CN115651477A - High-temperature-resistant wave-absorbing coating and preparation method thereof - Google Patents
High-temperature-resistant wave-absorbing coating and preparation method thereof Download PDFInfo
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Abstract
The invention provides a preparation method of a high-temperature-resistant wave-absorbing coating, belonging to the technical field of wave-absorbing materials; the preparation method comprises the following steps: s1, fully mixing iron-cobalt alloy powder, phenolic resin glue solution, organic solvent and silane coupling agent to obtain mixed slurry; s2, under the grinding condition, adding an organic solvent into the mixed slurry, and adjusting the viscosity of the mixed slurry to obtain the wave-absorbing coating; and S3, spraying the wave-absorbing coating on the surface of the substrate to obtain the high-temperature-resistant wave-absorbing coating. The preparation method is simple and controllable, and the prepared wave-absorbing coating has excellent high-temperature resistance, wave-absorbing performance and mechanical property and can meet the high-temperature requirement.
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.
Background
With the development of microwave technology, the system has higher and higher requirements on the high temperature resistance of microwave absorbing materials. However, the traditional wave-absorbing coating has the defects of poor temperature resistance, easy coating cracking at high temperature and reduced wave-absorbing performance, and cannot meet the high-temperature requirement.
Therefore, it is urgently needed to provide a wave-absorbing coating which is not easy to crack at high temperature and has excellent wave-absorbing performance.
Disclosure of Invention
Aiming at one or more technical problems in the prior art, the invention provides a high-temperature-resistant wave-absorbing coating, a preparation method thereof and a preparation method thereof.
The invention provides a preparation method of a high-temperature-resistant wave-absorbing coating in a first aspect, which comprises the following steps:
s1, sufficiently mixing iron-cobalt alloy powder, phenolic resin glue solution, organic solvent and silane coupling agent to obtain mixed slurry;
s2, under the grinding condition, adding an organic solvent into the mixed slurry, and adjusting the viscosity of the mixed slurry to obtain the wave-absorbing coating;
and S3, spraying the wave-absorbing coating on the surface of a substrate to obtain the high-temperature-resistant wave-absorbing coating.
Preferably, in step S1, after the iron-cobalt alloy powder and the phenolic resin glue solution are mixed, the organic solvent and the silane coupling agent are added under stirring to obtain the mixed slurry.
Preferably, in step S1, the mass ratio of the iron-cobalt alloy powder, the phenolic resin glue solution, the organic solvent and the silane coupling agent is (70-90): 17-55): 20-30): 0.02-0.08.
Preferably, in step S1, the particle size of the iron-cobalt alloy powder is 10 to 40 μm.
Preferably, in step S1, the phenolic resin glue solution is obtained by mixing phenolic resin and an organic solvent; the solid content of the phenolic resin glue solution is 50-70%.
Preferably, in step S2, under the grinding condition, an organic solvent is added to the mixed slurry, and the viscosity of the mixed slurry is adjusted to 10 to 30Pa · S, so as to obtain the wave-absorbing coating.
Preferably, in step S1, the silane coupling agent is γ -glycidoxypropyltrimethoxysilane; and/or
In step S1 and step S2, the organic solvent is one of ethyl acetate, n-butanol, and acetone.
Preferably, in the step S3, the wave-absorbing coating is put into a spray tank, and a spray gun is used for spraying the surface of the substrate for 50-150 times to obtain the high-temperature-resistant wave-absorbing coating; when spraying, the caliber of the spray gun is set to be 1-2 mm, the spraying pressure is 0.2-0.8 MPa, and the spraying distance is 10-50 cm.
Preferably, in step S3, the substrate is an alloy substrate; and/or the thickness of the high-temperature-resistant wave-absorbing coating is 0.5-2 mm.
The invention provides a high-temperature-resistant wave-absorbing coating in a second aspect, which is prepared by the preparation method in the first aspect.
Compared with the prior art, the invention at least has the following beneficial effects:
the wave-absorbing slurry is prepared by taking iron-cobalt alloy powder with high temperature resistance as an absorbent, phenolic resin as a base material and silane coupling agent as raw materials, uniformly dispersed mixed slurry of the iron-cobalt alloy powder and the phenolic resin is prepared, the viscosity of the mixed slurry is regulated and controlled, the wave-absorbing coating capable of being directly sprayed on the surface of a structural member is obtained, and the formed wave-absorbing coating has excellent high temperature resistance, wave-absorbing performance and mechanical property.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the description below are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
Fig. 1 is a reflectivity-frequency curve diagram of a semi-cured high temperature resistant wave-absorbing film provided in embodiment 1 of the present invention;
fig. 2 is a reflectivity-frequency curve diagram of the semi-cured high temperature resistant wave-absorbing film provided in embodiment 2 of the present invention;
fig. 3 is a reflectivity-frequency curve diagram of the semi-cured high temperature resistant wave-absorbing film provided in embodiment 3 of the present invention;
FIG. 4 is a reflectivity-frequency curve of the wave-absorbing film provided in comparative example 1 of the present invention;
FIG. 5 is a reflectivity-frequency curve diagram of the wave-absorbing film provided by comparative example 5 of the invention.
Detailed Description
To make the objects, technical solutions and advantages of the embodiments of the present invention clearer and more complete, the following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments, and all other embodiments obtained by a person of ordinary skill in the art without creative efforts based on the embodiments of the present invention belong to the protection scope of the present invention.
The invention provides a preparation method of a high-temperature-resistant wave-absorbing coating in a first aspect, which comprises the following steps:
s1, sufficiently mixing iron-cobalt alloy powder, phenolic resin glue solution, organic solvent and silane coupling agent to obtain mixed slurry; the wave-absorbing slurry takes the iron-cobalt alloy powder as an absorbent and the phenolic resin as a matrix material, and both are high-temperature resistant materials, so that after the iron-cobalt alloy powder and the phenolic resin are compounded, the prepared wave-absorbing coating can be ensured to have excellent high-temperature resistance, wave-absorbing performance and mechanical property.
S2, under the grinding condition, adding an organic solvent into the mixed slurry, and adjusting the viscosity of the mixed slurry to obtain the wave-absorbing coating; under the condition of grinding, the organic solvent is added into the mixed slurry to adjust the viscosity of the mixed slurry, so as to obtain the wave-absorbing coating suitable for spraying.
And S3, spraying the wave-absorbing coating on the surface of a matrix to obtain the high-temperature-resistant wave-absorbing coating.
The wave-absorbing slurry takes the iron-cobalt alloy powder with high temperature resistance as an absorbent, the phenolic resin as a matrix material and the silane coupling agent as raw materials to prepare the mixed slurry with the uniformly dispersed iron-cobalt alloy powder and the phenolic resin, and the wave-absorbing coating capable of being directly sprayed on the surface of a structural member is obtained by regulating and controlling the viscosity of the mixed slurry, so that the formed wave-absorbing coating has excellent high temperature resistance, wave-absorbing performance and mechanical property.
According to some preferred embodiments, in step S1, after the iron-cobalt alloy powder and the phenolic resin glue solution are mixed, the organic solvent and the silane coupling agent are added under stirring conditions, so as to obtain the mixed slurry.
According to some preferred embodiments, in the step S1, the mass ratio of the iron-cobalt alloy powder, the phenolic resin glue solution, the organic solvent and the silane coupling agent is (70-90): 17-55: (20-30): 0.02-0.08); according to the invention, the dosage of the iron-cobalt alloy powder, the phenolic resin glue solution, the organic solvent and the silane coupling agent is controlled within the above range, so that the mixed slurry with uniformly dispersed iron-cobalt alloy powder and phenolic resin is obtained, the prepared wave-absorbing coating is ensured to have excellent mechanical property, temperature resistance and wave-absorbing property, and can be directly sprayed on the surface of a structural member.
According to some preferred embodiments, in step S1, the particle size of the iron-cobalt alloy powder is 10 to 40 μm; the invention controls the grain diameter of the iron-cobalt alloy powder within the range, and can ensure that the iron-cobalt alloy powder is uniformly dispersed in the phenolic resin glue solution.
According to some preferred embodiments, in step S1, the phenolic resin glue solution is obtained by mixing phenolic resin and an organic solvent; the solid content of the phenolic resin glue solution is 50-70%;
according to some preferred embodiments, in step S2, under the grinding condition, adding an organic solvent to the mixed slurry, and adjusting the viscosity of the mixed slurry to 10 to 30Pa · S to obtain the wave-absorbing coating; according to the invention, the viscosity of the mixed slurry is regulated and controlled by adding the organic solvent, the specific dosage of the organic solvent is not limited, and the requirement that the viscosity of the wave-absorbing coating is controlled within a target range can be met; the viscosity of the wave-absorbing coating is controlled within the range, the obtained slurry is suitable for spraying, and the sprayed coating has excellent mechanical property and is not easy to crack; has stronger adhesive force with the surface of the structural member and is not easy to fall off.
According to some preferred embodiments, in step S1, the silane coupling agent is γ -glycidoxypropyltrimethoxysilane (KH 560); and/or
In step S1 and step S2, the organic solvent is one of ethyl acetate, n-butanol and acetone; in the step S1, the organic solvent mainly has the function of fully dispersing the iron-cobalt alloy powder, the phenolic resin glue solution and the silane coupling agent to obtain uniformly dispersed mixed slurry; in step S2, the organic solvent is used to adjust the viscosity of the mixed slurry, so as to obtain the wave-absorbing coating meeting the spraying requirement.
According to some preferred embodiments, in step S3, the wave-absorbing coating is put into a spray tank, and a spray gun is used for spraying the surface of the substrate for 50-150 times to obtain the high-temperature-resistant wave-absorbing coating; when spraying, the caliber of the spray gun is set to be 1-2 mm, the spraying pressure is 0.2-0.8 MPa, and the spraying distance is 10-50 cm. In the spraying process, the spraying times, the caliber of the spray gun, the spraying pressure and the spraying distance can be adjusted according to actual needs, and the related parameters of the spraying times, the caliber of the spray gun, the spraying pressure and the spraying distance are generally limited in the range, so that most requirements can be met.
According to some preferred embodiments, in step S3, the substrate is an alloy substrate; and/or the thickness of the high-temperature-resistant wave-absorbing coating is 0.5-2 mm. The thickness of the wave-absorbing coating can be selected according to actual requirements and application scenes, and the wave-absorbing coating with the thickness can be obtained by matching with corresponding spraying parameters.
In some specific embodiments, preparing the high temperature resistant and wave absorbing coating includes: s1, mixing the iron-cobalt alloy powder and the phenolic resin glue solution, stirring for 10-20 min at the rotating speed of 400-700 r/min, and adding the organic solvent and the silane coupling agent under the stirring condition to obtain mixed slurry; the mass ratio of the iron-cobalt alloy powder, the phenolic resin glue solution, the organic solvent and the silane coupling agent is (70-90): (17-55): 20-30): 0.02-0.08; s2, putting the mixed slurry into a three-roll grinding machine, grinding for 1-3 h at the rotating speed of 50-70 r/min, adding an organic solvent into the mixed slurry under the grinding condition, and adjusting the viscosity of the mixed slurry to 10-30 Pa.s to obtain the wave-absorbing coating; s3, putting the wave-absorbing coating into a spray tank, and spraying the surface of the substrate for 50-150 times by using a spray gun to obtain the high-temperature-resistant wave-absorbing coating; when spraying, the caliber of the spray gun is set to be 1-2 mm, the spraying pressure is 0.2-0.8 MPa, and the spraying distance is 10-50 cm.
The invention provides a high-temperature-resistant wave-absorbing coating in a second aspect, which is prepared by the preparation method in the first aspect.
The wave-absorbing coating prepared by the invention can be directly sprayed on the surface of a structural member, and the formed wave-absorbing coating has excellent temperature resistance and wave-absorbing performance, and the coating is not easy to crack; in the frequency band of 2-18 GHz, the reflectivity at 300 ℃ is not more than 5dB compared with the reflectivity at normal temperature.
In order to more clearly illustrate the technical solutions and advantages of the present invention, the present invention is further described below with reference to the following embodiments.
It should be noted that the materials and reagents of the present invention can be obtained by direct purchase or self-synthesis in the market, and the specific type is not limited.
The wave-absorbing performance test standard is as follows: reference is made to GJB 2038A-2011.
Example 1
S1, slowly adding 700g of iron-cobalt alloy powder with the particle size of 30um into 550g of phenolic resin with the solid content of 60%, stirring for 10min at the rotating speed of 400r/min by using a stirrer, and adding 200g of ethyl acetate and 0.2g of KH560 under the stirring condition to form mixed slurry;
s2, putting the mixed slurry into a three-roll grinder, grinding for 2 hours at the rotating speed of 50r/min, and grinding during grinding; adding ethyl acetate under the grinding condition until the viscosity is 30 Pa.s to form the wave-absorbing coating;
s3, weighing 500g of wave-absorbing coating, putting the wave-absorbing coating into a spray tank, and spraying 100 times on the surface of the metal piece by using a spray gun to obtain a high-temperature-resistant wave-absorbing coating with the thickness of 1.5 mm; during spraying, the caliber of a spray gun is set to be 1mm, the pressure intensity is set to be 0.6MPa, and the gun moving distance is set to be 20cm;
the high-temperature-resistant wave-absorbing coating can be directly sprayed on the surface of a structural member, and the obtained wave-absorbing coating has excellent temperature resistance and wave-absorbing performance and is not easy to crack; as shown in FIG. 1, the reflectivity does not increase by more than 3dB at 300 ℃ compared with the reflectivity at normal temperature in the 2-18 GHz band.
Example 2
S1, slowly adding 800g of iron-cobalt alloy powder with the particle size of 30um into 400g of phenolic resin with the solid content of 60%, stirring for 10min at the rotating speed of 500r/min by using a stirrer, and adding 300g of ethyl acetate and 0.6g of KH560 under the stirring condition to form mixed slurry;
s2, putting the mixed slurry into a three-roll grinder, grinding for 2 hours at the rotating speed of 70r/min, and grinding during grinding; adding ethyl acetate under the grinding condition until the viscosity is 30 Pa.s to form the wave-absorbing coating;
s3, weighing 500g of wave-absorbing coating, putting the wave-absorbing coating into a spray tank, and spraying the wave-absorbing coating on the surface of the metal piece for 100 times by using a spray gun to obtain a high-temperature-resistant wave-absorbing coating with the thickness of 1.5 mm; during spraying, the caliber of a spray gun is set to be 2mm, the pressure intensity is set to be 0.8MPa, and the gun moving distance is set to be 50cm;
the high-temperature-resistant wave-absorbing coating can be directly sprayed on the surface of a structural part, and the obtained wave-absorbing coating has excellent temperature resistance and wave-absorbing performance and is not easy to crack; as shown in FIG. 2, the reflectivity does not increase by more than 3dB at 300 ℃ compared with the reflectivity at normal temperature in the 2-18 GHz band.
Example 3
S1, slowly adding 900g of iron-cobalt alloy powder with the particle size of 30um into 170g of phenolic resin with the solid content of 60%, stirring for 10min at the rotating speed of 500r/min by using a stirrer, and adding 250g of ethyl acetate and 0.4g of KH560 under the stirring condition to form mixed slurry;
s2, putting the mixed slurry into a three-roller grinding machine, grinding for 2 hours at the rotating speed of 70r/min, and grinding during grinding; adding ethyl acetate under the grinding condition until the viscosity is 10 Pa.s to form the wave-absorbing coating;
s3, weighing 500g of wave-absorbing coating, putting the wave-absorbing coating into a spray tank, and spraying the wave-absorbing coating on the surface of the metal piece for 100 times by using a spray gun to obtain a high-temperature-resistant wave-absorbing coating with the thickness of 1.5 mm; during spraying, the caliber of a spray gun is set to be 2mm, the pressure intensity is set to be 0.8MPa, and the gun moving distance is set to be 50cm;
the high-temperature-resistant wave-absorbing coating can be directly sprayed on the surface of a structural member, so that the prepared wave-absorbing coating has excellent temperature resistance and wave-absorbing performance, and the coating is not easy to crack; as shown in FIG. 3, the reflectivity does not exceed 5dB at 300 ℃ compared with the reflectivity at normal temperature in the 2-18 GHz band.
Comparative example 1
S1, slowly adding 500g of iron-cobalt alloy powder with the particle size of 30 mu m into 550g of phenolic resin with the solid content of 60%, stirring for 20min at the rotating speed of 700r/min by using a stirrer, and adding 100g of ethyl acetate and 0.6g of KH560 under the stirring condition to form mixed slurry.
S2, putting the mixed slurry into a three-roll grinder, grinding for 2 hours at the rotating speed of 50r/min, and grinding during grinding; and adding ethyl acetate under the grinding condition until the viscosity is 30 Pa.s to form the wave-absorbing coating.
S3, weighing 500g of wave-absorbing coating, putting the wave-absorbing coating into a spray tank, and spraying the wave-absorbing coating on the surface of the metal piece for 100 times by using a spray gun to obtain a high-temperature-resistant wave-absorbing coating with the thickness of 0.6 mm; when spraying, setting the caliber of the spray gun to be 1.5mm, the pressure intensity to be 0.7MPa and the gun moving distance to be 50cm;
the high-temperature-resistant wave-absorbing coating can be directly sprayed on the surface of a structural member, as shown in figure 4, in a frequency range of 2-18 GHz, although the rising value of the reflectivity at 300 ℃ is not more than 3dB compared with the reflectivity at normal temperature, the wave-absorbing performance is poor.
Comparative example 2
Comparative example 2 is substantially the same as example 1 except that: in step S1, 800g of iron-cobalt alloy powder with the particle size of 30um, 400g of phenolic resin with the solid content of 60%, 300g of ethyl acetate and 0.6g of KH560 are stirred for 10min by a stirrer at the rotating speed of 400r/min to form mixed slurry.
The formed wave-absorbing coating is non-uniform in dispersion and poor in spraying effect, and a high-temperature-resistant wave-absorbing coating cannot be obtained.
Comparative example 3
Comparative example 3 is substantially the same as example 1 except that: in step S1, 800g of iron-cobalt alloy powder with the particle size of 30um, 400g of phenolic resin with the solid content of 60% and 300g of ethyl acetate are stirred for 10min at the rotating speed of 400r/min by a stirrer to form mixed slurry.
The wave-absorbing coating formed without adding the coupling agent is not uniformly dispersed, so that the high-temperature-resistant wave-absorbing coating cannot be obtained by spraying.
Comparative example 4
Comparative example 4 is essentially the same as example 1, except that: step S2 is not present.
The viscosity of the formed mixed slurry is too high, and the high-temperature resistant wave-absorbing coating cannot be obtained by spraying.
Comparative example 5
Comparative example 5 is substantially the same as example 1 except that: in step S1, the iron-cobalt alloy powder is replaced with carbonyl iron powder.
The wave-absorbing film prepared in the comparative example 5 has certain wave-absorbing performance at normal temperature, but the high-temperature wave-absorbing performance is poorer.
Comparative example 6
Comparative example 6 is substantially the same as example 1 except that: in step S1, the iron-cobalt alloy powder is replaced with ferrite.
The wave-absorbing film prepared in the comparative example 6 has certain wave-absorbing performance at normal temperature, but the high-temperature wave-absorbing performance is poorer.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of a high-temperature-resistant wave-absorbing coating is characterized by comprising the following steps:
s1, fully mixing iron-cobalt alloy powder, phenolic resin glue solution, organic solvent and silane coupling agent to obtain mixed slurry;
s2, under the grinding condition, adding an organic solvent into the mixed slurry, and adjusting the viscosity of the mixed slurry to obtain the wave-absorbing coating;
and S3, spraying the wave-absorbing coating on the surface of a matrix to obtain the high-temperature-resistant wave-absorbing coating.
2. The preparation method according to claim 1, wherein in step S1, after the iron-cobalt alloy powder and the phenolic resin glue solution are mixed, the organic solvent and the silane coupling agent are added under stirring to obtain the mixed slurry.
3. The production method according to claim 1 or 2, wherein in step S1, the mass ratio of the iron-cobalt alloy powder, the phenolic resin glue solution, the organic solvent and the silane coupling agent is (70-90): 17-55)/(20-30): 0.02-0.08.
4. The method according to claim 1 or 2, wherein in step S1, the particle size of the iron-cobalt alloy powder is 10 to 40 μm.
5. The preparation method according to claim 1 or 2, wherein in step S1, the phenolic resin glue solution is obtained by mixing phenolic resin and an organic solvent; the solid content of the phenolic resin glue solution is 50-70%.
6. The preparation method according to claim 1, wherein in step S2, under the grinding condition, an organic solvent is added to the mixed slurry, and the viscosity of the mixed slurry is adjusted to 10-30 Pa-S, so as to obtain the wave-absorbing coating.
7. The production method according to claim 1, wherein in step S1, the silane coupling agent is γ -glycidoxypropyltrimethoxysilane; and/or
In step S1 and step S2, the organic solvent is one of ethyl acetate, n-butanol, and acetone.
8. The preparation method according to claim 1, wherein in step S3, the wave-absorbing coating is placed in a spray tank, and the surface of the substrate is sprayed with a spray gun for 50 to 150 times to obtain the high-temperature-resistant wave-absorbing coating; when spraying, the caliber of the spray gun is set to be 1-2 mm, the spraying pressure is 0.2-0.8 MPa, and the spraying distance is 10-50 cm.
9. The production method according to claim 1 or 8, wherein in step S3, the substrate is an alloy substrate; and/or
The thickness of the high-temperature resistant wave-absorbing coating is 0.5-2 mm.
10. A high-temperature-resistant wave-absorbing coating which is characterized by being prepared by the preparation method of any one of claims 1 to 7.
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