CN111073296A - Wave-absorbing patch and preparation method thereof - Google Patents
Wave-absorbing patch and preparation method thereof Download PDFInfo
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- CN111073296A CN111073296A CN201811216268.3A CN201811216268A CN111073296A CN 111073296 A CN111073296 A CN 111073296A CN 201811216268 A CN201811216268 A CN 201811216268A CN 111073296 A CN111073296 A CN 111073296A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions 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; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- H—ELECTRICITY
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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Abstract
The invention provides a wave-absorbing patch and a preparation method thereof, wherein the wave-absorbing patch comprises the following steps: mixing the vinyl-containing organic silicon polymer, hydrogen-containing polysiloxane, an anti-aging agent and the expanded graphite coated by ferroferric oxide, uniformly stirring, mixing and rolling to obtain the wave-absorbing patch. The wave absorbing agent with the core-shell structure is formed by coating hollow ferroferric oxide on the surface of the expanded graphite, so that the density of the wave absorbing agent can be reduced, the hollow and core-shell structure can be utilized, the multiple reflection of electromagnetic waves in the wave absorbing agent can be increased, the reflection loss of the wave absorbing agent is increased, and the reflection performance is improved. The technical process provided by the invention is simple, the operation is convenient, the prepared wave-absorbing patch is environment-friendly and pollution-free, has low density and good absorption performance, and can be widely applied to the fields of aerospace, antenna radar, airplane stealth, electronic communication, medical appliances and the like.
Description
Technical Field
The invention relates to the field of wave-absorbing materials, in particular to a wave-absorbing patch and a preparation method thereof.
Background
With the development of modern science and technology, various electronic and electrical equipment provide high efficiency for social production and bring great convenience for daily life of people. Meanwhile, the electromagnetic radiation and interference generated in the working process of electronic and electrical equipment can influence the production and life of people, so that the electromagnetic environment of human living space is increasingly worsened, the electromagnetic radiation and interference becomes a new pollution source which has larger harm and is not easy to protect after water source, atmosphere and noise, the electromagnetic radiation and interference not only influences normal communication, but also directly threatens the health of human, and becomes a hot problem concerned by the society and the science community, and therefore, the electromagnetic radiation and interference wave absorbing material is of great importance for the research on the wave absorbing material for reducing the electromagnetic radiation harm. The electromagnetic absorbing material is highly regarded by people in all fields, and is increasingly applied to industry and military, and is also gradually applied to various civil electronic and electrical equipment.
The wave-absorbing patch is mainly prepared by mixing ferrite and metal alloy powder serving as absorbents with plastic according to a certain proportion, the polymer-based wave-absorbing material on the market is mainly prepared by vulcanization molding, and the vulcanized plastic has large smell and is polluted and not suitable for certain specific application fields. In addition, the wave absorbing performance of the material can be influenced by the content of the wave absorbing agent and the thickness of the patch, and although the larger filling amount and the larger thickness are beneficial to improving the wave absorbing performance, the material has higher density and cannot meet the requirement of weight reduction, so that the application of the wave absorbing material patch is limited to a certain extent.
Disclosure of Invention
Aiming at the problems in the related art, the invention researches a preparation method of a wave-absorbing patch so as to provide the wave-absorbing patch with good wave-absorbing performance.
The preparation method of the wave-absorbing patch provided by the invention comprises the following steps: mixing the vinyl-containing organic silicon polymer, hydrogen-containing polysiloxane, an anti-aging agent and the expanded graphite coated by ferroferric oxide, uniformly stirring, mixing and rolling to obtain the wave-absorbing patch.
In the above preparation method, the step of mixing the vinyl-containing organosilicon polymer, the hydrogen-containing polysiloxane, the age resistor, and the ferroferric oxide-coated expanded graphite comprises: according to the mass parts, 30-50 parts of the vinyl-containing organic silicon polymer, 40-60 parts of the hydrogen-containing polysiloxane, 4-10 parts of the anti-aging agent and 400-1000 parts of the ferroferric oxide-coated expanded graphite are mixed.
In the above preparation method, the step of uniformly stirring comprises: stirring the mixture in a high-speed mixer at the speed of 800-1200r/min for 40-60 min.
In the above production method, the method further comprises: and after the step of uniformly stirring, adding 0.5-1 part of chloroplatinic acid by mass.
In the preparation method, the mixing mode is selected from one or more of triangular bag making, pillow bag making and thin tube making.
In the preparation method, the structure of the ferroferric oxide is a hollow structure.
In the above preparation method, the vinyl-containing organosilicon polymer is selected from one or more of vinyl phenyl polysiloxane, polystyrene and acrylate-silane polymer.
In the above preparation method, the vinyl-containing organosilicon polymer is selected from one or more of vinyl phenyl polysiloxane, polystyrene and acrylate-silane polymer.
In the above production method, the aging inhibitor is selected from one or a combination of more of tris (1, 4-ditertiary) phosphite, polypropylene resin, bis (2, 4-di-t-butylphenyl) alcohol diphosphate, bis (octadecyl) pentaerythritol diester.
The invention also provides the wave-absorbing patch prepared by the method.
According to the preparation method of the wave-absorbing patch, the surface of the expanded graphite is coated with the hollow ferroferric oxide, and the graphite sheet is light in weight and good in dielectric property, and the surface of the graphite sheet is coated with the hollow ferroferric oxide particles with high magnetic conductivity to form the wave-absorbing agent with the core-shell structure, so that the density of the wave-absorbing agent can be reduced, multiple reflections of electromagnetic waves in the wave-absorbing agent can be increased by utilizing the hollow and core-shell structures, the reflection loss of the wave-absorbing agent is increased, and the reflection property is improved. The technical process provided by the invention is simple, the operation is convenient, the prepared wave-absorbing patch is environment-friendly and pollution-free, the density is low, and the absorption performance is good.
The wave-absorbing patch prepared by the invention can be widely applied to wave-absorbing materials in the technical fields of anti-electromagnetic radiation interference, microwave darkroom, shielding box and microwave radiation protection, such as mobile devices, display devices, computers, digital equipment, electronic products and the like; in the fields of aerospace, antenna radar, airplane stealth, electronic communication, medical appliances and the like, the wave-absorbing patch characteristic has important application value in the fields of electromagnetic wave absorption and electromagnetic shielding.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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.
The preparation method of the wave-absorbing patch provided by the invention comprises the following steps:
preparing expanded graphite: according to the mass parts, 5-50 parts of graphite is dissolved in 5-10 parts of 98% concentrated sulfuric acid and 80-120 parts of deionized water, then the graphite is mechanically stirred in a water bath kettle at 50-60 ℃ for 40-60min, then water washing is carried out for 3-5 times, then filtering and drying are carried out, then the obtained graphite is put into a muffle furnace which is heated to 800-1000 ℃ for heating for 5-10min, and the obtained graphite is taken out and cooled to prepare the expanded graphite.
Preparing ferroferric oxide coated expanded graphite: respectively weighing 5-8 parts of ammonia water and 10-20 parts of ethanolamine according to a certain volume ratio, and uniformly stirring and mixing; 200-300g of soluble iron salt (ferric chloride) is weighed and dissolved in the solution, and is uniformly mixed, then the solution is placed into a reaction kettle with the temperature of 200-250 ℃ for reaction for 5-10 hours, and then the solution is taken out and poured into a reaction vessel beaker. Weighing 10-20 parts of expanded graphite prepared by the method, adding the expanded graphite into 40-50 parts of the solution, adjusting the pH value to 10.5-11.5, mechanically stirring in an oil bath kettle at 90-120 ℃ for 8-12h, adsorbing a magnetic substance to the bottom of the beaker, removing supernatant, cleaning for 3-5 times again, and drying to obtain the hollow ferroferric oxide coated expanded graphite.
Preparing the wave-absorbing patch: mixing the vinyl-containing organic silicon polymer, hydrogen-containing polysiloxane, an anti-aging agent and the expanded graphite coated by ferroferric oxide, uniformly stirring, mixing and rolling to obtain the wave-absorbing patch. Specifically, according to the mass parts, 30-50 parts of vinyl-containing organosilicon polymer, 40-60 parts of hydrogen-containing polysiloxane, 4-10 parts of anti-aging agent RD, and 1000 parts of ferroferric oxide-coated expanded graphite are mixed, stirred at the room temperature of 800-1200r/min by a high-speed mixer for 40-60min, then added with 0.5-1 part of chloroplatinic acid for 20min, mixed to a sheet with the thickness of about 2-4 mm, and placed in a sheet mold for calendering to obtain the silica gel-based wave-absorbing patch with the thickness of 1-3 mm. In the step, the ferroferric oxide is in a hollow structure, and the filling rate of the wave absorbing agent in the patch can reach 90%. In this step, the vinyl-containing silicone polymer is selected from one or more of vinylphenyl polysiloxane, polystyrene, acrylate-silane polymer in combination, the hydrogen-containing polysiloxane is selected from one or more of dimethylpolysiloxane, diphenyl dimethylpolysiloxane, trifluoropropyldimethylpolysiloxane in combination, and the aging inhibitor is selected from one or more of tris (1, 4-ditertiary) phosphite, polypropylene resin, bis (2, 4-di-t-butylphenyl) alcohol diphosphate, bis (octadecyl) pentaerythritol diester in combination. The hollow ferroferric oxide coated expansion is found by measurementThe density of the wave-absorbing patch of the graphite is 526g/cm higher than that of the wave-absorbing patch of the ferroferric oxide coated expanded graphite3Reduced to 387g/cm3。
According to the invention, the surface of the expanded graphite is coated with the hollow ferroferric oxide, and the graphite flake is light in weight and good in dielectric property, and the surface of the graphite flake is coated with the hollow ferroferric oxide particles with high magnetic conductivity to form the wave absorber with the core-shell structure, so that the density of the wave absorber can be reduced, the hollow and core-shell structures can be utilized, the multiple reflection of electromagnetic waves in the wave absorber can be increased, the reflection loss of the wave absorber can be increased, and the reflection performance can be improved.
The method for testing the reflectivity of the wave-absorbing patch comprises the following steps: the wave-absorbing patch is cut into wave-absorbing patches with the size of 300mm multiplied by 1.5mm for testing the reflectivity, an arch field comprehensive testing system is adopted in a microwave dark room with the size of 4m multiplied by 4m for testing the reflectivity of the wave-absorbing patches, the testing temperature is 25 ℃, the relative humidity is 54%, a fan-shaped horn in 1-18GHz measures the reflection data of a metal back plate at an incident angle of 10 degrees, then the wave-absorbing patches are placed on the metal back plate for measuring the reflection data of the patches, and the reflectivity of the wave-absorbing patches can be obtained by subtracting the reflection data of the patches.
Example 1
According to the mass parts, 30 parts of vinylphenyl polysiloxane, 40 parts of dimethyl polysiloxane, 4 parts of tris (1, 4-di-tertiary group) phosphite ester and 400 parts of ferroferric oxide coated expanded graphite are mixed, stirred at the room temperature of 800r/min for 40min by a high-speed mixer, then 0.5 part of chloroplatinic acid is added for 20min, and the mixture is mixed to a sheet with the thickness of about 2mm and then placed into a sheet mold for calendering to obtain the silica gel-based wave-absorbing patch with the thickness of 1 mm.
Example 2
Mixing 50 parts of polystyrol, 60 parts of diphenyl dimethyl polysiloxane, 10 parts of polypropylene resin and 1000 parts of ferroferric oxide coated expanded graphite according to the mass parts, stirring the mixture at the room temperature of 1200r/min for 60min by using a high-speed mixer, then adding 1 part of chloroplatinic acid for 20min, mixing the mixture to obtain a sheet with the thickness of about 4mm, and then putting the sheet into a sheet mould for calendering to obtain the silica gel-based wave-absorbing patch with the thickness of 3 mm.
Example 3
Mixing 40 parts of acrylate-silane polymer, 50 parts of trifluoro-cyclopropyl dimethyl polysiloxane, 7 parts of bis (2, 4-di-tert-butylphenyl) alcohol diphosphate and 600 parts of ferroferric oxide-coated expanded graphite in parts by mass, stirring the mixture at the room temperature of 1000r/min for 50min by using a high-speed mixer, then adding 0.7 part of chloroplatinic acid for 20min, mixing the mixture to obtain a sheet with the thickness of about 3mm, and then putting the sheet into a sheet mold for calendering to obtain the silica gel-based wave-absorbing patch with the thickness of 1 mm.
Example 4
According to the mass parts, 35 parts of polystyrol, 45 parts of trifluoro cyclopropyl dimethyl polysiloxane, 6 parts of bis (octadecyl) pentaerythritol diester and 500 parts of ferroferric oxide coated expanded graphite are mixed, stirred at the room temperature of 900r/min for 45min by a high-speed mixer, then 0.6 part of chloroplatinic acid is added for 20min, the mixture is mixed to a sheet with the thickness of about 4mm, and the sheet is placed into a sheet mold for calendering to obtain the silica gel-based wave-absorbing patch with the thickness of 2 mm.
Example 5
According to the mass parts, 45 parts of vinyl phenyl polysiloxane, 55 parts of dimethyl polysiloxane, 8 parts of bis (2, 4-di-tert-butylphenyl) alcohol diphosphate and 800 parts of ferroferric oxide coated expanded graphite are mixed, stirred at the room temperature of 1100r/min for 55min by a high-speed mixer, then 0.8 part of chloroplatinic acid is added for 20min, and the mixture is mixed to a sheet with the thickness of about 3mm and then placed in a sheet mold for calendering to obtain the silica gel-based wave-absorbing patch with the thickness of 2 mm.
The wave-absorbing performance of the wave-absorbing patches prepared in the above examples 1-5 was tested to obtain the peak values of tensile strength, bending strength and reflectivity of the wave-absorbing patch, and the results are shown in table 1 below:
| serial number | Tensile strength | Bending strength | Reflectivity peak (GHz, dB) |
| Example 1 | 2.23MPa | 1.68MPa | (6.1，14.5) |
| Example 2 | 3.52MPa | 1.94MPa | (8.3，16.1) |
| Example 3 | 2.36MPa | 2.12MPa | (7.2，15.2) |
| Example 4 | 3.12MPa | 2.86MPa | (7.4，15.5) |
| Example 5 | 3.89MPa | 3.05MPa | (7.9，15.3) |
According to the experimental results, the wave-absorbing patch prepared by the method disclosed by the invention not only has good tensile strength and bending strength, but also has good wave-absorbing performance. The method can be widely applied to the fields of aerospace, antenna radar, airplane stealth, electronic communication, medical appliances and the like.
According to the invention, the surface of the expanded graphite is coated with the hollow ferroferric oxide, and the graphite flake is light in weight and good in dielectric property, and the surface of the graphite flake is coated with the hollow ferroferric oxide particles with high magnetic conductivity to form the wave absorber with the core-shell structure, so that the density of the wave absorber can be reduced, the hollow and core-shell structures can be utilized, the multiple reflection of electromagnetic waves in the wave absorber can be increased, the reflection loss of the wave absorber can be increased, and the reflection performance can be improved. The silicon-gum-based wave-absorbing patch is obtained by mixing the silicon-gum-based wave-absorbing patch with different components at room temperature, the process is simple, the operation is convenient, and the prepared wave-absorbing patch is pollution-free, low in density, good in wave-absorbing performance and suitable for different wave-absorbing fields.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. 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: mixing the vinyl-containing organic silicon polymer, hydrogen-containing polysiloxane, an anti-aging agent and the expanded graphite coated by ferroferric oxide, uniformly stirring, mixing and rolling to obtain the wave-absorbing patch.
2. The production method according to claim 1, wherein the step of mixing the vinyl-containing silicone polymer, the hydrogenpolysiloxane, the age resistor, and the ferrosoferric oxide-coated expanded graphite comprises: according to the mass parts, 30-50 parts of the vinyl-containing organic silicon polymer, 40-60 parts of the hydrogen-containing polysiloxane, 4-10 parts of the anti-aging agent and 400-1000 parts of the ferroferric oxide-coated expanded graphite are mixed.
3. The method of claim 1, wherein the step of stirring uniformly comprises: stirring the mixture in a high-speed mixer at the speed of 800-1200r/min for 40-60 min.
4. The method of manufacturing according to claim 1, further comprising: and after the step of uniformly stirring, adding 0.5-1 part of chloroplatinic acid by mass.
5. The method of claim 1, wherein the mixing is performed by one or more selected from the group consisting of triangular bagging, pillow bagging, and thining.
6. The preparation method according to claim 1, wherein the ferroferric oxide has a hollow structure.
7. The method of claim 1, wherein the vinyl-containing silicone polymer is selected from the group consisting of one or more of vinylphenyl polysiloxane, polystyrol, acrylate-silane polymer.
8. The method according to claim 1, wherein the hydrogenpolysiloxane is selected from one or more of dimethylpolysiloxane, diphenyldimethylpolysiloxane, and trifluoropropyldimethylpolysiloxane.
9. The method according to claim 1, wherein the anti-aging agent is selected from the group consisting of tris (1, 4-ditertiary) phosphite, polypropylene resin, bis (2, 4-di-t-butylphenyl) alcohol diphosphate, bis (octadecyl) pentaerythritol diester, and combinations of one or more thereof.
10. The wave-absorbing patch prepared by the preparation method according to any one of claims 1 to 9.
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| CN112029421A (en) * | 2020-09-11 | 2020-12-04 | 航天特种材料及工艺技术研究所 | Wave-absorbing adhesive film material and preparation method thereof |
| CN114516661A (en) * | 2020-11-19 | 2022-05-20 | 洛阳尖端技术研究院 | Hollow flaky carbonyl iron powder and preparation method thereof |
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