CN109822950B - Polymer material with anti-icing function and integrated forming method thereof - Google Patents
Polymer material with anti-icing function and integrated forming method thereof Download PDFInfo
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Abstract
An integrated forming method of a polymer material with an anti-icing function is characterized in that an anti-icing function structure and a polymer base material are integrally formed by designing a surface structure of a mold and adjusting hot-pressing parameters of composite material forming. The polymer material with the anti-icing function and the integrated forming method thereof provided by the invention have the following advantages: the two functions of preparing the polymer-based material and integrating the anti-icing microstructure on the material are simultaneously completed, and compared with the traditional technology, the preparation method has the advantages of simple operation, good structural formability and uniform microstructure distribution; the prepared polymer material has the surface super-hydrophobic characteristic to liquid water, and the freezing time of supercooled liquid drops is obviously prolonged, so that the supercooled liquid drops have enough time to separate from the surface; the coating has extremely low ice adhesion strength, can be peeled off from the surface of a material under the action of natural wind power or gravity, can be used for covering parts of the outer surface of machine equipment exposed in extreme environments, and has important practical significance for the development of anti-icing and deicing technologies of wind turbines and airplanes.
Description
Technical Field
The invention belongs to the technical field of composite material processing technology and surface modification, and particularly relates to a polymer material with an anti-icing function and an integrated forming method thereof.
Background
Polymer matrix composites generally refer to continuous fiber/short fiber reinforced resin matrix composites. The high strength and high modulus characteristics of the fibers make them ideal carriers. The matrix material has good adhesive properties, firmly bonds the fibers together, and simultaneously enables the load to be uniformly distributed and transferred to the fibers, allowing the fibers to bear compression and shear loads. The good composition between the fiber and the matrix shows respective advantages, can realize the optimal structural design, has the characteristics of light weight, high strength and high rigidity, and is widely applied to the fields of national defense and civil life. Such as glass fiber composites used in the united states for rocket motor casings, fuel autoclaves, helicopter rotor blades, and the like. Domestic C919 aircraft skins use a large number of composite laminates. The polymer-based composite material is mainly applied to the fields of aircraft surface skins and wind driven generators.
The icing of aircraft surfaces such as high-altitude unmanned aerial vehicle, manned passenger plane can influence the windage, causes the energy consumption increase, reduces the time of endurance by a wide margin, and critical position freezes and even has the risk of crash. The research on the anti-icing technology has important significance.
The ice coating prevention technology is a novel technology for blocking or delaying material surface bonding/ice coating by utilizing the intrinsic property of the material, and is different from active ice removing technologies such as electric heating, mechanical vibration and the like. There are two main ideas for improving the anti-icing performance of the material: 1) by constructing a hierarchical micro-nano structure and a low surface energy modification method, the super-hydrophobicity of the surface of the material is improved, the freezing of supercooled liquid drops is delayed, the freezing point of the material is lowered, and the supercooled liquid drops can leave the surface of an aircraft in time under the action of external force such as wind power, self gravity and the like before being frozen; 2) by arranging macroscopic and microscopic crack sources on the surface of the material, the ice adhesion strength between ice and a matrix is reduced, and the position and the shape of an ice layer are controlled, so that the ice layer is broken and separated from the surface of the material in the initial growth stage due to external forces such as wind power, self gravity and the like. The invention integrates the two design ideas.
The existing technical route for integrating the anti-icing function on the composite material is to prepare the composite material and then construct an anti-icing structure on the composite material. For example, in patent CN105504324A, a resin-based composite material with a super-hydrophobic bionic surface and a preparation method thereof, the preparation method requires cleaning and polishing the molded composite material, and then requires procedures such as laser processing of a microstructure and spraying of a hydrophobic coating, and has the disadvantages of complicated steps, high cost, and unstable strength of the microstructure.
Disclosure of Invention
The invention aims to provide a polymer material with an anti-icing function and an integrated forming method thereof, and aims to solve the problems of high cost, multiple steps and unstable performance when a composite material with the anti-icing function is prepared in the prior art.
Aiming at the method for constructing a functional micro-nano structure after forming a composite material by the traditional technical means, the invention provides a polymer material integrated forming method with an anti-icing function, which can realize passive protection on icing and comprises the following steps:
(1) preparing a closed metal die by a precision machining method, cleaning for later use, and precoating a release agent;
(2) cutting the fiber cloth to a proper shape, and then wrapping the core material to obtain a dry fiber prefabricated forming body;
(3) mixing resin, a curing agent and a low surface energy modifier to obtain a liquid polymer mixture;
(4) placing the dry fiber prefabricated molding body in the closed metal mold, injecting the mixed liquid polymer mixture into the dry fiber prefabricated molding after mold closing, and vacuumizing to obtain a workpiece;
(5) setting the pressure and temperature of a hot press, curing the workpiece in the closed metal die for a certain time, controlling the pressure and temperature of the curing, and slowly cooling after the curing is finished;
(6) and (3) after the temperature of the hot press is reduced to 80 ℃ or room temperature, unloading the pressure and opening the die, separating the solidified workpiece from the closed metal die, and cleaning burrs and fins to obtain the polymer material with the ice coating prevention function.
The polymer material with the surface microstructure prepared by the integrated forming method has the super-hydrophobic characteristic and extremely low ice adhesion strength, and the ice coating resistance of the composite material is greatly improved. Meanwhile, the integration method has the advantages of regular array, uniform organizational structure and accurate size, and avoids the defects of unstable size, irregular array, damage to the continuity of a matrix and fibers and the like possibly caused by the traditional method for processing the microstructure on the formed composite material.
As a preferable scheme, the die material of the closed metal die in the step (1) is corrosion-resistant steel, titanium alloy, and high-strength aluminum alloy.
More preferably, the closed metal mold in the step (1) has a microstructure with a special shape, and is an inverted pyramid, a round or a square pit; the included angle between the side surface and the bottom surface of the inverted pyramid pit is 45-54 degrees, and the size ranges of the length, the width and the height are 1-200 mu m; the size range of the length and the height of the square column pits is 1-200 mu m, the size range of the diameter and the depth of the circular pits is 1-200 mu m, and the distance range of two adjacent inverted pyramid, circular or square pits is 1-500 mu m.
More preferably, the fiber cloth in step (2) is made of one or more of glass fiber, carbon fiber, aramid fiber, asbestos fiber, potassium titanate fiber, silicon carbide fiber, natural fiber and hybrid fiber.
More preferably, the resin in step (3) comprises one or more of polyester, vinyl ester, epoxy, phenolic, polyphenylene sulfide, polyetheretherketone and polyetherimide.
More preferably, the material used for the low surface energy modifier in step (3) is heptadecafluorodecyltriethoxysilane or stearic acid.
More preferably, the liquid polymer mixture in step (3) is mixed with a discontinuous fiber or particle reinforcing phase, and the addition amount is 0.5-3% of the mass of the resin; the discontinuous fiber comprises metal or ceramic whiskers and carbon nanotubes, and the particle reinforcing phase comprises metal or ceramic nanoparticles and graphene.
More preferably, in the step (3), the addition amount of the curing agent is 10 to 25% of the mass of the resin, and the addition amount of the low surface energy modifier is 0.1 to 2% of the mass of the resin.
More preferably, the temperature of the curing process in step (5) is in the range of 120 ℃ to 200 ℃ and the pressure is in the range of 0.5 to 1.2 MPa.
The polymer material with the anti-icing function is prepared by any one of the methods.
The invention has the beneficial effects that the polymer material with the anti-icing function and the integrated forming method thereof provided by the invention have the following advantages:
① compared with the method of forming the composite material first and then heating to construct the structure by the traditional technical means, the method provided by the invention realizes the effect of simultaneously completing two functions of preparing the polymer material and integrating the anti-icing microstructure on the material, and has the advantages of simple operation, good structural formability and uniform microstructure distribution;
② A polymer material with ice-covering-proof function has super-hydrophobic property to liquid water, and can remarkably prolong the freezing time of supercooled liquid drop to make supercooled liquid drop have enough time to separate from surface;
③ A polymer material with ice-covering-proof function is made by the integrated molding method and has extremely low ice adhesion strength, and the ice can fall off from the surface of the polymer material under the action of natural wind or gravity;
④ the polymer material made by the integrated molding method of the polymer material with the function of ice coating prevention can be used as the outer surface covering piece of the machine equipment such as the aircraft, the wind driven generator blade and the like exposed in extreme environment, and has important practical significance for the development of the ice prevention and removal technology of the wind turbine and the aircraft, in particular to the development of the passive ice prevention and removal technology.
Drawings
FIG. 1 is a schematic process flow diagram of an integrated molding method of a polymer material with an anti-icing function in embodiment 1 of the present invention;
FIG. 2 is a schematic view of a polymer material with an anti-icing function prepared by an integrated molding method of the polymer material with the anti-icing function in example 1 of the present invention;
FIG. 3 is a schematic view of a microstructure array of a polymer material with an anti-icing function prepared by an integrated molding method of the polymer material with the anti-icing function in example 1 of the present invention;
FIG. 4 is a schematic structural diagram of the polymer material with an anti-icing function prepared by the method for integrally molding the polymer material with the anti-icing function in the invention when being embedded with a closed metal mold.
The meaning of the reference symbols in the figures: 1-closing metal mould, 2-polymer material with anti-icing function.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to fig. 1 to 4 of the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
An integrated molding method of a polymer material with an anti-icing function comprises the following steps:
(1) preparing a closed 7075 aluminum alloy die with a square pit array microstructure on the inner wall by using a precision numerical control lathe, cleaning for later use, and precoating a release agent;
(2) cutting the fiber cloth to a proper shape, and then wrapping the PVC foam core material to prepare a dry fiber prefabricated forming body; SW220 high-strength glass fiber is selected as the fiber cloth, PVC foam is selected as the core material, and the size of the PVC foam is 50mmx50mmx4 mm;
(3) according to the following steps of 3: 1: mixing 0.01 mass ratio of resin, curing agent and low surface energy modifier heptadecafluorodecyltriethoxysilane FAS-17 to obtain liquid polymer mixture;
(4) placing the dry fiber preform in the closed metal mold; injecting the liquid polymer mixture into the dry fiber prefabricated forming body after die assembly until no bubble-free liquid colloid flows out of the glue outlet, and vacuumizing to obtain a workpiece;
(5) setting the pressure of a hot press to be 0.8Mpa, preheating for 15min at the temperature of 120 ℃, then heating to 180 ℃, curing a workpiece in a closed metal mold for 150min, and slowly cooling after curing;
(6) and (3) after the temperature of the hot press is reduced to 80 ℃, unloading the pressure and opening the die, separating the solidified part from the closed metal die, and cleaning the defects of flash, burr and the like to obtain the polymer material with the ice coating prevention function.
One polymer material with an anti-icing function that can be obtained by the above method is a glass fiber reinforced epoxy resin composite material with an anti-icing function.
Example 2
An integrated molding method of a polymer material with an anti-icing function comprises the following steps:
(1) preparing a closed 7075 aluminum alloy die with an inverted pyramid pit array microstructure on the inner wall by using a precision numerical control lathe, cleaning for later use, and precoating a release agent;
(2) cutting the fiber cloth to a proper shape, and then wrapping the PVC foam core material to prepare a dry fiber prefabricated forming body; the fiber cloth is made of a high-strength carbon fiber material with the temperature of T700SC-12000-50 ℃, and the high-strength carbon fiber material is precoated with epoxy resin slurry; the core material is PVC foam with the size of 50mmx50mmx4 mm;
(3) according to the following steps of 3: 1: mixing 0.01 mass ratio of resin, curing agent and low surface energy modifier heptadecafluorodecyltriethoxysilane FAS-17 to obtain liquid polymer mixture;
(4) placing the dry fiber preform in the closed metal mold; injecting the liquid polymer mixture into the dry fiber prefabricated forming body after die assembly until no bubble-free liquid colloid flows out of the glue outlet, and vacuumizing to obtain a workpiece;
(5) setting the pressure of a hot press to be 0.8Mpa, preheating for 15min at the temperature of 120 ℃, then heating to 180 ℃, curing a workpiece in a closed metal mold for 150min, and slowly cooling after curing;
(6) and (3) after the temperature of the hot press is reduced to 80 ℃, unloading the pressure and opening the die, separating the solidified part from the closed metal die, and cleaning the defects of flash, burr and the like to obtain the polymer material with the ice coating prevention function.
One polymer material with an anti-icing function which can be obtained by the method is a carbon fiber reinforced epoxy resin composite material with an anti-icing function.
Example 3
An integrated molding method of a polymer material with an anti-icing function comprises the following steps:
(1) preparing a closed 7075 aluminum alloy die with a square pit array microstructure on the inner wall by using a precision numerical control lathe, cleaning for later use, and precoating a release agent;
(2) cutting the fiber cloth to a proper shape, and then wrapping the PVC foam core material to prepare a dry fiber prefabricated forming body; the fiber cloth is aramid fiber, the core material is PVC foam, and the size of the PVC foam is 50mmx50mmx4 mm;
(3) according to the following steps of 3: 1: mixing 0.01 mass ratio of resin, curing agent and low surface energy modifier heptadecafluorodecyltriethoxysilane FAS-17 to obtain liquid polymer mixture;
(4) placing the dry fiber preform in the closed metal mold; injecting the liquid polymer mixture into the dry fiber prefabricated forming body after die assembly until no bubble-free liquid colloid flows out of the glue outlet, and vacuumizing to obtain a workpiece;
(5) setting the pressure of a hot press to be 0.8Mpa and the temperature to be 120 ℃, preheating for 15min, then heating to 180 ℃, curing a workpiece in a closed metal mold for 150min, and slowly cooling after curing;
(6) and (3) after the temperature of the hot press is reduced to 80 ℃, unloading the pressure and opening the die, separating the solidified part from the closed metal die, and cleaning the defects of flash, burr and the like to obtain the polymer material with the ice coating prevention function.
The polymer material with the anti-icing function obtained by the method is an aramid fiber reinforced epoxy resin composite material with the anti-icing function.
Example 4
An integrated molding method of a polymer material with an anti-icing function comprises the following steps:
(1) preparing a closed 7075 aluminum alloy die with a micron-sized square pit array microstructure on the inner wall by using a precision numerical control lathe, cleaning for later use, and precoating a release agent;
(2) cutting the fiber cloth to a proper shape, and then wrapping the PVC foam core material to prepare a dry fiber prefabricated forming body; the fiber cloth is made of a high-strength carbon fiber material with the temperature of T700SC-12000-50 ℃, and the high-strength carbon fiber material is precoated with epoxy resin slurry; the core material is PVC foam with the size of 50mmx50mmx4 mm;
(3) according to the following steps of 3: 1: 0.01: mixing resin, curing agent, low surface energy modifier heptadecafluorodecyltriethoxysilane (FAS-17) and discontinuous fiber carbon nano tube at a ratio of 0.01 to obtain colloidal mixture; the diameter of the non-continuous fiber carbon nano tube is 2-20nm, and the length is 5-1000 μm;
(4) placing the dry fiber prefabricated forming body in the closed metal mold, injecting the mixed colloidal mixture into the dry fiber prefabricated forming body after mold closing, and vacuumizing to obtain a workpiece;
(5) setting the pressure of a hot press to be 0.8Mpa, preheating for 15min at the temperature of 120 ℃, then heating to 180 ℃, curing a workpiece in a closed metal mold for 150min, and slowly cooling after curing;
(6) and (3) after the temperature of the hot press is reduced to 80 ℃, unloading the pressure and opening the die, separating the solidified part from the closed metal die, and cleaning the defects of flash, burr and the like to obtain the polymer material with the ice coating prevention function.
The polymer material with the anti-icing function obtained by the method is a carbon fiber reinforced carbon nanotube dispersion-strengthened epoxy resin composite material with the anti-icing function.
Example 5
An integrated molding method of a polymer material with an anti-icing function comprises the following steps:
(1) preparing a closed 7075 aluminum alloy die with an inverted pyramid pit array microstructure on the inner wall by using a precision numerical control lathe, cleaning for later use, and precoating a release agent;
(2) cutting the fiber cloth to a proper shape, and then wrapping the PVC foam core material to prepare a dry fiber prefabricated forming body; the fiber cloth is made of a high-strength carbon fiber material with the temperature of T700SC-12000-50 ℃, and the high-strength carbon fiber material is precoated with epoxy resin slurry; the core material is PVC foam with the size of 50mmx50mmx4 mm;
(3) according to the following steps of 3: 1: mixing 0.01 mass ratio of resin, curing agent and low surface energy modifier heptadecafluorodecyltriethoxysilane FAS-17 to obtain liquid polymer mixture;
(4) placing the dry fiber preform in the closed metal mold; injecting the liquid polymer mixture into the dry fiber prefabricated forming body after die assembly until no bubble-free liquid colloid flows out of the glue outlet, and vacuumizing to obtain a workpiece;
(5) setting the pressure of a hot press to be 0.8Mpa, preheating for 15min at the temperature of 120 ℃, then heating to 180 ℃, curing a workpiece in a closed metal mold for 150min, and slowly cooling after curing;
(6) and (3) after the temperature of the hot press is reduced to 80 ℃, unloading the pressure and opening the die, separating the solidified part from the closed metal die, and cleaning the defects of flash, burr and the like to obtain the polymer material with the ice coating prevention function.
One polymer material with an anti-icing function which can be obtained by the method is a carbon fiber reinforced epoxy resin composite material with an anti-icing function.
The polymer materials with the ice coating prevention function prepared in examples 1 to 5 were subjected to performance tests, the test items include wetting angle, icing delay time and ice adhesion strength, and the test results are shown in table 1.
TABLE 1 polymer material Performance test results with anti-icing function
| Group of | Wetting angle (°) | Icing delay time(s) | Ice adhesion Strength (kpa) |
| Example 1 | 148.33 | 495 | 37.5 |
| Example 2 | 153.67 | 642 | 31.4 |
| Example 3 | 149.78 | 502 | 42.3 |
| Example 4 | 155.5 | 700 | 28.9 |
| Example 5 | 147.66 | 392 | 36.5 |
From the performance detection results, it can be seen that the polymer material with the anti-icing function prepared in the embodiments 1 to 5 has the characteristic that the surface has super-hydrophobic property to liquid water, and can significantly prolong the icing time of supercooled liquid drops, so that the supercooled liquid drops have enough time to separate from the surface; the composite material has the characteristics of extremely low ice adhesion strength and capability of falling off from the surface of the composite material under the action of natural wind power or gravity; the method can be used for covering the outer surface of the machine equipment exposed to extreme environments, such as aircraft and wind driven generator blades.
It should be understood that the above-described specific embodiments are merely illustrative of the present invention and are not intended to limit the present invention. Obvious variations or modifications which are within the spirit of the invention are possible within the scope of the invention.
Claims (8)
1. An integrated forming method of a polymer material with an ice-covering prevention function is characterized by comprising the following steps:
(1) preparing a closed metal die by a precision machining method, cleaning for later use, and precoating a release agent;
the die material of the closed metal die is corrosion-resistant steel, titanium alloy and high-strength aluminum alloy; the closed metal mold has a microstructure with a special shape, and is an inverted pyramid, a round or a square pit; the included angle between the side surface and the bottom surface of the inverted pyramid pit is 45-54 degrees, and the size ranges of the length, the width and the height are 1-200 mu m; the size range of the length and the height of the square pits is 1-200 mu m, the size range of the diameter and the depth of the round pits is 1-200 mu m, and the distance range of two adjacent inverted pyramids, round pits or square pits is 1-500 mu m;
(2) cutting the fiber cloth to a proper shape, and then wrapping the core material to obtain a dry fiber prefabricated forming body;
(3) mixing resin, a curing agent and a low surface energy modifier to obtain a liquid polymer mixture;
(4) placing the dry fiber prefabricated molding body in the closed metal mold, injecting the mixed liquid polymer mixture into the dry fiber prefabricated molding after mold closing, and vacuumizing to obtain a workpiece;
(5) setting the pressure and temperature of a hot press, curing the workpiece in the closed metal die for a certain time, controlling the pressure and temperature of the curing, and slowly cooling after the curing is finished;
(6) and (3) after the temperature of the hot press is reduced to 80 ℃ or room temperature, unloading the pressure and opening the die, separating the solidified workpiece from the closed metal die, and cleaning burrs and fins to obtain the polymer material with the ice coating prevention function.
2. The integrated forming method of polymer material with ice coating prevention function according to claim 1, wherein the material of the fiber cloth in the step (2) is one or more of glass fiber, carbon fiber, aramid fiber, asbestos fiber, potassium titanate fiber, silicon carbide fiber, natural fiber and hybrid fiber.
3. The integrated molding method of polymer material with ice covering prevention function of claim 1, wherein in step (3), the resin comprises one or more of polyester, vinyl ester, epoxy resin, phenolic resin, polyphenylene sulfide, polyether ether ketone and polyether imide.
4. The integrated molding method of polymer material with anti-icing function as claimed in claim 1, wherein the material used for the low surface energy modifier in step (3) is heptadecafluorodecyltriethoxysilane or stearic acid.
5. The integrated molding method of polymer material with ice coating prevention function as claimed in claim 1, wherein the liquid polymer mixture in step (3) is mixed with discontinuous fiber or particle reinforced phase, and the addition amount is 0.5-3% of the mass of resin; the discontinuous fiber comprises metal or ceramic whiskers and carbon nanotubes, and the particle reinforcing phase comprises metal or ceramic nanoparticles and graphene.
6. The integrated molding method of polymer material with anti-icing function according to claim 1, wherein the addition amount of the curing agent in the step (3) is 10-25% of the mass of the resin, and the addition amount of the low surface energy modifier is 0.1-2% of the mass of the resin.
7. The integrated molding method of polymer material with anti-icing function as claimed in claim 1, wherein the temperature range of the curing process in step (5) is 120 ℃ and 200 ℃, and the pressure range is 0.5-1.2 Mpa.
8. A polymer material with an anti-icing function, which is prepared by the method of any one of claims 1 to 7.
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| CN112950584B (en) * | 2021-03-01 | 2022-07-29 | 哈尔滨工程大学 | Coating surface defect identification method based on deep learning |
| CN113246560A (en) * | 2021-04-09 | 2021-08-13 | 南京航空航天大学 | Anti-icing and deicing composite material with electric heating/super-hydrophobic function and preparation method thereof |
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