CN116285660A - Multifunctional magnetic resin-based composite wave-absorbing coating and preparation method and application thereof - Google Patents

Multifunctional magnetic resin-based composite wave-absorbing coating and preparation method and application thereof Download PDF

Info

Publication number
CN116285660A
CN116285660A CN202310139571.2A CN202310139571A CN116285660A CN 116285660 A CN116285660 A CN 116285660A CN 202310139571 A CN202310139571 A CN 202310139571A CN 116285660 A CN116285660 A CN 116285660A
Authority
CN
China
Prior art keywords
absorbing coating
composite wave
based composite
wave
resin
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202310139571.2A
Other languages
Chinese (zh)
Other versions
CN116285660B (en
Inventor
车仁超
连刚杰
游文彬
张金仓
程一峰
赵彪
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhejiang Lab
Original Assignee
Zhejiang Lab
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Zhejiang Lab filed Critical Zhejiang Lab
Priority to CN202310139571.2A priority Critical patent/CN116285660B/en
Publication of CN116285660A publication Critical patent/CN116285660A/en
Application granted granted Critical
Publication of CN116285660B publication Critical patent/CN116285660B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18—Fireproof paints including high temperature resistant paints
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/23—Magnetisable or magnetic paints or lacquers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/32—Radiation-absorbing paints
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/47—Levelling agents
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

Abstract

The invention discloses a multifunctional magnetic resin-based composite wave-absorbing coating, a preparation method and application thereof, belonging to the technical field of wave-absorbing coating materials, wherein the composite wave-absorbing coating is prepared from the following raw materials in parts by mass: 35-70 wt% of magnetic alloy powder; 5-15 wt% of low-melting glass powder; 3-20wt% of glass fiber; 15-30wt% of organic silicon resin; 0.5 to 3 weight percent of silicone resin curing agent; 0.05 to 0.15 weight percent of leveling agent. The multifunctional magnetic resin-based composite wave-absorbing coating with low porosity, smooth surface, excellent wave-absorbing performance at high temperature and excellent electromagnetic performance is prepared by the selection of raw materials, the synergistic effect among the raw materials and a simple process, the mechanical performance and the binding force with a matrix are obviously improved at high temperature, the heat resistance is good, and the technical problems that the powder flattening and the like easily occur when the high-temperature-resistant wave-absorbing coating is prepared by a thermal spraying method in the prior art are solved.

Description

Multifunctional magnetic resin-based composite wave-absorbing coating and preparation method and application thereof
Technical Field
The invention belongs to the technical field of high-temperature-resistant wave-absorbing coating materials, and particularly relates to a multifunctional magnetic resin-based composite wave-absorbing coating, a preparation method and application thereof.
Background
The radar wave-absorbing material technology is an important technology in the field of military stealth, and is divided into a coating type wave-absorbing material, a patch type wave-absorbing material, a structural type wave-absorbing material and the like according to functions, and the coating type wave-absorbing material has the characteristics of no limitation of a component structure, easiness in construction and the like, so that the radar wave-absorbing material is widely studied at the earliest. The stealth parts are classified according to working temperature and can be classified into normal temperature and high temperature. The weapon is easy to generate the problem of air current burning in a high-speed flight state, which puts higher requirements on the stable service of the wave-absorbing material at high temperature, and is a key place for improving the safety and the striking capability of the weapon. Aiming at the differentiation requirement of the high-temperature-resistant wave-absorbing coating, the resin-based wave-absorbing material becomes a research hot spot because of simple preparation and forming process and easy control. The organic silicon resin has an organic-inorganic framework due to the Si-O-Si main chain structure, so that the organic silicon resin has excellent heat resistance, weather resistance and processability, but in the practical application process, the organic silicon resin still has outstanding problems, and the main performances are as follows: high curing temperature, long time, poor adhesion to the substrate, low mechanical strength of the paint film at high temperature, etc. Therefore, the silicone resin is usually subjected to chemical or physical modification by copolymerization or blending with other resins, but when the silicone resin is modified by conventional resins such as epoxy and acrylic acid, the temperature resistance of the silicone resin is certainly affected.
The magnetic loss type wave absorbing material is used as the wave absorbing agent of the silicon resin coating, so that the broadband strong absorption can be realizedThe magnetic wave absorbing agent has the advantages of high density, easy oxidation at high temperature, poor high-temperature stability, low Curie temperature and the like, and can not be used under the condition of high temperature directly. Along with the development of the medium-high entropy alloy, the complex interaction among elements causes the alloy to present a cocktail effect, and a large number of medium-high entropy alloys with excellent performances such as high Curie temperature, magnetism, antioxidation and the like are developed. The magnetic alloy containing Si and Cr elements in the magnetic material has the characteristics of large magnetic conductivity, higher dielectric property, good thermal stability, oxidation resistance and the like, and the high magnetic conductivity and the high magnetic loss enable the magnetic alloy to keep high absorption of low-frequency electromagnetic wave energy when the thickness of the wave-absorbing coating is smaller, so that the introduction of the high-temperature magnetic alloy is a necessary way for realizing light, thin, strong and wide of the high-temperature-resistant wave-absorbing coating. A common alloy is Fe-Si-Cr alloy (FSC), which contains Fe as a component 87 Si 6.5 Cr 6.5 However, due to the higher dielectric constant, the composite ceramic powder is usually subjected to means such as inorganic coating, organic coating, composite ceramic powder granulation and the like to achieve better impedance matching effect, and in addition, in order to meet the excellent performance of the resin-based composite wave-absorbing coating, the dosage of the wave-absorbing agent powder added into the resin matrix is often relatively large, the strength of the composite coating is reduced along with the increase of the filling quantity of the wave-absorbing agent powder, and the coating modification can enable the wave-absorbing agent powder to have strong adhesive force with the resin matrix, so that the composite wave-absorbing coating with higher strength is obtained.
For the preparation of the multifunctional high-temperature-resistant composite coating, the preparation is mainly divided into hot spraying and low-temperature cold spraying according to different spraying construction temperatures. The thermal spraying technology using plasma arc, electric arc and combustion flame as heat sources heats powder to a molten state, then impacts and deposits on a substrate at high speed, phase change, chemical reaction and other phenomena inevitably occur in the process, and the flaky appearance is the main appearance of the magnetic alloy in the coating after thermal spraying, on one hand, the flaky magnetic alloy has better high-frequency magnetic permeability due to the fact that the limit of Snock is overcome, but the corresponding dielectric constant is obviously increased, the impedance matching characteristic is poor, the high dielectric constant ensures that a conductive network is extremely easy to form in a coating tissue structure, the wave absorbing performance of the coating is influenced, and on the other hand, the appearance and the structure of the magnetic alloy are influenced by plastic deformation caused by flaky. Although the low-temperature cold spraying is not heated to a molten state, plastic deformation caused by high-speed impact also leads the magnetic alloy to be mainly in a flaky shape in a coating structure, and the shape and the structure of the modified magnetic alloy can be damaged. The resin-based composite material coating can be formed by brushing, spraying, calendaring and other preparation processes, and can realize normal-temperature or low-temperature curing reaction under the action of a curing agent, so that the appearance and the structure of the magnetic alloy are kept intact, and high-temperature oxidation can be avoided.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention provides the multifunctional magnetic resin-based composite wave-absorbing coating which is cured at low temperature and used at high temperature, has the characteristics of simple preparation process, low porosity, flat and smooth surface, excellent wave-absorbing performance at high temperature and excellent electromagnetic performance, and has obviously improved mechanical property and bonding force with a matrix at high temperature, good heat resistance and easy industrial production.
The technical scheme adopted is as follows:
a multifunctional magnetic resin-based composite wave-absorbing coating is prepared from the following raw materials in percentage by mass:
Figure BDA0004089587470000021
Figure BDA0004089587470000031
according to the invention, the high-temperature wave absorbing performance of the product composite wave absorbing coating is regulated and controlled by regulating the addition amount of the magnetic alloy powder, the service time of the coating at high temperature can be prolonged due to the synergistic effect of the low-melting glass powder and the organic silicon resin, the mechanical property of the coating can be enhanced due to the addition of the glass fiber, the curing time of the silicon resin can be regulated and controlled due to the regulation of the addition amount of the silicon resin curing agent, the porosity of the coating can be reduced due to the addition of the leveling agent, and the surface of the coating is flat and smooth; in addition, the curing agent is introduced to modify the organic silicon resin, so that after curing, the high-temperature thermal stability of the silicon resin is obviously improved, and the mass retention rate at different temperatures is obviously improved, thereby laying a foundation for preparing the high-temperature-resistant wave-absorbing coating. On the basis, the multifunctional magnetic resin-based composite wave-absorbing coating capable of being cured at low temperature is prepared through component design.
Further, when the coating raw materials comprise the following components: the magnetic alloy powder was 68.32wt%; the low-melting glass powder is 8.54wt%; 4.27wt% of glass fibers; 17.08wt% silicone resin; the silicone curing agent was 1.71wt%; when the leveling agent is 0.08wt%, the multifunctional magnetic resin-based composite wave-absorbing coating has better wave-absorbing performance and mechanical property, and better process formability. When the magnetic alloy powder accounts for more than 68.32wt%, the impedance matching is poor due to the fact that the dielectric constant is too high, the wave absorbing performance of the coating is reduced, and meanwhile, the adhesive force of the silicon resin to the substrate is gradually reduced along with the increase of the magnetic alloy powder. The leveling agent can reduce the surface energy of the silicon resin, so that the porosity of the coating is reduced, and the surface of the coating is flat and smooth; the silicone resin curing agent can generate a crosslinking reaction with the organic groups of the organic silicone resin, so that on one hand, the curing time can be reduced, the efficiency can be improved, and on the other hand, the heat resistance of the organic silicone resin can be improved through the crosslinking reaction.
The magnetic alloy powder is a magnetic alloy with Curie temperature more than 550 ℃, the grain diameter of the magnetic alloy powder is less than or equal to 5 mu m, and further preferably, the magnetic alloy powder is iron silicon chromium (FSC), the element component is similar to that of 410 stainless steel, the Curie temperature requirement can be met, and the adhesive force to a matrix is good after the magnetic alloy powder is combined with other raw materials to prepare a coating.
The melting range of the low-melting-point glass powder is less than 550 ℃; the inorganic binding force of the organic silicon resin is reduced under the high temperature condition, glass powder is required to be melted under the high temperature condition, a part of silicon resin is replaced to play a role of a binder under the high temperature condition, and the service time of the coating under the high temperature is prolonged.
The diameter of the glass fiber is 10-15 mu m, and the length is 0.8-3 mm. The adhesive force of the organic silicon resin to the matrix can be influenced by the too thick diameter of the glass fiber, on the other hand, the influence of the length of the glass fiber on the mechanical property of the coating is also larger, when the length of the reinforcing phase glass fiber is too short, the mechanical property of the coating is improved less, when the length of the reinforcing phase glass fiber is too long, the reinforcing phase glass fiber can be agglomerated, the function of the reinforcing phase glass fiber is lost, and the mechanical property of the coating is poorer.
The invention also provides a preparation method of the multifunctional magnetic resin-based composite wave-absorbing coating, which comprises the following steps:
s1, uniformly mixing magnetic alloy powder, low-melting-point glass powder and glass fibers, ball milling, adding organic silicon resin, a silicon resin curing agent and a leveling agent, and stirring in a rolling way to obtain slurry;
s2, preprocessing the surface of the matrix, coating the preprocessed matrix with a layer of slurry in the step S1, then placing the matrix into a corresponding mold, injecting the slurry, jolt-ramming, removing the redundant slurry, and curing at a low temperature to obtain the multifunctional magnetic resin matrix composite wave-absorbing coating.
Preferably, zirconia balls are used in the ball milling process, and the ball-to-material ratio is 1:1-5; the rotating speed of the rolling stirring is 80-90 r/min, and the stirring time is 1-2 h. The main purpose of controlling the lower ball-to-material ratio and the rotating speed is to ensure that the slurry meets the uniform mixing and simultaneously avoid flattening of the magnetic powder filler.
Preferably, the substrate is 410 stainless steel, the pretreatment step comprises ultrasonic cleaning and sand blasting treatment, preferably, the pretreatment step comprises ultrasonic cleaning with absolute ethyl alcohol and acetone sequentially to remove oil stains on the surface of the substrate, and the sand blasting treatment is used for further removing a surface oxide layer and improving the adhesive force of the coating.
Because the contact angle of the silicon resin to the matrix is larger, the invention adopts the process of coating a layer of uniform slurry in advance and then grouting, thereby avoiding the problem of poor combination of the slurry and the matrix caused by directly grouting the slurry, removing the redundant slurry by utilizing extrusion force, and enhancing the combination strength between the coating and the matrix.
Preferably, the thickness of the sizing agent on the matrix is 1-1.5 mm after the sizing agent is injected. If the thickness of the slurry is thicker, the drying rate is different in the drying chamber due to different contact modes between the interface and the inside and the air, and the surface and the inside of the coating can generate microcracks due to the excessive internal stress generated by the drying chamber.
Preferably, the compaction is carried out on a compaction table, the power of the compaction table is 70-85%, and the compaction time is 5-10 min. The jolt ramming process enables the slurry to be more uniformly dispersed, air mixed in when the slurry is injected is discharged, jolt ramming power and treatment time are not excessively long, or micro-deposition of the magnetic alloy powder filler is caused, and a gradient effect is formed.
The low temperature curing temperature is not more than 200 ℃.
Preferably, the parameters of the low temperature cure are: preserving heat for 0.2-5 h at 80-100 ℃ and preserving heat for 0.5-2 h at 200 ℃. The method can ensure the evaporation of the organic silicon resin solvent at the temperature of 80-100 ℃ and simultaneously avoid micro cracks on the surface and inside of the coating caused by internal stress generated by different drying rates of the coating; 200 ℃ can promote the curing of the silicone resin and avoid serious weightlessness phenomenon. The temperature and the holding time can be further adjusted according to the thickness of the coating.
The invention also provides application of the multifunctional magnetic resin-based composite wave-absorbing coating in the field of high-temperature-resistant wave-absorbing coatings, and particularly application of the multifunctional magnetic resin-based composite wave-absorbing coating at a high temperature exceeding 500 ℃.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the invention, the high-temperature wave absorbing performance of the product composite wave absorbing coating is regulated and controlled through the adjustment of the addition amount of the magnetic alloy powder, the use time of the coating at high temperature can be prolonged through the synergistic effect of the low-melting glass powder and the organic silicon resin, the mechanical property of the coating can be enhanced through the addition of the reinforced phase glass fiber, and the surface energy of the silicon resin can be reduced through the leveling agent, so that the porosity of the coating is reduced, and the surface of the coating is flat and smooth; the silicone resin curing agent can generate a crosslinking reaction with the organic groups of the organic silicone resin, so that on one hand, the curing time can be reduced, the efficiency can be improved, and on the other hand, the heat resistance of the organic silicone resin can be improved through the crosslinking reaction.
(2) The invention improves the problem of reduced bonding strength caused by structural damage of the multifunctional magnetic resin-based wave-absorbing material at high temperature through improving the components of the slurry, improves the reliability, and has very important significance for the preparation and the use of the high-temperature multifunctional magnetic resin-based composite wave-absorbing coating.
(3) The method can solve the problem of powder flattening caused by melting or impact of the magnetic powder which is easy to occur when the high-temperature-resistant wave-absorbing coating is prepared by a thermal spraying method, and effectively avoids the damage of spraying to the structure of the magnetic powder.
Drawings
FIG. 1 is an SEM image of a multifunctional magnetic resin-based composite wave-absorbing coating of example 1 after being subjected to high temperature treatment;
FIG. 2 is an SEM image of the wave-absorbing coating of comparative example 1;
FIG. 3 is an SEM image of the wave-absorbing coating of comparative example 2;
FIG. 4 shows electromagnetic parameters of the multifunctional magnetic resin-based composite wave-absorbing coating in the X-band in example 1;
FIG. 5 shows electromagnetic parameters in the X-band after the multifunctional magnetic resin-based composite wave-absorbing coating in example 1 is subjected to high temperature treatment;
FIG. 6 is a graph showing reflectance test before and after heat treatment of the multifunctional magnetic resin-based composite wave-absorbing coating in example 1;
FIG. 7 shows electromagnetic parameters of the multifunctional magnetic resin-based composite wave-absorbing coating in the X-band in example 2;
fig. 8 shows electromagnetic parameters of the multifunctional magnetic resin-based composite wave-absorbing coating in the X-band in example 3.
Detailed Description
The invention is further elucidated below in connection with the examples and the accompanying drawing. It is to be understood that these examples are for illustration of the invention only and are not intended to limit the scope of the invention.
In the following examples and comparative examples, iron-silicon-chromium FSC powder was obtained from Changsha metal materials Co., ltd, and the product was FeSiCr (Curie temperature: 700 ℃ C., particle size: 3 to 5 μm). Silicone resin (CAS No. 67763-03-5), curing agent (HP 2000), leveling agent (DC-51) were purchased from Hubei Long-Shengshai New Material Co., ltd., low melting glass frit (melting range 380 ℃ C. To 480 ℃ C.), glass fiber (diameter 10-15 μm, length 0.8-3 mm) were purchased from Anmi micro-nano New Material (Guangzhou Co., ltd., brands are GT40, BQ2000, respectively).
Example 1
Step one: slurry preparation
Adding 800g of FSC, 100g of low-melting glass powder and 50g of glass fiber into a V-shaped stirrer, stirring for 2 hours to uniformly mix, adding the mixed powder and 800g of zirconia balls into a ball milling tank, adding 200g of organic silicon resin, 10wt% of curing agent of the organic silicon resin and 0.5wt% of leveling agent of the organic silicon resin, and stirring for 2 hours in a rolling way at 80-90 r/min to obtain slurry.
Step two: coating preparation
And (3) ultrasonic washing of greasy dirt on the surface of the substrate by using ethanol, acetone and the like, sand blasting treatment is carried out on the stainless steel of the substrate 410, then the substrate after sand blasting treatment is fixed, a layer of slurry obtained in the step one is uniformly coated in advance, then the substrate is put into a mould with a corresponding size, slurry is injected, the thickness of the slurry is 1-1.5 mm, and after 80% power of a jolt stand is jolt for 5min, superfluous slurry on the surface is extruded and scraped.
Step three: low temperature curing
The substrate coated with the slurry is kept at 80 ℃ for 5 hours, and after the organosilicon solvent is dried, the curing reaction is carried out at 200 ℃ for 2 hours. Cooling to room temperature to obtain the FSC/organic silicon resin composite wave-absorbing coating used at low temperature and high temperature, namely the multifunctional magnetic resin-based composite wave-absorbing coating.
Step four: high temperature treatment
And (3) preserving the temperature of the substrate with the product coating prepared in the step (III) for 30min at 550 ℃, verifying the service performance of the substrate at high temperature, wherein the heating rate is 10 ℃/min, and naturally cooling.
Comparative example 1
The preparation method of the coating in comparative example 1 differs from that in example 1 only in that no leveling agent is added; it was also subjected to high temperature treatment by the method of step four in example 1.
Comparative example 2
The preparation method of the coating in comparative example 2 is different from the preparation method in example 1 only in that the thickness of the slurry is more than 2mm after the slurry is injected in the second step; the parameters of low-temperature curing in the third step are as follows: 80, keeping the temperature for 10 hours, and keeping the temperature at 200 ℃ for 2 hours; it was also subjected to high temperature treatment by the method of step four in example 1.
Example 2
700g of FSC, 100g of low-melting glass powder and 50g of glass fiber are added into a V-shaped stirrer and stirred for 2 hours to be uniformly mixed, then the mixed powder and 800g of zirconia balls are added into a ball milling tank, then 200g of organic silicon resin, 10wt% of curing agent of the organic silicon resin and 0.5wt% of leveling agent of the organic silicon resin are added, and the mixture is stirred for 2 hours in a rolling way at 80-90 r/min to obtain slurry.
Step two: coating preparation
And (3) ultrasonic washing of greasy dirt on the surface of the substrate by using ethanol, acetone and the like, sand blasting treatment is carried out on the stainless steel of the substrate 410, then the substrate after sand blasting treatment is fixed, a layer of slurry obtained in the step one is uniformly coated in advance, then the substrate is put into a mould with a corresponding size, slurry is injected, the thickness of the slurry is 1-1.5 mm, and after 80% power of a jolt stand is jolt for 5min, superfluous slurry on the surface is extruded and scraped.
Step three: low temperature curing
The substrate coated with the slurry is kept at 80 ℃ for 5 hours, and after the organosilicon solvent is dried, the curing reaction is carried out at 200 ℃ for 2 hours. Cooling to room temperature to obtain the FSC/organic silicon resin composite wave-absorbing coating used at low temperature and high temperature, namely the multifunctional magnetic resin-based composite wave-absorbing coating.
Step four: high temperature treatment
And (3) preserving the temperature of the substrate with the product coating prepared in the step (III) for 30min at 550 ℃, verifying the service performance of the substrate at high temperature, wherein the heating rate is 10 ℃/min, and naturally cooling.
Example 3
600g of FSC, 100g of low-melting glass powder and 50g of glass fiber are added into a V-shaped stirrer and stirred for 2 hours to be uniformly mixed, then the mixed powder and 800g of zirconia balls are added into a ball milling tank, then 200g of organic silicon resin, 10wt% of curing agent of the organic silicon resin and 0.5wt% of leveling agent of the organic silicon resin are added, and the mixture is stirred for 2 hours in a rolling way at 80-90 r/min to obtain slurry.
Step two: coating preparation
And (3) ultrasonic washing of greasy dirt on the surface of the substrate by using ethanol, acetone and the like, sand blasting treatment is carried out on the stainless steel of the substrate 410, then the substrate after sand blasting treatment is fixed, a layer of slurry obtained in the step one is uniformly coated in advance, then the substrate is put into a mould with a corresponding size, slurry is injected, the thickness of the slurry is 1-1.5 mm, and after 80% power of a jolt stand is jolt for 5min, superfluous slurry on the surface is extruded and scraped.
Step three: low temperature curing
The substrate coated with the slurry is kept at 80 ℃ for 5 hours, and after the organosilicon solvent is dried, the curing reaction is carried out at 200 ℃ for 2 hours. Cooling to room temperature to obtain the FSC/organosilicon resin composite wave-absorbing coating used at low temperature and high temperature, namely the multifunctional magnetic resin matrix composite wave-absorbing coating.
Step four: high temperature treatment
And (3) preserving the temperature of the substrate with the product coating prepared in the step (III) for 30min at 550 ℃, verifying the service performance of the substrate at high temperature, wherein the heating rate is 10 ℃/min, and naturally cooling.
Example 4
Step one: slurry preparation
Adding 800g of FSC, 100g of low-melting glass powder and 50g of glass fiber into a V-shaped stirrer, stirring for 2 hours to uniformly mix, adding the mixed powder and 800g of zirconia balls into a ball milling tank, adding 200g of organic silicon resin, 5wt% of curing agent of the organic silicon resin and 0.5wt% of leveling agent of the organic silicon resin, and stirring for 2 hours in a rolling way at 80-90 r/min to obtain slurry.
Step two: coating preparation
And (3) ultrasonic washing of greasy dirt on the surface of the substrate by using ethanol, acetone and the like, sand blasting treatment is carried out on the stainless steel of the substrate 410, then the substrate after sand blasting treatment is fixed, a layer of slurry obtained in the step one is uniformly coated in advance, then the substrate is put into a mould with a corresponding size, slurry is injected, the thickness of the slurry is 1-1.5 mm, and after 80% power of a jolt stand is jolt for 5min, superfluous slurry on the surface is extruded and scraped.
Step three: low temperature curing
The substrate coated with the slurry is kept at 80 ℃ for 5 hours, and after the organosilicon solvent is dried, the curing reaction is carried out at 200 ℃ for 2 hours. Cooling to room temperature to obtain the FSC/organic silicon resin composite wave-absorbing coating used at low temperature and high temperature, namely the multifunctional magnetic resin-based composite wave-absorbing coating.
Step four: high temperature treatment
And (3) preserving the temperature of the substrate with the product coating prepared in the step (III) for 30min at 550 ℃, verifying the service performance of the substrate at high temperature, wherein the heating rate is 10 ℃/min, and naturally cooling.
Example 5
Step one: slurry preparation
Adding 800g of FSC, 50g of low-melting glass powder and 50g of glass fiber into a V-shaped stirrer, stirring for 2 hours to uniformly mix, adding the mixed powder and 800g of zirconia balls into a ball milling tank, adding 200g of organic silicon resin, 5wt% of curing agent of the organic silicon resin and 0.5wt% of leveling agent of the organic silicon resin, and stirring for 2 hours in a rolling way at 80-90 r/min to obtain slurry.
Step two: coating preparation
And (3) ultrasonic washing of greasy dirt on the surface of the substrate by using ethanol, acetone and the like, sand blasting treatment is carried out on the stainless steel of the substrate 410, then the substrate after sand blasting treatment is fixed, a layer of slurry obtained in the step one is uniformly coated in advance, then the substrate is put into a mould with a corresponding size, slurry is injected, the thickness of the slurry is 1-1.5 mm, and after 80% power of a jolt stand is jolt for 5min, superfluous slurry on the surface is extruded and scraped.
Step three: low temperature curing
The substrate coated with the slurry is kept at 80 ℃ for 5 hours, and after the organosilicon solvent is dried, the curing reaction is carried out at 200 ℃ for 2 hours. Cooling to room temperature to obtain the FSC/organic silicon resin composite wave-absorbing coating used at low temperature and high temperature, namely the multifunctional magnetic resin-based composite wave-absorbing coating.
Step four: high temperature treatment
And (3) preserving the temperature of the substrate with the product coating prepared in the step (III) for 30min at 550 ℃, verifying the service performance of the substrate at high temperature, wherein the heating rate is 10 ℃/min, and naturally cooling.
Example 6
Step one: slurry preparation
Adding 800g of FSC, 50g of low-melting glass powder and 50g of glass fiber into a V-shaped stirrer, stirring for 2 hours to uniformly mix, adding the mixed powder and 800g of zirconia balls into a ball milling tank, adding 200g of organic silicon resin, 5wt% of curing agent of the organic silicon resin and 0.5wt% of leveling agent of the organic silicon resin, and stirring for 2 hours in a rolling way at 80-90 r/min to obtain slurry.
Step two: coating preparation
And (3) ultrasonic washing of greasy dirt on the surface of the substrate by using ethanol, acetone and the like, sand blasting treatment is carried out on the stainless steel of the substrate 410, then the substrate after sand blasting treatment is fixed, a layer of slurry obtained in the step one is uniformly coated in advance, then the substrate is put into a mould with a corresponding size, slurry is injected, the thickness of the slurry is 1-1.5 mm, and after 80% power of a jolt stand is jolt for 5min, superfluous slurry on the surface is extruded and scraped.
Step three: low temperature curing
The substrate coated with the slurry is kept at 80 ℃ for 2 hours, and after the organosilicon solvent is dried, the curing reaction is carried out at 200 ℃ for 2 hours. Cooling to room temperature to obtain the FSC/organic silicon resin composite wave-absorbing coating used at low temperature and high temperature, namely the multifunctional magnetic resin-based composite wave-absorbing coating.
Step four: high temperature treatment
And (3) preserving the temperature of the substrate with the product coating prepared in the step (III) for 30min at 550 ℃, verifying the service performance of the substrate at high temperature, wherein the heating rate is 10 ℃/min, and naturally cooling.
Sample analysis
Morphology observations were made for the coatings prepared in examples and comparative examples: FIG. 1 is an SEM image of a multifunctional magnetic resin-based composite wave-absorbing coating of example 1 after being subjected to high temperature treatment; from figure 1, it can be obviously observed that the coating is not dropped off after high-temperature treatment, the bonding condition of the coating and the matrix is good, no crack is generated, and in addition, the morphology of the magnetic alloy powder is kept good and no agglomeration phenomenon exists; FIGS. 2 and 3 are SEM images of the wave-absorbing coating layers of comparative examples 1 and 2, respectively; as can be seen from the comparison between fig. 1 and fig. 2, the silicon resin leveling agent is not added in the comparative example 1, so that a large amount of gaps exist in the wave-absorbing coating, and the wave-absorbing and mechanical properties of the coating are affected; from fig. 3 we intuitively observe that when the thickness of the coating is too thick, the surface of the coating cracks due to the excessive internal stress caused by the different drying rates at the air coating interface and inside the coating, if a high thickness coating is required, the preparation process of the invention can be repeated multiple times by using the principle of 'small number of times' to increase the thickness of the coating.
The usability of the multifunctional magnetic resin-based composite wave-absorbing coating prepared in the embodiment at high temperature is detected: FIGS. 4 and 5 are respectively the electromagnetic parameters of the multifunctional magnetic resin-based composite wave-absorbing coating in the X-band before and after the high temperature treatment in example 1; it is apparent from fig. 4 and 5 that the dielectric constant of the coating is increased by 7% as the silicone resin is thermally decomposed to lose weight in the high-temperature heat treatment, and the magnetic parameters are not significantly changed, and it is further demonstrated that the silicone resin effectively prevents oxidation of the magnetic alloy. FIG. 6 is a graph showing reflectance test before and after heat treatment of the multifunctional magnetic resin-based composite wave-absorbing coating in example 1; it can be seen from fig. 6 that the wave-absorbing properties of the coating after heat treatment are better than those of the coating before heat treatment at a coating thickness of 1mm, and the absorption peaks move to low frequencies, mainly because the impedance matching effect of the coating is optimized with an increase in dielectric constant on the one hand, and a large amount of air is present as the coating structure changes from a dense structure to a loose structure with partial weight loss of the silicone resin on the other hand. Of course, here we can design the ratio of the magnetic alloy powder by using the law before and after the heat treatment, so that it is more reasonable, and fig. 7 and fig. 8 are electromagnetic parameters of the multifunctional magnetic resin-based composite wave-absorbing coating obtained by adjusting and controlling the ratio of different magnetic alloy powder in embodiments 2 and 3 respectively.
While the foregoing embodiments have been described in detail in connection with the embodiments of the invention, it should be understood that the foregoing embodiments are merely illustrative of the invention and are not intended to limit the invention, and any modifications, additions, substitutions and the like made within the principles of the invention are intended to be included within the scope of the invention.

Claims (10)

1. The multifunctional magnetic resin-based composite wave-absorbing coating is characterized by being prepared from the following raw materials in percentage by mass:
Figure FDA0004089587460000011
2. the multifunctional magnetic resin-based composite wave-absorbing coating according to claim 1, wherein the magnetic alloy powder is a magnetic alloy with a curie temperature of >550 ℃ and a particle size of 5 μm or less.
3. The multifunctional magnetic resin-based composite wave-absorbing coating according to claim 1, wherein the melting range of the low-melting glass powder is less than 550 ℃.
4. The multifunctional magnetic resin-based composite wave-absorbing coating according to claim 1, wherein the glass fiber has a diameter of 10-15 μm and a length of 0.8-3 mm.
5. The method for preparing the multifunctional magnetic resin-based composite wave-absorbing coating according to any one of claims 1 to 4, comprising the following steps:
s1, uniformly mixing magnetic alloy powder, low-melting-point glass powder and glass fibers, ball milling, adding organic silicon resin, a silicon resin curing agent and a leveling agent, and stirring in a rolling way to obtain slurry;
s2, preprocessing the surface of the matrix, coating the preprocessed matrix with a layer of slurry in the step S1, then placing the matrix into a corresponding mold, injecting the slurry, jolt-ramming, removing the redundant slurry, and curing at a low temperature to obtain the multifunctional magnetic resin matrix composite wave-absorbing coating.
6. The method for preparing a multifunctional magnetic resin-based composite wave-absorbing coating according to claim 5, wherein the pretreatment step comprises ultrasonic cleaning and sand blasting.
7. The method for preparing the multifunctional magnetic resin-based composite wave-absorbing coating according to claim 5, wherein the thickness of the sizing agent on the substrate is 1-1.5 mm after the sizing agent is injected.
8. The method for preparing a multifunctional magnetic resin-based composite wave-absorbing coating according to claim 5, wherein the temperature of low-temperature curing is not more than 200 ℃.
9. The method for preparing the multifunctional magnetic resin-based composite wave-absorbing coating according to claim 5, wherein the parameters of low-temperature curing are as follows: preserving heat for 0.2-5 h at 80-100 ℃ and preserving heat for 0.5-2 h at 200 ℃.
10. The use of a multifunctional magnetic resin-based composite wave-absorbing coating according to any one of claims 1-4 in the field of high temperature resistant wave-absorbing coatings.
CN202310139571.2A 2023-02-08 2023-02-08 Multifunctional magnetic resin-based composite wave-absorbing coating and preparation method and application thereof Active CN116285660B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202310139571.2A CN116285660B (en) 2023-02-08 2023-02-08 Multifunctional magnetic resin-based composite wave-absorbing coating and preparation method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202310139571.2A CN116285660B (en) 2023-02-08 2023-02-08 Multifunctional magnetic resin-based composite wave-absorbing coating and preparation method and application thereof

Publications (2)

Publication Number Publication Date
CN116285660A true CN116285660A (en) 2023-06-23
CN116285660B CN116285660B (en) 2023-08-11

Family

ID=86797034

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202310139571.2A Active CN116285660B (en) 2023-02-08 2023-02-08 Multifunctional magnetic resin-based composite wave-absorbing coating and preparation method and application thereof

Country Status (1)

Country Link
CN (1) CN116285660B (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007217959A (en) * 2006-02-16 2007-08-30 Diatex Co Ltd Wave absorbing structural member and wave absorbing structural body
US20110293892A1 (en) * 2009-12-22 2011-12-01 Masanori Ogawa Heat-insulating and sound absorbing material for the heat-insulating and sound absorbing structure of a car body
CN114262567A (en) * 2021-11-23 2022-04-01 航天科工武汉磁电有限责任公司 Low-temperature-cured high-temperature-resistant wave-absorbing coating and preparation method thereof
CN114274623A (en) * 2021-12-23 2022-04-05 航天科工武汉磁电有限责任公司 High-temperature-resistant wave absorbing plate and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007217959A (en) * 2006-02-16 2007-08-30 Diatex Co Ltd Wave absorbing structural member and wave absorbing structural body
US20110293892A1 (en) * 2009-12-22 2011-12-01 Masanori Ogawa Heat-insulating and sound absorbing material for the heat-insulating and sound absorbing structure of a car body
CN114262567A (en) * 2021-11-23 2022-04-01 航天科工武汉磁电有限责任公司 Low-temperature-cured high-temperature-resistant wave-absorbing coating and preparation method thereof
CN114274623A (en) * 2021-12-23 2022-04-05 航天科工武汉磁电有限责任公司 High-temperature-resistant wave absorbing plate and preparation method thereof

Also Published As

Publication number Publication date
CN116285660B (en) 2023-08-11

Similar Documents

Publication Publication Date Title
CN102758164B (en) Temperature-resistant thermal-spray radar absorbing coating and preparation method of spraying powder thereof
CN111304578B (en) Heat insulation/radar wave absorption integrated composite coating, titanium alloy material with composite coating coated on surface and preparation method of titanium alloy material
CN111732457B (en) Anti-oxidation/infrared stealth coating on surface of fiber-reinforced ceramic matrix composite material with temperature resistance of 1650 ℃ and preparation method thereof
CN110117764B (en) Thermal barrier/high-temperature low-infrared-emissivity integrated coating, metal composite material with coating and preparation method of metal composite material
CN115231952B (en) Rain erosion resistant inorganic coating on surface of quartz fiber reinforced quartz-based composite material and preparation method thereof
CN108637263A (en) A kind of microwave sintering preparation TiB2The method of-M metal ceramic powders
CN114988895A (en) Impact-resistant thermal cycle and CMAS corrosion resistant complex phase eutectoid environmental barrier coating and preparation method thereof
CN115851070A (en) Anti-oxidation ablation-resistant coating and preparation method thereof
CN113735590B (en) Preparation method and product of high-temperature-resistant electromagnetic wave-absorbing ceramic matrix composite material
CN116285660B (en) Multifunctional magnetic resin-based composite wave-absorbing coating and preparation method and application thereof
CN113817946B (en) HEA-SiC high-temperature wave-absorbing material and preparation method thereof
CN115583835B (en) Low-porosity high-mechanical-strength carbon graphite material and preparation method thereof
CN108998689B (en) High-temperature-resistant metal ceramic wave-absorbing material and preparation method thereof
KR101431148B1 (en) Method of preparing ceramic coating material for low temperature sintering and coated product using the same
CN115057692B (en) Aluminum-carbon sliding brick added with ferrotitanium alloy and production method thereof
CN110404751B (en) Method for forming anti-ablation coating on surface of resin-based composite material
CN101220211B (en) Anti-laser composite resin and method for producing the same
CN1380489A (en) Exhaust tube of engine and its integral preparation process
CN114409408A (en) Silicon carbide composite powder for laser 3D printing and preparation method thereof
CN114086102A (en) Ba (Mg)1/3Ta2/3)O3-YSZ double-ceramic-layer thermal barrier coating and preparation method thereof
CN106116698B (en) A kind of low-heat leads SiCN-Y2SiO5Environment barrier preparation method of composite coating
CN108794015B (en) Preparation method and application of silicon carbide and titanium diboride composite ceramic material
CN116063102B (en) High-temperature-resistant coating capable of being repaired online and preparation method thereof
CN113276496B (en) Light-weight heat-insulation integrated carbon fiber reinforced phenolic resin composite material
Jun et al. A Study of Low-Density Heat-Resistant Coating for New-Generation Launch Vehicle Fairings

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant