CN113136131B - High-temperature-stability wave-absorbing coating and preparation method and application thereof - Google Patents
High-temperature-stability wave-absorbing coating and preparation method and application thereof Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 110
- 239000011248 coating agent Substances 0.000 title claims abstract description 100
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 113
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 86
- 239000002002 slurry Substances 0.000 claims abstract description 68
- 239000006260 foam Substances 0.000 claims abstract description 37
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 32
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000010521 absorption reaction Methods 0.000 claims abstract description 28
- 239000002131 composite material Substances 0.000 claims abstract description 28
- 239000003822 epoxy resin Substances 0.000 claims abstract description 24
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 24
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 8
- 238000010000 carbonizing Methods 0.000 claims abstract description 8
- 239000000758 substrate Substances 0.000 claims abstract description 8
- 238000005470 impregnation Methods 0.000 claims abstract description 6
- 238000003763 carbonization Methods 0.000 claims abstract description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 16
- 238000007598 dipping method Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000010907 mechanical stirring Methods 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000010298 pulverizing process Methods 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 230000001476 alcoholic effect Effects 0.000 claims 1
- 239000002250 absorbent Substances 0.000 abstract description 15
- 230000002745 absorbent Effects 0.000 abstract description 15
- 239000011268 mixed slurry Substances 0.000 abstract 2
- 239000000463 material Substances 0.000 description 13
- 238000003756 stirring Methods 0.000 description 10
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- 239000011358 absorbing material Substances 0.000 description 3
- 230000010354 integration Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- 238000004891 communication Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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- 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- 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
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Abstract
The invention discloses a high-temperature stable wave-absorbing coating and a preparation method thereof, and mainly solves the problems of poor temperature stability, narrow absorption band and the like of the microwave absorption performance of the conventional coating. The coating takes carbonyl iron and carbon foam as main absorbents, and the absorption bandwidth and the temperature stability of the absorption performance of the coating are adjusted by controlling the carbonization temperature of the carbon foam and the proportion of the carbon foam and the carbonyl iron. The preparation method comprises the following steps: 1. carbonizing melamine foam for 2-6h at 700 ℃, 800 ℃ and 900 ℃ respectively in an argon atmosphere; 2. preparing carbonyl iron and epoxy resin into mixed slurry according to a certain proportion; 3. vacuum impregnation of the carbon foam in the prepared mixed slurry; 4. coating the carbon foam/carbonyl iron composite slurry on a substrate by adopting a blade coating method, and curing at the temperature of 100-120 ℃ for 2-4h to obtain the coating. The coating obtained by the invention can keep an effective absorption frequency band above 8GHz from room temperature to 300 ℃, and the temperature stability of the effective absorption bandwidth and the microwave absorption performance is improved at the same time.
Description
Technical Field
The invention belongs to the technical field of wave-absorbing coating materials, and particularly relates to a high-temperature stable wave-absorbing coating as well as a preparation method and application thereof.
Background
The wave-absorbing material is a material capable of attenuating electromagnetic waves incident into the material and converting electromagnetic energy into heat energy or other forms of energy. Among a plurality of wave-absorbing materials, the wave-absorbing coating is widely applied due to the advantages of simple process, strong shape adaptability and the like. The main components of the wave-absorbing coating are absorbent and resin matrix. The absorbent is mainly divided into three types, namely a magnetic loss type absorbent, a conductive loss type absorbent and a dielectric loss type absorbent. The magnetic loss type absorbent has high absorption efficiency per unit thickness and wide effective absorption band frequency band, but the temperature stability of the absorption performance is poor, and the absorption efficiency of the conductive loss type absorbent and the dielectric loss type absorbent is low, so that the effective absorption band is narrow. Therefore, the wave-absorbing coating used at present has the problems of narrow effective bandwidth, poor temperature stability of wave-absorbing performance, large thickness and the like.
On the other hand, with the increasing degree of integration and miniaturization of various electronic devices, more heat radiation and electromagnetic interference can be generated in a narrow space. Therefore, the wave-absorbing coating is required to be capable of having a wide effective absorption frequency band and stable microwave absorption performance within the temperature of room temperature to 300 ℃ in many fields, and the thickness of the coating is less than 1.5 mm. Therefore, a wave-absorbing coating with thin thickness, wide effective absorption frequency band and high temperature stability of wave-absorbing performance needs to be developed, so that the requirements of development of various electronic devices can be met.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a wave-absorbing coating with high temperature stability, which simultaneously achieves multiple aims of widening an effective absorption frequency band, reducing the coating thickness, improving the temperature stability of microwave absorption performance and the like through compounding of magnetic and conductive absorbents.
The wave-absorbing coating with high temperature stability is prepared by curing carbon foam/carbonyl iron composite slurry, the volume ratio of carbon foam to carbonyl iron slurry in the raw materials of the wave-absorbing coating is 1:1-2:1, and the mass ratio of carbonyl iron to epoxy resin and curing agent in the carbonyl iron slurry is (1-3) 0.5: 0.6.
Further, in the technical scheme, the thickness of the coating is 1.0-1.1mm, and the effective absorption bandwidth of the coating is more than 8GHz within the 8-18GHz frequency band at the temperature of room temperature to 300 ℃.
The invention also provides a method for preparing the wave-absorbing coating with high temperature stability, which comprises the following steps:
step one, preparing carbon foam: ultrasonically cleaning melamine foam with an alcohol solution, drying in an oven for 12-24h, placing the obtained melamine foam in a tubular furnace, carbonizing for 2-6h in an argon atmosphere, and placing the obtained carbon foam in a pulverizer for pulverization to obtain carbon foam particles;
step two, preparing carbonyl iron slurry: uniformly mixing carbonyl iron, epoxy resin and a curing agent according to a certain mass ratio to obtain carbonyl iron slurry;
step three, preparing carbon foam/carbonyl iron composite slurry: vacuum-dipping carbon foam with a certain volume in the carbonyl iron slurry obtained in the step two to obtain carbon foam/carbonyl iron composite slurry;
step four, preparing the wave-absorbing coating: coating the carbon foam/carbonyl iron composite slurry obtained in the third step on a metal substrate by adopting a blade coating method, controlling the thickness of the coating by using a mould, and heating and curing to obtain the wave-absorbing coating with high temperature stability.
Preferably, the mass ratio of the distilled water to the ethanol in the alcohol solution in the step one is 1:1-1:3, the drying temperature is 80-100 ℃, the carbonization temperature of the melamine foam is 700-900 ℃, and the particle size of the carbon foam particles is 100-1000 μm.
Preferably, the mass ratio of the carbonyl iron to the epoxy resin and the curing agent in the carbonyl iron slurry in the step two is (1-3):0.5:0.6, and in order to ensure that the components are uniformly mixed, the carbonyl iron slurry is mechanically stirred and ultrasonically dispersed, the rotating speed of the mechanical stirring is 480-.
Preferably, the volume ratio of the carbon foam to the carbonyl iron slurry in the carbon foam/carbonyl iron composite slurry in the step three is 1:1-2:1, and in order to ensure that the carbonyl iron and the carbon foam are uniformly compounded, the vacuum impregnation pressure is less than 0.09MPa, the vacuum impregnation time is 30min, and the vacuum impregnation temperature is 30-50 ℃.
Preferably, the thickness of the wave-absorbing coating in the step four is controlled to be 1.0-1.1mm, the curing temperature of the coating is 100-120 ℃, and the curing time is 2-4 h.
According to the method for the high-temperature-stability wave-absorbing coating, the high-temperature-stability wave-absorbing coating can effectively generate a good electromagnetic wave absorption effect in mobile phone patches, electronic equipment with high miniaturization and integration level, the field of related aircrafts and electronic devices with large temperature fluctuation of working environments.
Compared with the prior art, the invention has the following advantages:
the high-temperature stable wave-absorbing coating disclosed by the invention takes a composite material consisting of carbon foam and carbonyl iron as an absorbent, and the prepared absorbent integrates multiple loss modes such as magnetic loss, electric conduction loss and the like, so that the wave-absorbing efficiency of the coating per unit thickness can be effectively improved. In addition, the three-dimensional skeleton structure of the carbon foam provides a large number of attachment sites and conductive paths for carbonyl iron, so that the effective absorption band of the coating can be effectively widened. The temperature characteristic of the microwave absorption performance of the coating can be adjusted by adjusting the carbonization temperature and the addition content of the carbon foam, and stable electromagnetic wave absorption can be realized within the range of room temperature to 300 ℃. The vacuum impregnation method is adopted in the preparation process of the coating, so that the high-temperature-resistant epoxy resin can be ensured to be fully contacted and soaked with the absorbent, and the problem of high-temperature oxidation of carbonyl iron is effectively solved; in addition, the use of the die blade coating method in the coating preparation process can effectively simplify the coating process of the coating and improve the flatness of the coating.
The high-temperature stable wave-absorbing coating can obtain an effective absorption frequency band of more than 8GHz within the range of room temperature to 300 ℃ under the condition that the thickness of the coating is 1.0-1.1mm, and covers all Ku wave bands and more than 57% of X wave bands. In addition, the wave absorption coating can show the best wave absorption performance in the whole temperature section, and has good temperature stability of microwave absorption performance. Therefore, the high-temperature stability wave-absorbing coating simultaneously realizes the optimization of multiple key indexes such as thin thickness, wide effective absorption frequency band, high-temperature stability and the like.
The invention is further described below with reference to the accompanying drawings and examples.
Drawings
FIG. 1 is a flow chart of the preparation of the high temperature stability wave-absorbing coating of the present invention.
FIG. 2 is a topographical view of the carbon foam prepared in example 3.
FIG. 3 is a topographical map of carbonyl iron used in example 1.
Fig. 4 is a morphology chart of the carbon foam/carbonyl iron composite absorbent prepared in example 1.
Fig. 5 is a temperature-varying reflection loss diagram of the wave-absorbing coating prepared in example 1. The variable-temperature reflection loss test is carried out according to a GJB 2038A-2011 radar wave-absorbing material reflectivity test method.
Fig. 6 is a thermal weight loss curve of the wave-absorbing coating and the epoxy resin prepared in example 5. The thermal weight loss test adopts a GB/T27761-2011 test method.
Table 1 shows the comparison of the microwave absorbing performance of the wave absorbing coating prepared in example 1 and the existing absorbent at the temperature of room temperature to 300 ℃.
Detailed Description
Example 1
The high-temperature stable wave-absorbing coating of the embodiment mainly comprises carbonyl iron (produced by Shanxi Xinghua group, Ltd.), epoxy resin (produced by Jiangsu Tai Er New Material science and technology Co., Ltd.), methyl hexahydrophthalic anhydride curing agent (produced by deep-creative chemical Co., Ltd.), and melamine foam (produced by Hebei Weisen New Material science and technology Co., Ltd.). The mixture ratio of various raw materials is as follows: the mass ratio of the carbonyl iron to the epoxy resin and the curing agent is 1.7:0.5:0.6, and the volume ratio of the carbon foam to the carbonyl iron slurry is 1.5: 1. The raw material of the carbonized foam used in this example is melamine foam, carbonyl iron is sheet carbonyl iron, and the aspect ratio of the powder is greater than 40 (as shown in fig. 3).
In this embodiment, the preparation method of the high-temperature stable wave-absorbing coating includes the following steps (see the preparation flow chart in fig. 1):
(1) preparing carbon foam: ultrasonically cleaning melamine foam in an alcohol solution with the mass fraction of 50% for 30min, drying in an oven for 24h at the drying temperature of 80 ℃, placing the obtained melamine foam in a tubular furnace, carbonizing the melamine foam for 2h at the temperature of 800 ℃ in an argon atmosphere, placing the obtained carbon foam in a crusher for pulverization, and obtaining carbon foam particles with the particle size of 100-1000 mu m;
(2) preparing carbonyl iron slurry: mixing carbonyl iron, epoxy resin and a curing agent according to a mass ratio of 1.7:0.5:0.6, and in order to ensure that all components are uniformly mixed, mechanically stirring and ultrasonically dispersing carbonyl iron slurry, wherein the rotating speed of mechanical stirring is 480r/min, the stirring time is 30min, and the ultrasonic dispersing time is 30 min;
(3) preparing carbon foam/carbonyl iron composite slurry: vacuum-dipping carbon foam with a certain volume in the carbonyl iron slurry obtained in the step (2), wherein the volume ratio of the carbon foam to the carbonyl iron slurry is 1.5:1, and the vacuum-dipping pressure is required to be less than 0.09MPa to ensure that carbonyl iron and the carbon foam are uniformly compounded to obtain carbon foam/carbonyl iron composite slurry;
(4) preparing a wave-absorbing coating: and (3) coating the carbon foam/carbonyl iron composite slurry obtained in the step (3) on a metal substrate by adopting a blade coating method, controlling the thickness of the coating to be 1mm by using a mould, heating and curing to obtain the wave-absorbing coating with high-temperature stability, wherein the curing temperature of the coating is 120 ℃, and the curing time is 4 hours.
Example 2
The high-temperature stable wave-absorbing coating of the embodiment mainly comprises carbonyl iron (produced by Shanxi Xinghua group, Ltd.), epoxy resin (produced by Jiangsu Tai Er New Material science and technology Co., Ltd.), methyl hexahydrophthalic anhydride curing agent (produced by deep-creative chemical Co., Ltd.), and melamine foam (produced by Hebei Weisen New Material science and technology Co., Ltd.). The mixture ratio of various raw materials is as follows: the mass ratio of the carbonyl iron to the epoxy resin and the curing agent is 1.7:0.5:0.6, and the volume ratio of the carbon foam to the carbonyl iron slurry is 1.5: 1. The raw material of the carbonized foam used in this example is melamine foam, carbonyl iron is sheet carbonyl iron, and the aspect ratio of the powder is greater than 40 (as shown in fig. 3).
In this embodiment, the preparation method of the high-temperature stable wave-absorbing coating includes the following steps (see the preparation flow chart in fig. 1):
(1) preparing carbon foam: ultrasonically cleaning melamine foam in an alcohol solution with the mass fraction of 50% for 30min, drying in an oven for 24h at the drying temperature of 80 ℃, placing the obtained melamine foam in a tubular furnace, carbonizing the melamine foam for 2h at the temperature of 900 ℃ in an argon atmosphere, placing the obtained carbon foam in a crusher for pulverization, and obtaining carbon foam particles with the particle size of 100-1000 mu m;
(2) preparing carbonyl iron slurry: mixing carbonyl iron, epoxy resin and a curing agent according to a mass ratio of 1.7:0.5:0.6, and in order to ensure that all components are uniformly mixed, mechanically stirring and ultrasonically dispersing carbonyl iron slurry, wherein the rotating speed of mechanical stirring is 720r/min, the stirring time is 30min, and the ultrasonic dispersing time is 30 min;
(3) preparing carbon foam/carbonyl iron composite slurry: vacuum-dipping carbon foam with a certain volume in the carbonyl iron slurry obtained in the step (2), wherein the volume ratio of the carbon foam to the carbonyl iron slurry is 1.5:1, and the vacuum-dipping pressure is required to be less than 0.09MPa to ensure that carbonyl iron and the carbon foam are uniformly compounded to obtain carbon foam/carbonyl iron composite slurry;
(4) preparing a wave-absorbing coating: and (3) coating the carbon foam/carbonyl iron composite slurry obtained in the step (3) on a metal substrate by adopting a blade coating method, controlling the thickness of the coating to be 1mm by using a mould, heating and curing to obtain the wave-absorbing coating with high-temperature stability, wherein the curing temperature of the coating is 120 ℃, and the curing time is 4 hours.
Example 3
The high-temperature stable wave-absorbing coating of the embodiment mainly comprises carbonyl iron (produced by Shanxi Xinghua group, Ltd.), epoxy resin (produced by Jiangsu Tai Er New Material science and technology Co., Ltd.), methyl hexahydrophthalic anhydride curing agent (produced by deep-creative chemical Co., Ltd.), and melamine foam (produced by Hebei Weisen New Material science and technology Co., Ltd.). The mixture ratio of various raw materials is as follows: the mass ratio of the carbonyl iron to the epoxy resin and the curing agent is 1.7:0.5:0.6, and the volume ratio of the carbon foam to the carbonyl iron slurry is 1.5: 1. The raw material of the carbonized foam used in this example is melamine foam, carbonyl iron is sheet carbonyl iron, and the aspect ratio of the powder is greater than 40 (as shown in fig. 3).
In this embodiment, the preparation method of the high-temperature stable wave-absorbing coating includes the following steps (see the preparation flow chart in fig. 1):
(1) preparing carbon foam: ultrasonically cleaning melamine foam in an alcohol solution with the mass fraction of 50% for 30min, drying in an oven for 24h at the drying temperature of 80 ℃, placing the obtained melamine foam in a tubular furnace, carbonizing the melamine foam for 2h at the temperature of 700 ℃ in an argon atmosphere, placing the obtained carbon foam in a crusher for pulverization, and obtaining carbon foam particles with the particle size of 100-1000 mu m;
(2) preparing carbonyl iron slurry: mixing carbonyl iron, epoxy resin and a curing agent according to a mass ratio of 1.7:0.5:0.6, and in order to ensure that all components are uniformly mixed, mechanically stirring and ultrasonically dispersing carbonyl iron slurry, wherein the rotating speed of mechanical stirring is 960r/min, the stirring time is 30min, and the ultrasonic dispersing time is 30 min;
(3) preparing carbon foam/carbonyl iron composite slurry: vacuum-dipping carbon foam with a certain volume in the carbonyl iron slurry obtained in the step (2), wherein the volume ratio of the carbon foam to the carbonyl iron slurry is 1.5:1, and the vacuum-dipping pressure is required to be less than 0.09MPa to ensure that carbonyl iron and the carbon foam are uniformly compounded to obtain carbon foam/carbonyl iron composite slurry;
(4) preparing a wave-absorbing coating: and (3) coating the carbon foam/carbonyl iron composite slurry obtained in the step (3) on a metal substrate by adopting a blade coating method, controlling the thickness of the coating to be 1mm by using a mould, heating and curing to obtain the wave-absorbing coating with high-temperature stability, wherein the curing temperature of the coating is 120 ℃, and the curing time is 4 hours.
Example 4
The high-temperature stable wave-absorbing coating of the embodiment mainly comprises carbonyl iron (produced by Shanxi Xinghua group, Ltd.), epoxy resin (produced by Jiangsu Tai Er New Material science and technology Co., Ltd.), methyl hexahydrophthalic anhydride curing agent (produced by deep-creative chemical Co., Ltd.), and melamine foam (produced by Hebei Weisen New Material science and technology Co., Ltd.). The mixture ratio of various raw materials is as follows: the mass ratio of the carbonyl iron to the epoxy resin and the curing agent is 1.7:0.5:0.6, and the volume ratio of the carbon foam to the carbonyl iron slurry is 1: 1. The raw material of the carbonized foam used in this example is melamine foam, carbonyl iron is sheet carbonyl iron, and the aspect ratio of the powder is greater than 40 (as shown in fig. 3).
In this embodiment, the preparation method of the high-temperature stable wave-absorbing coating includes the following steps (see the preparation flow chart in fig. 1):
(1) preparing carbon foam: ultrasonically cleaning melamine foam in an alcohol solution with the mass fraction of 50% for 30min, drying in an oven for 24h at the drying temperature of 80 ℃, placing the obtained melamine foam in a tubular furnace, carbonizing the melamine foam for 2h at the temperature of 800 ℃ in an argon atmosphere, placing the obtained carbon foam in a crusher for pulverization, and obtaining carbon foam particles with the particle size of 100-1000 mu m;
(2) preparing carbonyl iron slurry: mixing carbonyl iron, epoxy resin and a curing agent according to a mass ratio of 1.7:0.5:0.6, and in order to ensure that all components are uniformly mixed, mechanically stirring and ultrasonically dispersing carbonyl iron slurry, wherein the rotating speed of mechanical stirring is 960r/min, the stirring time is 30min, and the ultrasonic dispersing time is 30 min;
(3) preparing carbon foam/carbonyl iron composite slurry: vacuum-dipping carbon foam with a certain volume in the carbonyl iron slurry obtained in the step (2), wherein the volume ratio of the carbon foam to the carbonyl iron slurry is 1:1, and the vacuum-dipping pressure is less than 0.09MPa to ensure that carbonyl iron and carbon foam are uniformly compounded to obtain carbon foam/carbonyl iron composite slurry;
(4) preparing a wave-absorbing coating: and (3) coating the carbon foam/carbonyl iron composite slurry obtained in the step (3) on a metal substrate by adopting a blade coating method, controlling the thickness of the coating to be 1mm by using a mould, heating and curing to obtain the wave-absorbing coating with high-temperature stability, wherein the curing temperature of the coating is 120 ℃, and the curing time is 4 hours.
Example 5
The high-temperature stable wave-absorbing coating of the embodiment mainly comprises carbonyl iron (produced by Shanxi Xinghua group, Ltd.), epoxy resin (produced by Jiangsu Tai Er New Material science and technology Co., Ltd.), methyl hexahydrophthalic anhydride curing agent (produced by deep-creative chemical Co., Ltd.), and melamine foam (produced by Hebei Weisen New Material science and technology Co., Ltd.). The mixture ratio of various raw materials is as follows: the mass ratio of the carbonyl iron to the epoxy resin and the curing agent is 1.7:0.5:0.6, and the volume ratio of the carbon foam to the carbonyl iron slurry is 2: 1. The raw material of the carbonized foam used in this example is melamine foam, carbonyl iron is sheet carbonyl iron, and the aspect ratio of the powder is greater than 40 (as shown in fig. 3).
In this embodiment, the preparation method of the high temperature stability wave-absorbing coating includes the following steps (see fig. 1 for a preparation flow chart):
(1) preparing carbon foam: ultrasonically cleaning melamine foam in an alcohol solution with the mass fraction of 50% for 30min, drying in an oven for 24h at the drying temperature of 80 ℃, placing the obtained melamine foam in a tubular furnace, carbonizing the melamine foam for 2h at the temperature of 800 ℃ in an argon atmosphere, placing the obtained carbon foam in a crusher for pulverization, and obtaining carbon foam particles with the particle size of 100-1000 mu m;
(2) preparing carbonyl iron slurry: mixing carbonyl iron, epoxy resin and a curing agent according to a mass ratio of 1.7:0.5:0.6, and in order to ensure that all components are uniformly mixed, mechanically stirring and ultrasonically dispersing carbonyl iron slurry, wherein the rotating speed of mechanical stirring is 960r/min, the stirring time is 30min, and the ultrasonic dispersing time is 30 min;
(3) preparing carbon foam/carbonyl iron composite slurry: vacuum-dipping carbon foam with a certain volume in the carbonyl iron slurry obtained in the step (2), wherein the volume ratio of the carbon foam to the carbonyl iron slurry is 2:1, and the vacuum-dipping pressure is less than 0.09MPa to ensure that carbonyl iron and carbon foam are uniformly compounded to obtain carbon foam/carbonyl iron composite slurry;
(4) preparing a wave-absorbing coating: and (3) coating the carbon foam/carbonyl iron composite slurry obtained in the step (3) on a metal substrate by adopting a blade coating method, controlling the thickness of the coating to be 1mm by using a mould, heating and curing to obtain the wave-absorbing coating with high-temperature stability, wherein the curing temperature of the coating is 120 ℃, and the curing time is 4 hours.
TABLE 1
Reference to the literature
[1]H.Tian,H.-T.Liu,H.-F.Cheng,Composites Science and Technology 2014,90,202.
[2]H.Yang,M.Cao,Y.Li,H.Shi,Z.Hou,X.Fang,H.Jin,W.Wang,J.Yuan,Advanced Optical Materials 2014,2,214.
[3]X.Yuan,L.Cheng,Y.Zhang,S.Guo,L.Zhang,Materials&Design 2016,92,563.
[4]H.-J.Yang,W.-Q.Cao,D.-Q.Zhang,T.-J.Su,H.-L.Shi,W.-Z.Wang,J.Yuan,M.-S.Cao,ACS Applied Materials&Interfaces 2015,7,7073.
[5]X.Yuan,L.Cheng,S.Guo,L.Zhang,Ceramics International 2017,43,282.
[6]Y.Mu,W.Zhou,Y.Hu,H.Wang,F.Luo,D.Ding,Y.Qing,Journal of the European Ceramic Society 2015,35,2991.
[7]M.Han,X.Yin,W.Duan,S.Ren,L.Zhang,L.Cheng,Journal of the European Ceramic Society 2016,36,2695.
[8]W.-Q.Cao,X.-X.Wang,J.Yuan,W.-Z.Wang,M.-S.Cao,Journal of Materials Chemistry C 2015,3,10017.
[9]B.Wen,M.-S.Cao,Z.-L.Hou,W.-L.Song,L.Zhang,M.-M.Lu,H.-B.Jin,X.-Y.Fang,W.-Z.Wang,J.Yuan,Carbon 2013,65,124.
[10]M.-M.Lu,W.-Q.Cao,H.-L.Shi,X.-Y.Fang,J.Yang,Z.-L.Hou,H.-B.Jin,W.-Z.Wang,J.Yuan,M.-S.Cao,Journal of Materials Chemistry A 2014,2,10540.
[11]H.Wang,D.Zhu,W.Zhou,F.Luo,Journal of Alloys and Compounds 2015,648,313.
[12]L.Kong,X.Yin,M.Han,L.Zhang,L.Cheng,Ceramics International 2015,41,4906.
[13]J.Liu,M.-S.Cao,Q.Luo,H.-L.Shi,W.-Z.Wang,J.Yuan,ACS Applied Materials&Interfaces 2016,8,22615.
[14]Y.Li,M.-s.Cao,D.-w.Wang,J.Yuan,RSC Advances 2015,5,77184.
[15]Y.Li,X.Fang,M.Cao,Scientific Reports 2016,6,24837.
[16]G.Wang,X.Li,P.Wang,J.Zhang,D.Wang,L.Qiao,T.Wang,F.Li,Journal of Magnetism and Magnetic Materials 2018,456,92.
[17]M.-M.Lu,M.-S.Cao,Y.-H.Chen,W.-Q.Cao,J.Liu,H.-L.Shi,D.-Q.Zhang,W.-Z.Wang,J.Yuan,ACS Applied Materials&Interfaces 2015,7,19408.
[18]J.Liu,W.-Q.Cao,H.-B.Jin,J.Yuan,D.-Q.Zhang,M.-S.Cao,Journal of Materials Chemistry C 2015,3,4670.
[19]L.Kong,X.Yin,Q.Li,F.Ye,Y.Liu,G.Duo,X.Yuan,Journal of the American Ceramic Society 2013,96,2211.
[20]M.-S.Cao,W.-L.Song,Z.-L.Hou,B.Wen,J.Yuan,Carbon 2010,48,788.
[21]Z.Hou,X.Yin,H.Xu,H.Wei,M.Li,L.Cheng,L.Zhang,ACS Applied Materials&Interfaces 2019,11,5364.
[22]Y.-K.Dou,J.-B.Li,X.-Y.Fang,H.-B.Jin,M.-S.Cao,Applied Physics Letters 2014,104,052102.
[23]H.-J.Yang,J.Yuan,Y.Li,Z.-L.Hou,H.-B.Jin,X.-Y.Fang,M.-S.Cao,Solid State Communications 2013,163,1.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modifications, variations and equivalents of the above embodiments are intended to be included within the scope of the present invention.
Claims (7)
1. The high-temperature stable wave-absorbing coating is characterized by being prepared by curing carbon foam/carbonyl iron composite slurry, wherein the volume ratio of carbon foam to carbonyl iron slurry in the raw materials of the wave-absorbing coating is 1:1-2:1, and the mass ratio of carbonyl iron to epoxy resin and curing agent in the carbonyl iron slurry is (1-3) 0.5: 0.6;
the preparation method of the high-temperature stable wave-absorbing coating comprises the following steps:
step one, preparing carbon foam: ultrasonically cleaning melamine foam with an alcohol solution, drying in an oven for 12-24h, placing the obtained melamine foam in a tubular furnace, carbonizing for 2-6h in an argon atmosphere, and placing the obtained carbon foam in a pulverizer for pulverization to obtain carbon foam particles;
step two, preparing carbonyl iron slurry: uniformly mixing carbonyl iron, epoxy resin and a curing agent according to the mass ratio of (1-3) to 0.5:0.6 to obtain carbonyl iron slurry;
step three, preparing carbon foam/carbonyl iron composite slurry: vacuum-dipping carbon foam into the carbonyl iron slurry obtained in the second step, wherein the volume ratio of the carbon foam to the carbonyl iron slurry is 1:1-2:1, the vacuum-dipping time is 30min, and the vacuum-dipping temperature is 30-50 ℃, so as to obtain carbon foam/carbonyl iron composite slurry;
step four, preparing the wave-absorbing coating: coating the carbon foam/carbonyl iron composite slurry obtained in the third step on a metal substrate by adopting a blade coating method, controlling the thickness of the coating to be 1.0-1.1mm by using a mould, and heating and curing to obtain the wave-absorbing coating with high-temperature stability.
2. The high temperature stability wave-absorbing coating of claim 1, wherein the thickness of the coating is 1.0-1.1mm, and the coating can obtain an effective absorption bandwidth of more than 8GHz within a frequency band of 8-18GHz at a temperature of room temperature to 300 ℃.
3. The high temperature stability wave-absorbing coating as claimed in claim 1, wherein the mass ratio of distilled water to ethanol in the alcoholic solution of step one is 1:1-1:3, the drying temperature is 80-100 ℃, the carbonization temperature of melamine foam is 700-900 ℃, and the particle size of carbon foam particles is 100-1000 μm.
4. The high temperature stability wave-absorbing coating as claimed in claim 1, wherein the mass ratio of the carbonyl iron to the epoxy resin and the curing agent in the carbonyl iron slurry in the step two is (1-3):0.5:0.6, the carbonyl iron slurry is mechanically stirred and ultrasonically dispersed, the rotating speed of the mechanical stirring is 480-.
5. The high-temperature-stability wave-absorbing coating according to claim 1, wherein the volume ratio of the carbon foam to the carbonyl iron slurry in the carbon foam/carbonyl iron composite slurry in the third step is 1:1-2:1, and the pressure for vacuum impregnation is less than 0.09 MPa.
6. The high temperature stability microwave absorbing coating as claimed in claim 1, wherein the thickness of the microwave absorbing coating in step four is controlled to be 1.0-1.1mm, the curing temperature of the coating is 100 ℃ and 120 ℃, and the curing time is 2-4 h.
7. The high temperature stable microwave absorbing coating of any one of claims 1 to 6, for use in the field of cell phone patches, electronic devices and related aircraft.
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