CN115678333B - Wave-absorbing coating, preparation method and application thereof - Google Patents
Wave-absorbing coating, preparation method and application thereof Download PDFInfo
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- CN115678333B CN115678333B CN202211326831.9A CN202211326831A CN115678333B CN 115678333 B CN115678333 B CN 115678333B CN 202211326831 A CN202211326831 A CN 202211326831A CN 115678333 B CN115678333 B CN 115678333B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention provides a wave-absorbing coating and a preparation method thereof, wherein the wave-absorbing coating comprises a wave-absorbing coating A layer and a wave-absorbing coating B layer which are stacked on a substrate in a staggered manner; the raw materials of the wave-absorbing coating A layer comprise resin, carbonyl iron powder, auxiliary materials, thinner and curing agent; the raw materials of the wave-absorbing coating B comprise resin, glass flakes with alloy plated on the surface, auxiliary materials, thinner and curing agent. The carbonyl iron powder and the glass flakes with the alloy plated on the surfaces are arranged in a layering manner, so that the carbonyl iron powder absorbed in the coating can be promoted to be uniformly distributed, and stable wave absorbing performance and mechanical property are ensured after the solid coating is formed.
Description
Technical Field
The invention relates to the field of wave-absorbing materials, in particular to a wave-absorbing coating and a preparation method thereof.
Background
The wave absorbing material is also called as stealth material, and has important application value in military. Can be used for various weapon products, such as stealth aircraft, stealth ships and the like. There are many studies on wave-absorbing materials on stealth aircraft, but there are few stealth vessels. For the stealth ship, the requirements of high temperature resistance during exposure, corrosion resistance during sea water and the like are met, and the ship has the characteristics of impact resistance, fatigue resistance, high flexibility and the like during engineering application.
The density of the wave-absorbing material is generally larger, when the coating containing the wave-absorbing material is used for preparing the wave-absorbing coating by adopting a spraying process, the wave-absorbing material tends to be settled, so that the concentration of the wave-absorbing material in the bottom area of the coating is large, the concentration of the surface of the coating is small, the wave-absorbing performance of the coating is further reduced, and the mechanical performance of the bottom is reduced due to the large concentration of the wave-absorbing material.
Disclosure of Invention
The invention provides a wave-absorbing coating and a preparation method thereof, and the wave-absorbing performance of the coating is stable and uniform.
The technical scheme of the invention is that the wave-absorbing coating comprises a wave-absorbing coating A layer and a wave-absorbing coating B layer which are alternately stacked on a substrate, wherein the thickness of each wave-absorbing coating A layer and each wave-absorbing coating B layer is 13-40 mu m; the raw materials of the wave-absorbing coating A layer comprise 100 parts of resin, 100-200 parts of modified carbonyl iron powder, 0-20 parts of auxiliary materials, 1-200 parts of thinner and 10-30 parts of curing agent in parts by weight; the raw materials of the wave-absorbing coating B comprise 100 parts of resin, 30-100 parts of glass flakes with alloy plated on the surfaces, 0-20 parts of auxiliary materials, 1-200 parts of thinner and 10-30 parts of curing agent.
Further, when the modified carbonyl iron powder is prepared, the carbonyl iron powder and KH560 silane coupling agent are put into ethanol, stirred and mixed for 10-12 hours, and then the carbonyl iron powder is settled and dried to obtain the modified carbonyl iron powder; wherein the carbonyl iron powder: KH560 silane coupling agent: the mass ratio of the ethanol is 100:2-7:130-220. The mass concentration of the ethanol is more than 99.9 percent.
Further, the particle size of the modified carbonyl iron powder in the raw material of the wave-absorbing coating A is D10-11 mu m, D50-20 mu m and D90-40 mu m.
Further, the preparation method of the modified carbonyl iron powder comprises the following steps: putting carbonyl iron powder and KH560 silane coupling agent into 99.9% pure alcohol, stirring and mixing at high speed for 12 hours, and settling and drying the carbonyl iron powder to obtain modified carbonyl iron powder, wherein the carbonyl iron powder is prepared by the following steps: KH560 silane coupling agent: the mass ratio of the 99.9% pure alcohol is 100:2-7:130-220.
Further, the thickness of the glass flake of the modified surface plated alloy in the raw material of the wave-absorbing coating B is 1-3 mu m, and the grain diameter is 30-50 mu m.
Further, when preparing the glass flake with the modified surface plated with alloy, washing the glass flake with water, and then performing sensitization and activation pretreatment; then carrying out chemical plating alloy, finally filtering, washing and drying, then putting the glass flake with the surface plated alloy and KH560 silane coupling agent into ethanol, stirring and mixing at a high speed for 12 hours, and then settling and drying the glass flake with the surface plated alloy to obtain the glass flake with the modified surface plated alloy, wherein the glass flake with the surface plated alloy: KH560 silane coupling agent: the mass ratio of the ethanol is 100:7-15:100-150. The concentration of ethanol is above 99.9%.
Further, the alloy used in the electroless plating of the glass flakes is an iron-cobalt-nickel alloy.
Further, in the wave-absorbing coating, the mass ratio of the modified carbonyl iron powder to the glass flake with the modified surface alloy plating is controlled to be 1:0.3-0.5.
Further, the resin is epoxy resin, acrylic resin, fluorocarbon resin, alkyd resin or organic silicon resin, the auxiliary material is dispersing agent and/or coupling agent, and the thinner is dimethylbenzene and/or cyclohexanone.
The invention also relates to a method for preparing the wave-absorbing coating, comprising the following steps:
s1, taking resin, thinner and auxiliary materials, mixing uniformly, then adding modified carbonyl iron powder, mixing uniformly, and finally adding a curing agent, mixing uniformly to obtain the wave-absorbing coating A;
s2, taking resin, thinner and auxiliary materials, uniformly mixing, then adding the glass flakes with the modified surface plated with alloy, uniformly mixing, and finally adding a curing agent, and uniformly mixing to obtain the wave-absorbing coating B;
s3, respectively loading the wave-absorbing coating A and the wave-absorbing coating B into different spraying devices, spraying a wave-absorbing coating A layer on the substrate by adopting a staggered stacking spraying mode, spraying a wave-absorbing coating B layer after the surface of the coating is dried, and carrying out the next round of spraying after the surface of the wave-absorbing coating B layer is dried until the required thickness is reached, and carrying out curing treatment to obtain the required wave-absorbing coating.
Further, the thickness of each of the layer A and the layer B of the wave-absorbing coating is 13-40 μm.
The invention has the following beneficial effects:
according to the invention, the wave-absorbing coating is arranged into a structure that A, B coating layers are stacked alternately, wherein the A coating contains modified carbonyl iron powder, which has excellent wave-absorbing performance, but has larger density and is easy to subside; the coating B contains glass flakes with modified surface plated with alloy, and the glass flakes are flaky materials with high transverse-longitudinal ratio, but have no wave absorbing performance; the surface of the modified surface alloy is plated with the Fe-Ni-Co alloy, so that the modified surface alloy has higher dielectric constant and magnetic conductivity, has excellent low-frequency wave absorbing performance, obviously reduces the density compared with carbonyl iron powder, and has the effects of effectively blocking and carrying the sedimentation of the carbonyl iron powder of the level because the glass flake of the modified surface alloy is small in density and is subjected to the action of surface tension and buoyancy, and can not be settled in the coating, but can float to the outermost surface of the coating to be uniformly distributed. The last layer is the modified alloy-plated glass flake and the modified carbonyl iron powder which are suspended on the upper surface of the resin of the layer, and the like, so that the uniformly-spaced alloy-plated glass flake and carbonyl iron powder combined structure can be finally realized on the microstructure. Thus, the effect of uniform distribution of carbonyl iron powder absorbing waves in the coating is realized, and the uniformity and stability of the wave absorbing performance and mechanical property of the coating after curing and forming are further ensured. Meanwhile, the modified carbonyl iron powder and the glass flake with the modified surface plated with alloy are coated with a layer of KH560 coupling agent, the coupling agent enables the bonding force between the two powders and the resin to be better, and meanwhile, the uniformity of the distribution of the glass flake and the carbonyl iron powder is combined, so that the flexibility and the shock resistance of the coating are more excellent.
When the invention is practically applied to the modified carbonyl iron powder and the alloy-plated glass flake, the size particle diameter of the modified carbonyl iron powder and the alloy-plated glass flake is preferably controlled to be 1-3 mu m in thickness, the particle diameter is 30-50 mu m, the coating mechanical property is poor due to the too large particle diameter, the practical engineering application is not realized, and the particle diameter is too small to effectively block and accept the modified carbonyl iron powder. Preferably, the particle size D10 of the modified carbonyl iron powder is less than or equal to 11 mu m, D50 is less than or equal to 20 mu m, and D90 is less than or equal to 40 mu m. If the particle size of the carbonyl iron powder is larger, the mechanical property of the coating is poor, more importantly, the quality is too heavy when the particle size is too large, the glass flakes plated with the Fe-Ni-Co alloy are difficult to effectively block, and still the carbonyl iron powder is still caused to be settled.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention.
Example 1:
the modified carbonyl iron powder is prepared as follows: putting carbonyl iron powder and KH560 silane coupling agent into 99.9% pure alcohol, stirring and mixing at high speed for 12 hours, and settling and drying the carbonyl iron powder to obtain modified carbonyl iron powder, wherein the carbonyl iron powder is prepared by the following steps: KH560 silane coupling agent: the mass ratio of the 99.9% pure alcohol is 100:5:170.
S1, preparing a wave-absorbing coating A, wherein the raw materials comprise 100g of epoxy resin (102C-4H), 120g of modified carbonyl iron powder, 10g of coupling agent (A151), 150g of dimethylbenzene and 38g of curing agent (E44 curing agent). The preparation method comprises the following steps: taking epoxy resin, dimethylbenzene and a coupling agent, and stirring for 10min; and adding the modified carbonyl iron powder, stirring for 20min, adding the curing agent, stirring for 5min, and uniformly mixing to obtain the wave-absorbing coating A.
The particle size range of the modified magnetic powder was 10 μm for D10, 15 μm for D50 and 35 μm for D90.
S2, preparing a wave-absorbing coating B, wherein the raw materials comprise 100g of epoxy resin (102C-4H), 40g of glass flake with alloy plated on the surface, 10g of coupling agent (A151), 150g of dimethylbenzene and 38g of curing agent (E44 curing agent). The preparation steps of the wave-absorbing paint B are the same as those of the wave-absorbing paint A, and only the modified carbonyl iron powder is replaced by the glass flakes with the modified surface plated with alloy.
The preparation steps of the glass flake with the alloy plated on the surface are as follows:
1) Pretreating glass flakes, namely washing the glass flakes, filtering, sensitizing by an acidic stannous chloride solution, filtering, activating by a palladium chloride solution, and filtering to obtain pretreated glass flakes. Wherein the thickness of the glass flake is 2 mu m, the grain diameter is 40 mu m, the stannous chloride concentration is 14g/L, and the palladium chloride solution concentration is 0.2g/L.
2) And (3) performing electroless plating of Fe-Ni-Co alloy, immersing the pretreated glass flake in a mixed solution containing cobalt sulfate, nickel sulfate and ferrous sulfate, performing electroless plating for 20min, filtering, washing and drying to obtain the glass flake with Fe-Ni-Co on the surface. The pH value of the plating solution is kept at 9, and the temperature is 82 ℃. Then placing the glass flake with the surface plated alloy and KH560 silane coupling agent into 99.9% pure alcohol, stirring and mixing at high speed for 12 hours, and settling and drying the glass flake with the surface plated alloy to obtain the modified glass flake with the surface plated alloy, wherein the glass flake with the surface plated alloy: KH560 silane coupling agent: the mass ratio of the 99.9% pure alcohol is 100:12:130.
S3, spraying the target object by adopting a spraying process, wherein the steps are as follows: and respectively loading the wave-absorbing paint A and the wave-absorbing paint B into two groups of different spraying equipment, spraying the wave-absorbing paint A on the substrate material in a staggered spraying mode, spraying the wave-absorbing paint A with the thickness of 20 mu m, spraying the wave-absorbing paint B after the coating is dried, with the thickness of 20 mu m, continuing to wait until the coating is dried, spraying the wave-absorbing paint A with the thickness of 20 mu m, and so on, performing staggered spraying until the total thickness of the coating reaches 2 mm, and performing curing process treatment until the curing is complete. The required wave-absorbing coating is obtained.
The standard object is aluminum alloy plate, the thickness is about 5mm, and the length and width are 180mm. The obtained coating is tested for mechanical properties, high temperature resistance and electromagnetic wave absorption effect.
A. The coating template tests the reflectivity of the frequency band of 1 GHz-18 GHz according to GJB2038A-2011 'method for testing reflectivity of radar absorbing material'.
B. The coating panels were tested for flexibility according to GB/T1731-1993 and for impact strength according to GB/T1732-1993.
The test results were as follows: the average reflectivity of 1-18GHz is-8.5 dB, the flexibility is 3mm, and the impact strength is more than 140kg cm. The coating prepared by the coating has excellent mechanical property and stable and uniform wave absorbing property.
Example 2
The modified carbonyl iron powder is prepared as follows: putting carbonyl iron powder and KH560 silane coupling agent into 99.9% pure alcohol, stirring and mixing at high speed for 12 hours, and settling and drying the carbonyl iron powder to obtain modified carbonyl iron powder, wherein the carbonyl iron powder is prepared by the following steps: KH560 silane coupling agent: the mass ratio of the 99.9% pure alcohol is 100:6:180.
Preparation of the wave-absorbing coating:
s1, preparing a wave-absorbing coating A, wherein the raw materials comprise 100g of alkyd resin (BD 3108-70-F alkyd resin), 130g of flaked carbonyl iron powder, 10g of dispersing agent (byk) 10g, 180g of dimethylbenzene and 28g of curing agent (DX-35). The method comprises the following steps: taking alkyd resin, dimethylbenzene and a dispersing agent, and stirring for 15min; and adding carbonyl iron powder, stirring for 20min, adding a curing agent, stirring for 5min, and uniformly mixing to obtain the wave-absorbing coating A.
The particle size range of the flaked magnetic powder was 10 μm for D10, 15 μm for D50 and 35 μm for D90.
S2, preparing a wave-absorbing coating B, wherein the raw materials comprise 100g of alkyd resin (BD 3108-70-F alkyd resin), 35g of glass flakes with alloy plated on the surfaces, 10g of dispersing agent (byk), 180g of dimethylbenzene and 28g of curing agent (DX-35). The thickness of the glass flake was 2.5 μm and the particle size was 38. Mu.m.
The preparation procedure of the glass flake with alloy plated surface is the same as in example 1:
s3, spraying the target object by adopting a spraying process, wherein the steps are as follows: and respectively loading the wave-absorbing paint A and the wave-absorbing paint B into two groups of different spraying equipment, spraying the wave-absorbing paint A on the substrate material in a staggered spraying mode, spraying the wave-absorbing paint A with the thickness of 20 mu m, spraying the wave-absorbing paint B after the coating is dried, with the thickness of 20 mu m, continuing to wait until the coating is dried, spraying the wave-absorbing paint A with the thickness of 20 mu m, and so on, performing staggered spraying until the total thickness of the coating reaches 2 mm, and performing curing process treatment until the curing is complete. The required wave-absorbing coating is obtained.
The base material is aluminum alloy plate with the thickness of about 5mm and the length and width of 180mm. The obtained coating is tested for mechanical properties, high temperature resistance and electromagnetic wave absorption effect.
The test results were as follows: the average reflectivity of 1-18GHz is-8.1 dB, the flexibility is 3mm, and the impact strength is more than 120kg cm; the coating prepared by the coating has excellent mechanical property and stable and uniform wave absorbing property.
Example 3:
the modified carbonyl iron powder is prepared as follows: putting carbonyl iron powder and KH560 silane coupling agent into 99.9% pure alcohol, stirring and mixing at high speed for 12 hours, and settling and drying the carbonyl iron powder to obtain modified carbonyl iron powder, wherein the carbonyl iron powder is prepared by the following steps: KH560 silane coupling agent: the mass ratio of the 99.9% pure alcohol is 100:6:180.
Preparation of the wave-absorbing coating:
s1, preparing a wave-absorbing coating A, wherein the raw materials comprise 100g of fluorocarbon resin (pf-501 resin), 130g of modified carbonyl iron powder, 10g of dispersing agent (byk 151), 180g of dimethylbenzene and 33g of curing agent (N75). The method comprises the following steps: taking alkyd resin, dimethylbenzene and a dispersing agent, and stirring for 15min; and adding the modified carbonyl iron powder, stirring for 20min, adding the curing agent, stirring for 5min, and uniformly mixing to obtain the wave-absorbing coating A.
The particle size range of the modified magnetic powder was 10 μm for D10, 15 μm for D50 and 35 μm for D90.
S2, preparing a wave-absorbing coating B, wherein the raw materials comprise 100g of fluorocarbon resin (pf-501 resin), 35g of glass flake with alloy plated on the surface, 10g of dispersing agent (byk 151), 180g of dimethylbenzene and 33g of curing agent (N75). The thickness of the glass flake was 2.5 μm and the particle size was 38. Mu.m.
The preparation procedure of the glass flake with alloy plated surface is the same as in example 1:
s3, spraying the target object by adopting a spraying process, wherein the steps are as follows: and respectively loading the wave-absorbing paint A and the wave-absorbing paint B into two groups of different spraying equipment, spraying the wave-absorbing paint A on the substrate material in a staggered spraying mode, spraying the wave-absorbing paint A with the thickness of 20 mu m, spraying the wave-absorbing paint B after the coating is dried, with the thickness of 20 mu m, continuing to wait until the coating is dried, spraying the wave-absorbing paint A with the thickness of 20 mu m, and so on, performing staggered spraying until the total thickness of the coating reaches 2 mm, and performing curing process treatment until the curing is complete. The required wave-absorbing coating is obtained.
The base material is aluminum alloy plate with the thickness of about 5mm and the length and width of 180mm. The obtained coating is tested for mechanical properties, high temperature resistance and electromagnetic wave absorption effect.
The test results were as follows: the average reflectivity of 1-18GHz is-8.1 dB, the flexibility is 3mm, and the impact strength is more than 130kg cm; the coating prepared by the coating has excellent mechanical property and stable and uniform wave absorbing property.
Comparative example 1:
the wave-absorbing coating A and the wave-absorbing coating B of the coating are prepared in the same way as in the example 1, and the difference is that when the coating is prepared, the wave-absorbing coating A and the wave-absorbing coating B are firstly mixed and then stirred for 5min until the coating is uniform, the spraying thickness and the layer number are the same as in the example 1, and the finally obtained wave-absorbing coating is tested, and the test method is the same as in the example 1.
The test results were as follows: the average reflectivity of 1-18GHz is-7 dB, the flexibility is 10mm, and the impact strength is less than 80kg cm. The coating prepared by the coating has reduced mechanical properties (flexibility and impact strength) and reduced wave absorbing performance in the earlier stage.
Claims (8)
1. A wave-absorbing coating layer, which is characterized in that,the wave-absorbing coating is characterized by comprising a wave-absorbing coating A layer and a wave-absorbing coating B layer which are stacked on a substrate in a staggered manner, wherein the thickness of each wave-absorbing coating A layer and each wave-absorbing coating B layer is 13-40 mu m; the raw materials of the wave-absorbing coating A layer comprise 100 parts of resin, 100-200 parts of modified carbonyl iron powder, 0-20 parts of auxiliary materials, 1-200 parts of thinner and 10-30 parts of curing agent in parts by weight; wherein the particle size of the modified carbonyl iron powder is D 10 ≤11μm，D 50 ≤20μm，D 90 ≤40μm；
The raw materials of the wave-absorbing coating B layer comprise 100 parts of resin, 30-100 parts of glass flakes with alloy plated on the surface, 0-20 parts of auxiliary materials, 1-200 parts of thinner and 10-30 parts of curing agent; wherein the thickness of the glass flake plated with alloy on the surface is 1-3 mu m, and the grain diameter is 30-50 mu m.
2. The wave-absorbing coating of claim 1, wherein: when the modified carbonyl iron powder is prepared, the carbonyl iron powder and KH560 silane coupling agent are put into ethanol, stirred and mixed for 10-12 hours, and then the carbonyl iron powder is settled and dried to obtain the modified carbonyl iron powder; wherein the carbonyl iron powder: KH560 silane coupling agent: the mass ratio of the ethanol is 100:2-7:130-220.
3. The wave-absorbing coating of claim 1, wherein: when preparing the glass flake with the alloy plated on the surface, washing the glass flake with water, and then performing sensitization and activation pretreatment; and then carrying out electroless alloy plating, and finally filtering, washing and drying to obtain the alloy.
4. A wave-absorbing coating according to claim 3, characterized in that: the alloy adopted in the chemical plating of the glass flakes is Fe-Co-Ni alloy.
5. A wave-absorbing coating according to claim 3, characterized in that: the glass flake with the surface plated with the alloy is further modified, specifically, the glass flake with the surface plated with the alloy is prepared by putting the glass flake with the surface plated with the alloy and a KH560 silane coupling agent into ethanol, stirring and mixing the mixture for 10 to 12 hours, and then settling and drying the mixture to obtain the glass flake with the surface plated with the alloy, wherein the glass flake with the surface plated with the alloy: KH560 silane coupling agent: the mass ratio of the ethanol is 100:12:130.
6. The wave-absorbing coating according to any one of claims 1 to 5, characterized in that: in the wave-absorbing coating, the mass ratio of the modified carbonyl iron powder to the glass flake with the surface plated with the alloy is controlled to be 1:0.3-0.5.
7. The wave-absorbing coating of claim 1, wherein: the resin is epoxy resin, acrylic resin, fluorocarbon resin, alkyd resin or organic silicon resin, the auxiliary materials are dispersing agents and/or coupling agents, and the thinner materials are xylene and/or cyclohexanone.
8. A method for preparing the wave-absorbing coating according to any one of claims 1 to 7, comprising the steps of:
s1, taking resin, thinner and auxiliary materials, mixing uniformly, then adding modified carbonyl iron powder, mixing uniformly, and finally adding a curing agent, mixing uniformly to obtain the wave-absorbing coating A;
s2, taking resin, thinner and auxiliary materials, mixing uniformly, then adding glass flakes with alloy plated surfaces, mixing uniformly, and finally adding a curing agent, mixing uniformly to obtain the wave-absorbing coating B;
s3, respectively loading the wave-absorbing paint A and the wave-absorbing paint B into different spraying equipment, spraying a wave-absorbing paint A layer on the substrate by adopting a staggered stacking spraying mode, spraying a wave-absorbing paint B layer after the surface of the coating is dried, and carrying out the next round of spraying after the surface of the wave-absorbing paint B layer is dried until the required thickness is reached, and carrying out curing treatment to obtain the required wave-absorbing coating.
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