion structure has the anti-icing performance. As can be seen from fig. 7, the composite coating having a double inclusion structure was spray-treated to the coating under freezing conditions, and as a result, exhibited anti-icing properties.
Claims (8)
1. A preparation method of a multifunctional coating with self-cleaning, anti-icing and microwave absorption is characterized in that: the method comprises the following steps:
first, preparation of a nanoparticle oil dispersion with low surface energy
a. Weighing 4-6 g of NaOH and dissolving in 92.5mL of deionized water to prepare NaOH solution for later use, and respectively weighing 2.86-4.29 g of FeCl2·4H2O and 4.864-7.296 g of FeCl3·6H2Dissolving O in 70-110 mL of deionized water, ultrasonically dispersing into a uniform solution, transferring the solution into a flask for heating, when the temperature is raised to 40-60 ℃, dropwise adding NaOH solution into the flask at the rate of 1 drop/second, continuing to react for 1.5 hours at the temperature of 40-60 ℃ after dropwise adding is finished, cooling to 25 ℃ after the reaction is finished, ultrasonically washing the solution for a plurality of times by using deionized water to obtain magnetic particles, ultrasonically dispersing the magnetic particles into 250-350 mL of water/ethanol solution with the volume ratio of 1:4 to obtain stable Fe3O4A dispersion liquid;
b. 250mL of Fe was taken3O4Adding 10mL of ammonia water into the dispersion, stirring and dispersing for 1h, dropwise adding 4mL of ethyl silicate during stirring, stirring for 6h at 25 ℃, performing magnetic adsorption precipitation, washing with ethanol and distilled water to obtain Fe3O4@SiO2Core-shell structured composite nanoparticles of Fe3O4@SiO2Ultrasonically dispersing the core-shell structure composite nano particles in 150mL of deionized water to obtain Fe3O4@SiO2A core-shell structure composite nanoparticle dispersion;
c. 120mL of Fe was taken3O4@SiO2Adding 1-4 g of urea, 2-6 g of cationic surfactant, 4-10 mL of 1-pentanol, 100-150 mL of cyclohexane and 10g of ethyl silicate in turn into core-shell structure composite nanoparticle dispersion liquid, stirring for 0.5-6h at 25 ℃ to obtain a mixed solution, transferring the mixed solution into a reaction kettle, reacting for 5h at 110-150 ℃, cooling to 25 ℃, performing magnetic adsorption precipitation, washing with water and ethanol, and drying to obtain Fe3O4@SiO2/organic composite nanoparticles of Fe3O4@SiO2Dispersing organic composite nano particles in 150mL of toluene solution to obtain Fe3O4@SiO2Organic composite nano particle toluene dispersion;
d. 100mL of Fe was weighed3O4@SiO2Organic composite nano particle toluene dispersion liquid, adding 30-50 mL of n-octyl trimethoxy siloxane in 12 portionsCarrying out reflux reaction for 20-48 h at 0 ℃, carrying out magnetic adsorption precipitation, and washing with toluene and xylene to obtain Fe3O4@H-SiO2/organic composite nanoparticles of Fe3O4@H-SiO2Performing ultrasonic dispersion on organic composite nanoparticles in a solvent to obtain a low-surface-energy nanoparticle oily dispersion liquid with the solid content of 10.0-25.0 wt%;
second step, Fe3O4Preparation of/rGO/PANI/resin composite coating
a. Dissolving 0.01M aniline in 10mL hydrochloric acid solution with the concentration of 1M, performing ultrasonic dispersion for 15min to obtain mixed solution A, dissolving 0.01M ammonium persulfate in 10mL hydrochloric acid solution with the concentration of 1M, performing ultrasonic dispersion for 15min to obtain mixed solution B, pouring the mixed solution B into the mixed solution A, stirring for 2h at 20 ℃, obtaining a dark green solution after the reaction is finished, filtering the dark green solution to obtain a filtrate, washing for several times with water and methanol until the washing liquid is colorless, and dissolving the washed filtrate in deionized water to obtain PANI solution with the mass fraction of 1wt% -3 wt%;
b. measuring 10mL of 80% hydrazine hydrate and 20mL of absolute ethanol, and uniformly mixing to obtain a hydrazine hydrate mixed solution for later use; respectively measuring 400mL of 2.5mg/mL graphene oxide aqueous solution and 0.5g of polyvinylpyrrolidone, adding the graphene oxide aqueous solution and the polyvinylpyrrolidone into a beaker, uniformly dispersing by ultrasound, transferring the mixture into the flask, starting heating, starting dropwise adding a hydrazine hydrate mixed solution into the flask when the temperature reaches 80 ℃, reacting for 3 hours after the dropwise adding is finished, and cooling to 25 ℃ after the reaction is finished to obtain an rGO dispersion liquid; respectively adding 20-40 mL of Fe into 100-150 mL of rGO dispersion liquid3O4Adding a surface modifier into the dispersion liquid and 30-60 mL of PANI solution at 50-85 ℃, and reacting for 2-6 h to obtain Fe3O4An aqueous solution of/rGO/PANI composite magnetic particles;
c. adsorbing Fe by magnet3O4Aqueous solution of/rGO/PANI composite magnetic particles to make Fe3O4precipitating/rGO/PANI composite magnetic particles, and then washing with absolute ethyl alcohol for 3-5 times to obtain Fe3O4(rGO/PANI) magnetic particle slurry, mixing Fe3O4/rGAdding the O/PANI magnetic particle slurry into resin, and dispersing for 1.0h under stirring at the rotating speed of 1000-1500 rpm to obtain Fe with the concentration of 5-35 wt%3O4a/rGO/PANI/resin composite coating;
thirdly, preparing the multifunctional coating with self-cleaning, anti-icing and microwave absorbing functions
Mixing Fe3O4the/rGO/PANI/resin composite coating is uniformly sprayed on the surface of a metal substrate to serve as an inner coating, the metal substrate is placed in a 60 ℃ oven for 30-120 min, when the surface of the inner coating is not completely cured, the nano particle oil dispersion liquid with low surface energy is uniformly sprayed on the outer coating, and after further curing, the multifunctional coating with self-cleaning, anti-icing and microwave absorption functions is obtained.
2. The method of claim 1, wherein the multifunctional coating is selected from the group consisting of self-cleaning, anti-icing, and microwave absorbing: in the first step, the cationic surfactant in step c is any one of cetyltrimethylammonium bromide, dodecyltrimethylammonium bromide, tetradecyltrimethylammonium bromide, octadecyltrimethylammonium bromide and cetylpyridinium bromide.
3. The method of claim 1, wherein the multifunctional coating is selected from the group consisting of self-cleaning, anti-icing, and microwave absorbing: in the first step, step d, the solvent is ethyl acetate or xylene.
4. The method of claim 1, wherein the multifunctional coating is selected from the group consisting of self-cleaning, anti-icing, and microwave absorbing: in the second step, the surface modifier in step b is any one of KH550, KH560, KH570, sodium dodecyl sulfonate, sodium dodecyl benzene sulfonate and cetyltrimethylammonium bromide.
5. The method of claim 1, wherein the multifunctional coating is selected from the group consisting of self-cleaning, anti-icing, and microwave absorbing: in the step c of the second step, the resin is any one of 30.0 to 45.0wt% of epoxy resin, polyurethane resin and tetrafluoroethylene resin.
6. The method of claim 1, wherein the multifunctional coating is selected from the group consisting of self-cleaning, anti-icing, and microwave absorbing: in the third step, the spraying pressure of the inner coating is 0.1 MPa-0.25 MPa, and the spraying pressure of the outer coating is 0.25 MPa-0.35 MPa.
7. The method of claim 1, wherein the multifunctional coating is selected from the group consisting of self-cleaning, anti-icing, and microwave absorbing: in the third step, the further curing mode is curing in an oven at 60.0 ℃ for 4.0 to 8.0 hours or curing at 25 ℃ for 20.0 hours.
8. A multifunctional coating having self-cleaning, anti-icing and microwave absorbing properties prepared by the preparation method of any one of claims 1 to 7, wherein: comprises an inner coating and an outer coating which are sequentially sprayed on a metal substrate from inside to outside, wherein the inner coating is Fe3O4the/rGO/PANI/resin doped composite membrane has an outer coating which is a nano particle assembly membrane with low surface energy.
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