CN111135996A - Preparation method of medium-temperature broadband wave-absorbing coating - Google Patents
Preparation method of medium-temperature broadband wave-absorbing coating Download PDFInfo
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Abstract
The invention discloses a preparation method of a medium-temperature broadband wave-absorbing coating, which comprises the following steps: (1) carrying out sand blasting treatment on the surface of a workpiece base material, and cleaning after sand blasting; (2) coating or spraying a bonding layer on the surface of the base material in the step (1); (3) coating or spraying a ferromagnetic wave-absorbing layer on the bonding layer in the step (2); (4) and (4) coating or spraying a heat insulation layer on the ferromagnetic wave absorbing layer in the step (3). The wave-absorbing coating prepared by the invention consists of the bonding layer at the bottom layer, the ferromagnetic wave-absorbing layer at the middle layer and the heat-insulating layer at the surface layer, and the influence of the medium-temperature 500 ℃ environment on the wave-absorbing effect of the ferromagnetic wave-absorbing layer is solved and the problem that the ferromagnetic wave-absorbing layer cannot be used under the medium-temperature condition is solved through the composition of the heat-insulating layer and the ferromagnetic wave-absorbing layer in a double-layer structure.
Description
Technical Field
The invention belongs to the technical field of material surface treatment, and particularly relates to a preparation method of a medium-temperature broadband wave-absorbing coating.
Background
The wave-absorbing material has simple process, convenient construction, easy replacement and maintenance, and is the development direction of stealth technology, wherein the wave-absorbing coating is the main form, the components of the wave-absorbing coating mainly comprise a wave-absorbing agent and a wave-transmitting material, and the wave-absorbing principle is as follows: when electromagnetic waves act on the surface of the wave-absorbing coating, the wave-transmitting material in the coating can enable the electromagnetic waves to effectively penetrate, when the penetrated electromagnetic waves meet wave-absorbing agent units dispersed in the coating, interaction occurs, the energy loss mechanism mainly comprises a resistance loss type, a dielectric loss type and a magnetic loss type, and the energy of the electromagnetic waves is finally converted into heat energy through the action modes, so that the effective absorption is realized.
At present, the traditional wave-absorbing coating adopts an electromagnetic wave-absorbing agent, the wave-absorbing frequency band is wide, the wave-absorbing peak value is high, but due to the limitation of the Curie temperature point of a ferromagnetic material, the high temperature resistance is insufficient, the electromagnetic parameters of the ferromagnetic material are obviously reduced at 500 ℃, and the wave-absorbing effect is obviously reduced; the high-temperature-resistant wave-absorbing coating is mostly an electric loss type wave-absorbing material, mainly a ceramic high-temperature wave-absorbing coating, most of wave-absorbing agents are SiC fibers, Si, barium titanate, C/C materials and the like, the coating is widely applied to the field of high-temperature wave absorption at the temperature of more than 1000 ℃, and compared with a magnetic wave-absorbing material applied at normal temperature, the high-temperature wave-absorbing material has the characteristics of high temperature resistance, high strength, low creep deformation, low expansion coefficient and strong corrosion resistance, but has a narrow absorption frequency band and a poor low-frequency wave-absorbing effect. Meanwhile, the ceramic material has large change of dielectric constant with temperature, poor dielectric loss performance of the wave absorbing agent at the medium temperature of 500 ℃, difficult exertion of wave absorbing property, narrower absorbing frequency band and poorer effect.
Chinese patent CN106497313A discloses a high temperature resistant wave-absorbing coating and application thereof, the wave-absorbing coating disclosed in the patent can endure the temperature of about 350 ℃ and can not endure the high temperature of 500 ℃, and the wave-absorbing coating is not provided with a bonding layer on the surface of a substrate, so that the bonding strength between the obtained wave-absorbing coating and the substrate is not very high; the patent coats carbonyl iron powder, and the method is difficult to coat flaky or other wave absorbing agent powder and has low universality; the structure of the high-temperature-resistant wave-absorbing coating disclosed by the patent is a structure of a heat insulation layer, a wave-absorbing layer and a heat insulation layer, wherein resin materials of the heat insulation layer and the wave-absorbing layer respectively adopt phenolic resin and bisphenol A type epoxy resin, and the resin materials of the heat insulation layer and the wave-absorbing layer are inconsistent and are easy to peel off from each other; the curing process of the patent needs heating curing, and has influence on the selection of the size, the shape and the like of the protective matrix; in the heat insulation mode in the patent, the ceramic filler is matched with the high-temperature-resistant resin to reduce heat conduction, substances on the surface layer of the heat insulation layer cannot be combusted, and the heat insulation effect is not good; meanwhile, the heat insulation layer only plays a role in heat insulation and does not play a role in wave absorption, and the overall wave absorption effect of the coating is not good.
Disclosure of Invention
The invention provides a preparation method of a medium-temperature broadband wave-absorbing coating, the prepared wave-absorbing coating consists of a bonding layer at the bottom layer, a ferromagnetic wave-absorbing layer at the middle layer and a heat-insulating layer at the surface layer, the heat-insulating layer isolates heat transmission, reduces the influence of temperature on the ferromagnetic wave-absorbing layer, has a certain wave-absorbing effect at the same time, does not influence the transmission of electromagnetic waves to the ferromagnetic wave-absorbing layer, the ferromagnetic wave-absorbing layer is protected by the heat-insulating layer, the temperature in the layer is lower than Curie temperature, the ferromagnetic wave-absorbing agent is not influenced by temperature, the high-efficiency and broadband wave-absorbing characteristics of the ferromagnetic wave-absorbing agent are kept, the influence of the medium-temperature 500 ℃ environment on the wave-absorbing effect of the ferromagnetic wave-absorbing layer is solved through the compounding of the double.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a medium-temperature broadband wave-absorbing coating comprises the following steps:
(1) carrying out sand blasting treatment on the surface of a workpiece base material, and cleaning the surface of the base material after sand blasting to obtain a clean base material surface;
(2) bonding layer treatment process:
coating or spraying a bonding layer on the surface of the clean base material obtained in the step (1), wherein the insulating paint used for the bonding layer is organic silicon rubber resin, polytetrafluoroethylene or polyurethane;
(3) and (3) ferromagnetic wave-absorbing layer treatment process:
3.1) uniformly mixing one or more ferromagnetic wave absorbers to obtain a ferromagnetic wave absorber mixed filler, wherein the ferromagnetic wave absorbers comprise lamellar carbonyl iron and spherical carbonyl iron, and the size range of the ferromagnetic wave absorbers is from several micrometers to dozens of micrometers;
3.2) uniformly mixing the ferromagnetic wave absorbing agent mixed filler obtained in the step 3.1) with a wave-transparent matrix to obtain a ferromagnetic wave absorbing layer coating, wherein the wave-transparent matrix is high-temperature-resistant silicone rubber resin, and the ferromagnetic wave absorbing agent mixed filler accounts for 50-60% of the wave-transparent matrix by mass;
3.3) coating or spraying the ferromagnetic wave-absorbing layer coating obtained in the step 3.2) on the bonding layer obtained in the step 2 to obtain a ferromagnetic wave-absorbing layer, wherein the thickness of the ferromagnetic wave-absorbing layer is 1-1.5 mm;
(4) and (3) a heat insulation layer treatment process:
4.1) taking the modified organic silicon rubber resin as a matrix, taking one or more of quartz powder, aluminum hydroxide, boric acid and light ceramic hollow microspheres as a filler, mixing the one or more fillers to obtain a mixed filler, and adding a diluent;
4.2) uniformly mixing the mixed filler obtained in the step 4.1) with the modified organic silicon rubber resin to obtain a heat-insulating layer coating, wherein the mixed filler accounts for 50-60% of the modified organic silicon rubber resin by mass;
4.3) coating or spraying the heat insulation layer coating obtained in the step 4.2) on the ferromagnetic wave absorbing layer obtained in the step 3.3) to obtain a heat insulation layer, wherein the thickness of the heat insulation layer is 1.5-2.5 mm.
Further, in the step (1), when the surface of the workpiece base material is subjected to sand blasting treatment, the sand blasting pressure is 0.2-0.4MPa, the sand used for sand blasting is 70-120 meshes of brown corundum, the workpiece is placed into an acetone solution after sand blasting, and is dried by a blower after being ultrasonically cleaned in an ultrasonic cleaning testing machine for 30min, and is placed into an alcohol solution after being dried, and is ultrasonically cleaned in the ultrasonic cleaning testing machine for 30min, and finally is dried by the blower, so that the clean surface of the base material is obtained.
Further, the air conditioner is provided with a fan,
for the sheet/spherical ferromagnetic temperature-resistant wave-absorbing coating with the heat-insulating layer, the bonding layer treatment process in the step (2) is specifically as follows: putting the workpiece with the clean substrate material surface obtained in the step (1) into a spraying workshop, vibrating and mixing A, B components of polyurethane emulsion for 5min to obtain polyurethane emulsion, adding catalysts, namely ethyl orthosilicate and dibutyltin dilaurate, into the polyurethane emulsion according to a conventional ratio, uniformly mixing to obtain bonding layer coating, putting the bonding layer coating into a pneumatic spray gun, spraying the clean substrate material surface by using the pneumatic spray gun, adjusting the thickness of the bonding layer by spraying times, controlling the thickness of the bonding layer to be 100 mu m, and curing at normal temperature to obtain the bonding layer;
for the sheet/sheet ferromagnetic temperature-resistant wave-absorbing coating with the heat-insulating layer, the bonding layer treatment process in the step (2) is specifically as follows: putting the workpiece with the clean substrate material surface obtained in the step (1) into a spraying workshop, mixing organic silicon rubber resin and a solvent namely dimethylbenzene in a vibration mode for 5min, adding a catalyst namely ethyl orthosilicate and dibutyltin dilaurate into the mixed solution according to a conventional proportion, uniformly mixing to obtain a bonding layer coating, putting the bonding layer coating into a pneumatic spray gun, spraying the clean substrate material surface by using the pneumatic spray gun, adjusting the thickness of the bonding layer by spraying times, controlling the thickness of the bonding layer to be 100 microns, and obtaining the bonding layer by adopting normal-temperature curing treatment.
Further, the air conditioner is provided with a fan,
for the sheet/spherical ferromagnetic temperature-resistant wave-absorbing coating with the heat-insulating layer, the ferromagnetic wave-absorbing layer treatment process in the step (3) is specifically as follows:
3.1) mixing a flaky iron powder wave absorbing agent with the particle size of more than 10 microns with a spherical carbonyl iron powder wave absorbing agent with the particle size of 1-2 microns in a mass ratio of 1:1, mechanically stirring for 20min, ultrasonically vibrating for 10min, and circulating the operation for 2 times to uniformly mix the ferromagnetic wave absorbing agents with different sizes and shapes so as to obtain a ferromagnetic wave absorbing agent mixed filler;
3.2) mixing the ferromagnetic wave absorbing agent mixed filler obtained in the step 3.1) with a high-temperature-resistant silicon rubber resin wave-transmitting matrix, mechanically stirring for 10min, ultrasonically oscillating for 20min, and circulating the operation for 2 times, wherein the stirring speed and other parameters are uniformly mixed to obtain an original coating of a ferromagnetic wave absorbing layer, and the ferromagnetic wave absorbing agent mixed filler accounts for 50-60% of the high-temperature-resistant silicon rubber resin wave-transmitting matrix by mass;
3.3) adding catalysts, namely ethyl orthosilicate and dibutyltin dilaurate, into the original coating of the ferromagnetic wave-absorbing layer obtained in the step 3.2) according to the conventional proportion, uniformly mixing to obtain a coating of the ferromagnetic wave-absorbing layer, putting the coating of the ferromagnetic wave-absorbing layer into a pneumatic spray gun, spraying the bonding layer in the step (2) by using a pneumatic spray gun, wherein the pneumatic spraying adopts multiple spraying to meet the thickness requirement, and the moving speed of the pneumatic spray gun is adjusted according to the shape of the workpiece and the requirement of the thickness of each section of coating, the thickness of the coating in each reciprocating spraying period is 120 +/-2 mu m, the spraying is stopped for 3min and the workpiece does not stop rotating every 3-4 spraying periods, so as to be beneficial to leveling of the coating, volatilizing the solvent and carrying out primary curing, and repeating the spraying process after finishing, the pressure of the spraying gas is 0.2-0.4MPa until the thickness of the ferromagnetic absorbing layer reaches 1-1.5 mm;
for the sheet/sheet-shaped ferromagnetic temperature-resistant wave-absorbing coating with the heat-insulating layer, the ferromagnetic wave-absorbing layer treatment process in the step (3) is specifically as follows:
3.1) mixing the flaky iron powder wave absorbing agent with the particle size of more than 10 microns with the flaky iron powder wave absorbing agent with the particle size of 1-2 microns in a mass ratio of 1:1, mechanically stirring for 20min, ultrasonically vibrating for 10min, and circulating the operation for 2 times to uniformly mix the ferromagnetic wave absorbing agents with different sizes so as to obtain the ferromagnetic wave absorbing agent mixed filler;
3.2) mixing the ferromagnetic wave absorbing agent mixed filler obtained in the step 3.1) with a high-temperature-resistant silicon rubber resin wave-transmitting matrix, mechanically stirring for 10min, ultrasonically oscillating for 20min, and circulating the operation for 2 times, wherein the stirring speed and other parameters are uniformly mixed to obtain an original coating of a ferromagnetic wave absorbing layer, and the ferromagnetic wave absorbing agent mixed filler accounts for 50-60% of the high-temperature-resistant silicon rubber resin wave-transmitting matrix by mass;
3.3) adding catalysts, namely ethyl orthosilicate and dibutyltin dilaurate, into the original coating of the ferromagnetic wave-absorbing layer obtained in the step 3.2) according to the conventional proportion, uniformly mixing to obtain a coating of the ferromagnetic wave-absorbing layer, putting the coating of the ferromagnetic wave-absorbing layer into a pneumatic spray gun, spraying the bonding layer in the step (2) by using a pneumatic spray gun, wherein the pneumatic spraying adopts multiple spraying to meet the thickness requirement, and the moving speed of the pneumatic spray gun is adjusted according to the shape of the workpiece and the requirement of the thickness of each section of coating, the thickness of the coating in each reciprocating spraying period is 120 +/-2 mu m, the spraying is stopped for 3min and the workpiece does not stop rotating every 3-4 spraying periods, so as to be beneficial to leveling of the coating, volatilizing the solvent and carrying out primary curing, and repeating the spraying process after finishing, and the spraying gas pressure is 0.2-0.4MPa until the thickness of the ferromagnetic absorbing layer reaches 1-1.5 mm.
Further, the heat insulation layer treatment process in the step (4) specifically comprises the following steps:
4.1) taking the modified organic silicon rubber resin as a matrix, and mixing quartz powder: aluminum hydroxide: boric acid: mixing the light ceramic hollow microspheres in a mass ratio of 1:1:1:2 to obtain a mixed filler, and adding a diluent;
4.2) mixing the mixed filler obtained in the step 4.1) with the modified organic silicon rubber resin, mechanically stirring for 10min, ultrasonically oscillating for 20min, and circulating the operation for 2 times, wherein the stirring speed and other parameters are uniformly mixed to obtain the original coating of the heat-insulating layer, and the mass ratio of the mixed filler to the modified organic silicon rubber resin is 50-60%;
4.3) adding a catalyst, namely ethyl orthosilicate and dibutyltin dilaurate, into the original coating of the thermal insulation layer in the step 4.2) according to a conventional proportion, uniformly mixing to obtain a thermal insulation layer coating, putting the thermal insulation layer coating into a pneumatic spray gun, spraying the ferromagnetic wave absorbing layer in the step 3.3) by using the pneumatic spray gun, stopping spraying for 3min without stopping the rotation of the workpiece when the pneumatic spraying is carried out for 3-4 periods by adopting multiple spraying to meet the thickness requirement, adjusting the moving speed of the pneumatic spray gun according to the shape of the workpiece and the thickness of the coating of each period, wherein the thickness of the coating in each reciprocating spraying period is 120 +/-2 mu m, so that the leveling and solvent volatilization of the coating are facilitated, carrying out primary curing, and repeating the spraying process after finishing until the thickness of the thermal insulation layer reaches 1.5 mm.
Further, in step 4.1): the light ceramic hollow micro-beads are light ceramic SiO2Hollow micro-bead, light ceramic SiO2The hollow microspheres have a particle size of 120 μm and a bulk density of 0.3g/cm3And the diluent is 120# solvent oil.
The wave-absorbing coating prepared by the invention, which consists of the bonding layer at the bottom layer, the ferromagnetic wave-absorbing layer at the middle layer and the heat-insulating layer at the surface layer, keeps the high-efficiency absorption characteristic of the ferromagnetic wave-absorbing layer and simultaneously improves the environmental adaptability of the wave-absorbing coating, and the principle is as follows: under the high-speed flying environment, the surface of the wave-absorbing coating is heated due to air friction, the peak temperature reaches 500 ℃, the heat conduction of the heat-insulating layer is reduced by the filler such as light ceramic hollow microspheres distributed in the layer, the heat generated by friction is taken away through the surface combustion of the organic silicon rubber resin matrix, the heat reaching the surface of the ferromagnetic wave-absorbing layer is effectively reduced, the surface temperature of the ferromagnetic wave-absorbing layer is reduced to be below 200 ℃, the temperature of the ferromagnetic wave-absorbing layer is lower than the Curie temperature, so that the ferromagnetic wave-absorbing layer is prevented from being influenced by the temperature, meanwhile, the material of the heat-insulating layer has better compatibility with the ferromagnetic wave-absorbing layer, the matrix resin material adopted by the heat-insulating layer can be consistent with the matrix resin of the ferromagnetic wave-absorbing layer, the main body of the heat-insulating layer is a wave-permeable, after reaching the ferromagnetic wave-absorbing layer, the ferromagnetic material is protected by the heat-insulating layer, so that the broadband efficient absorption characteristic of the ferromagnetic material is kept, electromagnetic waves are further attenuated, electromagnetic wave gradient absorption is formed, meanwhile, the integral consistency of the coating structure can be improved due to the continuous resin matrix, so that the broadband efficient electromagnetic wave absorption can be kept at 500 ℃, meanwhile, impurities on the surface of the coating can be taken away along with the partial combustion of the surface of the heat-insulating layer, the influence of the impurities on the penetration of the electromagnetic waves is reduced, and the absorption effect of the coating on the electromagnetic waves is ensured.
Compared with the prior art, the invention has the beneficial effects that:
the heat insulation filler and the wave absorption filler are respectively added into the matrix resin to respectively obtain the heat insulation layer and the ferromagnetic wave absorption layer, the matrix resin of the heat insulation layer and the matrix resin of the ferromagnetic wave absorption layer adopt the same or similar resin systems, so that the heat insulation layer and the wave absorption layer have better consistency, the heat conduction is isolated through the heat insulation layer, the heat is taken away through the surface combustion consumption of the heat insulation layer, the surface temperature of the coating is reduced, the internal temperature of the ferromagnetic wave absorption layer is lower than the Curie temperature, the ferromagnetic wave absorption agent in the ferromagnetic wave absorption layer keeps the high absorption characteristic, the temperature resistance of the matrix is improved through the high-temperature resin, and the ferromagnetic wave absorption agent of the ferromagnetic wave absorption layer is kept to efficiently absorb electromagnetic waves, and the coating with: 1) the structural coating keeps the high-efficiency absorption characteristic of the ferromagnetic wave-absorbing layer in the environment of 500 ℃; 2) the surface of the heat insulation layer can take away heat and combustion impurities through combustion in a high-speed flying environment, so that the transmission characteristic of the surface of the coating to electromagnetic waves is ensured, and the absorption effect of the coating is improved; 3) part of the filler in the heat insulation layer has an electromagnetic wave absorption effect, and can improve the electromagnetic wave absorption effect and the frequency band; 4) the coating structure has good continuity, and the engineering application is more flexible and easy to operate;
in the invention, the bonding layer can improve the bonding strength of the ferromagnetic wave-absorbing layer and the matrix;
in the invention, the adopted wave absorbing agent is not subjected to special treatment such as coating, the application range is wide, and the absorption efficiency is favorably improved; the structure of the medium-temperature wide-band wave-absorbing coating disclosed by the invention is a structure comprising a bonding layer, a wave-absorbing layer and a heat-insulating layer, wherein the heat-insulating layer and the wave-absorbing layer are both made of silicone rubber resin, and the continuity of a resin matrix is good, so that the integrity and consistency of the whole coating can be improved, the interlayer peeling is not easy to occur, and the mechanical property is better; the curing mode in the invention is normal temperature curing, and the size, shape and the like of the matrix have little influence on the curing process; the heat insulation mode in the invention not only comprises a mode of reducing heat conduction, but also takes away heat by burning and consuming surface substances of the heat insulation layer, so that the heat insulation effect is better; the light ceramic hollow microsphere structure and other fillers contained in the heat-insulating layer have certain electromagnetic wave absorption effect, the heat-insulating layer can absorb part of electromagnetic waves, and multi-stage absorption is formed by the heat-insulating layer and the wave-absorbing layer, and meanwhile, the absorption frequency band of the coating of the invention basically covers 2-18GHZ, the peak power is high, and the overall absorption effect of the coating is better.
Drawings
FIG. 1 is a schematic diagram of the principle of absorbing electromagnetic waves by a heat-insulating layer and a wave-absorbing layer in the present invention;
FIG. 2 is a schematic illustration of the frictional heating of an insulation pack and the heat removal from the combustion of the insulation pack in accordance with the present invention during flight of an aircraft;
FIG. 3 is a schematic comparison of a wave-absorbing coating with a thermal insulation layer and a wave-absorbing coating without a thermal insulation layer after the temperature is increased;
FIG. 4 is a scanning electron microscope image of a double-layer structure formed by a heat-insulating layer and a wave-absorbing layer in the invention;
FIG. 5 is an XRD spectrum of a mixed flake iron powder (wave absorber) after treatment at different temperatures for 1h in example 2;
FIG. 6 is a wave-absorbing performance diagram of a wave-absorbing layer obtained by mixing flaky iron powder without a heat-insulating layer at different temperatures;
FIG. 7 is a wave-absorbing performance diagram of a mixed flaky iron powder temperature-resistant wave-absorbing layer with a 1.5mm thermal-insulating layer at different temperatures.
Detailed Description
Example 1
For a sheet/spherical ferromagnetic temperature-resistant wave-absorbing coating with a heat-insulating layer, a preparation method of a medium-temperature wide-band wave-absorbing coating comprises the following steps:
(1) the sand blasting pressure when the surface of a workpiece base material is subjected to sand blasting treatment is 0.2-0.4MPa, the sand used for sand blasting is brown corundum sand of 70-120 meshes, the workpiece is placed into an acetone solution after sand blasting, is subjected to ultrasonic cleaning in an ultrasonic cleaning testing machine for 30min and then is dried by a blower, the workpiece is placed into an alcohol solution after being dried, is subjected to ultrasonic cleaning in the ultrasonic cleaning testing machine for 30min and finally is dried by the blower, and the clean surface of the base material is obtained;
(2) bonding layer treatment process:
putting the workpiece with the clean substrate material surface obtained in the step (1) into a spraying workshop, vibrating and mixing A, B components of polyurethane emulsion for 5min to obtain polyurethane emulsion, adding catalysts, namely ethyl orthosilicate and dibutyltin dilaurate, into the polyurethane emulsion according to a conventional ratio, uniformly mixing to obtain bonding layer coating, putting the bonding layer coating into a pneumatic spray gun, spraying the clean substrate material surface by using the pneumatic spray gun, adjusting the thickness of the bonding layer by spraying times, controlling the thickness of the bonding layer to be 100 mu m, and curing at normal temperature to obtain the bonding layer;
(3) and (3) ferromagnetic wave-absorbing layer treatment process:
3.1) mixing a flaky iron powder wave absorbing agent with the particle size of more than 10 microns with a spherical carbonyl iron powder wave absorbing agent with the particle size of 1-2 microns in a mass ratio of 1:1, mechanically stirring for 20min, ultrasonically vibrating for 10min, and circulating the operation for 2 times to uniformly mix the ferromagnetic wave absorbing agents with different sizes and shapes so as to obtain a ferromagnetic wave absorbing agent mixed filler;
3.2) mixing the ferromagnetic wave absorbing agent mixed filler obtained in the step 3.1) with a high-temperature-resistant silicon rubber resin wave-transmitting matrix, mechanically stirring for 10min, ultrasonically oscillating for 20min, and circulating the operation for 2 times, wherein the stirring speed and other parameters are uniformly mixed to obtain an original coating of a ferromagnetic wave absorbing layer, and the ferromagnetic wave absorbing agent mixed filler accounts for 50-60% of the high-temperature-resistant silicon rubber resin wave-transmitting matrix by mass;
3.3) adding catalysts, namely ethyl orthosilicate and dibutyltin dilaurate, into the original coating of the ferromagnetic wave-absorbing layer obtained in the step 3.2) according to the conventional proportion, uniformly mixing to obtain a coating of the ferromagnetic wave-absorbing layer, putting the coating of the ferromagnetic wave-absorbing layer into a pneumatic spray gun, spraying the bonding layer in the step (2) by using a pneumatic spray gun, wherein the pneumatic spraying adopts multiple spraying to meet the thickness requirement, and the moving speed of the pneumatic spray gun is adjusted according to the shape of the workpiece and the requirement of the thickness of each section of coating, the thickness of the coating in each reciprocating spraying period is 120 +/-2 mu m, the spraying is stopped for 3min and the workpiece does not stop rotating every 3-4 spraying periods, so as to be beneficial to leveling of the coating, volatilizing the solvent and carrying out primary curing, and repeating the spraying process after finishing, the pressure of the spraying gas is 0.2-0.4MPa until the thickness of the ferromagnetic absorbing layer reaches 1-1.5 mm;
(4) and (3) a heat insulation layer treatment process:
4.1) taking the modified organic silicon rubber resin as a matrix, and mixing quartz powder: aluminum hydroxide: boric acid: mixing the light ceramic hollow microspheres in a mass ratio of 1:1:1:2 to obtain a mixed filler, and adding a diluent;
4.2) mixing the mixed filler obtained in the step 4.1) with the modified organic silicon rubber resin, mechanically stirring for 10min, ultrasonically oscillating for 20min, and circulating the operation for 2 times, wherein the stirring speed and other parameters are uniformly mixed to obtain the original coating of the heat-insulating layer, and the mass ratio of the mixed filler to the modified organic silicon rubber resin is 50-60%;
4.3) adding a catalyst, namely ethyl orthosilicate and dibutyltin dilaurate, into the original coating of the thermal insulation layer in the step 4.2) according to a conventional proportion, uniformly mixing to obtain a thermal insulation layer coating, putting the thermal insulation layer coating into a pneumatic spray gun, spraying the ferromagnetic wave absorbing layer in the step 3.3) by using the pneumatic spray gun, stopping spraying for 3min without stopping the rotation of the workpiece when the pneumatic spraying is carried out for 3-4 periods by adopting multiple spraying to meet the thickness requirement, adjusting the moving speed of the pneumatic spray gun according to the shape of the workpiece and the thickness of the coating of each period, wherein the thickness of the coating in each reciprocating spraying period is 120 +/-2 mu m, so that the leveling and solvent volatilization of the coating are facilitated, carrying out primary curing, and repeating the spraying process after finishing until the thickness of the thermal insulation layer reaches 1.5 mm.
Wherein, in the step 4.1), the light ceramic hollow microspheres are light ceramic SiO2Hollow micro-bead, light ceramic SiO2The hollow microspheres have a particle size of 120 μm and a bulk density of 0.3g/cm3And the diluent is 120# solvent oil.
Example 2
For a sheet/sheet ferromagnetic temperature-resistant wave-absorbing coating with a heat-insulating layer, a preparation method of a medium-temperature broadband wave-absorbing coating comprises the following steps:
(1) the sand blasting pressure when the surface of a workpiece base material is subjected to sand blasting treatment is 0.2-0.4MPa, the sand used for sand blasting is brown corundum sand of 70-120 meshes, the workpiece is placed into an acetone solution after sand blasting, is subjected to ultrasonic cleaning in an ultrasonic cleaning testing machine for 30min and then is dried by a blower, the workpiece is placed into an alcohol solution after being dried, is subjected to ultrasonic cleaning in the ultrasonic cleaning testing machine for 30min and finally is dried by the blower, and the clean surface of the base material is obtained;
(2) bonding layer treatment process:
putting the workpiece with the clean substrate material surface obtained in the step (1) into a spraying workshop, mixing organic silicon rubber resin and a solvent namely dimethylbenzene in a vibration mode for 5min, adding a catalyst namely ethyl orthosilicate and dibutyltin dilaurate into the mixed solution according to a conventional proportion, uniformly mixing to obtain a bonding layer coating, putting the bonding layer coating into a pneumatic spray gun, spraying the bonding layer coating on the clean substrate material surface by using the pneumatic spray gun, adjusting the thickness of the bonding layer by spraying times, controlling the thickness of the bonding layer to be 100 microns, and obtaining the bonding layer by adopting normal-temperature curing treatment;
(3) and (3) ferromagnetic wave-absorbing layer treatment process:
3.1) mixing the flaky iron powder wave absorbing agent with the particle size of more than 10 microns with the flaky iron powder wave absorbing agent with the particle size of 1-2 microns in a mass ratio of 1:1, mechanically stirring for 20min, ultrasonically vibrating for 10min, and circulating the operation for 2 times to uniformly mix the ferromagnetic wave absorbing agents with different sizes so as to obtain the ferromagnetic wave absorbing agent mixed filler;
3.2) mixing the ferromagnetic wave absorbing agent mixed filler obtained in the step 3.1) with a high-temperature-resistant silicon rubber resin wave-transmitting matrix, mechanically stirring for 10min, ultrasonically oscillating for 20min, and circulating the operation for 2 times, wherein the stirring speed and other parameters are uniformly mixed to obtain an original coating of a ferromagnetic wave absorbing layer, and the ferromagnetic wave absorbing agent mixed filler accounts for 50-60% of the high-temperature-resistant silicon rubber resin wave-transmitting matrix by mass;
3.3) adding catalysts, namely ethyl orthosilicate and dibutyltin dilaurate, into the original coating of the ferromagnetic wave-absorbing layer obtained in the step 3.2) according to the conventional proportion, uniformly mixing to obtain a coating of the ferromagnetic wave-absorbing layer, putting the coating of the ferromagnetic wave-absorbing layer into a pneumatic spray gun, spraying the bonding layer in the step (2) by using a pneumatic spray gun, wherein the pneumatic spraying adopts multiple spraying to meet the thickness requirement, and the moving speed of the pneumatic spray gun is adjusted according to the shape of the workpiece and the requirement of the thickness of each section of coating, the thickness of the coating in each reciprocating spraying period is 120 +/-2 mu m, the spraying is stopped for 3min and the workpiece does not stop rotating every 3-4 spraying periods, so as to be beneficial to leveling of the coating, volatilizing the solvent and carrying out primary curing, and repeating the spraying process after finishing, and the spraying gas pressure is 0.2-0.4MPa until the thickness of the ferromagnetic absorbing layer reaches 1-1.5 mm.
(4) And (3) a heat insulation layer treatment process:
4.1) taking the modified organic silicon rubber resin as a matrix, and mixing quartz powder: aluminum hydroxide: boric acid: mixing the light ceramic hollow microspheres in a mass ratio of 1:1:1:2 to obtain a mixed filler, and adding a diluent;
4.2) mixing the mixed filler obtained in the step 4.1) with the modified organic silicon rubber resin, mechanically stirring for 10min, ultrasonically oscillating for 20min, and circulating the operation for 2 times, wherein the stirring speed and other parameters are uniformly mixed to obtain the original coating of the heat-insulating layer, and the mass ratio of the mixed filler to the modified organic silicon rubber resin is 50-60%;
4.3) adding a catalyst, namely ethyl orthosilicate and dibutyltin dilaurate, into the original coating of the thermal insulation layer in the step 4.2) according to a conventional proportion, uniformly mixing to obtain a thermal insulation layer coating, putting the thermal insulation layer coating into a pneumatic spray gun, spraying the ferromagnetic wave absorbing layer in the step 3.3) by using the pneumatic spray gun, stopping spraying for 3min without stopping the rotation of the workpiece when the pneumatic spraying is carried out for 3-4 periods by adopting multiple spraying to meet the thickness requirement, adjusting the moving speed of the pneumatic spray gun according to the shape of the workpiece and the thickness of the coating of each period, wherein the thickness of the coating in each reciprocating spraying period is 120 +/-2 mu m, so that the leveling and solvent volatilization of the coating are facilitated, carrying out primary curing, and repeating the spraying process after finishing until the thickness of the thermal insulation layer reaches 1.5 mm.
Wherein, in the step 4.1): the light ceramic hollow micro-beads are light ceramic SiO2Hollow micro-bead, light ceramic SiO2The hollow microbead has a granularity of 120 mu m and a bulk density of 0.3 g/mlcm3And the diluent is 120# solvent oil.
As can be seen from fig. 3, the wave-absorbing coating with the thermal insulation layer generates heat by friction in high altitude, the surface of the thermal insulation layer burns to take away the heat, the mixed filler in the thermal insulation layer isolates the heat conduction, so that the temperature reaching the wave-absorbing layer is reduced, namely, the temperature of the wave-absorbing layer rises slowly, the temperature of the ferromagnetic wave-absorbing agent in the wave-absorbing layer is lower than the curie temperature, and the ferromagnetic wave-absorbing agent in the wave-absorbing layer can maintain the broadband efficient absorption characteristic; the wave-absorbing coating without the heat-insulating layer generates heat through friction in high altitude, so that the temperature is rapidly increased, and the ferromagnetic wave-absorbing agent loses efficacy after the temperature of the ferromagnetic wave-absorbing agent is higher than the Curie temperature.
As is clear from fig. 5, when the temperature of the ferromagnetic wave absorbing agent powder is increased to 200 degrees or more, oxidation starts to occur, and when the temperature is increased to 300 degrees or more, the ferromagnetic wave absorbing agent powder is significantly oxidized and loses ferromagnetism.
As can be seen from fig. 6, the reflection loss of the ferromagnetic wave-absorbing layer without the thermal insulation layer to the electromagnetic wave gradually decreases with the increase of the temperature, that is, the wave-absorbing performance of the ferromagnetic wave-absorbing layer without the thermal insulation layer to the electromagnetic wave gradually decreases with the increase of the temperature, when the temperature reaches 500 ℃, the reflection loss of the ferromagnetic wave-absorbing layer without the thermal insulation layer to the electromagnetic wave is substantially zero, that is, when the temperature reaches 500 ℃, the ferromagnetic wave-absorbing layer without the thermal insulation layer does not substantially absorb the electromagnetic wave.
As can be seen from fig. 7, the reflection loss of the mixed flaky iron powder temperature-resistant wave-absorbing layer with the 1.5mm heat-insulating layer to the electromagnetic wave does not change with the rise of the temperature basically, which shows that the heat-insulating layer protects the wave-absorbing layer so that the wave-absorbing layer is not affected by the temperature, and the wave-absorbing layer can still effectively absorb the electromagnetic wave even at the temperature of 500 ℃.
Claims (6)
1. A preparation method of a medium-temperature broadband wave-absorbing coating is characterized by comprising the following steps:
(1) carrying out sand blasting treatment on the surface of a workpiece base material, and cleaning the surface of the base material after sand blasting to obtain a clean base material surface;
(2) bonding layer treatment process:
coating or spraying a bonding layer on the surface of the clean base material obtained in the step (1), wherein the insulating paint used for the bonding layer is organic silicon rubber resin, polytetrafluoroethylene or polyurethane;
(3) and (3) ferromagnetic wave-absorbing layer treatment process:
3.1) uniformly mixing one or more ferromagnetic wave absorbers to obtain a ferromagnetic wave absorber mixed filler, wherein the ferromagnetic wave absorbers comprise lamellar carbonyl iron and spherical carbonyl iron, and the size range of the ferromagnetic wave absorbers is from several micrometers to dozens of micrometers;
3.2) uniformly mixing the ferromagnetic wave absorbing agent mixed filler obtained in the step 3.1) with a wave-transparent matrix to obtain a ferromagnetic wave absorbing layer coating, wherein the wave-transparent matrix is high-temperature-resistant silicone rubber resin, and the ferromagnetic wave absorbing agent mixed filler accounts for 50-60% of the wave-transparent matrix by mass;
3.3) coating or spraying the ferromagnetic wave-absorbing layer coating obtained in the step 3.2) on the bonding layer obtained in the step 2 to obtain a ferromagnetic wave-absorbing layer, wherein the thickness of the ferromagnetic wave-absorbing layer is 1-1.5 mm;
(4) and (3) a heat insulation layer treatment process:
4.1) taking the modified organic silicon rubber resin as a matrix, taking one or more of quartz powder, aluminum hydroxide, boric acid and light ceramic hollow microspheres as a filler, mixing the one or more fillers to obtain a mixed filler, and adding a diluent;
4.2) uniformly mixing the mixed filler obtained in the step 4.1) with the modified organic silicon rubber resin to obtain a heat-insulating layer coating, wherein the mixed filler accounts for 50-60% of the modified organic silicon rubber resin by mass;
4.3) coating or spraying the heat insulation layer coating obtained in the step 4.2) on the ferromagnetic wave absorbing layer obtained in the step 3.3) to obtain a heat insulation layer, wherein the thickness of the heat insulation layer is 1.5-2.5 mm.
2. The method for preparing a medium-temperature broadband wave-absorbing coating according to claim 1, wherein in the step (1), the sand blasting pressure is 0.2-0.4MPa when the surface of a workpiece base material is subjected to sand blasting, the sand used for sand blasting is 70-120 meshes of brown corundum, the workpiece is placed into an acetone solution after sand blasting, and is subjected to ultrasonic cleaning in an ultrasonic cleaning tester for 30min and then is dried by a blower, the workpiece is placed into an alcohol solution after drying, and is subjected to ultrasonic cleaning in the ultrasonic cleaning tester for 30min and finally is dried by the blower, and a clean surface of the base material is obtained.
3. The preparation method of the medium-temperature broadband wave-absorbing coating according to claim 2, characterized in that:
for the sheet/spherical ferromagnetic temperature-resistant wave-absorbing coating with the heat-insulating layer, the bonding layer treatment process in the step (2) is specifically as follows: putting the workpiece with the clean substrate material surface obtained in the step (1) into a spraying workshop, vibrating and mixing A, B components of polyurethane emulsion for 5min to obtain polyurethane emulsion, adding catalysts, namely ethyl orthosilicate and dibutyltin dilaurate, into the polyurethane emulsion according to a conventional ratio, uniformly mixing to obtain bonding layer coating, putting the bonding layer coating into a pneumatic spray gun, spraying the clean substrate material surface by using the pneumatic spray gun, adjusting the thickness of the bonding layer by spraying times, controlling the thickness of the bonding layer to be 100 mu m, and curing at normal temperature to obtain the bonding layer;
for the sheet/sheet ferromagnetic temperature-resistant wave-absorbing coating with the heat-insulating layer, the bonding layer treatment process in the step (2) is specifically as follows: putting the workpiece with the clean substrate material surface obtained in the step (1) into a spraying workshop, mixing organic silicon rubber resin and a solvent namely dimethylbenzene in a vibration mode for 5min, adding a catalyst namely ethyl orthosilicate and dibutyltin dilaurate into the mixed solution according to a conventional proportion, uniformly mixing to obtain a bonding layer coating, putting the bonding layer coating into a pneumatic spray gun, spraying the clean substrate material surface by using the pneumatic spray gun, adjusting the thickness of the bonding layer by spraying times, controlling the thickness of the bonding layer to be 100 microns, and obtaining the bonding layer by adopting normal-temperature curing treatment.
4. The preparation method of the medium-temperature wide-band wave-absorbing coating according to claim 3, characterized in that:
for the sheet/spherical ferromagnetic temperature-resistant wave-absorbing coating with the heat-insulating layer, the ferromagnetic wave-absorbing layer treatment process in the step (3) is specifically as follows:
3.1) mixing a flaky iron powder wave absorbing agent with the particle size of more than 10 microns with a spherical carbonyl iron powder wave absorbing agent with the particle size of 1-2 microns in a mass ratio of 1:1, mechanically stirring for 20min, ultrasonically vibrating for 10min, and circulating the operation for 2 times to uniformly mix the ferromagnetic wave absorbing agents with different sizes and shapes so as to obtain a ferromagnetic wave absorbing agent mixed filler;
3.2) mixing the ferromagnetic wave absorbing agent mixed filler obtained in the step 3.1) with a high-temperature-resistant silicon rubber resin wave-transmitting matrix, mechanically stirring for 10min, ultrasonically oscillating for 20min, and circulating the operation for 2 times, wherein the stirring speed and other parameters are uniformly mixed to obtain an original coating of a ferromagnetic wave absorbing layer, and the ferromagnetic wave absorbing agent mixed filler accounts for 50-60% of the high-temperature-resistant silicon rubber resin wave-transmitting matrix by mass;
3.3) adding catalysts, namely ethyl orthosilicate and dibutyltin dilaurate, into the original coating of the ferromagnetic wave-absorbing layer obtained in the step 3.2) according to the conventional proportion, uniformly mixing to obtain a coating of the ferromagnetic wave-absorbing layer, putting the coating of the ferromagnetic wave-absorbing layer into a pneumatic spray gun, spraying the bonding layer in the step (2) by using a pneumatic spray gun, wherein the pneumatic spraying adopts multiple spraying to meet the thickness requirement, and the moving speed of the pneumatic spray gun is adjusted according to the shape of the workpiece and the requirement of the thickness of each section of coating, the thickness of the coating in each reciprocating spraying period is 120 +/-2 mu m, the spraying is stopped for 3min and the workpiece does not stop rotating every 3-4 spraying periods, so as to be beneficial to leveling of the coating, volatilizing the solvent and carrying out primary curing, and repeating the spraying process after finishing, the pressure of the spraying gas is 0.2-0.4MPa until the thickness of the ferromagnetic absorbing layer reaches 1-1.5 mm;
for the sheet/sheet-shaped ferromagnetic temperature-resistant wave-absorbing coating with the heat-insulating layer, the ferromagnetic wave-absorbing layer treatment process in the step (3) is specifically as follows:
3.1) mixing the flaky iron powder wave absorbing agent with the particle size of more than 10 microns with the flaky iron powder wave absorbing agent with the particle size of 1-2 microns in a mass ratio of 1:1, mechanically stirring for 20min, ultrasonically vibrating for 10min, and circulating the operation for 2 times to uniformly mix the ferromagnetic wave absorbing agents with different sizes so as to obtain the ferromagnetic wave absorbing agent mixed filler;
3.2) mixing the ferromagnetic wave absorbing agent mixed filler obtained in the step 3.1) with a high-temperature-resistant silicon rubber resin wave-transmitting matrix, mechanically stirring for 10min, ultrasonically oscillating for 20min, and circulating the operation for 2 times, wherein the stirring speed and other parameters are uniformly mixed to obtain an original coating of a ferromagnetic wave absorbing layer, and the ferromagnetic wave absorbing agent mixed filler accounts for 50-60% of the high-temperature-resistant silicon rubber resin wave-transmitting matrix by mass;
3.3) adding catalysts, namely ethyl orthosilicate and dibutyltin dilaurate, into the original coating of the ferromagnetic wave-absorbing layer obtained in the step 3.2) according to the conventional proportion, uniformly mixing to obtain a coating of the ferromagnetic wave-absorbing layer, putting the coating of the ferromagnetic wave-absorbing layer into a pneumatic spray gun, spraying the bonding layer in the step (2) by using a pneumatic spray gun, wherein the pneumatic spraying adopts multiple spraying to meet the thickness requirement, and the moving speed of the pneumatic spray gun is adjusted according to the shape of the workpiece and the requirement of the thickness of each section of coating, the thickness of the coating in each reciprocating spraying period is 120 +/-2 mu m, the spraying is stopped for 3min and the workpiece does not stop rotating every 3-4 spraying periods, so as to be beneficial to leveling of the coating, volatilizing the solvent and carrying out primary curing, and repeating the spraying process after finishing, and the spraying gas pressure is 0.2-0.4MPa until the thickness of the ferromagnetic absorbing layer reaches 1-1.5 mm.
5. The preparation method of the medium-temperature broadband wave-absorbing coating according to claim 1 or 4, wherein the treatment process of the heat-insulating layer in the step (4) is as follows:
4.1) taking the modified organic silicon rubber resin as a matrix, and mixing quartz powder: aluminum hydroxide: boric acid: mixing the light ceramic hollow microspheres in a mass ratio of 1:1:1:2 to obtain a mixed filler, and adding a diluent;
4.2) mixing the mixed filler obtained in the step 4.1) with the modified organic silicon rubber resin, mechanically stirring for 10min, ultrasonically oscillating for 20min, and circulating the operation for 2 times, wherein the stirring speed and other parameters are uniformly mixed to obtain the original coating of the heat-insulating layer, and the mass ratio of the mixed filler to the modified organic silicon rubber resin is 50-60%;
4.3) adding a catalyst, namely ethyl orthosilicate and dibutyltin dilaurate, into the original coating of the thermal insulation layer in the step 4.2) according to a conventional proportion, uniformly mixing to obtain a thermal insulation layer coating, putting the thermal insulation layer coating into a pneumatic spray gun, spraying the ferromagnetic wave absorbing layer in the step 3.3) by using the pneumatic spray gun, stopping spraying for 3min without stopping the rotation of the workpiece when the pneumatic spraying is carried out for 3-4 periods by adopting multiple spraying to meet the thickness requirement, adjusting the moving speed of the pneumatic spray gun according to the shape of the workpiece and the thickness of the coating of each period, wherein the thickness of the coating in each reciprocating spraying period is 120 +/-2 mu m, so that the leveling and solvent volatilization of the coating are facilitated, carrying out primary curing, and repeating the spraying process after finishing until the thickness of the thermal insulation layer reaches 1.5 mm.
6. The preparation method of the medium-temperature wide-band wave-absorbing coating according to claim 1, wherein in step 4.1): the light ceramic hollow micro-beads are light ceramic SiO2Hollow micro-bead, light ceramic SiO2The hollow microspheres have a particle size of 120 μm and a bulk density of 0.3g/cm3And the diluent is 120# solvent oil.
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Application publication date: 20200512 |