CN115873440A - High-temperature-resistant wave-absorbing coating and preparation method thereof, broadband wave-absorbing material and preparation method thereof - Google Patents
High-temperature-resistant wave-absorbing coating and preparation method thereof, broadband wave-absorbing material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-temperature-resistant wave-absorbing coating and a preparation method thereof, and a broadband wave-absorbing material and a preparation method thereof, wherein the high-temperature-resistant wave-absorbing coating comprises 200-400 parts of an absorbent, 80-200 parts of a modified adhesive, 1-25 parts of an auxiliary agent and 1-120 parts of a solvent, wherein the absorbent is a magnetic alloy material, and the modified adhesive can be cured at room temperature. The high-temperature-resistant wave-absorbing coating provided by the invention can be suitable for various base materials, has high-temperature resistance and good electromagnetic wave absorption performance, and particularly shows that after being treated at the high temperature of 400-650 ℃, the surface of the coating does not have falling and obvious defects, and the coating shows excellent electromagnetic wave absorption performance, and the absorption performance can be improved by 2-10%.
Description
Technical Field
The invention relates to the technical field of wave-absorbing materials, in particular to a high-temperature-resistant wave-absorbing coating and a preparation method thereof, and a broadband wave-absorbing material and a preparation method thereof.
Background
With the rapid development of aerospace technology, in order to meet the requirement of rapid striking, the speed of an aircraft is faster and faster, the surface temperature of the aircraft is rapidly increased under the influence of air resistance at high speed, when the temperature reaches 300-650 ℃, the traditional wave-absorbing material can cause the wave-absorbing performance to be reduced due to the problems of surface oxidation, microstructure change and the like, the stealth capability of the aircraft is seriously influenced, and the wave-absorbing material becomes the bottleneck problem of stealth of airplanes and missiles, and the high-temperature wave-absorbing material is a key technology for solving the bottleneck problem. The wave-absorbing coating researched at present is mainly applied to normal temperature conditions, does not have wave-absorbing performance and high temperature resistance, and limits the application of the wave-absorbing coating on high-temperature parts to a great extent. Therefore, the research on the high-temperature wave-absorbing coating is developed, so that the coating has both broadband traveling wave inhibition performance and high-temperature resistance, and has important practical significance and military application prospect.
Disclosure of Invention
The invention mainly aims to provide a high-temperature-resistant wave-absorbing coating and a preparation method thereof, a broadband wave-absorbing material and a preparation method thereof, and aims to provide the broadband wave-absorbing material with high-temperature resistance and broadband traveling wave inhibition performance.
In order to achieve the purpose, the invention provides a high-temperature-resistant wave-absorbing coating which comprises, by mass, 200-400 parts of an absorbent, 80-200 parts of a modified adhesive, 1-25 parts of an auxiliary agent and 1-120 parts of a solvent, wherein the absorbent is a magnetic alloy material, and the modified adhesive can be cured at room temperature.
Optionally, the magnetic alloy material has a curie temperature above 700 ℃ and an average grain size of 4.0-40.0 μm.
Optionally, the magnetic alloy material includes a metal element and a nonmetal element, the metal element includes iron and at least one of cobalt, nickel, chromium, molybdenum and aluminum, and the nonmetal element includes silicon.
Optionally, the preparation step of the magnetic alloy material comprises:
putting the powder raw materials into a smelting furnace for smelting and vacuum atomization to prepare spherical alloy powder, then sintering for 1-10 h at 180-220 ℃, and then ball-milling and sieving to prepare the magnetic alloy material.
Optionally, the modified binder comprises at least one of modified silicate, modified silica sol, modified alumina sol and modified phosphate; and/or the presence of a gas in the gas,
the auxiliary agent comprises an anti-settling agent and a defoaming agent; and/or the presence of a gas in the atmosphere,
the solvent includes at least one of water and a water-based sol.
Optionally, the step of preparing the modified adhesive comprises:
mixing the adhesive and organic silicon, and stirring at 25-90 ℃ for 0.5-8 h to prepare a modified adhesive; wherein the addition amount of the organic silicon is 1-10% of the mass of the adhesive.
Further, the invention also provides a preparation method of the high-temperature-resistant wave-absorbing coating, which comprises the following steps:
stirring the modified adhesive at the speed of 3000-10000 rpm for 3-10 min, and then standing for 2-10 min for curing;
and adding a magnetic alloy material, a solvent and an auxiliary agent into the cured modified adhesive, and homogenizing until the magnetic alloy material, the solvent and the auxiliary agent are uniformly dispersed to prepare the high-temperature-resistant wave-absorbing coating.
Furthermore, the invention also provides a broadband wave-absorbing material, which comprises a base material and a wave-absorbing coating coated on the surface of the base material, wherein the wave-absorbing coating is formed by the high-temperature-resistant wave-absorbing coating, and the base material comprises any one of a stainless steel base material, a titanium alloy base material, an aluminum alloy base material, a quartz base material and an aluminum silicate base material.
Optionally, the thickness of the wave-absorbing coating is 0.8-3 mm.
In addition, the invention also provides a preparation method of the broadband wave-absorbing material, which comprises the following steps:
providing the high-temperature-resistant wave-absorbing coating;
and spraying the high-temperature-resistant wave-absorbing coating on the surface of a base material by using an air pressure spray gun, and curing at room temperature to obtain the broadband wave-absorbing material.
The high-temperature-resistant wave-absorbing coating provided by the invention can be suitable for various base materials, has high-temperature resistance and good electromagnetic wave absorption performance, and particularly shows that after the high-temperature treatment at 400-650 ℃, the surface of the coating does not fall off or has obvious defects, and the high-temperature-resistant wave-absorbing coating has excellent electromagnetic wave absorption performance, and the absorption performance can be improved by 2-10%.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other related drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is an appearance diagram of a coating of a broadband wave-absorbing material prepared in example 8 of the present invention before and after high temperature treatment;
FIG. 2 is a coating reflectivity curve before and after high temperature treatment of the broadband wave-absorbing material prepared in embodiment 8 of the present invention;
FIG. 3 is a coating reflectivity curve chart of the broadband wave-absorbing material prepared in embodiment 9 before and after high-temperature treatment;
FIG. 4 is a scanning electron microscope image of the coating surface before and after high temperature treatment of the broadband wave-absorbing material prepared in example 10 of the present invention;
FIG. 5 is a coating reflectivity curve chart of the broadband wave-absorbing material prepared in embodiment 11 before and after high-temperature treatment;
fig. 6 is a coating reflectivity curve chart of the broadband wave-absorbing material prepared in embodiment 12 before and after high-temperature treatment.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially. In addition, the meaning of "and/or" appearing throughout includes three juxtapositions, exemplified by "A and/or B", including either A or B or both A and B. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a high-temperature-resistant wave-absorbing coating which comprises an absorbent, a modified adhesive, an auxiliary agent and a solvent, wherein the absorbent is a magnetic alloy material, and the modified adhesive can be cured at room temperature. The research shows that with the increase of the dosage of the absorbent in the system, the adhesive components are reduced, on one hand, the adhesive force among the components is weakened, the surface of the coating is easy to fall off, on the other hand, the difficulty of the coating in the spraying process is increased, and the apparent performance of the coating is influenced. Preferably, in an embodiment of the high temperature resistant wave-absorbing coating provided by the invention, the mass parts of the absorbent, the modified adhesive, the auxiliary agent and the solvent are 200-400 parts, 80-200 parts, 1-25 parts and 1-120 parts, respectively.
The high-temperature-resistant wave-absorbing coating provided by the invention can be suitable for various substrates, has high-temperature resistance and good electromagnetic wave absorption performance, particularly shows that after high-temperature treatment at 400-650 ℃, the surface of the coating has no drop and obvious defects, shows excellent electromagnetic wave absorption performance, can improve the absorption performance by 2-10%, can realize high-temperature-resistant protection and broadband stealth requirements of the surface of a large-area complex-structure part, meets the application requirements of military and civil use on high-temperature-resistant broadband wave-absorbing materials of different substrates, and has wide market application prospect.
In recent years, high-temperature wave absorbers such as SiC-based oxygen-free ceramic materials, ternary layered compounds (MAX phase non-metallic carbides or nitrides), metal oxides (represented by Zn, sn, and Ti), carbon materials (MWCNTs, G, CF, and C black), and magnetic metal alloys have been attracting attention. Silicon carbide is the most extensive non-oxide high-temperature resistant material, has stable chemical property, high heat conductivity coefficient, small thermal expansion coefficient and excellent wear resistance, but is a pure dielectric material, almost has no magnetic loss effect and has poor broadband absorption effect. The ternary layered compound is a carbide or nitride with a close-packed hexagonal structure, also commonly referred to as MAX phase material, and can be represented by the formula M n+1 AX n To indicate. Wherein M represents a transition metal element, A represents a main group element, and X is a C or N element. Wherein, with Ti 3 SiC 2 The steel has the characteristics of most extensive research, corrosion resistance, high temperature resistance, high hardness and high strength. However, the pure MAX phase material has high conductivity and strong electromagnetic wave reflection, which results in the decrease of wave-absorbing performance, and the synthetic process has high process requirements and high price, and is difficult to meet the use requirements of mass production. The carbon-based wave-absorbing material mainly comprises carbon black, carbon fiber, carbon nano tube, graphite and the like, and has the advantages of good corrosion resistance, low density, high conductivity and the like, but the impedance mismatch between a single carbon material and a free space is easy to occurAnd the problem of oxidation failure in a high-temperature oxygen-containing environment, and the defects of complex oxidation resistance process, poor uniformity and stability and the like exist, so that the application of the antioxidant in the high-temperature field is limited. The metal oxide absorbent is mainly a semiconductor oxide of Zn, sn and Ti, has the advantages of low infrared radiation, high temperature resistance and low cost, but the low conductivity of the metal oxide absorbent causes the metal oxide absorbent to have weak electrical loss capability and poorer wave-absorbing performance. The absorbent materials are dielectric high-temperature resistant absorbents which are difficult to meet the actual service performance requirements such as high temperature resistance and broadband absorption, and the conductivity and impedance matching of the absorbent materials are mainly regulated and controlled by means of doping, surface coating, multi-layer structure and porous structure design at present, so that the wave-absorbing performance is improved.
The magnetic alloy material selected in the invention is an alloy material which takes an iron-based material as a main temperature-resistant metal and a nonmetal as auxiliary materials, so that the requirements of high temperature resistance and broadband absorption which are difficult to meet by a single absorbent are made up, the practical application requirements of low cost, simplified process, universality on various base materials and the like can be realized, and the magnetic alloy material is the preferred absorbent material in the invention. Specifically, in some embodiments of the present invention, the magnetic alloy material has a Curie temperature above 700 ℃ and an average grain size of 4.0 to 40.0 μm.
Further, in some embodiments of the present invention, the magnetic alloy material includes a metal element and a nonmetal element, the metal element includes iron and at least one of cobalt, nickel, chromium, molybdenum, and aluminum, and the nonmetal element includes silicon. Still further, in some preferred embodiments of the present invention, the magnetic alloy material is an iron-cobalt-nickel-chromium-molybdenum-silicon-aluminum alloy powder, wherein the mass fractions of iron, cobalt, nickel, chromium, molybdenum, silicon and aluminum are 34 to 89%, 3 to 20%, 1 to 10%, 3 to 8%, 2 to 8%, 1 to 12% and 1 to 8% in this order.
In addition, in some embodiments of the present invention, a method for preparing the magnetic alloy material is further provided, which mainly includes four steps of batching, smelting, flaking and sieving, and the specific implementation manner is as follows: putting the powder raw materials into a smelting furnace for smelting and vacuum atomization to prepare spherical alloy powder, then sintering for 1-10 h at 180-220 ℃, and then ball-milling and sieving to prepare the magnetic alloy material.
Weighing powder raw materials according to a proportion (the purity of the powder raw materials is preferably higher than 99.9%), putting the powder raw materials into a vacuum induction melting furnace for melting, then carrying out vacuum atomization to obtain spherical alloy powder, then placing the spherical alloy powder at the temperature of 180-220 ℃ for sintering for 1-10 h, then carrying out ball milling on the sintered alloy powder by a ball mill to carry out flakiness to obtain flakiness powder, and then sieving by a 300-mesh sieve to obtain the magnetic alloy powder with the average particle size of 4.0-40.0 mu m. The magnetic alloy powder prepared by the invention can form multi-size interactive distribution through smelting and ball milling processes, can play a role in connection and bridging in a binder system after subsequent homogenization, and can form uniform dispersion in the system, so that the stability of performance is ensured, and the multi-size distribution absorbent can regulate and control the electromagnetic parameters of the material, so that the material has a broadband absorption effect. In summary, the magnetic alloy powder prepared by the invention has the characteristics of high temperature resistance and broadband absorption when being used as an absorbent in a high-temperature-resistant wave-absorbing coating, and iron is used as a main component to be doped with other metal elements and non-metal elements, so that the high-temperature resistance, fatigue resistance and impact resistance of the absorbent can be improved, the magnetic conductivity and dielectric constant of the metal powder can be adjusted, and the problem of poor impedance matching performance of a single magnetic metal absorbent is solved.
When the alloy powder is ball-milled, the longer the ball-milling time is, the more likely surface defects inevitably occur in the microstructure of the alloy powder. In some embodiments of the invention, the time of ball milling is preferably 2 to 10 hours. In addition, it is also conceivable to increase the electromagnetic absorption performance of the magnetic alloy powder by increasing the specific surface area of the magnetic alloy powder or by increasing the dielectric properties of the magnetic alloy powder without affecting the magnetic permeability.
With the development of excellent performance, low cost and environmental protection in the coating industry, inorganic coatings show superiority which organic coatings do not have, and attract extensive attention and intensive research. Silicate and phosphate compounds are used as adhesives which are widely used at present, but the bottleneck problems of poor water resistance, low strength, high brittleness, high curing temperature, poor acid and alkali resistance and the like which need to be solved still exist. The modified adhesive selected by the invention adopts organic silicon as a modifier to modify the adhesives such as silicate or phosphate, and the like, and utilizes the coupling and crosslinking action among intermolecular hydroxyl groups to enable organic-inorganic materials to form a crosslinking network structure in molecules to form a compact, tough and high-adhesion film, so that on one hand, the flexibility, the water resistance and the acid and alkali resistance of the inorganic coating are improved, on the other hand, the curing temperature of the coating is reduced, the coating can be cured at room temperature, and the process flow of preparing the broadband wave-absorbing material by subsequently adopting the high-temperature-resistant wave-absorbing coating is facilitated to be simplified.
Specifically, in some embodiments of the present invention, the modified binder includes at least one of modified silicate, modified silica sol, modified alumina sol, and modified phosphate, which may be any one of the above substances, or a mixture of any two or more of the above substances, and all of them fall within the protection scope of the present invention.
In addition, the invention also provides a preparation method of the modified adhesive, which specifically comprises the following steps: mixing the adhesive and organic silicon, and stirring for 0.5-8 h at 25-90 ℃ to prepare a modified adhesive; wherein the addition amount of the organic silicon is 1-10% of the mass of the adhesive. It is to be understood that, when the modified binder includes two or more of modified silicate, modified silica sol, modified alumina sol, and modified phosphate, the step of mixing the binder and the silicone may be a step of mixing the binder with only one binder, and mixing different modified binders after performing a plurality of binder modifications to obtain different modified binders, or may be a step of mixing two or more of silicate, silica sol, alumina sol, and phosphate to obtain the modified binder directly by one modification.
The modified adhesive prepared by the invention is obtained by modifying an inorganic coating by adopting an organic silicon material, the inorganic material and the organic material can load a large amount of active hydroxyl groups on the surface in an aqueous medium, the active hydroxyl groups form a coupling or crosslinking structure on the surface of a molecule in the modification and subsequent curing processes, and a compact crosslinking network structure is gradually formed along with the volatilization of moisture, so that the strong adhesion performance, the good water resistance and the high temperature resistance are realized, and the modified adhesive has the characteristics of room temperature curability, water resistance, acid and alkali resistance and stable high temperature resistance.
Additionally, in some embodiments of the present invention, the adjunct comprises an anti-settling agent and an anti-foaming agent. Specifically, the anti-settling agent may be, for example, a hollow micro powder anti-settling agent, and the mass of the anti-settling agent accounts for 5% of the solid component in the high temperature-resistant wave-absorbing coating. The defoaming agent can be a vegetable oil defoaming agent, and the mass of the defoaming agent accounts for 0.5% of the solid components in the high-temperature resistant wave-absorbing coating.
In addition, in some embodiments of the present invention, the solvent includes at least one of water and a water-based sol, and the water may be used alone or in combination with the water-based sol. Further, when the solvent is a mixture formed by mixing water and a water-based sol, it is preferable that the water and the water-based sol are mixed at a mass ratio of 1.
Based on the high-temperature-resistant wave-absorbing coating provided by the invention, the invention also provides a preparation method of the high-temperature-resistant wave-absorbing coating, which comprises the following steps:
stirring the modified adhesive at the speed of 3000-10000 rpm for 3-10 min, and then standing for 2-10 min for curing;
and adding a magnetic alloy material, a solvent and an auxiliary agent into the cured modified adhesive, and homogenizing until the magnetic alloy material, the solvent and the auxiliary agent are uniformly dispersed to prepare the high-temperature-resistant wave-absorbing coating.
Firstly, stirring the modified adhesive at a high speed of 3000-10000 rpm for 3-10 min, and then standing for 2-10 min at room temperature for curing; and sequentially adding a magnetic alloy material, a solvent and an auxiliary agent into the cured modified adhesive in proportion, and placing the mixture into a homogeneous emulsifier for homogenization treatment for 5-20 min until the solid raw materials are completely and uniformly dispersed to obtain the homogenized high-temperature-resistant wave-absorbing coating. The raw materials and the process used in the preparation method of the high-temperature-resistant wave-absorbing coating provided by the invention are environment-friendly, non-toxic, simple in process and easy to operate, and the prepared high-temperature-resistant wave-absorbing coating can be homogenized so as to ensure the stable coating process and performance of the coating.
In addition, based on the high-temperature-resistant wave-absorbing coating or the preparation method of the high-temperature-resistant wave-absorbing coating provided by the invention, the invention also provides a broadband wave-absorbing material, the broadband wave-absorbing material comprises a base material and a wave-absorbing coating coated on the surface of the base material, the wave-absorbing coating is formed by the high-temperature-resistant wave-absorbing coating, and the composition or the preparation method of the high-temperature-resistant wave-absorbing coating refers to the embodiment. It can be understood that, since the broadband wave-absorbing material provided by the invention adopts all the embodiments of the high-temperature-resistant wave-absorbing coating or the preparation method of the high-temperature-resistant wave-absorbing coating, at least all the beneficial effects brought by the embodiments are achieved, and no further description is given here. The high-temperature-resistant wave-absorbing coating provided by the invention can be suitable for various base materials, the base materials comprise any one of a stainless steel base material, a titanium alloy base material, an aluminum alloy base material, a quartz base material and an aluminum silicate base material, and a coating formed on the surface of the base material by the high-temperature-resistant wave-absorbing coating has good performance, so that a broadband wave-absorbing material with excellent performance and good stability can be obtained.
For the high-temperature resistant coating material, the thicker the coating thickness is, the higher the requirement on the high-temperature resistance of the material is, the paint spraying usually needs to be formed by multiple thin spraying, and the thicker the coating thickness is, the more challenging the adhesion force at high temperature is. The experimental research shows that the thickness of the wave-absorbing coating is preferably 0.8-3 mm, and the high-temperature resistance and the spraying process of the wave-absorbing coating can be considered at the same time.
In addition, based on the preparation method of the broadband wave-absorbing material or the high-temperature-resistant wave-absorbing coating provided by the invention, the invention also provides a preparation method of the broadband wave-absorbing material, which comprises the following steps:
step S10, providing a high-temperature-resistant wave-absorbing coating, wherein the composition or the preparation method of the high-temperature-resistant wave-absorbing coating refers to the embodiment;
and S20, spraying the high-temperature-resistant wave-absorbing coating on the surface of a base material by using an air pressure spray gun, and curing at room temperature to obtain the broadband wave-absorbing material.
It can be understood that, because the preparation method of the broadband wave-absorbing material provided by the invention adopts all the embodiments of the high-temperature-resistant wave-absorbing coating or the preparation method of the high-temperature-resistant wave-absorbing coating provided by the invention, at least all the beneficial effects brought by the embodiments are achieved, and the details are not repeated herein. The preparation method of the broadband wave-absorbing material provided by the invention has a simple process, and can be cured at room temperature, so that the process energy consumption and the production cost are greatly reduced.
The technical solutions of the present invention are further described in detail below with reference to specific examples and drawings, it should be understood that the following examples are merely illustrative of the present invention and are not intended to limit the present invention.
Example 1
(1) Weighing iron, silicon and chromium with the purity higher than 99.9 percent according to the proportion (the mass fractions of the iron, the silicon and the chromium are respectively 88 percent, 6 percent and 6 percent), mixing the materials, putting the materials into a vacuum induction smelting furnace for smelting for a period of time, then carrying out vacuum atomization to obtain spherical alloy powder, then sintering for 4 hours at 200 ℃, then carrying out ball milling on the sintered alloy powder for 2 hours by adopting a ball mill, and sieving the sintered alloy powder by a 300-mesh sieve to obtain the magnetic alloy powder with the average size of 4.0-10.0 mu m.
(2) Mixing the silica sol with organic silicon (the mass of the organic silicon is 5 percent of that of the silica sol), and stirring for 6 hours at 70 ℃ to prepare the modified adhesive.
(3) Weighing 100 parts of modified adhesive, stirring at a high speed of 5000rpm for 8min, and standing at room temperature for 8min for curing; and then sequentially adding 300 parts of magnetic alloy powder, 30 parts of solvent (water) and 10 parts of auxiliary agent (comprising a hollow micro powder anti-settling agent and a vegetable oil defoaming agent, wherein the mass ratio of the anti-settling agent to the defoaming agent is 10: 1) into the cured modified adhesive, and placing the mixture into a homogeneous emulsifier for homogenization treatment for 5min until the solid raw materials are completely and uniformly dispersed to prepare the homogenized high-temperature-resistant wave-absorbing coating.
Example 2
(1) Weighing iron, silicon, chromium, molybdenum and aluminum with the purity higher than 99.9 percent according to the proportion (the mass fractions of the iron, the silicon, the chromium, the molybdenum and the aluminum are respectively 86 percent, 5 percent, 6 percent and 3 percent), mixing the materials, putting the materials into a vacuum induction smelting furnace to be smelted for a period of time, then carrying out vacuum atomization to obtain spherical alloy powder, then sintering the spherical alloy powder for 2 hours at 200 ℃, then carrying out ball milling on the sintered alloy powder for 6 hours by adopting a ball mill, and sieving the sintered alloy powder by a 300-mesh sieve to obtain the magnetic alloy powder with the average size of 6.0 to 15.0 mu m.
(2) Mixing silicate and organic silicon (the mass of the organic silicon is 1 percent of that of the silicate), and stirring for 2.5 hours at 40 ℃ to prepare the modified adhesive.
(3) Weighing 120 parts of modified adhesive, stirring at a high speed of 8000rpm for 8min, and standing at room temperature for 8min for curing; and sequentially adding 280 parts of magnetic alloy powder, 60 parts of solvent (water-based sol) and 10 parts of auxiliary agent (comprising a hollow micro powder anti-settling agent and a vegetable oil defoaming agent, wherein the mass ratio of the anti-settling agent to the defoaming agent is 10: 1) into the cured modified adhesive, and placing the mixture into a homogeneous emulsifier for homogenization treatment for 8min until the solid raw materials are completely and uniformly dispersed to prepare the homogenized high-temperature-resistant wave-absorbing coating.
Example 3
(1) Weighing iron, cobalt, nickel, chromium, molybdenum, silicon and aluminum with the purity higher than 99.9 percent according to the proportion (the mass fractions of the iron, the cobalt, the nickel, the chromium, the molybdenum, the silicon and the aluminum are respectively 88 percent, 3 percent, 1 percent, 3 percent, 2 percent, 1 percent and 2 percent), mixing the materials, putting the materials into a vacuum induction smelting furnace for smelting for a period of time, carrying out vacuum atomization to obtain spherical alloy powder, then sintering for 6 hours at 200 ℃, ball-milling the sintered alloy powder for 10 hours by using a ball mill, and sieving by using a 300-mesh sieve to obtain the magnetic alloy powder with the average size of 8.0-30.0 mu m.
(2) Mixing silica sol and organic silicon (the mass of the organic silicon is 2 percent of that of the silica sol), and stirring for 4 hours at 60 ℃ to prepare the modified adhesive.
(3) Weighing 200 parts of modified adhesive, stirring at a high speed of 10000rpm for 10min, and standing at room temperature for 10min for curing; and then sequentially adding 200 parts of magnetic alloy powder, 20 parts of solvent (water and water-based sol are mixed in equal mass ratio) and 20 parts of auxiliary agent (comprising a hollow micro powder anti-settling agent and a vegetable oil defoaming agent, wherein the mass ratio of the anti-settling agent to the defoaming agent is 10.
Example 4
(1) Weighing iron, cobalt, silicon and aluminum with the purity higher than 99.9 percent according to the proportion (the mass fractions of the iron, the cobalt, the silicon and the aluminum are respectively 79 percent, 5 percent, 10 percent and 6 percent), mixing the materials, putting the materials into a vacuum induction smelting furnace for smelting for a period of time, then carrying out vacuum atomization to obtain spherical alloy powder, then sintering for 5 hours at 200 ℃, then carrying out ball milling on the sintered alloy powder for 2 hours by adopting a ball mill, and sieving by using a 300-mesh sieve to obtain the magnetic alloy powder with the average size of 15.0-25.0 mu m.
(2) And (3) mixing phosphate with organic silicon (the mass of the organic silicon is 1 percent of that of the phosphate), and stirring at 90 ℃ for 0.5h to prepare the modified adhesive.
(3) Weighing 150 parts of modified adhesive, stirring at 6000rpm for 6min at high speed, and standing at room temperature for 6min for curing; and then sequentially adding 250 parts of magnetic alloy powder, 20 parts of solvent (water and water-based sol are mixed in equal mass ratio) and 15 parts of auxiliary agent (comprising a hollow micro powder anti-settling agent and a vegetable oil defoaming agent, wherein the mass ratio of the anti-settling agent to the defoaming agent is 10: 1) into the cured modified adhesive, and placing the mixture into a homogeneous emulsifier for homogenization treatment for 16min until the solid raw materials are completely and uniformly dispersed to prepare the homogenized high-temperature-resistant wave-absorbing coating.
Example 5
(1) Weighing iron, chromium, silicon and molybdenum with the purity higher than 99.9 percent according to the proportion (the mass fractions of the iron, the chromium, the silicon and the molybdenum are respectively 85 percent, 8 percent, 3 percent and 4 percent), mixing the materials, putting the materials into a vacuum induction smelting furnace to be smelted for a period of time, then carrying out vacuum atomization to obtain spherical alloy powder, then sintering the spherical alloy powder for 3 hours at 200 ℃, then carrying out ball milling on the sintered alloy powder for 7 hours by adopting a ball mill, and sieving the sintered alloy powder by a 300-mesh sieve to obtain the magnetic alloy powder with the average size of 10.0 to 15.0 mu m.
(2) Mixing silicate and organic silicon (the mass of the organic silicon is 6 percent of that of the silicate), and stirring for 1h at 40 ℃ to prepare the modified adhesive.
(3) Weighing 160 parts of modified adhesive, stirring at 6000rpm for 5min at a high speed, and standing at room temperature for 5min for curing; and then adding 240 parts of magnetic alloy powder, 50 parts of solvent (water and water-based sol are mixed in equal mass ratio) and 9 parts of auxiliary agent (comprising hollow micro powder anti-settling agent and vegetable oil defoaming agent, wherein the mass ratio of the anti-settling agent to the defoaming agent is 10.
Example 6
The preparation procedure was the same as in example 1, except that the ball milling time in step (1) was extended to 8 hours, to obtain a magnetic alloy powder having an average size of 6.0 to 15.0. Mu.m.
Example 7
The preparation steps are the same as those of example 5, except that 80 parts of modified binder, 320 parts of magnetic alloy powder, 25 parts of assistant and 80 parts of solvent are used in step (3).
Example 8
(1) Weighing iron, cobalt, nickel, chromium, molybdenum, silicon and aluminum with the purity higher than 99.9 percent according to the proportion (the mass fractions of the iron, the cobalt, the nickel, the chromium, the molybdenum, the silicon and the aluminum are respectively 75 percent, 3 percent, 4 percent, 5 percent, 3 percent, 6 percent and 4 percent), mixing the materials, putting the mixture into a vacuum induction smelting furnace for smelting for a period of time, then carrying out vacuum atomization to obtain spherical alloy powder, then sintering for 4 hours at 180 ℃, then carrying out ball milling on the sintered alloy powder for 4 hours by a ball mill, and sieving by a 300-mesh sieve to obtain the magnetic alloy powder with the average particle size of 25.0-40.0 mu m.
(2) Mixing silica sol and organic silicon (the mass of the organic silicon is 10 percent of that of the silica sol), and stirring for 5 hours at 25 ℃ to prepare the modified adhesive.
(3) Weighing 140 parts of modified adhesive, stirring at 3000rpm for 3min at high speed, and standing at room temperature for 6min for curing; and then sequentially adding 350 parts of magnetic alloy powder, 60 parts of solvent (water) and 2.5 parts of auxiliary agent (comprising a hollow micro powder anti-settling agent and a vegetable oil defoaming agent, wherein the mass ratio of the anti-settling agent to the defoaming agent is 10: 1) into the cured modified adhesive, and placing the mixture into a homogeneous emulsifier for homogenization treatment for 10min until the solid raw materials are completely and uniformly dispersed to prepare the homogenized high-temperature-resistant wave-absorbing coating.
Example 9
(1) Weighing iron, cobalt, nickel, chromium, molybdenum, silicon and aluminum with the purity higher than 99.9 percent according to the proportion (the mass fractions of the iron, the cobalt, the nickel, the chromium, the molybdenum, the silicon and the aluminum are respectively 80 percent, 5 percent, 1 percent, 5 percent, 3 percent and 1 percent), mixing the materials, putting the materials into a vacuum induction smelting furnace for smelting for a period of time, carrying out vacuum atomization to obtain spherical alloy powder, then sintering for 2 hours at 220 ℃, ball-milling the sintered alloy powder for 8 hours by using a ball mill, and sieving by using a 300-mesh sieve to obtain the magnetic alloy powder with the average grain diameter of 10.0-25.0 mu m.
(2) Mixing silica sol and organic silicon (the mass of the organic silicon is 8 percent of that of the silica sol), and stirring for 5 hours at 50 ℃ to prepare the modified adhesive.
(3) Weighing 180 parts of modified adhesive, stirring at a high speed of 8000rpm for 4min, and standing at room temperature for 4min for curing; and then sequentially adding 400 parts of magnetic alloy powder, 120 parts of solvent (water-based sol) and 12 parts of auxiliary agent (comprising a hollow micro powder anti-settling agent and a vegetable oil defoaming agent, wherein the mass ratio of the anti-settling agent to the defoaming agent is 10: 1) into the cured modified adhesive, and placing the mixture into a homogeneous emulsifier for homogenization treatment for 10min until the solid raw materials are completely and uniformly dispersed to prepare the homogenized high-temperature-resistant wave-absorbing coating.
Example 10
And (2) spraying the high-temperature-resistant wave-absorbing coating prepared in the embodiment 1 on the surface of a titanium alloy base material by using an air pressure spray gun, and curing at room temperature to form a wave-absorbing coating with the thickness of 1.3mm to prepare the broadband wave-absorbing material.
And testing the reflectivity of the coating on the surface of the broadband wave-absorbing material, then placing the broadband wave-absorbing material in a high-temperature oven to be treated at 650 ℃ for 20min, then cooling to room temperature, observing the apparent condition of the coating, and testing the reflectivity.
FIG. 1 shows the comparison of the appearance of the coating before and after high temperature treatment, and it can be seen that the coating surface is intact and has no obvious defects after high temperature treatment.
Fig. 2 shows the reflectance curve of the coating before and after the high temperature treatment, and it can be seen that the reflection loss of the coating after the high temperature treatment is improved by 6% as compared with that before the high temperature treatment.
Example 11
The high-temperature resistant wave-absorbing coating prepared in the embodiment 2 is sprayed on the surface of a quartz substrate by an air pressure spray gun, and the coating is cured at room temperature to form a wave-absorbing coating with the thickness of 0.8mm, so that the broadband wave-absorbing material is prepared.
And testing the reflectivity of the surface coating of the broadband wave-absorbing material, then placing the broadband wave-absorbing material in a high-temperature oven to be treated for 60min at 500 ℃, then cooling to room temperature, observing the apparent condition of the coating, and testing the reflectivity.
Observation of coating appearance: after high-temperature treatment, the coating surface is intact and has no obvious defects.
Fig. 3 shows the reflectance curve of the coating before and after the high temperature treatment, and it can be seen that the reflection loss of the coating after the high temperature treatment is improved by 2% compared to that before the high temperature treatment.
Example 12
And (3) spraying the high-temperature-resistant wave-absorbing coating prepared in the embodiment 3 on the surface of a titanium alloy base material by using an air pressure spray gun, and curing at room temperature to form a wave-absorbing coating with the thickness of 1.5mm to prepare the broadband wave-absorbing material.
And testing the reflectivity of the coating on the surface of the broadband wave-absorbing material, then placing the broadband wave-absorbing material in a high-temperature oven to be treated for 60min at 400 ℃, then cooling to room temperature, observing the apparent condition of the coating, and testing the reflectivity.
Observation of coating appearance: after high-temperature treatment, the coating surface is intact and has no obvious defects.
FIG. 4 is a scanning electron microscope image of the surface of the coating before and after the high temperature treatment, and it can be seen that the surface of the coating is not significantly changed after the high temperature treatment.
Tests show that after high-temperature treatment, the reflection loss of the coating is improved by 5 percent compared with that before high-temperature treatment.
Example 13
The high temperature resistant wave-absorbing coating prepared in the embodiment 4 is sprayed on the surface of a stainless steel base material by an air pressure spray gun, and the coating is cured at room temperature to form a wave-absorbing coating with the thickness of 2mm, so that the broadband wave-absorbing material is prepared.
And testing the reflectivity of the coating on the surface of the broadband wave-absorbing material, then placing the broadband wave-absorbing material in a high-temperature oven to be treated for 10min at 650 ℃, then cooling to room temperature, observing the apparent condition of the coating, and testing the reflectivity.
Observation of coating appearance: after high-temperature treatment, the surface of the coating is intact and has no obvious defects.
Fig. 5 shows the reflectance curve of the coating before and after the high temperature treatment, and it can be seen that the reflection loss of the coating after the high temperature treatment is improved by 2% compared to that before the high temperature treatment.
Example 14
The high-temperature resistant wave-absorbing coating prepared in the embodiment 5 is sprayed on the surface of a titanium alloy base material by an air pressure spray gun, and the coating is cured at room temperature to form a wave-absorbing coating with the thickness of 1.2mm, so that the broadband wave-absorbing material is prepared.
And testing the reflectivity of the coating on the surface of the broadband wave-absorbing material, then placing the broadband wave-absorbing material in a high-temperature oven to be treated at 650 ℃ for 20min, then cooling to room temperature, observing the apparent condition of the coating, and testing the reflectivity.
Observation of apparent condition of coating: after high-temperature treatment, the coating surface is intact and has no obvious defects.
Fig. 6 shows the reflectance curve of the coating before and after the high temperature treatment, and it can be seen that the reflection loss of the coating after the high temperature treatment is improved by 10% as compared to that before the high temperature treatment.
Example 15
The high-temperature resistant wave-absorbing coating prepared in the embodiment 6 is sprayed on the surface of a titanium alloy base material by an air pressure spray gun, and the coating is cured at room temperature to form a wave-absorbing coating with the thickness of 1.3mm, so that the broadband wave-absorbing material is prepared.
And testing the reflectivity of the coating on the surface of the broadband wave-absorbing material, then placing the broadband wave-absorbing material in a high-temperature oven to be treated at 650 ℃ for 20min, then cooling to room temperature, observing the apparent condition of the coating, and testing the reflectivity.
Observation of coating appearance: after high-temperature treatment, the surface of the coating is intact and has no obvious defects.
Tests show that after high-temperature treatment, the reflection loss of the coating is slightly improved compared with that before high-temperature treatment.
Example 16
And (3) spraying the high-temperature-resistant wave-absorbing coating prepared in the embodiment 7 on the surface of a titanium alloy base material by using an air pressure spray gun, and curing at room temperature to form a wave-absorbing coating with the thickness of 1.3mm to prepare the broadband wave-absorbing material.
And testing the reflectivity of the coating on the surface of the broadband wave-absorbing material, then placing the broadband wave-absorbing material in a high-temperature oven to be treated at 650 ℃ for 20min, then cooling to room temperature, observing the apparent condition of the coating, and testing the reflectivity.
Observation of coating appearance: after high-temperature treatment, the coating surface is intact and has no obvious defects.
Tests show that after high-temperature treatment, the reflection loss of the coating is slightly improved compared with that before high-temperature treatment.
Example 17
The high-temperature resistant wave-absorbing coating prepared in the embodiment 5 is sprayed on the surface of a titanium alloy base material by an air pressure spray gun, and the coating is cured at room temperature to form a wave-absorbing coating with the thickness of 2.5mm, so that the broadband wave-absorbing material is prepared.
And then, the broadband wave-absorbing material is placed in a high-temperature oven to be treated for 20min at the temperature of 650 ℃, then the temperature is reduced to room temperature, and the apparent condition of the coating is observed.
Observation of coating appearance: after high temperature treatment, slight cracks appear on the surface of the coating.
Example 18
The high-temperature resistant wave-absorbing coating prepared in the embodiment 8 is sprayed on the surface of an aluminum alloy base material by an air pressure spray gun, and the coating is cured at room temperature to form a wave-absorbing coating with the thickness of 1.0mm, so that the broadband wave-absorbing material is prepared.
And testing the reflectivity of the coating on the surface of the broadband wave-absorbing material, then placing the broadband wave-absorbing material in a high-temperature oven to be treated at 650 ℃ for 20min, then cooling to room temperature, observing the apparent condition of the coating, and testing the reflectivity.
Observation of apparent condition of coating: after high-temperature treatment, the coating surface is intact and has no obvious defects. Tests show that after high-temperature treatment, the reflection loss of the coating is slightly improved compared with that before high-temperature treatment.
Example 19
The high temperature resistant wave-absorbing coating prepared in the embodiment 9 is sprayed on the surface of the titanium alloy base material by an air pressure spray gun, and the coating is cured at room temperature to form a wave-absorbing coating with the thickness of 3.0mm, so that the broadband wave-absorbing material is prepared.
And testing the reflectivity of the surface coating of the broadband wave-absorbing material, then placing the broadband wave-absorbing material in a high-temperature oven to be treated for 20min at 650 ℃, then cooling to room temperature, observing the apparent condition of the coating, and testing the reflectivity.
Observation of apparent condition of coating: after high-temperature treatment, the coating surface is intact and has no obvious defects.
Tests show that after high-temperature treatment, the reflection loss of the coating is slightly improved compared with that before high-temperature treatment.
Comparative example 1
(1) Weighing iron, silicon and chromium with the purity higher than 99.9 percent according to the proportion (the mass fractions of the iron, the silicon and the chromium are respectively 80 percent, 12 percent and 8 percent), mixing the materials, putting the materials into a vacuum induction smelting furnace for smelting for a period of time, then carrying out vacuum atomization to obtain spherical alloy powder, then sintering for 4 hours at 200 ℃, then carrying out ball milling on the sintered alloy powder for 2 hours by adopting a ball mill, and sieving the sintered alloy powder by a 300-mesh sieve to obtain the magnetic alloy powder with the average size of 4.0-10.0 mu m.
(2) Mixing the silica sol with organic silicon (the mass of the organic silicon is 5 percent of that of the silica sol), and stirring for 6 hours at 70 ℃ to prepare the modified adhesive.
(3) Weighing 100 parts of modified adhesive, stirring at a high speed of 5000rpm for 8min, and standing at room temperature for 8min for curing; and sequentially adding 420 parts of magnetic alloy powder, 30 parts of solvent and 10 parts of auxiliary agent into the cured modified adhesive, and placing the mixture into a homogeneous emulsifier for homogenization treatment for 5min until the solid raw materials are completely and uniformly dispersed to prepare the homogenized high-temperature-resistant wave-absorbing coating.
(4) And spraying the prepared high-temperature-resistant wave-absorbing coating on the surface of a titanium alloy base material by using an air pressure spray gun, and curing at room temperature to form a wave-absorbing coating with the thickness of 1.3mm to prepare the broadband wave-absorbing material.
And then, the broadband wave-absorbing material is placed in a high-temperature oven to be treated for 20min at the temperature of 650 ℃, then the temperature is reduced to room temperature, and the apparent condition of the coating is observed.
Observation of apparent condition of coating: after high-temperature treatment, the coating surface comes off.
Comparative example 2
(1) Weighing iron, silicon and chromium with the purity higher than 99.9 percent according to the proportion (the mass fractions of the iron, the silicon and the chromium are respectively 85 percent, 9 percent and 6 percent), mixing the materials, putting the materials into a vacuum induction smelting furnace for smelting for a period of time, then carrying out vacuum atomization to obtain spherical alloy powder, then sintering the spherical alloy powder for 4 hours at 200 ℃, then carrying out ball milling on the sintered alloy powder for 2 hours by adopting a ball mill, and sieving the spherical alloy powder with a 300-mesh sieve to obtain the magnetic alloy powder with the average size of 4.0-10.0 mu m.
(2) Mixing the silica sol with organic silicon (the mass of the organic silicon is 5 percent of that of the silica sol), and stirring for 6 hours at 70 ℃ to prepare the modified adhesive.
(3) Weighing 100 parts of modified adhesive, stirring at a high speed of 8000rpm for 8min, and standing at room temperature for 8min for curing; and sequentially adding 300 parts of magnetic alloy powder, 30 parts of solvent and 10 parts of auxiliary agent into the cured modified adhesive, and placing the mixture into a homogeneous emulsifier for homogenization treatment for 5min until the solid raw materials are completely and uniformly dispersed to prepare the homogenized high-temperature-resistant wave-absorbing coating.
(4) And spraying the prepared high-temperature-resistant wave-absorbing coating on the surface of a titanium alloy base material by using an air pressure spray gun, and curing at room temperature to form a wave-absorbing coating with the thickness of 3.2mm to prepare the broadband wave-absorbing material.
And then, the broadband wave-absorbing material is placed in a high-temperature oven to be treated for 20min at 650 ℃, then the temperature is reduced to room temperature, and the apparent condition of the coating is observed.
Observation of coating appearance: after high-temperature treatment, the coating surface slightly falls off. In addition, the spray process of the coating material is difficult to be increased compared to example 10.
The above are only preferred embodiments of the present invention, and do not limit the scope of the present invention, and it is obvious to those skilled in the art that various modifications and variations can be made in the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall be included in the scope of the present invention.
Claims (10)
1. The high-temperature-resistant wave-absorbing coating is characterized by comprising, by mass, 200-400 parts of an absorbent, 80-200 parts of a modified adhesive, 1-25 parts of an auxiliary agent and 1-120 parts of a solvent, wherein the absorbent is a magnetic alloy material, and the modified adhesive can be cured at room temperature.
2. The high temperature resistant wave absorbing coating of claim 1, wherein the magnetic alloy material has a Curie temperature of greater than 700 ℃ and an average particle size of 4.0-40.0 μm.
3. The high temperature resistant wave absorbing coating of claim 1 wherein the magnetic alloy material comprises metallic elements and non-metallic elements, the metallic elements comprise iron and at least one of cobalt, nickel, chromium, molybdenum, and aluminum, and the non-metallic elements comprise silicon.
4. The high temperature resistant wave absorbing coating of claim 3, wherein the preparation of the magnetic alloy material comprises:
putting the powder raw materials into a smelting furnace for smelting and vacuum atomization to prepare spherical alloy powder, then sintering for 1-10 h at 180-220 ℃, and then ball-milling and sieving to prepare the magnetic alloy material.
5. The high temperature resistant wave absorbing coating of claim 1, wherein the modified binder comprises at least one of modified silicate, modified silica sol, modified alumina sol, modified phosphate; and/or the presence of a gas in the gas,
the auxiliary agent comprises an anti-settling agent and a defoaming agent; and/or the presence of a gas in the atmosphere,
the solvent includes at least one of water and a water-based sol.
6. The high temperature resistant wave absorbing coating of claim 5, wherein the modified binder is prepared by the steps of:
mixing the adhesive and organic silicon, and stirring at 25-90 ℃ for 0.5-8 h to prepare a modified adhesive; wherein the addition amount of the organic silicon is 1-10% of the mass of the adhesive.
7. A method for preparing the high temperature resistant wave-absorbing coating as claimed in any one of claims 1 to 6, characterized by comprising the following steps:
stirring the modified adhesive at the speed of 3000-10000 rpm for 3-10 min, and then standing for 2-10 min for curing;
and adding a magnetic alloy material, a solvent and an auxiliary agent into the cured modified adhesive, and homogenizing until the magnetic alloy material, the solvent and the auxiliary agent are uniformly dispersed to prepare the high-temperature-resistant wave-absorbing coating.
8. A broadband wave-absorbing material is characterized by comprising a base material and a wave-absorbing coating coated on the surface of the base material, wherein the wave-absorbing coating is formed by the high-temperature-resistant wave-absorbing coating according to any one of claims 1 to 6, and the base material comprises any one of a stainless steel base material, a titanium alloy base material, an aluminum alloy base material, a quartz base material and an aluminum silicate base material.
9. The broadband wave-absorbing material of claim 8, wherein the thickness of the wave-absorbing coating is 0.8-3 mm.
10. A method for preparing a broadband wave absorbing material according to any one of claims 8 to 9, comprising the following steps:
providing a high temperature resistant wave absorbing coating according to any one of claims 1 to 6;
and spraying the high-temperature-resistant wave-absorbing coating on the surface of a base material by using an air pressure spray gun, and curing at room temperature to obtain the broadband wave-absorbing material.
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