CN116162272B - Shape memory ice-preventing and-removing composite material film and preparation method and application thereof - Google Patents
Shape memory ice-preventing and-removing composite material film and preparation method and application thereof Download PDFInfo
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- CN116162272B CN116162272B CN202310321077.8A CN202310321077A CN116162272B CN 116162272 B CN116162272 B CN 116162272B CN 202310321077 A CN202310321077 A CN 202310321077A CN 116162272 B CN116162272 B CN 116162272B
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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Abstract
The invention provides a shape memory ice-preventing and removing composite material film, and a preparation method and application thereof, belonging to the technical field of composite materials, wherein the preparation method comprises the following steps: adding micro-nano filler particles and a hydrophobic modifier into an organic solvent, and stirring and mixing to obtain a solution A; adding a binder into the solution A, and stirring and mixing to obtain a solution B, wherein the binder comprises a shape memory resin-based material; adding a curing agent into the solution B, and uniformly stirring and mixing to obtain a solution C; spraying the solution C on the surface of a die by adopting a spray gun, drying and curing, and stripping the cured film from the surface of the die to obtain the shape memory ice control composite material film; wherein the mass ratio of the micro-nano filler particles to the binder is 1 (11-30). The preparation method provided by the invention has simple process, can be completely attached to a complex surface, has good deicing performance, avoids the problem of difficult replacement when a coating fails, and has wide engineering application prospect.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a shape memory ice-preventing and removing composite material film, and a preparation method and application thereof.
Background
Inspired by the hydrophobic characteristics of plants and insect body surfaces in the nature, such as lotus leaves, rose petals, rice leaves, butterfly wings, compound eyes of mosquitoes and the like, the super-hydrophobic material has proved to have wide application in the aspects of rain protection, ice/snow protection, stain resistance, corrosion resistance and the like. Among these, surface chemistry and micro-nanostructures have been demonstrated to be two major factors affecting the wettability of superhydrophobic surfaces.
At present, researchers have developed various preparation methods of micro-nano structures, including etching methods, template methods, chemical vapor deposition methods, electrostatic spinning methods, electrochemical deposition methods, layer-by-layer assembly methods, solution immersion methods, phase separation methods and corrosion methods, but most of the preparation methods are expensive, have severe preparation conditions, and are difficult to realize large-area coating. The spraying method is one of common coating modes, is simple in process operation and easy to realize, is suitable for preparing large-area coatings, is an important mode of functional coating engineering and industrialization, but the surface coatings are easy to damage, the damaged coatings need to be polished and then are sprayed again for repair, and the technical difficulty is high for some large-scale special equipment.
Along with the development of the preparation process of the film material, the film formation of various materials has become a general development trend, and especially the requirements for functional film materials are increasingly increased, for example, a conductive film, a high polymer permeable film, an oil-water separation film and the like, and the replaceable film material is beneficial to realizing the repair of the damage of the surface of the structure, however, the film of the soft material is easy to damage after being attached to the surface, and the hard material film has the problem of being difficult to be attached to a complex curved surface, so that the application prospect is limited.
Disclosure of Invention
The invention solves the problem of providing a preparation method of a composite material film which can be well attached to a complex curved surface and has good mechanical properties.
In order to solve at least one aspect of the above problems, the present invention provides a method for preparing a shape memory ice preventing and removing composite film, comprising the steps of:
step S1, adding micro-nano filler particles and a hydrophobic modifier into an organic solvent, and uniformly stirring and mixing to obtain a solution A;
s2, adding a binder into the solution A, and uniformly stirring and mixing to obtain a solution B, wherein the binder comprises a shape memory resin-based material;
s3, adding a curing agent into the solution B, and uniformly stirring and mixing to obtain a solution C;
s4, spraying the solution C on the surface of a die by adopting a spray gun, drying and curing, and stripping the cured film from the surface of the die to obtain the shape memory ice control composite material film;
wherein the mass ratio of the micro-nano filler particles to the binder is 1 (11-30).
Preferably, in the step S2, the binder further includes polydimethylsiloxane, and a mass ratio of the polydimethylsiloxane to the shape memory resin-based material is 5:1-1:30.
Preferably, in the step S1, the hydrophobic modifier includes at least one of hexadecyltrimethoxysilane and triethoxy-1 h,2 h-tridecafluoro-N-octylsilane.
Preferably, in the step S1, the organic solvent includes at least one of ethyl acetate and toluene.
Preferably, in the step S4, the material of the mold includes a release cloth or polytetrafluoroethylene.
Preferably, in the step S4, the spraying pressure of the spray gun is 0.1-1.1MPa, and the distance between the spray gun and the die is 100-400mm.
Preferably, in the steps S1-S3, the stirring speed is 500-1000r/min, and the stirring time is 0.5-48h.
Preferably, in the step S4, drying and curing are performed at 50-200 ℃ for 10-300min.
According to the invention, the micro-nano filler particles and the hydrophobic modifier are added into the organic solvent and stirred and mixed uniformly, so that the micro-nano filler particles can be subjected to hydrophobic modification, and then the binder and the curing agent are sequentially added into the solution, wherein the binder comprises a shape memory resin-based material, so that the finally obtained shape memory ice prevention and removal composite material film has shape memory performance, the prepared mixed solution is sprayed on the surface of a mold in a spraying manner, dried and cured to form a film, and the shape memory ice prevention and removal composite material film is obtained after being peeled off from the surface of the mold. The preparation method of the shape memory ice-preventing and removing composite material film provided by the invention is simple in process, and the prepared shape memory ice-preventing and removing composite material film can be completely attached to a complex surface, has good ice-preventing and removing performance, avoids the problem of difficult replacement when a coating fails, and has wide engineering application prospects.
The invention also provides a shape memory deicing composite material film, which is prepared by adopting the preparation method of the shape memory deicing composite material film.
Compared with the prior art, the shape memory ice-preventing and removing composite material film has the beneficial effects that are the same as those of the preparation method of the shape memory ice-preventing and removing composite material film, and are not repeated here.
The invention also provides application of the shape memory ice-preventing and removing composite material film in the fields of aviation, automobiles and ocean industry.
Compared with the prior art, the application of the shape memory ice-preventing and removing composite material film has the beneficial effects that the application is the same as the preparation method of the shape memory ice-preventing and removing composite material film, and the application is not repeated here.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing a shape memory deicing composite material film in an embodiment of the invention;
FIG. 2 is a block diagram of a shape memory ice protection and detachment composite film in accordance with an embodiment of the present invention;
FIG. 3 is a second block diagram of a shape memory ice protection and detachment composite film in accordance with an embodiment of the present invention;
FIG. 4 is a SEM image of a shape memory ice protection and detachment composite film in accordance with an embodiment of the present invention;
FIG. 5 is a SEM image of a shape memory ice protection and detachment composite film of a comparative example of the present invention;
FIG. 6 is a graph of contact angle test results for a shape memory anti-icing composite film in an embodiment of the present invention;
FIG. 7 is a graph showing the results of a roll angle test of a shape memory ice protection and detachment composite film in accordance with an embodiment of the present invention;
FIG. 8 is a graph of bending test results of a shape memory deicing composite material film in an embodiment of the present invention;
FIG. 9 is a graph of the load test results of a shape memory ice protection and detachment composite film in accordance with an embodiment of the present invention;
FIG. 10 is a graph showing the force tear results of a shape memory ice protection and detachment composite film in a comparative example of the present invention;
FIG. 11 is a graph showing the results of a test of the hydrophobicity of a shaped shape memory ice protection and removal composite film according to an embodiment of the present invention;
FIG. 12 is a graph of wheel crush test results of a shape memory ice protection and detachment composite film in accordance with an embodiment of the present invention;
FIG. 13 is a graph showing the results of an anti-icing performance test for a shape memory anti-icing composite film according to an embodiment of the present invention;
FIG. 14 is a graph showing the results of deicing performance test of a shape memory deicing composite material film in an embodiment of the present invention.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more readily apparent, a more particular description of embodiments of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
It should be noted that, without conflict, features in the embodiments of the present invention may be combined with each other. The terms "comprising," "including," "containing," and "having" are intended to be non-limiting, as other steps and other ingredients not affecting the result may be added. The above terms encompass the terms "consisting of … …" and "consisting essentially of … …". Materials, equipment, reagents are commercially available unless otherwise specified. In addition, although the steps in the preparation are described in the forms of S1, S2, S3, S4, etc., the description is only for the convenience of understanding, and the forms of S1, S2, S3, S4, etc. do not represent a limitation of the sequence of the steps.
The embodiment of the invention provides a preparation method of a shape memory ice-preventing and removing composite material film, which is shown in figure 1 and comprises the following steps:
step S1, adding micro-nano filler particles and a hydrophobic modifier into an organic solvent, and uniformly stirring and mixing to obtain a solution A;
s2, adding a binder into the solution A, and uniformly stirring and mixing to obtain a solution B, wherein the binder comprises a shape memory resin-based material;
s3, adding a curing agent into the solution B, and uniformly stirring and mixing to obtain a solution C;
s4, spraying the solution C on the surface of a die by adopting a spray gun, drying and curing, and stripping the cured film from the surface of the die to obtain the shape memory ice control composite material film;
wherein the mass ratio of the micro-nano filler particles to the binder is 1 (11-30).
According to the embodiment of the invention, the micro-nano filler particles and the hydrophobic modifier are added into the organic solvent and stirred and mixed uniformly, so that the micro-nano filler particles can be subjected to hydrophobic modification, and then the binder and the curing agent are sequentially added into the solution, wherein the binder comprises a shape memory resin matrix material, so that the finally obtained shape memory ice preventing and removing composite material film has shape memory performance, the prepared mixed solution is sprayed on the surface of a mold in a spraying mode, dried and cured to form a film, and the film is peeled off from the surface of the mold, so that the shape memory ice preventing and removing composite material film is obtained. The shape memory ice-preventing and removing composite material film provided by the embodiment of the invention has simple preparation process, can be completely attached to a complex surface, has good ice-preventing and removing performance, avoids the problem of difficult replacement when a coating fails, and has wide engineering application prospect.
In the step S1, micro-nano filler particles and a hydrophobic modifier are added into an organic solvent, and are stirred and mixed to obtain a solution A, so that the micro-nano filler particles can be subjected to hydrophobic modification, wherein the micro-nano filler particles can enable the surface of the prepared shape memory anti-icing and deicing composite material film to have a micro-nano structure, and the hydrophobically modified micro-nano filler particles can provide good hydrophobic performance for the shape memory anti-icing and deicing composite material film.
In one embodiment, the hydrophobic modifier includes at least one of hexadecyltrimethoxysilane and triethoxy-1H, 2H-tridecafluoro-N-octylsilane. Hexadecyltrimethoxysilane and triethoxy-1H, 2H-tridecafluoro-N-octylsilane have long chain alkyl groups, which, when used for hydrophobic modification, are capable of forming hydrophobic layers.
In one embodiment, the micro-nano filler particles include at least one of Carbon Nanotubes (CNTs) and multi-walled carbon nanotubes (MWCNTs). The CNT and the MWCNT have rich micro-nano structures, so that the surface of the prepared shape memory ice-proof composite material film has rich micro-nano structures, and the hydrophobicity is improved.
In one embodiment, the organic solvent includes at least one of ethyl acetate and toluene. Ethyl acetate is capable of dissolving the hydrophobic modifier, binder and curing agent.
In one embodiment, the micro-nano filler particles and the hydrophobic modifier are added into the organic solvent and then stirred for 0.5 to 48 hours under the stirring speed of 500 to 1000r/min, so that the hydrophobic modifier and the micro-nano filler particles are fully mixed for hydrophobic modification.
In step S2, adding a binder into the solution A, and stirring and mixing uniformly to obtain a solution B, wherein the binder comprises a shape memory resin-based material. The shape memory resin-based material is used as a binder, so that the shape memory performance can be provided for the shape memory ice preventing and removing composite material film, when the shape memory ice preventing and removing composite material film is required to be attached to the surface of a complex structure, the hard material is softened by heating to a temperature above the glass transition temperature, so that complete attachment is realized, after the attachment is completed, the hard state of the shape memory ice preventing and removing composite material film can be restored below the glass transition temperature, the mechanical performance of the shape memory ice preventing and removing composite material film is improved, and damage in the use process is reduced.
In one embodiment, the binder further comprises polydimethylsiloxane, the mass ratio of the polydimethylsiloxane to the shape memory resin-based material being from 5:1 to 1:30. In order to ensure that the shape memory ice-preventing and-removing composite material film has good mechanical properties while having shape memory properties, the binder comprises Polydimethylsiloxane (PDMS) and a shape memory resin-based material, and the mass ratio of the Polydimethylsiloxane (PDMS) to the shape memory resin-based material is 30:1-1:5.
In one embodiment, after the binder is added to solution A, stirring is performed at a stirring speed of 500-1000r/min for a period of 0.5-48 hours. The binder was uniformly dispersed in the solution a by stirring.
In one embodiment, after the step S1, before the step S2, the method further includes:
mixing the binder and the diluent according to the volume ratio of 1 (1-20) to obtain a pretreatment binder;
the step S2 includes:
and adding the pretreatment binder into the solution A, and stirring and uniformly mixing to obtain the solution B.
Illustratively, the diluents include one or more of ethanol, ethyl acetate, and toluene.
Before the binder is added into the solution A, the binder and the diluent are mixed according to the volume ratio of 1 (1-20), so that the viscosity of the binder can be reduced, the binder is more uniformly dispersed, and the uniformity of the prepared shape memory ice-preventing and removing composite material film is improved.
The mass ratio of the micro-nano filler particle material to the binder is 1 (11-30), when the addition amount of the micro-nano filler particle material is low, the surface of the prepared shape memory ice-preventing and removing composite material film cannot form enough micro-nano structure, the hydrophobic property of the film is influenced, and when the addition amount of the micro-nano filler particle material is high, the mechanical property of the prepared shape memory ice-preventing and removing composite material film is poor and the film is easy to damage.
In the step S3, a curing agent is added into the solution B, and the solution C is obtained after stirring and mixing uniformly.
Specifically, the curing agent is Sylgard 184 curing agent, and after the curing agent is added, the mixture is stirred for 0.5 to 48 hours under the condition that the stirring speed is 500 to 1000r/min, so that the curing agent is uniformly dispersed in the solution.
And S4, spraying the solution C on the surface of a die by adopting a spray gun, drying and curing, and stripping the cured film from the surface of the die to obtain the shape memory ice control composite material film.
Among them, the mold is made of a material having a low surface energy and being smooth and flat, and the composite film is easily peeled off from the surface thereof, preferably a release cloth or polytetrafluoroethylene.
In one embodiment, when the solution C is sprayed on the surface of the die by adopting a spray gun, the spraying pressure is set to be 0.1-1.1MPa, the distance between the spray gun and the die is 100-400mm, and the spray gun is uniformly and uniformly arranged, so that the shape memory anti-icing composite material film with uniform texture is obtained.
It should be noted that the number of spraying times can be adjusted according to the thickness requirement of the shape memory deicing film.
In one embodiment, after the solution C is sprayed on the surface of the mold, the mold is placed into a drying oven for drying and curing, the curing temperature is 50-200 ℃, the curing time is 10-300min, and the solvent in the solution C is evaporated and the binder is crosslinked and cured through the drying and curing process to form the composite material film.
In order to further improve the ice preventing and removing performance of the shape memory ice preventing and removing composite material film, a heating electrode can be placed on the surface of the template before spraying the solution C, the shape memory ice preventing and removing composite material film with the heating electrode can be formed after spraying is finished and drying and solidifying are carried out, the heating electrode can be powered to heat so as to melt the ice layer on the surface of the shape memory ice preventing and removing composite material film, and the melted ice layer falls off from the surface of the shape memory ice preventing and removing composite material film due to the hydrophobicity of the shape memory ice preventing and removing composite material film, so that the ice preventing and removing performance of the shape memory ice preventing and removing composite material is further improved.
Another embodiment of the present invention provides a shape memory ice protection and detachment composite film, made by the method of making a shape memory ice protection composite film as described above.
Compared with the prior art, the shape memory ice-preventing and removing composite material film has the beneficial effects that are the same as those of the preparation method of the shape memory ice-preventing and removing composite material film, and the detailed description is omitted.
Yet another embodiment of the present invention provides the use of a shape memory ice protection and detachment composite film as described above in the aeronautical, automotive, marine industry.
Compared with the prior art, the application of the shape memory ice-preventing and removing composite material film has the beneficial effects that the application is the same as the preparation method of the shape memory ice-preventing and removing composite material film, and the application is not repeated here.
The invention will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. The experimental methods, which do not address specific conditions in the following examples, are generally in accordance with the conditions recommended by the manufacturer.
Example 1
1.1, adding 0.5g of multi-wall carbon nano tube (MWCNT) and 1g of hexadecyl trimethoxy silane into 100mL of ethyl acetate solution, stirring for 2h at 800r/min, and fully hydrophobically modifying the MWCNT to obtain solution A;
1.2, adding 2g of epoxy resin into the solution A under the stirring condition, continuously stirring at the stirring speed of 800r/min at room temperature for 14h, then adding 6g of PDMS, and continuously stirring at the same rotating speed for 14h to obtain a solution B;
1.3, adding 0.6g of Sylgard 184 curing agent into the solution B, and continuously stirring at room temperature for 60min at 800r/min to obtain a solution C;
1.4, selecting release cloth with a flat and smooth surface, cleaning the surface of the release cloth, and removing impurities on the surface to obtain a pretreatment die;
1.5, spraying the solution C on the surface of a pretreatment die by adopting a W-100-102G type high-micronization spray gun, wherein the spraying pressure is 0.3MPa, the distance between the spray gun and the pretreatment die is 350mm, the spray gun is uniformly and consistently arranged, the spray gun is sprayed for 10 times, and then the spray gun is placed into a drying oven for curing, the curing temperature is 80 ℃, and the curing time is 200min;
and 1.6, stripping the cured film from the surface of the pretreatment die to obtain the shape memory ice control composite material film.
Example 2
2.1, adding 0.7g of multi-walled carbon nanotube (MWCNT) and 1g of 1H, 2H-perfluorooctyl triethoxysilane into 100mL of ethyl acetate solution, stirring for 12h at 500r/min, and fully hydrophobically modifying the MWCNT to obtain solution A;
2.2, adding 6g of epoxy resin into the solution A under the stirring condition, continuously stirring at the stirring speed of 1000r/min for 12 hours at room temperature, then adding 2g of PDMS, and continuously stirring at the same rotating speed for 12 hours to obtain a solution B;
2.3, adding 0.2g of Sylgard 184 curing agent into the solution B, and continuously stirring at 500r/min for 40min at room temperature to obtain a solution C;
2.4, selecting a polytetrafluoroethylene mould with a smooth surface, cleaning the surface of the polytetrafluoroethylene mould, and removing impurities on the surface to obtain a pretreatment mould;
2.5, spraying the solution C on the surface of a pretreatment die by adopting a W-100-102G type high-micronization spray gun, wherein the spraying pressure is 0.2MPa, the distance between the spray gun and the pretreatment die is 200mm, the spray gun is uniformly and consistently arranged, spraying is carried out for 10 times, and then the spray gun is placed into a drying oven for curing, the curing temperature is 100 ℃, and the curing time is 120min;
and 2.6, stripping the cured film from the surface of the pretreatment die to obtain the shape memory ice control composite material film.
Fig. 2 and 3 are photographs of the resulting shape memory ice protection and detachment composite films of different sizes, respectively.
Example 3
3.1, adding 0.6g of multi-walled carbon nanotube (MWCNT) and 1g of 1H, 2H-perfluorooctyl triethoxysilane into 100mL of ethyl acetate solution, stirring for 1.5h at 800r/min, and fully hydrophobically modifying the MWCNT to obtain a solution A;
3.2, adding 8g of epoxy resin into the solution A under the stirring condition, continuously stirring at the stirring speed of 800r/min for 24 hours at room temperature, then adding 4g of PDMS, and continuously stirring at the same rotating speed for 12 hours to obtain a solution B;
3.3, adding 0.4g of Sylgard 184 curing agent into the solution B, and continuously stirring at room temperature for 40min at 800r/min to obtain a solution C;
selecting a polytetrafluoroethylene mould with a smooth surface, cleaning the surface of the polytetrafluoroethylene mould, and removing impurities on the surface to obtain a pretreatment mould;
3.5, spraying the solution C on the surface of a pretreatment die by adopting a W-100-102G type high-micronization spray gun, wherein the spraying pressure is 0.2MPa, the distance between the spray gun and the pretreatment die is 350mm, the spray gun is uniformly and consistently arranged, spraying is carried out for 10 times, and then the spray gun is placed into a drying oven for curing, the curing temperature is 120 ℃, and the curing time is 150min;
and 3.6, stripping the cured film from the surface of the pretreatment die to obtain the shape memory ice control composite material film.
Example 4
4.1, adding 0.65g of multi-walled carbon nanotube (MWCNT) and 1g of hexadecyl trimethoxy silane into 100mL of toluene solution, stirring for 1.5h at 800r/min to enable the MWCNT to be fully hydrophobically modified, and obtaining solution A, wherein the hexadecyl trimethoxy silane is added according to the mass ratio of 3%;
4.2, adding 8g of epoxy resin into the solution A under the stirring condition, continuously stirring at the stirring speed of 500r/min for 10 hours at room temperature, then adding 1g of PDMS, and continuously stirring at the same rotating speed for 20 hours to obtain a solution B;
4.3, adding 0.8g of Sylgard 184 curing agent into the solution B, and continuously stirring at 500r/min for 15min at room temperature to obtain a solution C;
4.4, selecting a polytetrafluoroethylene mould with a smooth surface, cleaning the surface of the polytetrafluoroethylene mould, and removing impurities on the surface to obtain a pretreatment mould;
4.5, spraying the solution C on the surface of the pretreatment die by adopting a W-100-102G type high-micronization spray gun, wherein the spraying pressure is 0.3MPa, the distance between the spray gun and the pretreatment die is 200mm, the spray gun is uniformly and consistently arranged, spraying is carried out for 10 times, and then the spray gun is placed into a drying oven for curing, the curing temperature is 150 ℃, and the curing time is 60 minutes;
and 4.6, stripping the cured film from the surface of the pretreatment die to obtain the shape memory ice control composite material film.
Comparative example 1
5.1, adding 0.75g of multi-walled carbon nanotube (MWCNT) and 1g of 1H, 2H-perfluorooctyl triethoxysilane into 100mL of ethyl acetate solution, stirring for 12h at 500r/min, and fully hydrophobically modifying the MWCNT to obtain solution A;
5.2, adding 6g of epoxy resin into the solution A under the stirring condition, continuously stirring at the stirring speed of 500r/min for 12 hours at room temperature, then adding 2g of PDMS, and continuously stirring at the same rotating speed for 12 hours to obtain a solution B;
5.3, adding 0.2g of Sylgard 184 curing agent into the solution B, and continuously stirring at 500r/min for 40min at room temperature to obtain a solution C;
5.4, selecting a polytetrafluoroethylene mould with a smooth surface, cleaning the surface of the polytetrafluoroethylene mould, and removing impurities on the surface to obtain a pretreatment mould;
5.5, spraying the solution C on the surface of a pretreatment die by adopting a W-100-102G type high-micronization spray gun, wherein the spraying pressure is 0.2MPa, the distance between the spray gun and the pretreatment die is 200mm, the spray gun is uniformly and consistently arranged, spraying is carried out for 10 times, and then the spray gun is placed into a drying oven for curing, the curing temperature is 100 ℃, and the curing time is 120min;
and 5.6, stripping the cured film from the surface of the pretreatment die to obtain the shape memory ice control composite material film.
Experimental example 1
The shape memory ice protection and detachment prevention composite film prepared in example 2 was observed under a scanning electron microscope, and the results are shown in fig. 4 and 5.
Fig. 4 is an SEM image observed at 1000 x, and fig. 5 is an SEM image observed at 50000 x, as shown in fig. 4 and 5, the surface of the shape memory ice protection and detachment prevention composite film has a micro-nano structure.
Experimental example 2
The contact angle of the shape memory deicing composite material film prepared in example 2 was measured, and the specific method was as follows: the measurement results are shown in fig. 6, and 5 μl of the water drop was dropped on the surface to be measured placed horizontally and characterized by a contact angle meter.
As can be seen from fig. 6, the shape memory ice preventing and removing composite material film prepared in example 2 has a contact angle of 152.4 ° and excellent superhydrophobic performance.
The roll angle of the shape memory ice-preventing and removing composite material film prepared in the example 2 is measured, and the specific method is as follows: and 5 mu L of water drops are dripped on the surface to be measured which is horizontally placed, the surface to be measured is characterized by utilizing a contact angle measuring instrument, a storage table is slowly inclined in the measuring process, the dynamic rolling process of the water drops and the inclination angle of the surface to be measured relative to the horizontal position are recorded, and the measuring result is shown in figure 7.
As can be seen from fig. 7, when the inclined surface is inclined at an angle of 6.5 °, the water drops rapidly roll off, which means that the shape memory ice preventing and removing composite film prepared in example 2 has super-hydrophobic low adhesion properties.
Experimental example 3
The toughness of the shape memory ice protection and detachment composite film prepared in example 2 was tested, and the shape memory ice protection and detachment composite film prepared in example 2 was bent, and the results are shown in fig. 8.
As can be seen from fig. 8, when the sample is bent, no fracture or breakage occurs, which indicates that the shape memory ice preventing and removing composite film prepared by the embodiment of the present invention has good toughness.
The shape memory ice preventing and removing composite film prepared in example 2 was tested for load bearing properties, one end of the sample was fixed to glass, and the other end was connected to a 500g weight by a clip, so that the weight was in a free sagging state, and the results are shown in fig. 9.
As can be seen from fig. 9, the shape memory ice preventing and removing composite material film prepared in the embodiment 2 of the present invention can bear the weight of a 500g weight, and has no breakage, which indicates that the composite material film has good bearing performance.
The mechanical properties of the shape memory ice protection and detachment composite films prepared in example 2 and comparative example 1 were respectively tested, and the two shape memory ice protection and detachment composite films were respectively torn. The results are shown in FIG. 10.
As can be seen from fig. 10, the shape memory ice preventing and removing composite film prepared in comparative example 1 is torn by force, while the shape memory ice preventing and removing composite film prepared in example 2 is not torn, which indicates that the shape memory ice preventing and removing composite film prepared in the example of the present invention has better mechanical properties than the sample prepared in comparative example 1.
Experimental example 4
The shape memory ice control and deicing composite material film prepared in example 2 was tested for its hydrophobic property after shaping, the shape memory ice control and deicing composite material film was heated to 80 ℃, shaped after it was softened, then rapidly cooled to below room temperature to fix its shape, and water droplets were dropped onto the surface of the shaped shape memory ice control and deicing composite material film, as shown in fig. 11.
From fig. 11, it can be seen that the water drops quickly drop on the shaped shape memory ice control composite material film, which indicates that the shaped shape memory ice control composite material film still has super-hydrophobic low adhesion performance and can realize complex curved surface shaping.
The shape memory ice protection and detachment prevention composite film prepared in example 2 was subjected to a wheel crush test, and a sample was placed on the ground so that the wheel crushed the sample, and the result is shown in fig. 12.
As can be seen from FIG. 12, the shape memory ice preventing and removing composite material film rolled by the wheels has complete structure and no damage, which indicates that the shape memory ice preventing and removing composite material film prepared by the embodiment of the invention has good mechanical properties.
Experimental example 5
The shape memory ice preventing and removing composite material film prepared in the embodiment 2 is attached to one of the wings of a metal model airplane, supercooled water drops are respectively dripped on the two wings at the ambient temperature of-14 ℃, and the surface temperature of the two wings is measured by a thermal imager, so that the result is shown in fig. 13.
As shown in fig. 13 (i), the black wing is a wing to which the shape memory anti-icing and deicing composite film is attached, and the white wing is a wing to which the shape memory anti-icing and deicing composite film is not attached, and as can be seen from fig. 13 (i), when supercooled water drops drop onto the black wing, supercooled water drops quickly roll, and when supercooled water drops drop onto the white wing, supercooled water drops adhere to the surface and freeze to form ice bodies.
As shown in fig. 13 (ii), the right wing is a wing to which the shape memory anti-icing and deicing composite film is attached, and the left wing is a wing to which the shape memory anti-icing and deicing composite film is not attached, as can be seen from fig. 13 (ii), the average surface temperature of the wing to which the shape memory anti-icing and deicing composite film is attached exceeds 5 ℃, and the average surface temperature of the wing to which the shape memory anti-icing and deicing composite film is not attached is about-5 ℃, and the adhesion of supercooled water drops can be effectively reduced due to the higher surface temperature, so that excellent anti-icing performance is shown.
The shape memory ice preventing and removing composite material film prepared in the embodiment 2 is attached to one wing of a metal model airplane, the model airplane is placed in an outdoor environment at the environment temperature of minus 10 ℃, the model airplane is covered by snow falling through a natural snow falling process, then the surfaces of the two wings are respectively irradiated by near infrared light with the wavelength of 808nm, the model airplane is acted by air flow, and the air flow direction is the front-to-back direction of the model airplane, and the result is shown in fig. 14.
Fig. 14 (i) is a state diagram of a model aircraft before irradiation of near infrared light, in which a black wing is a wing to which a shape memory deicing prevention composite material film is attached, and a white wing is not attached, in which fig. 14 (ii) is a picture of irradiation of the wing with near infrared light, and fig. 14 (iii) is a picture of the wing of the model aircraft after irradiation of the wing with air flow.
As can be seen from fig. 14 (i), in the initial state, the wings on both sides are covered by snow falling, as can be seen from fig. 14 (ii), after being irradiated by near infrared light, the snow on the surfaces of the black wings is melted to form spherical water drops, so that the surface snow is quickly eliminated, while as can be seen from fig. 14 (iii), after being acted by air flow, the spherical water drops are removed due to the small contact area between the spherical water drops and the surfaces of the wings, so that the snow-free effect is realized, but the white wings cannot melt the snow even if being irradiated by near infrared light for a long time. The shape memory deicing-preventing composite material film prepared by the embodiment of the invention has good deicing performance, can improve the flight stability of an aircraft in the running process of the aircraft, ensures the flight safety and has wide application prospect.
Although the present disclosure is described above, the scope of protection of the present disclosure is not limited thereto. Various changes and modifications may be made by one skilled in the art without departing from the spirit and scope of the disclosure, and these changes and modifications will fall within the scope of the invention.
Claims (8)
1. The preparation method of the shape memory deicing composite material film is characterized by comprising the following steps of:
step S1, adding micro-nano filler particles and a hydrophobic modifier into an organic solvent, and uniformly stirring and mixing to obtain a solution A;
s2, adding a binder into the solution A, and uniformly stirring and mixing to obtain a solution B, wherein the binder comprises a shape memory resin-based material;
s3, adding a curing agent into the solution B, and uniformly stirring and mixing to obtain a solution C;
s4, spraying the solution C on the surface of a die by adopting a spray gun, drying and curing, and stripping the cured film from the surface of the die to obtain the shape memory ice control composite material film;
wherein the mass ratio of the micro-nano filler particles to the binder is 1 (11-30);
in the step S2, the binder further includes polydimethylsiloxane, and the mass ratio of the polydimethylsiloxane to the shape memory resin-based material is 5:1-1:30;
the micro-nano filler particles comprise at least one of carbon nanotubes and multi-wall carbon nanotubes;
in the step S4, the material of the mold includes a release cloth or polytetrafluoroethylene.
2. A method of preparing a shape memory ice control and deicing composite film according to claim 1, wherein in step S1, the hydrophobic modifier comprises at least one of hexadecyltrimethoxysilane and triethoxy-1 h,2 h-tridecafluoro-N-octylsilane.
3. The method for producing a shape memory ice preventing and removing composite material film according to claim 1, wherein in said step S1, said organic solvent comprises at least one of ethyl acetate and toluene.
4. The method for producing a shape memory ice preventing and removing composite material film according to claim 1, wherein in said step S4, the spraying pressure of said spray gun is 0.1 to 1.1MPa, and the distance between said spray gun and said mold is 100 to 400mm.
5. The method for preparing a shape memory ice preventing and removing composite material film according to claim 1, wherein in the steps S1 to S3, the stirring speed is 500-1000r/min, and the stirring time is 0.5-48h.
6. The method for preparing a shape memory ice preventing and removing composite material film according to claim 1, wherein in the step S4, drying and curing are performed at 50-200 ℃ for 10-300min.
7. A shape memory ice protection and detachment composite film produced by the method of producing a shape memory ice protection composite film as claimed in any one of claims 1 to 6.
8. Use of the shape memory ice protection and detachment composite film of claim 7 in the aeronautical, automotive, marine industry field.
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