CN110982421B - High-temperature-resistant wave-absorbing coating and preparation method thereof - Google Patents
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Abstract
The invention provides a high-temperature-resistant wave-absorbing coating and a preparation method thereof, and relates to the field of radar wave-absorbing functional coatings. The high-temperature-resistant wave-absorbing coating is prepared by using organic silicon resin as a binder, a carbonyl iron powder absorbent subjected to ball milling treatment, a solvent, an auxiliary agent, a toughening agent and the like, and adding a silane coupling agent for auxiliary curing when in use. The wave-absorbing coating has good electromagnetic wave absorption performance, simultaneously meets the requirement of small change of the reflectivity of the electromagnetic wave after continuous test for 100 hours at the high temperature of 200 ℃, has good mechanical property, can solve the problem of insufficient high temperature resistance of the existing wave-absorbing coating, improves the environmental adaptability of the wave-absorbing coating and prolongs the service life of the wave-absorbing coating.
Description
Technical Field
The invention belongs to the field of radar wave-absorbing coatings, and particularly relates to a high-temperature-resistant functional coating with a radar wave-absorbing effect for an aircraft and a preparation method thereof.
Background
Along with the increasing development of aerospace equipment technology, the application technology of radar wave-absorbing materials is more and more important, and the radar wave-absorbing coating is the most widely used radar wave-absorbing material, has a better wave-absorbing effect and is easy to construct. For an aircraft, the heat generated by friction with air in the high-speed flight process can enable the coating material to withstand high temperature, and although the common wave-absorbing coating material has good electromagnetic shielding and electromagnetic absorption effects, the common wave-absorbing coating material is often difficult to withstand high temperature.
The radar is one of the main technical means of modern aerospace investigation, and is widely applied to the fields of spacecraft detection, investigation, tracking and the like. The radar wave absorbing effect of the spacecraft is improved, and the method is very important for improving the survival capacity of the spacecraft. After the radar wave-absorbing coating is coated, the radar scattering area (RCS) on the surface of the spacecraft is reduced, so that the spacecraft is difficult to be detected by a radar system, and the radar stealth effect is achieved.
The invention provides a coating material which can resist high temperature and has excellent mechanical property and radar wave absorption performance and a preparation method thereof based on the current situation that the existing radar wave absorption coating material does not have the capability of resisting high temperature for a long time or has the defects of serious performance reduction after high temperature resistance, no use value and the like.
Disclosure of Invention
Aiming at the problems or defects in the prior art, one of the purposes of the invention is to provide a radar wave-absorbing coating material which can resist high temperature, has excellent mechanical property and radar wave-absorbing property, and can solve the problems that the existing radar wave-absorbing coating has poor high temperature resistance, and the performance of the radar wave-absorbing coating material is reduced or the function is invalid under the high temperature condition.
The invention also aims to provide a preparation method of the coating with the function, the method has simple process, and the prepared coating material has stable and reliable performance and excellent performance.
The invention achieves the first purpose by the following technical means:
the high-temperature-resistant radar wave-absorbing coating comprises a base material A component and an auxiliary material B component, wherein the base material A component consists of an absorbent, matrix resin, an organic solvent and an auxiliary agent, and the auxiliary agent comprises the following components in parts by weight: the auxiliary material component B is a hardening agent; the auxiliary agent comprises a toughening agent, a flatting agent and an anti-settling agent; the absorbent is carbonyl iron powder with typical electromagnetic parameters; the real part of the complex dielectric constant of the carbonyl iron powder is 20-24, the imaginary part of the complex dielectric constant is 0.5-1.0, the real part of the complex permeability is 4.8-5.5, and the imaginary part of the complex permeability is 2.0-2.7.
Further, according to the technical scheme, the mass ratio of the base material to the auxiliary materials is 100: 0.1 to 1, preferably 100: 0.4 to 0.6.
Further, according to the technical scheme, the base material A component comprises the following components in percentage by mass:
further, according to the technical scheme, the carbonyl iron powder is obtained by a specific ball milling process, and the specific processing process comprises the following steps: ball milling is carried out by adopting a 10L planetary ball mill, the weight of carbonyl iron powder in each can is about 0.4kg, and the weight of carbonyl iron powder in each can is 1.5kg
Steel balls and 1.5kg weight
Steel balls, 4 cans in total; setting ball milling frequency of 40Hz and ball milling time of 15-30 min, and then screening by using a 100-mesh screen to obtain the available carbonyl iron powder absorbent.
Further, in the above technical scheme, the matrix resin comprises a silicone resin and a modified silicone resin, and the silicone resin may be polyalkyl silicone resin, polyaryl silicone resin and polyalkyl aryl silicone resin; the modified organic silicon resin can adopt epoxy modified organic silicon resin, acrylic acid modified organic silicon resin, polyurethane modified organic silicon resin and the like; the matrix resin can be used singly or compounded according to a certain proportion.
Further, according to the technical scheme, the organic solvent is two or more of xylene, n-butanol, butyl acetate and propylene glycol methyl ether acetate which are compounded according to a certain proportion.
Furthermore, in the technical scheme, the leveling agent can adopt acrylate copolymer or polyester modified polydimethylsiloxane substances.
Further, in the above technical means, the anti-settling agent may be any one of modified polyurea compounds, fumed silica, organic bentonite and the like.
Further, according to the above technical scheme, the toughening agent may be one of diisobutyl phthalate, dioctyl phthalate, diisodecyl phthalate, and the like.
Further, in the technical scheme, the auxiliary material B component is a silane coupling agent, and can adopt any one of gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, gamma-mercaptopropyltrimethoxysilane and the like.
The second purpose of the invention is to provide a preparation method of the high-temperature-resistant radar wave-absorbing coating, which comprises the following steps:
the method comprises the following steps: mixing the matrix resin, the organic solvent and the auxiliary agent according to the designed formula amount, and fully stirring until the solid is completely dissolved;
step two: and adding a weighed carbonyl iron powder absorbent into the mixed liquid obtained in the step one under the stirring state, dispersing at a high speed for 20-30 min, and obtaining the component A of the usable wave-absorbing coating base material after confirming that the mixture is uniform and free of agglomeration.
Step three: and mixing the base material A component and the auxiliary material B component according to the design amount of the formula, and uniformly stirring to obtain the high-temperature-resistant radar wave-absorbing coating.
Further, according to the technical scheme, the stirring speed in the first step is 500-800 rpm, and the stirring time is 10-20 min.
Further, in the above technical scheme, the high-speed dispersion in the second step specifically adopts a high-speed shearing dispersion machine, and the stirring rotation speed is set to 1000rpm to 1500 rpm.
Compared with the prior art, the invention has the following beneficial effects:
(1) the high-temperature-resistant radar wave-absorbing coating provided by the invention adopts the carbonyl iron powder absorbent treated by the ball milling process, has high flakiness degree, good anisotropy, low dielectric constant and high magnetic conductivity, and has a good broadband absorption effect.
(2) The organic silicon resin adopted by the invention is used as a binder, the high temperature resistance is good, but the coating using the organic silicon resin alone needs higher baking temperature (generally reaching 150 ℃), and is difficult to reach higher dry film thickness of the coating at one time, so that the construction efficiency and the use adaptability are greatly restricted. In view of the above, the invention adopts the silane coupling agent as the hardening agent, which can generate silanol condensation reaction with the organic silicon resin to form a cross-linked network structure, thereby enhancing the mechanical strength of the paint film, meeting the construction requirement of thicker coatings and reducing the baking and curing temperature of the coatings.
(3) The invention adopts phthalate ester substances as the toughening agent, can improve the flexibility of the coating, and ensures that the coating still has better flexibility after the coating resists high temperature. The toughening agent contains more straight-chain alkyl groups, and the groups have higher bond energy and can resist certain high and low temperature changes. When the coating expands and contracts, the molecular structure formed by the group has better rotatability and elasticity, so that the coating has better toughening effect.
Drawings
FIG. 1 is a graph showing the results of the electromagnetic parameter tests of carbonyl iron powder subjected to ball milling treatment in examples 1 to 3 of the present invention.
Detailed Description
The present invention will be described in further detail below with reference to examples. The present invention is implemented on the premise of the technology of the present invention, and the detailed embodiments and specific procedures are given to illustrate the inventive aspects of the present invention, but the scope of the present invention is not limited to the following embodiments.
Various modifications to the precise description of the invention will be readily apparent to those skilled in the art from the information contained herein without departing from the spirit and scope of the appended claims. It is to be understood that the scope of the invention is not limited to the procedures, properties, or components defined, as these embodiments, as well as others described, are intended to be merely illustrative of particular aspects of the invention. Indeed, various modifications of the embodiments of the invention which are obvious to those skilled in the art or related fields are intended to be covered by the scope of the appended claims.
For a better understanding of the invention, and not as a limitation on the scope thereof, all numbers expressing quantities, percentages, and other numerical values used in this application are to be understood as being modified in all instances by the term "about". Accordingly, unless expressly indicated otherwise, the numerical parameters set forth in the specification and attached claims are approximations that may vary depending upon the desired properties sought to be obtained. At the very least, each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques.
The invention provides a high-temperature-resistant wave-absorbing coating and a preparation method thereof, the high-temperature-resistant wave-absorbing coating is prepared by taking organic silicon resin as a binder, a carbonyl iron powder absorbent with typical electromagnetic parameters after ball milling treatment, a solvent, an auxiliary agent, a toughening agent and the like, and a silane coupling agent is added for auxiliary curing when in use. The wave-absorbing coating has good electromagnetic wave absorption performance, simultaneously meets the requirement of small change of the reflectivity of the electromagnetic wave after continuous test for 100 hours at the high temperature of 200 ℃, has good mechanical property, can solve the problem of insufficient high temperature resistance of the existing wave-absorbing coating, improves the environmental adaptability of the wave-absorbing coating and prolongs the service life of the wave-absorbing coating.
The carbonyl iron powder absorbent adopted in the following embodiments 1 to 3 needs to be treated by a specific ball milling process, and the specific treatment process is as follows: ball milling is carried out by adopting a 10L planetary ball mill, the weight of carbonyl iron powder in each tank is about 0.4kg, each tank is matched with a steel ball with the diameter of 6mm and a steel ball with the diameter of 8mm, the weight of the steel ball is 1.5kg, and 4 tanks are matched together. Setting the frequency to be 40Hz, and ball milling for 15-30 min. Then screening the powder by using a 100-mesh screen to obtain the usable carbonyl iron powder absorbent. Fig. 1 shows typical electromagnetic parameters of carbonyl iron powder absorbent after ball milling process. Table 1 shows the range of variation of the electromagnetic parameters of the carbonyl iron powder after the ball milling treatment.
TABLE 1 variation range of electromagnetic parameters of carbonyl iron powder after ball milling treatment
Example 1
The high-temperature-resistant radar wave-absorbing coating comprises a base material A component and an auxiliary material B component, wherein the base material A component comprises 600g of an absorbent, 250g of organic silicon resin, 15g of xylene, 5g of n-butyl alcohol, 15g of butyl acetate, 15g of propylene glycol methyl ether acetate, 30g of diisobutyl phthalate, 8g of a polyester modified polydimethylsiloxane leveling agent and 4g of an organobentonite anti-settling agent, and the auxiliary material B is 5g of gamma-aminopropyltriethoxysilane; the absorbent is carbonyl iron powder with typical electromagnetic parameters; wherein: the real part of the complex dielectric constant of the carbonyl iron powder is 20-24, the imaginary part of the complex dielectric constant is 0.5-1.0, the real part of the complex permeability is 4.8-5.5, and the imaginary part of the complex permeability is 2.0-2.7.
The high-temperature-resistant radar wave-absorbing coating is prepared by the following method, comprising the following steps:
250g of organic silicon resin, 15g of dimethylbenzene, 5g of n-butyl alcohol, 15g of butyl acetate, 15g of propylene glycol methyl ether acetate, 30g of diisobutyl phthalate, 8g of polyester modified polydimethylsiloxane and 4g of organic bentonite are sequentially added into a beaker, the stirring speed is set to be 500-800 rpm, and the stirring is carried out for 10-20 min until the mixture is completely uniform. Adding 600g of carbonyl iron powder absorbent into the uniformly mixed resin solvent liquid under the stirring state, and dispersing for 20-30 min by adopting a high-speed shearing dispersion machine at the stirring speed of 1000-1500 rpm until the mixture is uniform and has no agglomeration phenomenon to obtain the usable wave-absorbing coating base material A component. 5g of the wave-absorbing coating auxiliary material B component (gamma-aminopropyl triethoxysilane) is weighed into the dispersed wave-absorbing coating base material A component, and the mixture is continuously stirred uniformly, so that the usable high-temperature resistant radar wave-absorbing coating is obtained.
Example 2
The high-temperature-resistant radar wave-absorbing coating comprises a base material A component and an auxiliary material B component, wherein the base material A component comprises 700g of an absorbent, 250g of organic silicon resin, 40g of dimethylbenzene, 30g of butyl acetate, 35g of dioctyl phthalate, 8g of a polyester modified polydimethylsiloxane leveling agent and 4g of a fumed silica anti-settling agent, and the auxiliary material B is 5g of gamma- (methacryloyloxy) propyl trimethoxy silane; the absorbent is carbonyl iron powder with typical electromagnetic parameters; wherein: the real part of the complex dielectric constant of the carbonyl iron powder is 20-24, the imaginary part of the complex dielectric constant is 0.5-1.0, the real part of the complex permeability is 4.8-5.5, and the imaginary part of the complex permeability is 2.0-2.7.
The high-temperature-resistant radar wave-absorbing coating is prepared by the following method, comprising the following steps:
adding 250g of organic silicon resin, 40g of dimethylbenzene, 30g of butyl acetate, 35g of dioctyl phthalate, 8g of polyester modified polydimethylsiloxane and 4g of fumed silica into a beaker in sequence, setting the stirring speed to be 500-800 rpm, and stirring for 10-20 min to be in a completely uniform state. Adding 700g of carbonyl iron powder absorbent into the uniformly mixed resin solvent liquid under the stirring state, and dispersing for 20-30 min by adopting a high-speed shearing dispersion machine at the stirring speed of 1000-1500 rpm until the mixture is uniform and has no agglomeration phenomenon to obtain the usable wave-absorbing coating base material A component. 5g of wave-absorbing coating auxiliary material B component (gamma- (methacryloyloxy) propyl trimethoxy silane) is weighed into the dispersed wave-absorbing coating base material A component, and the mixture is continuously stirred uniformly, so that the usable high-temperature resistant radar wave-absorbing coating is obtained.
Example 3
The high-temperature-resistant radar wave-absorbing coating comprises a base material component A and an auxiliary material component B, wherein the base material component A is composed of 780g of an absorbent, 220g of organic silicon resin, 40g of n-butanol, 30g of propylene glycol monomethyl ether acetate, 35g of diisodecyl phthalate, 8g of a polyacrylate copolymer flatting agent and 5g of an organic bentonite anti-settling agent, and the auxiliary material B is 4g of gamma-mercaptopropyl trimethoxy silane; the absorbent is carbonyl iron powder with typical electromagnetic parameters; wherein: the real part of the complex dielectric constant of the carbonyl iron powder is 20-24, the imaginary part of the complex dielectric constant is 0.5-1.0, the real part of the complex permeability is 4.8-5.5, and the imaginary part of the complex permeability is 2.0-2.7.
The high-temperature-resistant radar wave-absorbing coating is prepared by the following method, comprising the following steps:
220g of organic silicon resin, 40g of n-butyl alcohol, 30g of propylene glycol methyl ether acetate, 35g of diisodecyl phthalate, 8g of polyacrylate copolymer and 5g of organic bentonite are sequentially added into a beaker, the stirring speed is set to be 500 rpm-800 rpm, and the stirring is carried out for 10 min-20 min until the mixture is completely uniform. Adding 780g of carbonyl iron powder absorbent into the uniformly mixed resin solvent liquid while keeping stirring, and dispersing for 20-30 min by adopting a high-speed shearing dispersion machine at the stirring speed of 1000-1500 rpm until the mixture is uniform and has no agglomeration phenomenon to obtain the usable wave-absorbing coating base material A component. Weighing 4g of the auxiliary material B (gamma-mercaptopropyl-trimethoxysilane) of the wave-absorbing paint into the dispersed component A of the base material of the wave-absorbing paint, and continuously stirring the mixture uniformly to obtain the usable high-temperature resistant radar wave-absorbing paint.
For comparison, the invention designs a comparative example 1 and a comparative example 2 according to the following formula, prepares the radar absorbing coating, and the preparation method is similar to the method for preparing the coating in the examples and is not described in detail.
Comparative example 1
The radar wave-absorbing coating of the comparative example consists of the following components in percentage by mass:
Comparative example 2
The radar wave-absorbing coating of the comparative example consists of the following components in percentage by mass:
And (3) performance testing:
the wave-absorbing coating provided by the embodiments 1-3 and the comparative examples 1-2 is coated on the surface of a corresponding component (comprising a metal material or a non-metal material coated with a conductive primer on the surface) to obtain a high-temperature-resistant wave-absorbing coating. The method comprises the steps of selecting an aluminum alloy plate as a base material, coating a wave-absorbing coating on one surface of the aluminum alloy plate after surface treatment to obtain a coating sample plate, testing the mechanical property, the high temperature resistance and the electromagnetic wave absorption effect of the obtained coating, and evaluating whether the coating meets the requirements of the high temperature resistance and the radar wave absorption performance according to the test result, wherein the thickness of the aluminum alloy plate is about 5mm, and the length and the width of the aluminum alloy plate are all 180 mm.
The wave-absorbing coatings prepared by the radar wave-absorbing coatings obtained in the examples 1-3 and the comparative examples 1-2 were tested by adopting the following standards:
A. the coating sample plate is used for testing the reflectivity of the 8 GHz-18 GHz frequency band according to the GJB2038A-2011 radar wave-absorbing material reflectivity test method.
B. The coating template was tested for flexibility according to GB/T1731-.
C. And (3) performing a high temperature resistance test on the coating sample plate for 2h at 200 ℃, and testing the reflectivity and the mechanical property of the sample plate after high temperature resistance according to the standards in A and B.
D. And (3) performing a high temperature resistance test on the coating sample plate at 200 ℃ for 100h, and testing the reflectivity and the mechanical property of the sample plate after high temperature resistance according to the standards in A and B.
The test results are shown in tables 2 and 3.
Table 2 table for testing high temperature resistance of wave absorbing coating prepared from radar wave absorbing coating obtained in examples 1 to 3 and comparative examples 1 to 2
Note: the comparative example can not bear the environment with the temperature of 200 ℃ for 100 hours and is damaged.
Table 3 setting result table of broadband wave absorption performance of wave absorbing coating prepared from radar wave absorbing coating obtained in embodiments 1 to 3
| Examples | Bandwidth (GHz) with reflectivity less than or equal to-10 dB |
| Example 1 | 6.5 |
| Example 2 | 5.4 |
| Example 3 | 5.8 |
According to the test results in tables 2 and 3, the coatings obtained by the three groups of embodiments of the invention after high temperature test still have good flexibility and impact strength, and the reflectivity changes little, and still have good electromagnetic wave absorption effect, so that the wave absorption performance of the aircraft in a high temperature state can be satisfied. The test results of the two groups of comparative examples show that the high-temperature resistance of the coating material is poor, and the specific expression is that the flexibility and the impact strength of the coating are greatly reduced, and the reflectivity is also reduced to different degrees.
Claims (5)
1. A high temperature resistant radar wave-absorbing coating comprises a base material A component and an auxiliary material B component, and is characterized in that: the base material A component consists of an absorbent, matrix resin, an organic solvent and an auxiliary agent, wherein: the auxiliary material component B is a hardening agent; the auxiliary agent is a toughening agent, a flatting agent and an anti-settling agent; the absorbent is carbonyl iron powder with typical electromagnetic parameters; the real part of the complex dielectric constant of the carbonyl iron powder is 20-24, the imaginary part of the complex dielectric constant is 0.5-1.0, the real part of the complex permeability is 4.8-5.5, and the imaginary part of the complex permeability is 2.0-2.7; the mass ratio of the base material A component to the auxiliary material B component is 100: 0.1 to 1; the auxiliary material component B is a silane coupling agent; the base material A component comprises the following components in percentage by mass:
50 to 70 percent of absorbent
15 to 30 percent of matrix resin
5 to 10 percent of organic solvent
3 to 10 percent of toughening agent
0.5 to 1 percent of flatting agent
0.2 to 0.5 percent of anti-settling agent, and the sum of the mass percent of the components is 100 percent;
the matrix resin comprises organic silicon resin and modified organic silicon resin; the organic silicon resin adopts polyalkyl organic silicon resin, polyaryl organic silicon resin and polyalkyl aryl organic silicon resin; the modified organic silicon resin adopts epoxy modified organic silicon resin, acrylic acid modified organic silicon resin and polyurethane modified organic silicon resin.
2. The high temperature resistant radar absorbing coating of claim 1, wherein: the carbonyl iron powder is obtained by a specific ball milling process, and the specific processing process comprises the following steps: ball milling is carried out by adopting a 10L planetary ball mill, the weight of carbonyl iron powder filled in each tank is about 0.4kg, each tank is matched with a phi 6mm steel ball with the weight of 1.5kg and a phi 8mm steel ball with the weight of 1.5kg, and 4 tanks are matched together; setting ball milling frequency of 40Hz and ball milling time of 15-30 min, and then screening by using a 100-mesh screen to obtain the available carbonyl iron powder absorbent.
3. The high temperature resistant radar absorbing coating of claim 1, wherein: the organic solvent is two or more of dimethylbenzene, n-butyl alcohol, butyl acetate and propylene glycol methyl ether acetate which are compounded according to a certain proportion.
4. The high temperature resistant radar absorbing coating of claim 1, wherein: the flatting agent adopts acrylic copolymer or polyester modified polydimethylsiloxane substances; the anti-settling agent is any one of modified polyurea compounds, fumed silica and organic bentonite; the toughening agent is one of diisobutyl phthalate, dioctyl phthalate and diisodecyl phthalate.
5. The preparation method of the high temperature resistant radar wave absorbing coating of any one of claims 1 to 4, characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: mixing the matrix resin, the organic solvent and the auxiliary agent according to the designed formula amount, and fully stirring until the solid is completely dissolved;
step two: adding a weighed carbonyl iron powder absorbent into the mixed liquid obtained in the step one under the stirring state, dispersing at a high speed for 20-30 min, and preparing an available wave-absorbing coating base material A component after confirming that the mixture is uniform and free of agglomeration;
step three: and mixing the base material A component and the auxiliary material B component according to the design amount of the formula, and uniformly stirring to obtain the high-temperature-resistant radar wave-absorbing coating.
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| CN111748233A (en) * | 2020-07-21 | 2020-10-09 | 和爱电磁兼容科技(安徽)有限公司 | Low-reflectivity wave-absorbing material and preparation method thereof |
| CN111969330B (en) * | 2020-07-31 | 2023-02-10 | 航天科工武汉磁电有限责任公司 | Radar wave-absorbing material with unit structure pattern and preparation method thereof |
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