CN112048239B - Barium ferrite-Al2O3Porous SiC-loaded polyaniline wave-absorbing coating and preparation method thereof - Google Patents
Barium ferrite-Al2O3Porous SiC-loaded polyaniline wave-absorbing coating and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of polyaniline wave-absorbing coating, and discloses barium ferrite-Al2O3The porous SiC loaded polyaniline wave-absorbing coating comprises the following formula raw materials: barium ferrite-Al2O3The composite material comprises-SiC composite material, silane coupling agent, ammonium persulfate, aniline, o-anisidine and emulsifier. The barium ferrite-Al2O3Porous SiC-loaded polyaniline wave-absorbing coating, Al2O3The composite material is loaded on the surface of the SiC hollow microsphere to form a composite material, a large amount of electric dipole moment is generated, the interface polarization capability is enhanced, the SiC hollow microsphere structure can reflect and attenuate electromagnetic waves for multiple times, the lanthanum doping adjusts the barium ferrite magnetic crystal anisotropy field, the saturation magnetization intensity is improved, the magnetic conductivity and the magnetic loss capability of the barium ferrite are enhanced, the barium ferrite forms a three-dimensional conductive network on the surface of the SiC hollow microsphere to generate leakage loss to attenuate the electromagnetic waves, and the N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane improves the barium ferrite-Al2O3Dispersibility and compatibility of the-SiC composite material in polyaniline.
Description
Technical Field
The invention relates to the technical field of polyaniline wave-absorbing coating, in particular to barium ferrite-Al2O3Porous SiC loaded polyaniline wave-absorbing coating and a preparation method thereof.
Background
The electromagnetic wave is an oscillating particle wave which is derived and emitted in space by an electric field and a magnetic field which are the same and vertical to each other, and is an electromagnetic field which is transmitted in a wave form, the interference transmission path of the electromagnetic wave mainly comprises conduction interference and radiation interference, the electromagnetic wave can generate electronic radiation pollution to influence the normal work of electronic equipment, the electromagnetic wave also has great harm to human bodies, and the electromagnetic radiation is one of the main causes of cardiovascular diseases, diabetes and cancer mutation.
In order to prevent and inhibit the interference of electromagnetic waves, technical methods such as reasonably designing a circuit, filtering, shielding and the like are mainly adopted, the shielding technology is widely applied as a basic means for inhibiting the radiation of the electromagnetic waves, the radiation energy is limited in a specific area, or the radiation energy is prevented from entering another specific area, a wave absorbing material and a shielding material are key points of high and low shielding efficiency, polyaniline conductive polymers have the advantages of light weight, low density, good corrosion resistance, adjustable conductivity, special conjugated large pi system and the like, the great development potential is shown in the field of the wave absorbing material, but the absorption capacity of the conductive polymers to the electromagnetic waves is very limited by the conductive polymers, so that the polyaniline conductive polymers and other inorganic dielectric materials such as ferrite, strontium ferrite, ferroferric oxide, aluminum trioxide and the like are formed into composite materials, and the excellent electrical properties of the conductive polymers are utilized, and then the electromagnetic parameters of the material are regulated and controlled, the impedance matching of the material is improved, and the wave-absorbing performance of the material is improved, but the compatibility and the dispersibility of the inorganic dielectric material in the polyaniline are poor, so that the wave-absorbing performance of the polyaniline material is greatly reduced.
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides barium ferrite-Al2O3The polyaniline wave-absorbing coating loaded with porous SiC and the preparation method thereof solve the problem of poor wave-absorbing performance of polyaniline materials and the problem of poor compatibility and dispersibility of inorganic dielectric materials in polyaniline.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: barium ferrite-Al2O3The porous SiC loaded polyaniline wave-absorbing coating comprises the following formula raw materials in parts by weight: 6-18 parts of barium ferrite-Al2O3The composite material comprises-SiC composite material, 1-3 parts of silane coupling agent, 32-34 parts of ammonium persulfate, 17-19 parts of aniline, 30-33 parts of o-anisidine and 2-5 parts of emulsifier.
Preferably, the silane coupling agent is N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane.
Preferably, the emulsifier is dodecylbenzene sulfonic acid.
Preferably, the barium ferrite-Al2O3The preparation method of the-SiC composite material comprises the following steps:
(1) adding a mixed solvent of distilled water and ethanol into a reaction bottle, adding m-diphenol and paraformaldehyde, stirring at a constant speed until the mixture is dissolved, placing the reaction bottle into an ultrasonic treatment instrument, performing ultrasonic dispersion treatment at 40-50 ℃ for 40-60min, adding an ammonia water solution with the mass fraction of 20-25%, wherein the volume ratio of the distilled water to the ethanol to the ammonia water solution is 20-26:3-4:1, stirring at a constant speed for 6-8h, slowly dropwise adding tetraethoxysilane, placing the reaction bottle into a constant-temperature water bath, heating to 40-50 ℃, stirring at a constant speed for reaction for 25-30h, removing the solvent from the solution through a high-speed centrifuge, washing a solid product with distilled water and ethanol, fully drying, placing the solid product into an atmosphere resistance furnace, heating at the rate of 5-10 ℃/min, heating to 550-, calcining for 6-8h in air atmosphere under heat preservation, and then calcining in N2Heating to 620-plus-650 ℃ in the atmosphere, carrying out heat preservation calcination for 2-3h, heating to 1300-plus-1320 ℃ in the Ar atmosphere, carrying out heat preservation calcination for 2-3h, finally cooling to 720-plus-750 ℃, introducing air, carrying out heat preservation calcination for 1-2h, wherein the calcination product is the porous nano SiC hollow microspheres.
(2) Adding ethanol solvent, porous nano SiC hollow microspheres and nano Al into a reaction bottle2O3Placing a reaction bottle in an ultrasonic treatment instrument, performing ultrasonic dispersion treatment for 1-2h at 40-50 ℃, concentrating the solution under reduced pressure to remove the solvent and drying, placing the solid mixture in an atmosphere resistance furnace, introducing Ar, heating at the rate of 5-10 ℃/min, performing heat preservation and calcination for 3-4h at the temperature of 1420-1460 ℃, wherein the calcination product is SiC hollow microsphere loaded nano Al2O3。
(3) Distilled water and SiC hollow microsphere loaded with nano Al are added into a reaction bottle2O3、FeCl3、BaCl2And LaCl3Stirring for dissolving, adding polyvinylpyrrolidone, stirring at constant speed for 1-2 hr, adding urea, placing the reaction bottle in an ultrasonic treatment instrument, performing ultrasonic dispersion treatment at 50-70 deg.C for 2-3 hr, transferring the solution into a polytetrafluoroethylene reaction kettle, placing in a reaction kettle heating box, heating to 150 deg.C and 180 deg.C, reacting for 15-20 hr, cooling to room temperature, filtering to remove solvent, and allowing the solution to pass throughWashing the solid product with distilled water and ethanol, fully drying, placing the solid product in an atmosphere resistance furnace, heating at a rate of 5-10 ℃/min, calcining at 1050-1100 ℃ for 3-4h, wherein the calcined product is lanthanum-doped barium ferrite-SiC hollow microsphere loaded with nano Al2O3I.e. barium ferrite-Al2O3-a SiC composite material.
Preferably, the constant temperature water-bath includes the pot body, the inside swing joint of the pot body has a pot courage, the top swing joint of pot courage has the lid, the front of the pot body is provided with control panel, control panel's the outside is provided with the voltage control button, control panel's the outside is provided with the temperature control button, control panel's outside swing joint has the power key, the pot body is the design of radius angle for cuboid shape and its outside, the shape and the size of lid all with pot courage looks adaptation, and the cross sectional shape of lid is isosceles trapezoid, the four corners of pot body bottom all is provided with the cushion, the specification and size homogeneous phase of four cushion just is the stereoplasm rubber material.
Preferably, the mass ratio of the m-diphenol to the paraformaldehyde to the ethyl orthosilicate is 1:1.2-1.5: 6-7.
Preferably, the porous nano SiC hollow microspheres and nano Al2O3The mass ratio is 4-6: 1.
Preferably, the SiC hollow microspheres load nano Al2O3、FeCl3、BaCl2And LaCl3The mass ratio of the four is 30-40:28-47:3-5: 1.
Preferably, the barium ferrite-Al2O3The preparation method of the porous SiC loaded polyaniline wave-absorbing coating comprises the following steps:
(1) adding ethanol solvent and 6-18 parts of barium ferrite-Al into a reaction bottle2O3Placing a reaction bottle in a constant-temperature water bath, heating to 50-60 ℃, uniformly stirring for reaction for 30-40h, carrying out reduced pressure concentration on the solution to remove the solvent, washing the solid product with distilled water, and preparing the modified barium ferrite-Al2O3-a SiC composite material.
(2) Adding hydrochloric acid solution with the substance amount concentration of 1-1.5mol/L into a reaction bottle, adding 17-19 parts of aniline, 30-33 parts of o-methoxyaniline and 32-34 parts of ammonium persulfate, placing the reaction bottle into a low-temperature cooler, uniformly stirring and reacting for 15-20h at-5-0 ℃, filtering the solution to remove the solvent, washing the solid product with a proper amount of distilled water, and fully drying to prepare the aniline copolymer.
(3) Adding N, N-dimethylformamide solvent, aniline copolymer and modified barium ferrite-Al into a reaction bottle2O3-SiC composite material, placing a reaction bottle in an ultrasonic treatment instrument, performing ultrasonic dispersion treatment for 3-5h at the ultrasonic frequency of 25-35KHz, then stirring at constant speed for 2-4h, adding distilled water into the reaction bottle until a large amount of precipitate is generated, filtering to remove solvent, washing a solid product by using distilled water and ethanol, fully drying, adding a solid product solution in a toluene solvent, controlling the solid-liquid ratio to be 40-60%, then adding 2-5 parts of emulsifier, and stirring at constant speed for 4-6h to prepare barium ferrite-Al2O3Porous SiC loaded polyaniline wave-absorbing coating.
(III) advantageous technical effects
Compared with the prior art, the invention has the following beneficial technical effects:
the barium ferrite-Al2O3The polyaniline wave-absorbing coating loaded with porous SiC, resorcinol and paraformaldehyde and formed phenolic aldehyde oligomer as hollow templates and pore-making agents are prepared into porous nano SiC hollow microspheres by a high-temperature carbonization method, the surfaces of the porous nano SiC hollow microspheres have rich mesoporous structures and huge specific surface areas, the dielectric constant of SiC is very high, Al is added into the porous nano SiC hollow microspheres2O3Has excellent electrical insulation and low dielectric loss, Al2O3The composite material is loaded on the surface of the SiC hollow microsphere to generate a large amount of electric dipole moment, so that the interface polarization capability is enhanced, the impedance matching performance and the wave absorbing performance of the SiC are improved, and the SiC hollow microsphere structure can reflect electromagnetic waves for multiple times and has the effect of losing the electromagnetic waves.
The barium ferrite-Al2O3Porous SiC-loaded polyaniline wave-absorbing coating and barium ferriteThe body is spinel type ferrite, the barium ferrite forms hexagonal system ferrite with better wave-absorbing performance by doping lanthanum, the lanthanum has good electromagnetic structure and property, the anisotropic field and the electromagnetic parameters of the barium ferrite magnetic crystal are adjusted, the saturation magnetization intensity of the barium ferrite is improved, the coercive force is reduced, the magnetic conductivity and the magnetic loss capability of the barium ferrite are improved, and the lanthanum doping enables the barium ferrite to form a three-dimensional conductive network on the surface of the SiC hollow microsphere, so that the leakage loss can be generated to effectively attenuate electromagnetic waves.
The barium ferrite-Al2O3Porous SiC-loaded polyaniline wave-absorbing coating, silane coupling agent N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane and Al2O3The hydroxyl on the surface is bonded, and the amino and imino in the silane coupling agent and the imino in the polyaniline form hydrogen bonds and van der Waals force, so that the barium ferrite-Al is greatly improved2O3The dispersibility and the compatibility of the-SiC composite material in polyaniline avoid barium ferrite-Al2O3the-SiC composite material is agglomerated and agglomerated, so that the electromagnetic loss capacity and the wave absorbing performance of the polyaniline are enhanced.
Drawings
FIG. 1 is a perspective view of a connection structure of the present invention;
FIG. 2 is a left side view of the connection structure of the present invention;
FIG. 3 is a front view of the connection of the present invention;
fig. 4 is a top view of the connection structure of the present invention.
In the figure: 1-pot body, 2-pot container, 3-cover body, 4-control panel, 5-voltage control button, 6-temperature control button and 7-power key.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: barium ferrite-Al2O3The porous SiC loaded polyaniline wave-absorbing coating comprises the following formula raw materials in parts by weight: 6-18 parts of barium ferrite-Al2O3-SiC composite material, 1-3 parts of silane coupling agent, 32-34 parts of ammonium persulfate, 17-19 parts of aniline, 30-33 parts of o-methoxyaniline, 2-5 parts of emulsifier and silane coupling agentThe emulsifier is N- (beta-aminoethyl) -gamma-aminopropyl trimethoxy silane and the emulsifier is dodecyl benzene sulfonic acid.
Barium ferrite-Al2O3The preparation method of the-SiC composite material comprises the following steps:
(1) adding a mixed solvent of distilled water and ethanol into a reaction bottle, adding m-diphenol and paraformaldehyde, stirring at a constant speed until the m-diphenol and the paraformaldehyde are dissolved, placing the reaction bottle into an ultrasonic treatment instrument, performing ultrasonic dispersion treatment at 40-50 ℃ for 40-60min, adding an ammonia water solution with the mass fraction of 20-25%, wherein the volume ratio of the distilled water to the ethanol to the ammonia water solution is 20-26:3-4:1, stirring at a constant speed for 6-8h, slowly dropwise adding ethyl orthosilicate, wherein the mass ratio of the m-diphenol to the paraformaldehyde to the ethyl orthosilicate is 1:1.2-1.5:6-7, placing the reaction bottle into a constant-temperature water bath kettle, wherein the constant-temperature water bath kettle comprises a kettle body, the inner part of the kettle body is movably connected with a kettle liner, a cover body is movably connected above the kettle liner, a control panel is arranged on the front surface of the kettle body, and a voltage control button is arranged on the outer side of the control panel, the outer side of the control panel is provided with a temperature control button, the outer side of the control panel is movably connected with a power key, the pot body is in a cuboid shape, the outer side of the pot body is in a fillet design, the shape and the size of the cover body are matched with those of the pot liner, the cross section of the cover body is in an isosceles trapezoid shape, the four corners of the bottom of the pot body are provided with cushion blocks, the four cushion blocks are same in specification and size and are made of hard rubber materials, the pot body is heated to 40-50 ℃, stirred and reacted for 25-30h at a constant speed, the solution is passed through a high-speed centrifuge to remove a solvent, the solid product is washed by using distilled water and ethanol and is fully dried, the solid product is placed in an atmosphere resistance furnace, the heating rate is 5-10 ℃/min, the temperature is increased to 550 ℃; 580 ℃, the pot body is subjected to heat preservation and calcination for 6-8h in an air atmosphere, and then the pot is subjected to N2Heating to 620-plus-650 ℃ in the atmosphere, carrying out heat preservation calcination for 2-3h, heating to 1300-plus-1320 ℃ in the Ar atmosphere, carrying out heat preservation calcination for 2-3h, finally cooling to 720-plus-750 ℃, introducing air, carrying out heat preservation calcination for 1-2h, wherein the calcination product is the porous nano SiC hollow microspheres.
(2) Adding ethanol solvent, porous nano SiC hollow microspheres and nano Al into a reaction bottle2O3The mass ratio of the two is 4-6:1, the reaction bottle is placed in an ultrasonic treatment instrument, and ultrasonic dispersion is carried out at the temperature of 40-50 DEG CConcentrating the solution under reduced pressure for 1-2h to remove the solvent, drying, placing the solid mixture in an atmosphere resistance furnace, introducing Ar, heating at the rate of 5-10 ℃/min, performing heat preservation and calcination at the temperature of 1420-2O3。
(3) Distilled water and SiC hollow microsphere loaded with nano Al are added into a reaction bottle2O3、FeCl3、BaCl2And LaCl3The mass ratio of the four is 30-40:28-47:3-5:1, polyvinylpyrrolidone is added after stirring and dissolving, then the mixture is stirred at a constant speed for 1-2h, then urea is added, a reaction bottle is placed in an ultrasonic treatment instrument, ultrasonic dispersion treatment is carried out for 2-3h at the temperature of 50-70 ℃, the solution is transferred into a polytetrafluoroethylene reaction kettle and placed in a reaction kettle heating box, the reaction is carried out for 15-20h after heating to the temperature of 150 ℃ and 180 ℃, the solution is cooled to the room temperature, the solvent is removed by filtration, distilled water and ethanol are used for washing a solid product, the solid product is fully dried, the solid product is placed in an atmosphere resistance furnace, the heating rate is 5-10 ℃/min, the heat preservation and the calcination are carried out for 3-4h at the temperature of 1050 ℃ and 1100 ℃, and the calcination product is lanthanum-doped barium ferrite-SiC hollow microspheres loaded with nano Al2O3I.e. barium ferrite-Al2O3-a SiC composite material.
Barium ferrite-Al2O3The preparation method of the porous SiC loaded polyaniline wave-absorbing coating comprises the following steps:
(1) adding ethanol solvent and 6-18 parts of barium ferrite-Al into a reaction bottle2O3Placing a reaction bottle in a constant-temperature water bath, heating to 50-60 ℃, uniformly stirring for reaction for 30-40h, carrying out reduced pressure concentration on the solution to remove the solvent, washing the solid product with distilled water, and preparing the modified barium ferrite-Al2O3-a SiC composite material.
(2) Adding hydrochloric acid solution with the substance amount concentration of 1-1.5mol/L into a reaction bottle, adding 17-19 parts of aniline, 30-33 parts of o-methoxyaniline and 32-34 parts of ammonium persulfate, placing the reaction bottle into a low-temperature cooler, uniformly stirring and reacting for 15-20h at-5-0 ℃, filtering the solution to remove the solvent, washing the solid product with a proper amount of distilled water, and fully drying to prepare the aniline copolymer.
(3) Adding N, N-dimethylformamide solvent, aniline copolymer and modified barium ferrite-Al into a reaction bottle2O3-SiC composite material, placing a reaction bottle in an ultrasonic treatment instrument, performing ultrasonic dispersion treatment for 3-5h at the ultrasonic frequency of 25-35KHz, then stirring at constant speed for 2-4h, adding distilled water into the reaction bottle until a large amount of precipitate is generated, filtering to remove solvent, washing a solid product by using distilled water and ethanol, fully drying, adding a solid product solution in a toluene solvent, controlling the solid-liquid ratio to be 40-60%, then adding 2-5 parts of emulsifier, and stirring at constant speed for 4-6h to prepare barium ferrite-Al2O3Porous SiC loaded polyaniline wave-absorbing coating.
Example 1
(1) Preparing a porous nano SiC hollow microsphere component 1: adding a mixed solvent of distilled water and ethanol into a reaction bottle, adding m-diphenol and paraformaldehyde, stirring at a constant speed until the m-diphenol and the paraformaldehyde are dissolved, placing the reaction bottle into an ultrasonic treatment instrument, performing ultrasonic dispersion treatment at 40 ℃ for 40min, adding an aqueous ammonia solution with the mass fraction of 20%, slowly dropwise adding tetraethoxysilane after stirring at a constant speed for 6h, wherein the mass ratio of the m-diphenol, the paraformaldehyde and the tetraethoxysilane is 1:1.2:6, placing the reaction bottle into a constant-temperature water bath kettle, wherein the constant-temperature water bath kettle comprises a kettle body, the inner part of the kettle body is movably connected with a kettle liner, a cover body is movably connected above the kettle liner, a control panel is arranged on the front surface of the kettle body, a voltage control button is arranged on the outer side of the control panel, a temperature control button is arranged on the outer side of the control panel, a power key is movably connected with the outer side of the control panel, the pot body is cuboid shape and its outside is the design of radius angle, the shape and the size of lid all with pot courage looks adaptation to the cross-sectional shape of lid is isosceles trapezoid, the four corners of pot body bottom all is provided with the cushion, the specification and size homogeneous phase of four cushions is the same and is the stereoplasm rubber material, heat to 40 ℃, at the uniform velocity stirring reaction 25h, with solution through high speed centrifuge remove solvent, use distilled water and ethanol washing solid product, and fully dry, the solid product is arranged in atmosphere resistance furnace, the rate of rise of temperature is forHeating to 550 ℃ at the temperature of 5 ℃/min, carrying out heat preservation calcination for 6h in the air atmosphere, and then carrying out calcination in N2Heating to 620 ℃ in the atmosphere, carrying out heat preservation calcination for 2h, heating to 1300 ℃ in the Ar atmosphere, carrying out heat preservation calcination for 2h, finally cooling to 720 ℃, introducing air, carrying out heat preservation calcination for 1h, wherein the calcination product is the porous nano SiC hollow microsphere component 1.
(2) Preparation of SiC hollow microsphere loaded with nano Al2O3Component 1: adding ethanol solvent, porous nano SiC hollow microsphere component 1 and nano Al into a reaction bottle2O3Placing a reaction bottle in an ultrasonic treatment instrument, performing ultrasonic dispersion treatment at 40 ℃ for 1h, concentrating the solution under reduced pressure to remove the solvent, drying, placing the solid mixture in an atmosphere resistance furnace, introducing Ar, heating at the rate of 5 ℃/min, performing heat preservation and calcination at 1420 ℃ for 3h to obtain a calcined product, namely the SiC hollow microspheres loaded with nano Al2O3And (3) component 1.
(3) Preparation of barium ferrite-Al2O3-SiC composite material 1: distilled water and SiC hollow microsphere loaded with nano Al are added into a reaction bottle2O3Component 1, FeCl3、BaCl2And LaCl3Stirring and dissolving, adding polyvinylpyrrolidone, stirring at a constant speed for 1h, adding urea, placing a reaction bottle in an ultrasonic treatment instrument, performing ultrasonic dispersion treatment at 50 ℃ for 2h, transferring the solution into a polytetrafluoroethylene reaction kettle, placing the reaction kettle in a reaction kettle heating box, heating to 150 ℃ for reaction for 15h, cooling the solution to room temperature, filtering to remove the solvent, washing a solid product with distilled water and ethanol, fully drying, placing the solid product in an atmosphere resistance furnace, heating at a rate of 5 ℃/min, performing heat preservation and calcination at 1050 ℃ for 3h, wherein the calcination product is lanthanum-doped barium ferrite-SiC hollow microspheres loaded with nano Al2O3I.e. barium ferrite-Al2O3-SiC composite 1.
(4) Preparation of modified barium ferrite-Al2O3-SiC composite material 1: adding ethanol solvent and 18 parts of barium ferrite-Al into a reaction bottle2O31 part of-SiC composite material and 1 part of silane coupling agent which is N- (beta-aminoethyl) -gamma-aminopropyl trimethoxy siliconAlkane, placing the reaction bottle in a constant-temperature water bath kettle, heating to 50 ℃, uniformly stirring for reaction for 30 hours, decompressing and concentrating the solution to remove the solvent, washing the solid product with distilled water, and preparing the modified barium ferrite-Al2O3-SiC composite 1.
(5) Preparation of aniline copolymer component 1: adding a hydrochloric acid solution with the substance amount concentration of 1mol/L into a reaction bottle, adding 17 parts of aniline, 30-o-methoxyaniline and 32 parts of ammonium persulfate, placing the reaction bottle in a low-temperature cooling instrument, stirring at a constant speed at 0 ℃ for reaction for 15 hours, filtering the solution to remove a solvent, washing a solid product with a proper amount of distilled water, and fully drying to prepare the aniline copolymer component 1.
(6) The barium ferrite-Al is prepared2O3Porous SiC-loaded polyaniline wave-absorbing coating 1: adding N, N-dimethylformamide solvent, aniline copolymer component 1 and modified barium ferrite-Al into a reaction bottle2O3Placing a reaction bottle in an ultrasonic treatment instrument, performing ultrasonic dispersion treatment for 3 hours at the ultrasonic frequency of 25KHz, then stirring at a constant speed for 2 hours, adding distilled water into the reaction bottle until a large amount of precipitate is generated, filtering to remove the solvent, washing the solid product with distilled water and ethanol, fully drying, adding the solid product solution in a toluene solvent, controlling the solid-liquid ratio to be 40%, then adding 2 parts of emulsifier, and stirring at a constant speed for 4 hours to prepare the barium ferrite-Al composite material 12O3Porous SiC-loaded polyaniline wave-absorbing coating 1.
Example 2
(1) Preparing a porous nano SiC hollow microsphere component 2: adding a mixed solvent of distilled water and ethanol into a reaction bottle, adding m-diphenol and paraformaldehyde, stirring at a constant speed until the m-diphenol and the paraformaldehyde are dissolved, placing the reaction bottle into an ultrasonic treatment instrument, performing ultrasonic dispersion treatment at 40 ℃ for 40min, adding an ammonia water solution with the mass fraction of 20%, slowly dropwise adding ethyl orthosilicate after stirring at a constant speed for 6h, wherein the mass ratio of the m-diphenol, the paraformaldehyde and the ethyl orthosilicate is 1:1.2:6, placing the reaction bottle into a constant-temperature water bath kettle, wherein the constant-temperature water bath kettle comprises a kettle body, the interior of the kettle body is movably connected with a kettle liner, and the upper part of the kettle liner is movably connected with the kettle linerThe pot body is movably connected with a cover body, a control panel is arranged on the front face of the pot body, a voltage control button is arranged on the outer side of the control panel, a temperature control button is arranged on the outer side of the control panel, a power key is movably connected to the outer side of the control panel, the pot body is in a cuboid shape, the outer side of the pot body is in a fillet design, the shape and the size of the cover body are matched with those of a pot liner, the cross section of the cover body is in an isosceles trapezoid shape, cushion blocks are arranged on four corners of the bottom of the pot body, the four cushion blocks are identical in specification and size and made of hard rubber materials, the temperature is heated to 40 ℃, the solution is stirred at a constant speed for reaction for 25 hours, the solvent is removed through a high-speed centrifugal machine, the solid product is washed by using distilled water and ethanol and is fully dried, the solid product is placed in an atmosphere resistance furnace, the heating rate is 5 ℃/min, the temperature is increased to 550 ℃, the temperature is kept and calcined for 6 hours in the air atmosphere, and then the N is carried out2Heating to 620 ℃ in the atmosphere, carrying out heat preservation calcination for 2h, heating to 1300 ℃ in the Ar atmosphere, carrying out heat preservation calcination for 2h, finally cooling to 720 ℃, introducing air, carrying out heat preservation calcination for 1h, wherein the calcination product is the porous nano SiC hollow microsphere component 2.
(2) Preparation of SiC hollow microsphere loaded with nano Al2O3And (2) component: adding ethanol solvent, porous nano SiC hollow microsphere component 2 and nano Al into a reaction bottle2O3Placing a reaction bottle in an ultrasonic treatment instrument, performing ultrasonic dispersion treatment at 40 ℃ for 1h, concentrating the solution under reduced pressure to remove the solvent, drying, placing the solid mixture in an atmosphere resistance furnace, introducing Ar, heating at the rate of 5 ℃/min, performing heat preservation and calcination at 1420 ℃ for 3h to obtain a calcined product, namely the SiC hollow microspheres loaded with nano Al2O3And (3) component 2.
(3) Preparation of barium ferrite-Al2O3-SiC composite 2: distilled water and SiC hollow microsphere loaded with nano Al are added into a reaction bottle2O3Component 2, FeCl3、BaCl2And LaCl3The mass ratio of the four is 40:28:5:1, the polyvinylpyrrolidone is added after stirring and dissolving, the uniform stirring is carried out for 1h, then the urea is added, the reaction bottle is placed in an ultrasonic treatment instrument, the ultrasonic dispersion treatment is carried out for 2h at the temperature of 70 ℃, the solution is transferred into a polytetrafluoroethylene reaction kettle and placed in a reaction kettle heating box, and the heating is carried out until the solution is heated to the temperature of 40:28:5:1Reacting for 20 hours at 180 ℃, cooling the solution to room temperature, filtering to remove the solvent, washing the solid product with distilled water and ethanol, fully drying, placing the solid product in an atmosphere resistance furnace, heating at a rate of 10 ℃/min, carrying out heat preservation calcination at 1050 ℃ for 4 hours, wherein the calcination product is lanthanum-doped barium ferrite-SiC hollow microspheres loaded with nano Al2O3I.e. barium ferrite-Al2O3-SiC composite 2.
(4) Preparation of modified barium ferrite-Al2O3-SiC composite 2: adding ethanol solvent and 15 parts of barium ferrite-Al into a reaction bottle2O3Placing a reaction bottle in a constant-temperature water bath kettle, heating to 60 ℃, uniformly stirring for reaction for 30 hours, carrying out reduced pressure concentration on the solution to remove the solvent, washing the solid product with distilled water, and preparing the modified barium ferrite-Al2O3-SiC composite 2.
(5) Preparation of aniline copolymer component 2: adding a hydrochloric acid solution with the substance amount concentration of 1.5mol/L into a reaction bottle, adding 17.5 parts of aniline, 31-o-methoxyaniline and 32.5 parts of ammonium persulfate, placing the reaction bottle in a low-temperature cooling instrument, uniformly stirring and reacting at 0 ℃ for 15 hours, filtering the solution to remove the solvent, washing the solid product with a proper amount of distilled water, and fully drying to prepare the aniline copolymer component 2.
(6) The barium ferrite-Al is prepared2O3Porous SiC-loaded polyaniline wave-absorbing coating 2: adding N, N-dimethylformamide solvent, aniline copolymer component 2 and modified barium ferrite-Al into a reaction bottle2O3Placing a reaction bottle in an ultrasonic treatment instrument, performing ultrasonic dispersion treatment for 3 hours at the ultrasonic frequency of 35KHz, then stirring at a constant speed for 4 hours, adding distilled water into the reaction bottle until a large amount of precipitate is generated, filtering to remove the solvent, washing the solid product with distilled water and ethanol, fully drying, adding the solid product solution into a toluene solvent, controlling the solid-liquid ratio to be 45%, then adding 2.5 parts of emulsifier, and stirring at a constant speed for 6 hours to prepare the barium ferrite-Al composite material 22O3Porous SiC-loaded polyaniline wave-absorbing coatingAnd (3) feeding 2.
Example 3
(1) Preparing a porous nano SiC hollow microsphere component 3: adding a mixed solvent of distilled water and ethanol into a reaction bottle, adding m-diphenol and paraformaldehyde, stirring at a constant speed until the m-diphenol and the paraformaldehyde are dissolved, placing the reaction bottle into an ultrasonic treatment instrument, performing ultrasonic dispersion treatment at 45 ℃ for 50min, adding an ammonia water solution with the mass fraction of 22%, wherein the volume ratio of the distilled water, the ethanol and the ammonia water solution is 23:3.5:1, stirring at a constant speed for 7h, slowly dropwise adding tetraethoxysilane, wherein the mass ratio of the m-diphenol, the paraformaldehyde and the tetraethoxysilane is 1:1.4:6.5, placing the reaction bottle into a constant-temperature water bath kettle, wherein the constant-temperature water bath kettle comprises a kettle body, the inner part of the kettle body is movably connected with a kettle liner, a cover body is movably connected above the kettle liner, a control panel is arranged on the front surface of the kettle body, a voltage control button is arranged on the outer side of the control panel, a temperature control button is arranged on the outer side of the control panel, a power key is movably connected with the control panel, the pot body is in a cuboid shape, the outer side of the pot body is designed to be a fillet, the shape and the size of the cover body are matched with the pot liner, the cross section of the cover body is in an isosceles trapezoid shape, cushion blocks are arranged at four corners of the bottom of the pot body, the four cushion blocks are identical in specification and size and made of hard rubber materials, the pot body is heated to 45 ℃, the pot body is stirred at a constant speed for reaction for 28 hours, a solution is subjected to solvent removal through a high-speed centrifuge, a solid product is washed by using distilled water and ethanol and is fully dried, the solid product is placed in an atmosphere resistance furnace, the heating rate is 8 ℃/min, the temperature is increased to 560 ℃, the pot body is subjected to heat preservation and calcination for 7 hours in the air atmosphere, and then the pot body is subjected to N-phase reaction2Heating to 635 ℃ in the atmosphere, carrying out heat preservation calcination for 2.5h, heating to 1310 ℃ in the Ar atmosphere, carrying out heat preservation calcination for 2.5h, finally cooling to 740 ℃, introducing air, carrying out heat preservation calcination for 1.5h, wherein the calcination product is a porous nano SiC hollow microsphere component 3.
(2) Preparation of SiC hollow microsphere loaded with nano Al2O3And (3) component: adding ethanol solvent, porous nano SiC hollow microsphere component 3 and nano Al into a reaction bottle2O3Placing the reaction bottle in an ultrasonic treatment instrument, performing ultrasonic dispersion treatment at 45 deg.C for 1.5 hr, concentrating the solution under reduced pressure to remove solvent, drying, placing the solid mixture in an atmosphere resistorIntroducing Ar into the furnace, heating up at the rate of 8 ℃/min, and calcining at 1440 ℃ for 3.5h in a heat preservation way, wherein the calcined product is SiC hollow microspheres loaded with nano Al2O3And (3) component.
(3) Preparation of barium ferrite-Al2O3-SiC composite 3: distilled water and SiC hollow microsphere loaded with nano Al are added into a reaction bottle2O3Component 3, FeCl3、BaCl2And LaCl3The mass ratio of the four is 35:38:3.5:1, polyvinylpyrrolidone is added after stirring and dissolving, then the mixture is stirred at a constant speed for 1.5h, then urea is added, a reaction bottle is placed in an ultrasonic treatment instrument, ultrasonic dispersion treatment is carried out for 2.5h at the temperature of 60 ℃, the solution is transferred into a polytetrafluoroethylene reaction kettle and placed in a reaction kettle heating box, the reaction is carried out for 18h after heating to the temperature of 160 ℃, the solution is cooled to the room temperature, the solvent is removed by filtration, the solid product is washed by distilled water and ethanol and is fully dried, the solid product is placed in an atmosphere resistance furnace, the heating rate is 7 ℃/min, the heat preservation and calcination are carried out for 3.5h at the temperature of 1080 ℃, and the calcination product is lanthanum-doped barium ferrite-SiC hollow microspheres loaded with nano Al2O3I.e. barium ferrite-Al2O3-SiC composite 3.
(4) Preparation of modified barium ferrite-Al2O3-SiC composite 3: adding ethanol solvent and 12.5 parts of barium ferrite-Al into a reaction bottle2O33 parts of-SiC composite material and 2 parts of silane coupling agent N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, placing the reaction bottle in a constant-temperature water bath, heating to 55 ℃, uniformly stirring for reaction for 35 hours, decompressing and concentrating the solution to remove the solvent, washing the solid product with distilled water, and preparing the modified barium ferrite-Al2O3-SiC composite 3.
(5) Preparation of aniline copolymer component 3: adding a hydrochloric acid solution with the substance amount concentration of 1.2mol/L into a reaction bottle, adding 18 parts of aniline, 31-o-methoxyaniline and 33 parts of ammonium persulfate, placing the reaction bottle in a low-temperature cooling instrument, stirring at a constant speed at-2 ℃ for reacting for 18 hours, filtering the solution to remove the solvent, washing the solid product with a proper amount of distilled water, and fully drying to prepare the aniline copolymer component 3.
(6) The barium ferrite-Al is prepared2O3Porous SiC-loaded polyaniline wave-absorbing coating 3: adding N, N-dimethylformamide solvent, aniline copolymer component 3 and modified barium ferrite-Al into a reaction bottle2O3-SiC composite material 3, placing a reaction bottle in an ultrasonic treatment instrument, performing ultrasonic dispersion treatment for 4 hours at the ultrasonic frequency of 30KHz, then stirring at a constant speed for 3 hours, adding distilled water into the reaction bottle until a large amount of precipitate is generated, filtering to remove the solvent, washing the solid product with distilled water and ethanol, fully drying, adding the solid product solution into a toluene solvent, controlling the solid-liquid ratio to be 50%, then adding 3.5 parts of emulsifier, and stirring at a constant speed for 5 hours to prepare barium ferrite-Al2O3And a porous SiC-loaded polyaniline wave-absorbing coating 3.
Example 4
(1) Preparing a porous nano SiC hollow microsphere component 4: adding a mixed solvent of distilled water and ethanol into a reaction bottle, adding m-diphenol and paraformaldehyde, stirring at a constant speed until the m-diphenol and the paraformaldehyde are dissolved, placing the reaction bottle into an ultrasonic treatment instrument, performing ultrasonic dispersion treatment at 50 ℃ for 40min, adding an ammonia water solution with the mass fraction of 25%, slowly dropwise adding tetraethoxysilane after stirring at a constant speed for 6h, wherein the mass ratio of the m-diphenol, the paraformaldehyde and the tetraethoxysilane is 1:1.5:7, placing the reaction bottle into a constant-temperature water bath kettle, which comprises a kettle body, wherein the inner part of the kettle body is movably connected with a kettle liner, a cover body is movably connected above the kettle liner, a control panel is arranged on the front surface of the kettle body, a voltage control button is arranged on the outer side of the control panel, a temperature control button is arranged on the outer side of the control panel, and a power key is movably connected on the outer side of the control panel, the pot body is cuboid shape and its outside is the design of radius angle, the shape and the size of lid all with pot courage looks adaptation to the cross-sectional shape of lid is isosceles trapezoid, the four corners of pot body bottom all is provided with the cushion, the specification and size of four cushions are the same and are the rigid rubber material, heat to 40 ℃, at the uniform velocity stirring reaction 25h, pass through high speed centrifuge with solution and remove the solvent, use distilled water and ethanol washing solid product, and fully dry, solid product is arranged in atmosphere resistance furnace, the rate of rise of temperature is 5 DEG CHeating to 580 deg.C for 8h in air atmosphere, calcining in N2Heating to 650 ℃ in the atmosphere, carrying out heat preservation calcination for 2h, heating to 1320 ℃ in the Ar atmosphere, carrying out heat preservation calcination for 3h, finally cooling to 720 ℃, introducing air, carrying out heat preservation calcination for 2h, wherein the calcination product is a porous nano SiC hollow microsphere component 4.
(2) Preparation of SiC hollow microsphere loaded with nano Al2O3And (4) component: adding ethanol solvent, porous nano SiC hollow microsphere component 4 and nano Al into a reaction bottle2O3Placing a reaction bottle in an ultrasonic treatment instrument, performing ultrasonic dispersion treatment at 50 ℃ for 1h, concentrating the solution under reduced pressure to remove the solvent, drying, placing the solid mixture in an atmosphere resistance furnace, introducing Ar, heating at the rate of 10 ℃/min, performing heat preservation and calcination at 1420 ℃ for 4h to obtain a calcined product, namely the SiC hollow microspheres loaded with nano Al2O3And (4) component.
(3) Preparation of barium ferrite-Al2O3-SiC composite 4: distilled water and SiC hollow microsphere loaded with nano Al are added into a reaction bottle2O3Component 4, FeCl3、BaCl2And LaCl3Stirring and dissolving, adding polyvinylpyrrolidone, stirring at a constant speed for 2 hours, adding urea, placing a reaction bottle in an ultrasonic treatment instrument, performing ultrasonic dispersion treatment at 70 ℃ for 2 hours, transferring the solution into a polytetrafluoroethylene reaction kettle, placing the reaction kettle in a reaction kettle heating box, heating to 180 ℃ for reaction for 15 hours, cooling the solution to room temperature, filtering to remove the solvent, washing a solid product with distilled water and ethanol, fully drying, placing the solid product in an atmosphere resistance furnace, heating at a rate of 5 ℃/min, performing heat preservation and calcination at 1100 ℃ for 4 hours, wherein the calcination product is lanthanum-doped barium ferrite-SiC hollow microspheres loaded with nano Al2O3I.e. barium ferrite-Al2O3-SiC composite 4.
(4) Preparation of modified barium ferrite-Al2O3-SiC composite 4: adding ethanol solvent and 9.5 parts of barium ferrite-Al into a reaction bottle2O34 portions of-SiC composite material and 2.5 portions of silane coupling agent which is N- (beta-aminoethyl) -gamma-aminopropyl trimethoxy silanePlacing a reaction bottle in a constant-temperature water bath kettle, heating to 60 ℃, stirring at a constant speed for reaction for 30 hours, decompressing and concentrating the solution to remove the solvent, washing the solid product with distilled water, and preparing the modified barium ferrite-Al2O3-SiC composite 4.
(5) Preparation of aniline copolymer component 4: adding a hydrochloric acid solution with the substance amount concentration of 1mol/L into a reaction bottle, adding 18.5 parts of aniline, 32 o-methoxyaniline and 33.5 parts of ammonium persulfate, placing the reaction bottle in a low-temperature cooler, uniformly stirring at 0 ℃ for reaction for 15 hours, filtering the solution to remove the solvent, washing the solid product with a proper amount of distilled water, and fully drying to prepare the aniline copolymer component 4.
(6) The barium ferrite-Al is prepared2O3Porous SiC-loaded polyaniline wave-absorbing coating 4: adding N, N-dimethylformamide solvent, aniline copolymer component 4 and modified barium ferrite-Al into a reaction bottle2O3-SiC composite material 4, placing a reaction bottle in an ultrasonic treatment instrument, performing ultrasonic dispersion treatment for 5 hours at the ultrasonic frequency of 30KHz, then stirring at a constant speed for 4 hours, adding distilled water into the reaction bottle until a large amount of precipitate is generated, filtering to remove the solvent, washing the solid product with distilled water and ethanol, fully drying, adding the solid product solution in a toluene solvent, controlling the solid-liquid ratio to be 55%, then adding 4 parts of emulsifier, and stirring at a constant speed for 6 hours to prepare barium ferrite-Al2O3And a porous SiC-loaded polyaniline wave-absorbing coating 4.
Example 5
(1) Preparing a porous nano SiC hollow microsphere component 5: adding a mixed solvent of distilled water and ethanol into a reaction bottle, adding m-diphenol and paraformaldehyde, stirring at a constant speed until the m-diphenol and the paraformaldehyde are dissolved, placing the reaction bottle into an ultrasonic treatment instrument, performing ultrasonic dispersion treatment at 50 ℃ for 60min, adding an ammonia water solution with the mass fraction of 25%, wherein the volume ratio of the distilled water to the ethanol to the ammonia water solution is 26:4:1, stirring at a constant speed for 8h, slowly dropwise adding ethyl orthosilicate, wherein the mass ratio of the m-diphenol to the paraformaldehyde to the ethyl orthosilicate is 1:1.5:7, placing the reaction bottle into a constant-temperature water bath kettle, wherein the constant-temperature water bath kettle comprises a kettle body, the inner part of the kettle body is movably connected with a kettle liner, and the upper part of the kettle liner is arranged in the constant-temperature water bath kettleA cover body is movably connected, a control panel is arranged on the front surface of the pot body, a voltage control button is arranged on the outer side of the control panel, a temperature control button is arranged on the outer side of the control panel, a power key is movably connected on the outer side of the control panel, the pot body is cuboid-shaped, the outer side of the pot body is in a fillet design, the shape and the size of the cover body are matched with the pot liner, the cross section of the cover body is isosceles trapezoid, the four corners of the bottom of the pot body are provided with cushion blocks, the four cushion blocks have the same specification and size and are made of hard rubber materials, the mixture is heated to 50 ℃, stirred at a constant speed for reaction for 30 hours, the solution is passed through a high-speed centrifuge to remove the solvent, distilled water and ethanol are used for washing the solid product, and fully drying, placing the solid product in an atmosphere resistance furnace, heating to 580 ℃ at the heating rate of 10 ℃/min, carrying out heat preservation and calcination for 8h in the air atmosphere, and then carrying out N reaction.2Heating to 650 ℃ in the atmosphere, carrying out heat preservation calcination for 3h, heating to 1320 ℃ in the Ar atmosphere, carrying out heat preservation calcination for 3h, finally cooling to 750 ℃, introducing air, carrying out heat preservation calcination for 2h, wherein the calcination product is the porous nano SiC hollow microsphere component 5.
(2) Preparation of SiC hollow microsphere loaded with nano Al2O3And (5) component: adding ethanol solvent, porous nano SiC hollow microsphere component 5 and nano Al into a reaction bottle2O3Placing a reaction bottle in an ultrasonic treatment instrument, performing ultrasonic dispersion treatment at 50 ℃ for 2h, concentrating the solution under reduced pressure to remove the solvent, drying, placing the solid mixture in an atmosphere resistance furnace, introducing Ar, heating at a rate of 10 ℃/min, performing heat preservation and calcination at 1460 ℃ for 4h to obtain a calcined product, namely the SiC hollow microsphere loaded nano Al2O3And (5) component.
(3) Preparation of barium ferrite-Al2O3-SiC composite 5: distilled water and SiC hollow microsphere loaded with nano Al are added into a reaction bottle2O3Component 5, FeCl3、BaCl2And LaCl3The mass ratio of the four is 40:47:5:1, the polyvinylpyrrolidone is added after stirring and dissolving, the mixture is stirred at a constant speed for 2 hours, then the urea is added, the reaction bottle is placed in an ultrasonic treatment instrument, ultrasonic dispersion treatment is carried out for 3 hours at the temperature of 70 ℃, the solution is transferred into a polytetrafluoroethylene reaction kettle and placed in a reaction kettle heating box, and heating is carried outReacting for 20h at 180 ℃, cooling the solution to room temperature, filtering to remove the solvent, washing the solid product with distilled water and ethanol, fully drying, placing the solid product in an atmosphere resistance furnace, heating at a rate of 10 ℃/min, and calcining at 1100 ℃ for 4h while keeping the temperature, wherein the calcined product is lanthanum-doped barium ferrite-SiC hollow microspheres loaded with nano Al2O3I.e. barium ferrite-Al2O3-SiC composite 5.
(4) Preparation of modified barium ferrite-Al2O3-SiC composite 5: adding ethanol solvent and 6 parts of barium ferrite-Al into a reaction bottle2O35 parts of-SiC composite material and 3 parts of silane coupling agent N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, placing a reaction bottle in a constant-temperature water bath, heating to 60 ℃, uniformly stirring for reaction for 40 hours, decompressing and concentrating the solution to remove the solvent, washing the solid product with distilled water, and preparing the modified barium ferrite-Al2O3-SiC composite 5.
(5) Preparation of aniline copolymer component 5: adding a hydrochloric acid solution with the substance amount concentration of 1.5mol/L into a reaction bottle, adding 19 parts of aniline, 33 o-methoxyaniline and 34 parts of ammonium persulfate, placing the reaction bottle in a low-temperature cooling instrument, stirring at a constant speed at-5 ℃ for reaction for 20 hours, filtering the solution to remove the solvent, washing the solid product with a proper amount of distilled water, and fully drying to prepare the aniline copolymer component 5.
(6) The barium ferrite-Al is prepared2O3Porous SiC-loaded polyaniline wave-absorbing coating 5: adding N, N-dimethylformamide solvent, aniline copolymer component 5 and modified barium ferrite-Al into a reaction bottle2O3-SiC composite material 5, placing a reaction bottle in an ultrasonic treatment instrument, performing ultrasonic dispersion treatment for 5 hours at the ultrasonic frequency of 35KHz, then stirring at a constant speed for 4 hours, adding distilled water into the reaction bottle until a large amount of precipitate is generated, filtering to remove the solvent, washing the solid product with distilled water and ethanol, fully drying, adding the solid product solution in a toluene solvent, controlling the solid-liquid ratio to be 60%, then adding 5 parts of emulsifier, and stirring at a constant speed for 6 hours to prepare barium ferrite-Al2O3And the polyaniline wave-absorbing coating 5 is loaded with porous SiC.
Barium ferrite-Al in the examples2O31-5 of the porous SiC-loaded polyaniline wave-absorbing coating is cured to form a film, the film is cut into an annular film with the thickness of 3mm, and an E5071C network analyzer is used for testing the wave-absorbing performance and the electromagnetic shielding performance of the film material, wherein the test standard is GB/T35575-2017.
In summary, the barium ferrite-Al2O3The polyaniline wave-absorbing coating loaded with porous SiC, resorcinol and paraformaldehyde and formed phenolic aldehyde oligomer as hollow templates and pore-making agents are prepared into porous nano SiC hollow microspheres by a high-temperature carbonization method, the surfaces of the porous nano SiC hollow microspheres have rich mesoporous structures and huge specific surface areas, the dielectric constant of SiC is very high, Al is added into the porous nano SiC hollow microspheres2O3Has excellent electrical insulation and low dielectric loss, Al2O3The composite material is loaded on the surface of the SiC hollow microsphere to generate a large amount of electric dipole moment, so that the interface polarization capability is enhanced, the impedance matching performance and the wave absorbing performance of the SiC are improved, and the SiC hollow microsphere structure can reflect electromagnetic waves for multiple times and has the effect of losing the electromagnetic waves.
The barium ferrite is spinel type ferrite, the barium ferrite forms hexagonal system ferrite with better wave-absorbing performance by doping lanthanum, the lanthanum has good electromagnetic structure and property, the anisotropic field and the electromagnetic parameters of the barium ferrite magnetic crystal are adjusted, the saturation magnetization intensity of the barium ferrite is improved, the coercive force is reduced, the magnetic conductivity and the magnetic loss capability of the barium ferrite are improved, and the lanthanum doping enables the barium ferrite to form a three-dimensional conductive network on the surface of the SiC hollow microsphere, so that the leakage loss can be generated to effectively attenuate electromagnetic waves.
Silane coupling agent N- (beta-aminoethyl) -gamma-aminopropyl trimethoxy silane and Al2O3The hydroxyl on the surface is bonded, and the amino and imino in the silane coupling agent and the imino in the polyaniline form hydrogen bonds and van der Waals force, so that the barium ferrite-Al is greatly improved2O3The dispersibility and the compatibility of the-SiC composite material in polyaniline avoid barium ferrite-Al2O3the-SiC composite material is agglomerated and agglomerated, so that the electromagnetic loss capacity and the wave absorbing performance of the polyaniline are enhanced.
Claims (1)
1. Barium ferrite-Al2O3The porous SiC loaded polyaniline wave-absorbing coating comprises the following formula raw materials in parts by weight, and is characterized in that: 6-18 parts of barium ferrite-Al2O3-SiC composite material, 1-3 parts of silane coupling agent, 32-34 parts of ammonium persulfate, 17-19 parts of aniline, 30-33 parts of o-anisidine and 2-5 parts of emulsifier;
the silane coupling agent isN- (β -aminoethyl) - γ -aminopropyltrimethoxysilane;
the emulsifier is dodecyl benzene sulfonic acid;
the barium ferrite-Al2O3The preparation method of the-SiC composite material comprises the following steps:
(1) adding resorcinol and paraformaldehyde into a mixed solvent of distilled water and ethanol, stirring at a constant speed until the mixture is dissolved, performing ultrasonic dispersion treatment on the solution at 40-50 ℃ for 40-60min, then adding an ammonia water solution with the mass fraction of 20-25%, wherein the volume ratio of the distilled water, the ethanol and the ammonia water solution is 20-26:3-4:1, stirring at a constant speed for 6-8h, slowly dropwise adding tetraethoxysilane, heating the solution to 40-50 ℃ in a constant-temperature water bath, reacting for 25-30h, removing the solvent from the solution, washing a solid product, drying, placing the solid product into an atmosphere resistance furnace, heating at the rate of 5-10 ℃/min, heating to 550 ℃ and 580 ℃, performing heat preservation and calcination in an air atmosphere for 6-8h, and then performing N-substituted phenol-N-substituted phenol-substituted formaldehyde-added with the mixture of the same solvent2Heating to 650 ℃ in 620-plus-one atmosphere, carrying out heat preservation calcination for 2-3h, heating to 1320 ℃ in 1300-plus-one atmosphere in Ar atmosphere, carrying out heat preservation calcination for 2-3h, finally cooling to 750 ℃ in 720-plus-one atmosphere, introducing air, carrying out heat preservation calcination for 1-2h, wherein the calcination product is porous nano SiC hollow microspheres;
(2) adding porous nano SiC hollow microspheres and nano Al into ethanol solvent2O3Ultrasonic dispersing the solution at 40-50 deg.C for 1-2 hr, removing solvent from the solution, drying, and placing the solid mixture in atmosphereIntroducing Ar into the resistance furnace, heating at the rate of 5-10 ℃/min, carrying out heat preservation and calcination at the temperature of 1420-1460 ℃ for 3-4h to obtain a calcined product which is SiC hollow microsphere loaded with nano Al2O3；
(3) Adding SiC hollow microspheres loaded with nano Al into distilled water2O3、FeCl3、BaCl2And LaCl3Stirring and dissolving, adding polyvinylpyrrolidone, stirring at constant speed for 1-2h, adding urea, performing ultrasonic dispersion treatment on the solution at 50-70 ℃ for 2-3h, transferring the solution into a hydrothermal reaction kettle, heating to 150-2O3I.e. barium ferrite-Al2O3-a SiC composite;
the constant-temperature water bath kettle comprises a kettle body (1), a kettle liner (2) is movably connected inside the kettle body (1), a cover body (3) is movably connected above the kettle liner (2), a control panel (4) is arranged on the front side of the kettle body (1), a voltage control button (5) is arranged on the outer side of the control panel (4), a temperature control button (6) is arranged on the outer side of the control panel (4), a power key (7) is movably connected on the outer side of the control panel (4), the kettle body (1) is cuboid-shaped, the outer side of the kettle body is in a chamfered angle design, the shape and the size of the cover body (3) are matched with the kettle liner (2), the cross section of the cover body (3) is isosceles trapezoid, cushion blocks are arranged at four corners of the bottom of the kettle body (1), and the four cushion blocks are identical in specification and size and are made of hard rubber;
the mass ratio of the m-diphenol, the paraformaldehyde and the ethyl orthosilicate is 1:1.2-1.5: 6-7;
the porous nano SiC hollow microspheres and nano Al2O3The mass ratio is 4-6: 1;
the SiC hollow microspheres load nano Al2O3、FeCl3、BaCl2And LaCl3Four, theThe mass ratio is 30-40:28-47:3-5: 1;
the barium ferrite-Al2O3The preparation method of the porous SiC loaded polyaniline wave-absorbing coating comprises the following steps:
(1) adding 6-18 parts of barium ferrite-Al into an ethanol solvent2O3-SiC composite material and 1-3 parts of silane coupling agentNHeating the solution to 50-60 ℃ to react for 30-40h, removing the solvent from the solution, washing a solid product and drying to prepare the modified barium ferrite-Al2O3-a SiC composite;
(2) adding 17-19 parts of aniline, 30-33 parts of o-anisidine and 32-34 parts of ammonium persulfate into a hydrochloric acid solution with the mass concentration of 1-1.5mol/L, reacting the solution at-5-0 ℃ for 15-20h, removing the solvent from the solution, washing a solid product, and fully drying to prepare an aniline copolymer;
(3) to the direction ofN,NAdding aniline copolymer and modified barium ferrite-Al into dimethylformamide solvent2O3-SiC composite material, carrying out ultrasonic dispersion treatment on the solution for 3-5h with ultrasonic frequency of 25-35KHz, then stirring at constant speed for 2-4h, adding distilled water into the solution until a large amount of precipitate is generated, filtering to remove the solvent, washing the solid product, drying, dissolving the solid product in toluene solvent, controlling the solid-to-liquid ratio to be 40-60%, then adding 2-5 parts of emulsifier, and stirring at constant speed for 4-6h to prepare barium ferrite-Al2O3Porous SiC loaded polyaniline wave-absorbing coating.
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