CN111073295A - Preparation method of wave-absorbing patch - Google Patents
Preparation method of wave-absorbing patch Download PDFInfo
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- CN111073295A CN111073295A CN201811214966.XA CN201811214966A CN111073295A CN 111073295 A CN111073295 A CN 111073295A CN 201811214966 A CN201811214966 A CN 201811214966A CN 111073295 A CN111073295 A CN 111073295A
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/05—Polysiloxanes containing silicon bound to hydrogen
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/05—Polysiloxanes containing silicon bound to hydrogen
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- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3412—Heterocyclic compounds having nitrogen in the ring having one nitrogen atom in the ring
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- C08K5/3437—Six-membered rings condensed with carbocyclic rings
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Abstract
The invention provides a preparation method of a wave-absorbing patch, which comprises the following steps: the method comprises the following steps: carrying out ball milling treatment on carbonyl iron powder, and heating and drying to obtain carbonyl iron ball milled powder; step two: grinding and mixing the vinyl-containing organosilicon polymer, hydrogen-containing polysiloxane, an anti-aging agent, chloroplatinic acid and carbonyl iron balls into sheets; and a third step: and putting the sheet into a sheet-loading die for calendering to obtain the wave-absorbing patch. The invention aims to at least improve the wave absorbing performance of the wave absorbing patch on the basis of environmental protection.
Description
Technical Field
The invention relates to the field of wave absorption, in particular to a preparation method of a wave-absorbing patch.
Background
The wave-absorbing patch is mainly prepared by mixing ferrite and metal alloy powder as an absorbent with plastic according to a certain proportion. The polymer-based wave-absorbing material on the market is mainly prepared by vulcanization molding treatment, and the vulcanized plastic has large smell and pollution and is not suitable for some specific application occasions. In addition, the filling amount of the wave absorbing agent in the patch and the thickness of the patch can greatly influence the wave absorbing performance, and the application frequency range of the patch can be influenced if the filling amount of the patch is small, so that the practical application of the wave absorbing material patch is limited to a certain extent.
In industrial production, some exploration and attempts are made to solve the problems of pollution, environmental pollution, insufficient filling amount of the wave absorbing agent and the like of the wave absorbing patch. But the problems that the adding amount effect of the wave-absorbing powder is not obvious, the vulcanization process generates large smell and pollution, the wave-absorbing performance and the physical performance of the patch obtained by coating are required to be improved and the like still exist.
Disclosure of Invention
Aiming at the problems in the related art, the invention aims to provide a preparation method of a wave-absorbing patch, so as to at least improve the wave-absorbing performance of the wave-absorbing patch on the basis of environmental protection.
In order to achieve the purpose, the invention provides a preparation method of a wave-absorbing patch, which comprises the following steps: the method comprises the following steps: carrying out ball milling treatment on carbonyl iron powder, and heating and drying to obtain carbonyl iron ball milled powder; step two: grinding and mixing the vinyl-containing organosilicon polymer, hydrogen-containing polysiloxane, an anti-aging agent, chloroplatinic acid and carbonyl iron balls into sheets; and a third step: and putting the sheet into a sheet-loading die for calendering to obtain the wave-absorbing patch.
According to an embodiment of the present invention, the step one further comprises: carbonyl iron powder and absolute ethyl alcohol are mixed and then put into a ball milling tank with a plurality of agate beads for wet milling, so that slurry with carbonyl iron ball milled powder is obtained.
According to one embodiment of the invention, the carbonyl iron powder has a particle size of 10 to 20 μm.
According to one embodiment of the invention, the ball milling time of the ball milling treatment is 15-20 h.
According to one embodiment of the invention, the heating and drying temperature is 40-80 ℃, and the heating and drying time is 5-8 h.
According to one embodiment of the invention, the ball milling tank is arranged in a horizontal planetary ball mill, and the rotating speed of the horizontal planetary ball mill is 200-400 r/min.
According to one embodiment of the invention, the ratio of carbonyl iron powder to absolute ethyl alcohol is 200-600 g: 800-1000 mL.
According to one embodiment of the invention, the mass ratio of the agate beads to the carbonyl iron powder is 8-15: 1, the mass ratio of the agate beads is 2-5: 25-40: the agate beads are 50-70 mm in diameter, 20mm in diameter, 10mm in diameter and 6mm in diameter, and the total mass of the agate beads is 2.5 kg.
According to an embodiment of the present invention, the method further comprises mixing 30 to 50 parts of a vinyl-containing silicone polymer, 40 to 60 parts of a hydrogen-containing polysiloxane, 4 to 10 parts of an anti-aging agent, and 400 to 1000 parts of carbonyl iron balls, stirring the mixture at room temperature for 40 to 60 minutes by using a high speed mixer at a speed of 800 to 1200r/min, adding 0.5 to 1 part of chloroplatinic acid, stirring the mixture for 20 minutes, and mixing the mixture to obtain the sheet.
According to one embodiment of the invention, the thickness of the sheet is 2 mm.
The invention has the beneficial technical effects that:
according to the preparation method of the wave-absorbing patch, carbonyl iron powder is subjected to ball milling, so that the shape of the carbonyl iron powder is changed into a sheet structure with a certain width-thickness ratio, the purposes of having anisotropic characteristics, inhibiting eddy current effect and improving magnetic conductivity are achieved, and the wave-absorbing performance is improved. The carbonyl iron ball milled powder is mixed with different components at room temperature to obtain the silica-based wave-absorbing patch, and the process is simple and convenient to operate. The finally prepared wave-absorbing patch is pollution-free and good in wave-absorbing performance, and is suitable for different wave-absorbing fields.
Drawings
Fig. 1 is a process flow chart for preparing the wave-absorbing patch according to the embodiment of the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments that can be derived by one of ordinary skill in the art from the embodiments given herein are intended to be within the scope of the present invention.
As shown in fig. 1, in an embodiment of the present invention, a method 100 for preparing a wave-absorbing patch includes the following steps: the method comprises the following steps: carrying out ball milling treatment on carbonyl iron powder, and heating and drying to obtain carbonyl iron ball milled powder; step two: grinding and mixing the vinyl-containing organosilicon polymer, hydrogen-containing polysiloxane, an anti-aging agent RD, chloroplatinic acid and carbonyl iron balls into sheets; and a third step: and putting the sheet into a sheet-loading die for calendering to obtain the wave-absorbing patch. That is, in the method 100 for preparing the wave-absorbing patch of the present invention, carbonyl iron powder is ball-milled and then kneaded.
According to an embodiment of the present invention, the step one further comprises: uniformly mixing carbonyl iron powder and absolute ethyl alcohol, and then putting the mixture into a ball milling tank with a plurality of agate beads for wet milling to obtain slurry with carbonyl iron ball milled powder. Filtering the agate beads in the slurry, and heating and drying to obtain the carbonyl iron ball milled powder.
According to one embodiment of the present invention, the carbonyl iron powder has a particle size of 10 to 20 μm. The ball milling tank is arranged in a horizontal planetary ball mill, the rotating speed of the horizontal planetary ball mill is 200-400 r/min, and the ball milling time of ball milling treatment is 15-20 h. The heating and drying temperature is 40-80 ℃, and the heating and drying time is 5-8 h.
According to one embodiment of the invention, the ratio of carbonyl iron powder to absolute ethyl alcohol is 200-600 g: 800-1000 mL. The mass ratio of the agate beads to the carbonyl iron powder in the ball milling tank is 8-15: 1, the mass ratio of the agate beads is 2-5: 25-40: the agate beads are 50-70 mm in diameter, 20mm in diameter, 10mm in diameter and 6mm in diameter, and the total mass of the agate beads is 2.5 kg.
According to an embodiment of the present invention, the method further comprises mixing 30 to 50 parts of a vinyl-containing silicone polymer, 40 to 60 parts of a hydrogen-containing polysiloxane, 4 to 10 parts of an anti-aging agent RD, and 400 to 1000 parts of carbonyl iron balls, stirring the mixture at room temperature for 40 to 60 minutes by using a high speed mixer at a speed of 800 to 1200r/min, adding 0.5 to 1 part of chloroplatinic acid, stirring the mixture for 20 minutes, and mixing the mixture to obtain a sheet with a thickness of 2 mm.
In an embodiment of the present invention, the method 100 for preparing the wave-absorbing patch specifically includes:
performing ball milling treatment on carbonyl iron powder, uniformly stirring and mixing the carbonyl iron powder with the particle size of 10-20 mu m and absolute ethyl alcohol, and then putting the mixture into a ball milling tank for wet milling. Specifically, ball milling is carried out in a horizontal planetary ball mill, the rotating speed of the ball mill is 200-400 r/min, and the ball milling time is 15-20 h. Wherein the ratio of the carbonyl iron powder to the absolute ethyl alcohol is respectively 200-600 g: 800-1000 mL. A plurality of agate beads are further arranged in the ball milling tank, and the mass ratio of the agate beads to the carbonyl iron powder is 8-15: the agate beads comprise three kinds of agate beads with the diameters of 20mm, 10mm and 6mm, namely large, medium and small beads, and the mass ratio of the agate beads to the agate beads is 2-5: 25-40: 50-70, and the total weight of the agate beads is 2-3 kg. And (3) taking out the slurry after the ball milling is finished, filtering out agate beads, and heating and drying at the temperature of 40-80 ℃ for 5-8 h to obtain the carbonyl iron ball milled powder.
30-50 parts of vinyl-containing organic silicon polymer, 40-60 parts of hydrogen-containing polysiloxane, 4-10 parts of anti-aging agent RD and 400-1000 parts of carbonyl iron balls are ground and mixed. Stirring the mixture for 40-60 min at room temperature by adopting a high-speed mixer at the rotating speed of 800-1200 r/min, then adding 0.5-1 part of chloroplatinic acid, continuously stirring for 20min, mixing the mixture into a sheet with the thickness of about 2mm, and then putting the sheet into a sheet mould for calendering to obtain the silica-based wave-absorbing patch.
The prepared wave-absorbing patch is cut into a wave-absorbing patch with the size of 300mm multiplied by 1.5mm to test the reflectivity of the wave-absorbing patch, an arch field comprehensive test system is adopted to test the reflectivity of the wave-absorbing patch in a microwave dark room with the size of 4m multiplied by 4m, the test temperature is 25 ℃, the relative humidity is 54%, a fan-shaped horn in 1-18 GHz is used for testing the reflection data of the metal back plate at an incident angle of 10 degrees, then the wave-absorbing patch is placed on the metal back plate to test the common reflection data of the wave-absorbing patch and the metal back plate, and the reflectivity of the wave-absorbing patch can. The following are three specific examples of the invention, which respectively test the properties of the wave-absorbing patches prepared by the invention.
Example 1
Performing ball milling treatment on carbonyl iron powder, uniformly stirring and mixing the carbonyl iron powder with the particle size of 10-20 mu m and absolute ethyl alcohol, and then putting the mixture into a ball milling tank for wet milling. Specifically, ball milling is carried out in a horizontal planetary ball mill, the rotating speed of the ball mill is 250r/min, and the ball milling time is 20 h. Wherein the ratio of the carbonyl iron powder to the absolute ethyl alcohol is respectively 300 g: 800mL, wherein the mass ratio of a plurality of agate beads to carbonyl iron powder in the ball milling tank is 8: the agate beads comprise three kinds of agate beads with the diameters of 20mm, 10mm and 6mm, namely large, medium and small beads, and the mass ratio of the agate beads to the small beads is 5: 25: 70, the total weight of the three components is 2.5 kg. And (3) after the ball milling is finished, taking out the slurry, filtering out agate beads, and heating and drying at the temperature of 80 ℃ for 6 hours to obtain the carbonyl iron ball milled powder. And (2) grinding and mixing 45 parts of vinyl-containing organic silicon polymer, 50 parts of hydrogen-containing polysiloxane, 5 parts of anti-aging agent RD and 500 parts of carbonyl iron balls, stirring at room temperature for 60min at the rotating speed of 1000r/min by using a high-speed mixer, then adding 0.5 part of chloroplatinic acid, continuously stirring for 20min, mixing to obtain a sheet with the thickness of about 2mm, and then putting the sheet into a sheet mould for calendering to obtain the silicon-based wave-absorbing patch.
Example 2
Performing ball milling treatment on carbonyl iron powder, uniformly stirring and mixing the carbonyl iron powder with the particle size of 10-20 mu m and absolute ethyl alcohol, and then putting the mixture into a ball milling tank for wet milling. Specifically, the ball milling is carried out in a horizontal planetary ball mill, the rotating speed of the ball mill is 350r/min, and the ball milling time is 18 h. Wherein the ratio of the carbonyl iron powder to the absolute ethyl alcohol is respectively 400 g: 800mL, wherein the mass ratio of a plurality of agate beads to carbonyl iron powder in the ball milling tank is 12: the agate beads comprise three kinds of agate beads with the diameters of 20mm, 10mm and 6mm, namely large, medium and small beads, and the mass ratio of the agate beads to the small beads is 15: 25: 60, the total weight of the three components is 2.5 kg. And (3) after the ball milling is finished, taking out the slurry, filtering out agate beads, and heating and drying at the temperature of 80 ℃ for 6 hours to obtain the carbonyl iron ball milled powder. 50 parts of vinyl-containing organic silicon polymer, 45 parts of hydrogen-containing polysiloxane, 5 parts of anti-aging agent RD and 800 parts of carbonyl iron balls are ground and mixed, a high-speed mixer is adopted to stir at room temperature for 60min at the rotating speed of 1200r/min, then 0.8 part of chloroplatinic acid is added to continue stirring for 20min, the mixture is mixed into a sheet with the thickness of about 2mm, and the sheet is placed into a sheet mold to be calendered, so that the silicon-based wave-absorbing patch is obtained.
Example 3
Performing ball milling treatment on carbonyl iron powder, uniformly stirring and mixing the carbonyl iron powder with the particle size of 10-20 mu m and absolute ethyl alcohol, and then putting the mixture into a ball milling tank for wet milling. Specifically, the ball milling is carried out in a horizontal planetary ball mill, the rotating speed of the ball mill is 400r/min, and the ball milling time is 15 h. Wherein the ratio of the carbonyl iron powder to the absolute ethyl alcohol is respectively 500 g: 1000mL, the mass ratio of a plurality of agate beads to carbonyl iron powder in the ball milling tank is 15: 1. the agate beads comprise three kinds of agate beads with the diameters of 20mm, 10mm and 6mm, namely large, medium and small agate beads, and the mass ratio of the agate beads to the small agate beads is 20: 40: 40, the total weight of the three components is 2.5 kg. And (3) after the ball milling is finished, taking out the slurry, filtering out agate beads, and heating and drying at the temperature of 80 ℃ for 6h to obtain the ball milling powder of carbonyl iron. And (2) grinding and mixing 45 parts of vinyl-containing organic silicon polymer, 45 parts of hydrogen-containing polysiloxane, 10 parts of anti-aging agent RD and 900 parts of carbonyl iron balls, stirring at room temperature for 60min at the rotating speed of 1200r/min by using a high-speed mixer, then adding 1 part of chloroplatinic acid, continuously stirring for 20min, mixing into a sheet with the thickness of about 2mm, and then putting the sheet into a sheet mould for calendering to obtain the silicon-based wave-absorbing patch.
And (3) carrying out performance test on the three prepared wave-absorbing patches:
the reflectivity test of the wave-absorbing patch prepared in the embodiment 1 shows that the wave-absorbing patch obtained by ball-milling carbonyl iron powder has the wave-absorbing performance bandwidth of 2.71GHz less than or equal to 10dB and the peak intensity of 36.7dB at 4.26 GHz. The filling rate of the wave absorbing agent in the patch can reach 83.3 percent. The tensile strength of the material is 3.16MPa and the bending strength of the material is 2.89MPa through conventional mechanical tests.
The reflectivity test of the wave-absorbing patch prepared in the embodiment 2 shows that the wave-absorbing patch obtained by ball-milling carbonyl iron powder has the wave-absorbing performance bandwidth of 2.14GHz less than or equal to 10dB and the peak intensity of 28.9dB at 3.65 GHz. The filling rate of the wave absorbing agent in the patch can reach 88.8%. The tensile strength of the alloy is 1.97MPa and the bending strength of the alloy is 1.74MPa through conventional mechanical tests.
The reflectivity test of the wave-absorbing patch prepared in the embodiment 3 shows that the wave-absorbing patch obtained by ball milling carbonyl iron powder has the wave-absorbing performance bandwidth of 1.83GHz less than or equal to 10dB and the peak intensity of 20.4dB at 2.78 GHz. The filling rate of the wave absorbing agent in the patch can reach 90%. The tensile strength of the alloy is 1.88MPa and the bending strength of the alloy is 1.76MPa through conventional mechanical tests.
The preparation method 100 of the wave-absorbing patch is environment-friendly and pollution-free, and the filling amount of the absorbent is large, so that the wave-absorbing patch can be widely applied to wave-absorbing materials in the technical fields of anti-electromagnetic radiation interference, microwave darkrooms, shielding boxes and microwave radiation protection of mobile devices, display devices, computers, digital equipment, electronic products and the like. In addition, in the fields of radar, communication and aerospace, the wave-absorbing patch has wide application space in the aspects of improving the compatibility of airborne and airborne radar equipment, improving the performance of the whole machine and the like.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a wave-absorbing patch is characterized by comprising the following steps:
the method comprises the following steps: carrying out ball milling treatment on carbonyl iron powder, and heating and drying to obtain carbonyl iron ball milled powder;
step two: grinding and mixing a vinyl-containing organosilicon polymer, hydrogen-containing polysiloxane, an anti-aging agent, chloroplatinic acid and the carbonyl iron balls into sheets; and
step three: and putting the sheet into a sheet-mounted die for calendering to obtain the wave-absorbing patch.
2. The method according to claim 1, further comprising, in the first step: carbonyl iron powder and absolute ethyl alcohol are mixed and then put into a ball milling tank with a plurality of agate beads for wet milling, so that slurry with the carbonyl iron ball milled powder is obtained.
3. The method according to claim 1, wherein the carbonyl iron powder has a particle size of 10 to 20 μm.
4. The preparation method of claim 1, wherein the ball milling time of the ball milling treatment is 15-20 h.
5. The preparation method according to claim 1, wherein the temperature for heating and drying is 40-80 ℃, and the time for heating and drying is 5-8 h.
6. The preparation method according to claim 2, wherein the ball milling pot is arranged in a horizontal planetary ball mill, and the rotation speed of the horizontal planetary ball mill is 200-400 r/min.
7. The preparation method according to claim 2, wherein the ratio of carbonyl iron powder to absolute ethyl alcohol is 200-600 g: 800-1000 mL.
8. The preparation method according to claim 2, wherein the mass ratio of the agate beads to the carbonyl iron powder is 8-15: 1, the agate beads comprise the following components in a mass ratio of 2-5: 25-40: the agate beads are 50-70 agate beads with the diameters of 20mm, 10mm and 6mm respectively, and the total mass of the agate beads is 2.5 kg.
9. The method according to claim 1, further comprising mixing 30 to 50 parts of the vinyl-containing silicone polymer, 40 to 60 parts of the hydrogen-containing polysiloxane, 4 to 10 parts of the anti-aging agent, and 400 to 1000 parts of the carbonyl iron balls, milling the mixture, stirring the mixture at room temperature for 40 to 60 minutes at a speed of 800 to 1200r/min by a high speed mixer, adding 0.5 to 1 part of the chloroplatinic acid, stirring the mixture for 20 minutes, and kneading the mixture to obtain the sheet.
10. The method of claim 1, wherein the sheet has a thickness of 2 mm.
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