CN111647272A - High-thermal-conductivity modified silicone rubber composite wave-absorbing material and preparation method thereof - Google Patents
High-thermal-conductivity modified silicone rubber composite wave-absorbing material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of wave-absorbing materials, and discloses a high-thermal-conductivity modified silicone rubber composite wave-absorbing material which comprises the following formula raw materials and components: barium-cobalt ferrite-carbon nanotube composite material, silane coupling agent, hydroxyl silicone oil, cross-linking agent and catalyst. According to the high-heat-conductivity modified silicon rubber composite wave-absorbing material, lanthanum is doped to replace partial crystal lattices of barium, the dielectric constant and saturation magnetization of lanthanum-doped barium-cobalt ferrite are large, magnetic loss and dielectric loss are generated on electromagnetic waves, a carbon nano tube forms a micro three-dimensional conductive network to generate leakage conduction loss, the impedance matching performance of the material is enhanced under the combined action of the lanthanum-doped barium-cobalt ferrite and the carbon nano tube, a polysiloxane coating layer and hydroxyl silicone oil have good compatibility, the dispersity and compatibility of the barium-cobalt ferrite-carbon nano tube composite material in silicon rubber are improved, and the wave-absorbing performance, the thermal diffusion coefficient and the heat conductivity of a silicon rubber material are improved.
Description
Technical Field
The invention relates to the technical field of wave-absorbing materials, in particular to a high-thermal-conductivity modified silicone rubber composite wave-absorbing material and a preparation method thereof.
Background
The electromagnetic wave is an electromagnetic field propagated in a wave form, the electromagnetic wave is one kind of energy, objects generally higher than absolute zero release the electromagnetic wave, the higher the temperature is, the shorter the wavelength of the emitted electromagnetic wave is, the electromagnetic wave has electromagnetic radiation characteristics including radio wave, microwave, infrared ray, visible light, ultraviolet ray, X ray, gamma ray and the like, the electromagnetic radiation is a way of transferring energy, the radiation types can be free radiation, non-free radiation with thermal effect, non-free radiation without thermal effect and base station electromagnetic wave are not free radiation wave, the long-term electromagnetic radiation can cause harm to human immune function, reproductive system, cardiovascular system and the like, can cause human metabolism disorder, immunity reduction even induce various cancers and the like, and the electromagnetic wave can act with the electronic component to generate the interfered phenomenon, which affects the normal operation of the electronic device.
The wave-absorbing material can absorb or weaken the electromagnetic wave energy projected on the surface of the wave-absorbing material so as to reduce the interference of the electromagnetic wave, the loss mechanism of the wave-absorbing material is divided into resistance type loss, dielectric loss and magnetic loss, ferrite wave-absorbing materials such as barium ferrite, manganese zinc ferrite, cobalt ferrite and the like have excellent performance, have the characteristics of high absorption frequency band, high absorption rate, thin matching thickness and the like, the ferrite wave-absorbing material is applied to electronic equipment to absorb the electromagnetic radiation and play a role in eliminating the electromagnetic interference, the silicon rubber has good electrical insulation, oxidation resistance, aging resistance, light resistance, mildew resistance, chemical stability and the like, and has wide application in the fields of medical supplies, automobile manufacturing, electronic appliances and the like, but the current silicon rubber does not have the wave-absorbing performance, has poor absorption and shielding performance on the electromagnetic wave, and greatly reduces the practicability of the silicon rubber material, and the dispersibility and poor compatibility of inorganic wave-absorbing materials such as ferrite and the like in the silicon rubber can influence the mechanical properties of the silicon rubber material.
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a high-thermal-conductivity modified silicon rubber composite wave-absorbing material and a preparation method thereof, which solve the problem of poor wave-absorbing performance of silicon rubber and solve the problem of poor dispersibility and compatibility of a ferrite inorganic wave-absorbing material in the silicon rubber.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: a high-thermal-conductivity modified silicone rubber composite wave-absorbing material comprises the following formula raw materials in parts by weight: 2-6 parts of barium-cobalt ferrite-carbon nanotube composite material, 6-16 parts of silane coupling agent, 69-86 parts of hydroxyl silicone oil, 4-6 parts of cross-linking agent and 2-3 parts of catalyst.
Preferably, the silane coupling agent is vinyltriethoxysilane.
Preferably, the cross-linking agent is tetraethoxysilane.
Preferably, the catalyst is dibutyltin dilaurate.
Preferably, the preparation method of the barium-cobalt ferrite-carbon nanotube composite material comprises the following steps:
(1) adding carboxylated carbon nano tube and Ba (NO) into a reaction bottle3)2、CoCl2、FeCl3And La (NO)3)3Placing the reaction bottle into an ultrasonic treatment instrument after uniformly stirring, carrying out ultrasonic dispersion treatment for 20-40min at 40-50 ℃, adding a dispersing agent citric acid, carrying out ultrasonic dispersion treatment for 1-2h, placing the reaction bottle into a constant-temperature water bath kettle, heating to 50-70 ℃, carrying out uniform stirring reaction for 4-8h, adding ammonia water to adjust the pH value of the solution to be neutral, carrying out uniform stirring to form sol, placing the reaction bottle into an oven, and drying water to prepare the gel precursor.
(2) Placing the gel precursor in a resistance furnace, heating the gel precursor at the rate of 5-10 ℃/min, carrying out heat treatment at the temperature of 520-550 ℃ for 1-2h, heating the gel precursor to 1260-1300 ℃, carrying out heat preservation and calcination for 6-8h, washing the calcination product with distilled water, drying, then placing the product in a planetary ball mill for ball milling, wherein the revolution speed of the ball mill is 600-1500-mesh sieve rpm, and the rotation speed is 300-325-mesh sieve until the material passes through 1000-1500-mesh sieve, thereby preparing the barium-cobalt-ferrite-carbon nanotube composite material.
Preferably, the ultrasonic treatment appearance includes the host computer, installs ultrasonic generrator on the host computer, and ultrasonic generrator's bottom fixed mounting has ultrasonic probe, and ultrasonic generrator places on the cassette of host computer through the buckle, and the right side of host computer is provided with the pushing hands, the bottom fixedly connected with evenly distributed's of host computer roof, and the bottom activity of roof articulates there is the board of supporting, installs the extension spring on the board of supporting, supports the positive fixedly connected with footboard of board, and the bottom movable mounting of host computer has wheel components.
Preferably, the length of the carboxylated carbon nanotube is 10-30um, the diameter is less than or equal to 8nm, the carboxyl content is 2-3.8 percent, and FeCl is added3And the mass ratio of the carboxylated carbon nano tube is 5-8: 1.
Preferably, said Ba (NO)3)2、CoCl2、FeCl3And La (NO)3)3The mass ratio of the barium ferrite to the lanthanum-doped barium cobalt ferrite is 2.6-2.9:0.1-0.4:2:24, and the chemical expression is La0.1-0.4Ba2.6-2.9Co2Fe24O41。
Preferably, the preparation method of the high-thermal-conductivity modified silicone rubber composite wave-absorbing material comprises the following steps:
(1) adding a tetrahydrofuran solvent and 2-6 parts of barium-cobalt-ferrite-carbon nanotube composite material into a reaction bottle, carrying out ultrasonic dispersion treatment for 1-2h at 40-50 ℃, adding 6-16 parts of silane coupling agent vinyl triethoxysilane, placing the reaction bottle into a constant-temperature water bath, heating to 70-80 ℃, carrying out irradiation, stirring at a constant speed for reaction for 10-18h, cooling the solution to room temperature, carrying out reduced pressure distillation to remove the solvent, washing the solid product with ethanol and acetone, and fully drying to prepare the polysiloxane-coated barium-cobalt-ferrite-carbon nanotube composite material.
(2) Adding a tetrahydrofuran solvent into a reaction bottle, then adding a polysiloxane-coated barium-cobalt ferrite-carbon nano tube composite material, 69-86 parts of hydroxyl silicone oil and 4-6 parts of cross-linking agent ethyl orthosilicate, stirring uniformly, then adding 2-3 parts of catalyst dibutyltin dilaurate, placing the reaction bottle into an oil bath pot, heating to 80-100 ℃, stirring at a constant speed for reaction for 4-8 hours, pouring the solution into a mold, standing and curing at 40-50 ℃, and thus obtaining the high-thermal-conductivity modified silicone rubber composite wave-absorbing material.
Drawings
FIG. 1 is a schematic view of a support plate according to the present invention;
FIG. 2 is a schematic view of the roller supporting state of the present invention;
FIG. 3 is a side view of the present invention.
In the figure: 1. a host; 2. an ultrasonic generator; 3. an ultrasonic probe; 4. buckling; 5. a card holder; 6. a pushing handle; 7. a top plate; 8. a resisting plate; 9. a tension spring; 10. a pedal; 11. a roller assembly.
(III) advantageous technical effects
Compared with the prior art, the invention has the following beneficial technical effects:
the modified silicon rubber composite wave-absorbing material with high heat conductivity takes a carboxylated carbon nano tube as a substrate, a layer of lanthanum-doped barium-cobalt ferrite is uniformly formed on the surface of the carbon nano tube by an in-situ synthesis method, lanthanum is doped to replace partial crystal lattices of barium, compared with common ferroferric oxide and barium-cobalt ferrite, the lanthanum-doped barium-cobalt ferrite has higher dielectric constant and saturation magnetization intensity, effectively generates magnetic loss and dielectric loss on electromagnetic waves, has excellent conductivity of the carbon nano tube, forms a trace three-dimensional conductive network to generate leakage loss, converts electromagnetic energy of the electromagnetic waves into heat energy through resistance type loss to be dissipated, greatly enhances the impedance matching performance of the material under the combined action of the magnetic loss and the dielectric loss of the lanthanum-doped barium-cobalt ferrite and the leakage loss generated by the carbon nano tube, and enables the electromagnetic waves to be more fully incident into the wave-absorbing material, and the continuous reflection and loss are carried out, so that the wave absorbing performance of the material is enhanced.
The modified silicon rubber composite wave-absorbing material with high thermal conductivity is prepared by reacting vinyltriethoxysilane with active carboxyl on the surface of a carbon nano tube, irradiating the vinyltriethoxysilane, the polysiloxane-coated barium-cobalt ferrite-carbon nano tube is formed by self-polymerization, the polysiloxane coating layer has good compatibility with hydroxyl silicone oil, the hydroxyl silicone oil is polymerized to generate silicon rubber, under the coating action of polysiloxane, the dispersibility and compatibility of the barium-cobalt-ferrite-carbon nanotube composite material in the silicone rubber are greatly improved, the influence on the wave absorbing performance and the mechanical performance of the silicone rubber material due to uneven dispersion of the barium-cobalt-ferrite-carbon nanotube is avoided, meanwhile, the barium-cobalt ferrite and the carbon nano tube have high heat conductivity coefficients, and the uniformly dispersed barium-cobalt ferrite-carbon nano tube composite material improves the heat diffusion coefficient and the heat conductivity of the silicon rubber material.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: a high-thermal-conductivity modified silicone rubber composite wave-absorbing material comprises the following formula raw materials in parts by weight: 2-6 parts of barium-cobalt ferrite-carbon nanotube composite material, 6-16 parts of silane coupling agent, 69-86 parts of hydroxyl silicone oil, 4-6 parts of cross-linking agent and 2-3 parts of catalyst, wherein the silane coupling agent is vinyl triethoxysilane, the cross-linking agent is ethyl orthosilicate, and the catalyst is dibutyltin dilaurate.
The preparation method of the barium-cobalt ferrite-carbon nanotube composite material comprises the following steps:
(1) adding carboxylated carbon nano tube and Ba (NO) into a reaction bottle3)2、CoCl2、FeCl3And La (NO)3)3Wherein the length of the carboxylated carbon nanotube is 10-30um, the diameter is less than or equal to 8nm, the carboxyl content is 2-3.8 percent, and FeCl3The mass ratio of the carbon nano tube to the carboxylated carbon nano tube is 5-8:1, and Ba (NO) is added3)2、CoCl2、FeCl3And La (NO)3)3The mass ratio of the barium ferrite to the lanthanum-doped barium cobalt ferrite is 2.6-2.9:0.1-0.4:2:24, and the chemical expression is La0.1-0.4Ba2.6-2.9Co2Fe24O41The reaction bottle is arranged in the ultrasonic treatment instrument after being uniformly stirred, the ultrasonic treatment instrument comprises a host, an ultrasonic generator is installed on the host, an ultrasonic probe is fixedly installed at the bottom of the ultrasonic generator, the ultrasonic generator is placed on a clamping seat of the host through a buckle, a pushing hand is arranged on the right side of the host, a top plate is fixedly connected with the bottom of the host and uniformly distributed, a supporting plate is movably hinged to the bottom of the top plate, a tension spring is installed on the supporting plate, a pedal is fixedly connected to the front of the supporting plate, and a roller assembly is movably installed at the bottom of the host and is 40-50Performing ultrasonic dispersion treatment at the temperature of 50-70 ℃ for 20-40min, adding a dispersing agent citric acid, performing ultrasonic dispersion treatment for 1-2h, placing a reaction bottle in a constant-temperature water bath, heating to 50-70 ℃, uniformly stirring for reaction for 4-8h, adding ammonia water to adjust the pH of the solution to be neutral, uniformly stirring to form sol, placing the reaction bottle in an oven, and drying to obtain the gel precursor.
(2) Placing the gel precursor in a resistance furnace, heating the gel precursor at the rate of 5-10 ℃/min, carrying out heat treatment at the temperature of 520-550 ℃ for 1-2h, heating the gel precursor to 1260-1300 ℃, carrying out heat preservation and calcination for 6-8h, washing the calcination product with distilled water, drying, then placing the product in a planetary ball mill for ball milling, wherein the revolution speed of the ball mill is 600-1500-mesh sieve rpm, and the rotation speed is 300-325-mesh sieve until the material passes through 1000-1500-mesh sieve, thereby preparing the barium-cobalt-ferrite-carbon nanotube composite material.
The preparation method of the high-thermal-conductivity modified silicone rubber composite wave-absorbing material comprises the following steps:
(1) adding a tetrahydrofuran solvent and 2-6 parts of barium-cobalt-ferrite-carbon nanotube composite material into a reaction bottle, carrying out ultrasonic dispersion treatment for 1-2h at 40-50 ℃, adding 6-16 parts of silane coupling agent vinyl triethoxysilane, placing the reaction bottle into a constant-temperature water bath, heating to 70-80 ℃, carrying out irradiation, stirring at a constant speed for reaction for 10-18h, cooling the solution to room temperature, carrying out reduced pressure distillation to remove the solvent, washing the solid product with ethanol and acetone, and fully drying to prepare the polysiloxane-coated barium-cobalt-ferrite-carbon nanotube composite material.
(2) Adding a tetrahydrofuran solvent into a reaction bottle, then adding a polysiloxane-coated barium-cobalt ferrite-carbon nano tube composite material, 69-86 parts of hydroxyl silicone oil and 4-6 parts of cross-linking agent ethyl orthosilicate, stirring uniformly, then adding 2-3 parts of catalyst dibutyltin dilaurate, placing the reaction bottle into an oil bath pot, heating to 80-100 ℃, stirring at a constant speed for reaction for 4-8 hours, pouring the solution into a mold, standing and curing at 40-50 ℃, and thus obtaining the high-thermal-conductivity modified silicone rubber composite wave-absorbing material.
Example 1
(1) Preparation of gel precursor 1: adding carboxylated carbon nano tube and Ba (NO) into a reaction bottle3)2、CoCl2、FeCl3And La (NO)3)3，FeCl3And carboxylated carbon nanotubes at a mass ratio of 5:1, Ba (NO)3)2、CoCl2、FeCl3And La (NO)3)3The mass ratio of (A) is 2.9:0.1:2:24, the barium-cobalt ferrite is lanthanum-doped barium-cobalt ferrite, and the chemical expression is La0.1Ba2.9Co2Fe24O41After being uniformly stirred, the reaction bottle is placed in an ultrasonic treatment instrument which comprises a host machine, an ultrasonic generator is arranged on the host machine, an ultrasonic probe is fixedly arranged at the bottom of the ultrasonic generator, the ultrasonic generator is placed on a clamping seat of the host machine through a buckle, a pushing hand is arranged at the right side of the host machine, a top plate which is uniformly distributed is fixedly connected at the bottom of the host machine, a supporting plate is movably hinged at the bottom of the top plate, a tension spring is arranged on the supporting plate, a pedal is fixedly connected at the front of the supporting plate, a roller component is movably arranged at the bottom of the host machine, ultrasonic dispersion treatment is carried out for 20min at 40 ℃, a dispersing agent citric acid is added, ultrasonic dispersion treatment is carried out for 1h, the reaction bottle is placed in a constant-temperature water bath kettle, the reaction is heated to 50 ℃, stirring reaction is carried out at a constant speed for 4h, ammonia water is added to, to prepare a gel precursor 1.
(2) Preparing a barium-cobalt ferrite-carbon nanotube composite material 1: placing the gel precursor 1 in a resistance furnace, heating at a heating rate of 5 ℃/min, carrying out heat treatment at 520 ℃ for 1h, heating to 1260 ℃, carrying out heat preservation and calcination for 6h, washing the calcination product with distilled water, drying, then placing in a planetary ball mill for ball milling, wherein the revolution speed of the ball mill is 600rpm, the rotation speed of the ball mill is 300rpm, and obtaining the barium-cobalt ferrite-carbon nanotube composite material 1 until the material passes through a 1000-mesh screen.
(3) Preparing a polysiloxane-coated barium cobalt ferrite-carbon nanotube composite material 1: adding a tetrahydrofuran solvent and a 2 barium cobalt ferrite-carbon nanotube composite material 1 into a reaction bottle, performing ultrasonic dispersion treatment for 1h at 40 ℃, adding 6 parts of silane coupling agent vinyl triethoxysilane, placing the reaction bottle into a constant-temperature water bath kettle, heating to 70 ℃, performing irradiation, stirring at a constant speed for 10h, cooling the solution to room temperature, performing reduced pressure distillation to remove the solvent, washing a solid product with ethanol and acetone, and fully drying to prepare the polysiloxane-coated barium cobalt ferrite-carbon nanotube composite material 1.
(4) Preparing a high-thermal-conductivity modified silicone rubber composite wave-absorbing material 1: adding a tetrahydrofuran solvent into a reaction bottle, then adding 1 part of polysiloxane-coated barium-cobalt ferrite-carbon nano tube composite material, 86 parts of hydroxyl silicone oil and 4 parts of cross-linking agent ethyl orthosilicate, stirring uniformly, then adding 2 parts of catalyst dibutyltin dilaurate, placing the reaction bottle into an oil bath pot, heating to 80 ℃, stirring at a constant speed for reaction for 4 hours, pouring the solution into a mold, standing and curing at 40 ℃, and preparing the high-thermal-conductivity modified silicone rubber composite wave-absorbing material 1.
Example 2
(1) Preparation of gel precursor 2: adding carboxylated carbon nano tube and Ba (NO) into a reaction bottle3)2、CoCl2、FeCl3And La (NO)3)3，FeCl3The mass ratio of the carbon nano tube to the carboxylated carbon nano tube is 8:1, Ba (NO)3)2、CoCl2、FeCl3And La (NO)3)3The mass ratio of (A) is 2.8:0.2:2:24, the barium-cobalt ferrite is lanthanum-doped barium-cobalt ferrite, and the chemical expression is La0.2Ba2.8Co2Fe24O41After being uniformly stirred, the reaction bottle is arranged in an ultrasonic treatment instrument which comprises a host machine, an ultrasonic generator is arranged on the host machine, an ultrasonic probe is fixedly arranged at the bottom of the ultrasonic generator, the ultrasonic generator is arranged on a clamping seat of the host machine through a buckle, a pushing hand is arranged at the right side of the host machine, a top plate which is uniformly distributed is fixedly connected at the bottom of the host machine, a supporting plate is movably hinged at the bottom of the top plate, a tension spring is arranged on the supporting plate, a pedal is fixedly connected at the front of the supporting plate, and a roller component is movably arranged at the bottom of the host machine, performing ultrasonic dispersion treatment at 40 deg.C for 40min, adding dispersant citric acid, performing ultrasonic dispersion treatment for 2 hr, placing the reaction bottle in a constant temperature water bath, heating to 50 deg.C, stirring at constant speed for 4 hr, adding ammonia water to adjust pH to neutral, stirring at constant speed to form sol, and placing the reaction flask in oven to dry water.And (4) preparing the gel precursor 2.
(2) Preparing a barium-cobalt ferrite-carbon nanotube composite material 2: and (2) placing the gel precursor 2 in a resistance furnace, heating at the rate of 10 ℃/min, carrying out heat treatment at 550 ℃ for 2h, heating to 1300 ℃, carrying out heat preservation and calcination for 6h, washing the calcination product with distilled water, drying, then placing in a planetary ball mill for ball milling, wherein the revolution speed of the ball mill is 600rpm, and the rotation speed of the ball mill is 300rpm, and obtaining the barium-cobalt-ferrite-carbon nanotube composite material 2 until the material passes through a 1000-mesh screen.
(3) Preparing a polysiloxane-coated barium cobalt ferrite-carbon nanotube composite material 2: adding a tetrahydrofuran solvent and 2.8 parts of barium-cobalt-ferrite-carbon nanotube composite material 2 into a reaction bottle, performing ultrasonic dispersion treatment for 1h at 50 ℃, adding 8.5 parts of silane coupling agent vinyl triethoxysilane, placing the reaction bottle into a constant-temperature water bath, heating to 80 ℃, performing irradiation, stirring at a constant speed for 10h, cooling the solution to room temperature, performing reduced pressure distillation to remove the solvent, washing the solid product with ethanol and acetone, and fully drying to obtain the polysiloxane-coated barium-cobalt-ferrite-carbon nanotube composite material 2.
(4) Preparing a high-thermal-conductivity modified silicone rubber composite wave-absorbing material 2: adding a tetrahydrofuran solvent into a reaction bottle, then adding 2 parts of polysiloxane-coated barium-cobalt ferrite-carbon nano tube composite material, 82 parts of hydroxyl silicone oil and 4.5 parts of ethyl orthosilicate as a cross-linking agent, stirring uniformly, then adding 2.2 parts of dibutyltin dilaurate as a catalyst, placing the reaction bottle into an oil bath pot, heating to 80 ℃, stirring at a constant speed for reaction for 8 hours, pouring the solution into a mold, standing and curing at 50 ℃, and thus preparing the high-thermal-conductivity modified silicone rubber composite wave-absorbing material 2.
Example 3
(1) Preparation of gel precursor 3: adding carboxylated carbon nano tube and Ba (NO) into a reaction bottle3)2、CoCl2、FeCl3And La (NO)3)3，FeCl3The mass ratio of the carbon nano tube to the carboxylated carbon nano tube is 8:1, Ba (NO)3)2、CoCl2、FeCl3And La (NO)3)3The mass ratio of (A) to (B) is 2.7:0.3:2:24, barium cobalt ironThe ferrite is lanthanum-doped barium-cobalt ferrite with a chemical expression of La0.3Ba2.7Co2Fe24O41After being uniformly stirred, the reaction bottle is placed in an ultrasonic treatment instrument, the ultrasonic treatment instrument comprises a host machine, an ultrasonic generator is arranged on the host machine, an ultrasonic probe is fixedly arranged at the bottom of the ultrasonic generator, the ultrasonic generator is placed on a clamping seat of the host machine through a buckle, a pushing hand is arranged on the right side of the host machine, a top plate which is uniformly distributed is fixedly connected at the bottom of the host machine, a supporting plate is movably hinged at the bottom of the top plate, a tension spring is arranged on the supporting plate, a pedal is fixedly connected at the front of the supporting plate, a roller component is movably arranged at the bottom of the host machine, ultrasonic dispersion treatment is carried out for 40min at 50 ℃, a dispersing agent citric acid is added, ultrasonic dispersion treatment is carried out for 1h, the reaction bottle is placed in a constant-temperature water bath kettle, the reaction is heated to 50 ℃, stirring reaction is carried out for 8h at a constant speed, ammonia, to prepare a gel precursor 3.
(2) Preparing a barium-cobalt ferrite-carbon nanotube composite material 3: and (3) placing the gel precursor 3 in a resistance furnace, heating at the rate of 10 ℃/min, carrying out heat treatment at 550 ℃ for 1h, heating to 1300 ℃, carrying out heat preservation and calcination for 6h, washing the calcination product with distilled water, drying, then placing in a planetary ball mill for ball milling, wherein the revolution speed of the ball mill is 650rpm, and the rotation speed is 325rpm, and obtaining the barium-cobalt-ferrite-carbon nanotube composite material 3 until the material passes through a 1500-mesh screen.
(3) Preparing a polysiloxane-coated barium cobalt ferrite-carbon nanotube composite material 3: adding a tetrahydrofuran solvent and 4 barium-cobalt-ferrite-carbon nanotube composite material 3 into a reaction bottle, performing ultrasonic dispersion treatment for 2h at 50 ℃, adding 11 parts of silane coupling agent vinyl triethoxysilane, placing the reaction bottle in a constant-temperature water bath, heating to 70 ℃, performing irradiation, stirring at a constant speed for 10h, cooling the solution to room temperature, performing reduced pressure distillation to remove the solvent, washing the solid product with ethanol and acetone, and fully drying to obtain the polysiloxane-coated barium-cobalt-ferrite-carbon nanotube composite material 3.
(4) Preparing a high-thermal-conductivity modified silicone rubber composite wave-absorbing material 3: adding a tetrahydrofuran solvent into a reaction bottle, then adding 3 parts of polysiloxane-coated barium-cobalt ferrite-carbon nano tube composite material, 77 parts of hydroxyl silicone oil and 5.5 parts of ethyl orthosilicate as a cross-linking agent, stirring uniformly, then adding 2.5 parts of dibutyltin dilaurate as a catalyst, placing the reaction bottle into an oil bath pot, heating to 100 ℃, stirring at a constant speed for reaction for 4 hours, pouring the solution into a mold, standing and curing at 50 ℃, and thus preparing the high-thermal-conductivity modified silicone rubber composite wave-absorbing material 3.
Example 4
(1) Preparation of gel precursor 4: adding carboxylated carbon nano tube and Ba (NO) into a reaction bottle3)2、CoCl2、FeCl3And La (NO)3)3，FeCl3And carboxylated carbon nanotubes at a mass ratio of 5:1, Ba (NO)3)2、CoCl2、FeCl3And La (NO)3)3The mass ratio of the barium ferrite to the lanthanum-doped barium cobalt ferrite is 2.65:0.35:2:24, and the chemical expression is La0.35Ba2.65Co2Fe24O41After being uniformly stirred, the reaction bottle is placed in an ultrasonic treatment instrument which comprises a main machine, an ultrasonic generator is arranged on the main machine, an ultrasonic probe is fixedly arranged at the bottom of the ultrasonic generator, the ultrasonic generator is placed on a clamping seat of the main machine through a buckle, a pushing hand is arranged at the right side of the main machine, a top plate which is uniformly distributed is fixedly connected at the bottom of the main machine, a supporting plate is movably hinged at the bottom of the top plate, a tension spring is arranged on the supporting plate, a pedal is fixedly connected at the front of the supporting plate, a roller component is movably arranged at the bottom of the main machine, ultrasonic dispersion treatment is carried out for 30min at 45 ℃, a dispersing agent citric acid is added, ultrasonic dispersion treatment is carried out for 1.5h, the reaction bottle is placed in a constant-temperature water bath kettle, the reaction bottle is heated to 60 ℃, stirred at a constant speed for 6h, ammonia water is added to adjust the pH, to prepare the gel precursor 4.
(2) Preparing a barium-cobalt ferrite-carbon nanotube composite material 4: and (3) placing the gel precursor 4 in a resistance furnace, heating at the rate of 7 ℃/min, carrying out heat treatment at 535 ℃ for 1.5h, heating to 1280 ℃, carrying out heat preservation and calcination for 7h, washing the calcination product with distilled water, drying, then placing in a planetary ball mill for ball milling, wherein the revolution speed of the ball mill is 620rpm, the rotation speed is 310rpm, and the material passes through a 1200-mesh screen to prepare the barium-cobalt-ferrite-carbon nanotube composite material 4.
(3) Preparing a polysiloxane-coated barium cobalt ferrite-carbon nanotube composite material 4: adding a tetrahydrofuran solvent and 5 parts of barium-cobalt-ferrite-carbon nanotube composite material 4 into a reaction bottle, performing ultrasonic dispersion treatment for 1.5h at 45 ℃, adding 14.3 parts of silane coupling agent vinyl triethoxysilane, placing the reaction bottle into a constant-temperature water bath, heating to 75 ℃, performing irradiation, stirring at a constant speed for 14h, cooling the solution to room temperature, performing reduced pressure distillation to remove the solvent, washing the solid product with ethanol and acetone, and fully drying to obtain the polysiloxane-coated barium-cobalt-ferrite-carbon nanotube composite material 4.
(4) Preparing a high-thermal-conductivity modified silicone rubber composite wave-absorbing material 4: adding a tetrahydrofuran solvent into a reaction bottle, adding 4 parts of polysiloxane-coated barium-cobalt ferrite-carbon nano tube composite material, 72.5 parts of hydroxy silicone oil and 5.5 parts of cross-linking agent ethyl orthosilicate, stirring uniformly, adding 2.7 parts of catalyst dibutyltin dilaurate, placing the reaction bottle into an oil bath, heating to 90 ℃, stirring at a constant speed for reaction for 6 hours, pouring the solution into a mold, standing and curing at 45 ℃, and preparing the high-thermal-conductivity modified silicone rubber composite wave-absorbing material 4.
Example 5
(1) Preparation of a gel precursor 5: adding carboxylated carbon nano tube and Ba (NO) into a reaction bottle3)2、CoCl2、FeCl3And La (NO)3)3，FeCl3The mass ratio of the carbon nano tube to the carboxylated carbon nano tube is 8:1, Ba (NO)3)2、CoCl2、FeCl3And La (NO)3)3The mass ratio of (A) to (B) is 2.6:0.4:2:24, the barium-cobalt ferrite is lanthanum-doped barium-cobalt ferrite, and the chemical expression is La0.4Ba2.6Co2Fe24O41After being stirred uniformly, the reaction bottle is placed in an ultrasonic treatment instrument for ultrasonic dispersion treatment for 40min at the temperature of 50 ℃, and then dispersant citric acid is addedAnd (3) performing ultrasonic dispersion treatment for 2h, placing the reaction bottle in a constant-temperature water bath, heating to 70 ℃, uniformly stirring for reaction for 8h, adding ammonia water to adjust the pH of the solution to be neutral, uniformly stirring to form a sol, placing the reaction bottle in an oven, and drying to obtain a gel precursor 5.
(2) Preparing a barium-cobalt ferrite-carbon nanotube composite material 5: and (3) placing the gel precursor 5 in a resistance furnace, heating at the rate of 10 ℃/min, carrying out heat treatment at 550 ℃ for 2h, heating to 1300 ℃, carrying out heat preservation and calcination for 8h, washing the calcination product with distilled water, drying, then placing in a planetary ball mill for ball milling, wherein the revolution speed of the ball mill is 650rpm, and the rotation speed of the ball mill is 325rpm, and obtaining the barium-cobalt-ferrite-carbon nanotube composite material 5 until the material passes through a 1500-mesh screen.
(3) Preparing a polysiloxane-coated barium cobalt ferrite-carbon nanotube composite material 5: adding a tetrahydrofuran solvent and a 6 barium cobalt ferrite-carbon nanotube composite material 5 into a reaction bottle, performing ultrasonic dispersion treatment for 2 hours at 50 ℃, adding 16 parts of silane coupling agent vinyl triethoxysilane, placing the reaction bottle into a constant-temperature water bath kettle, heating to 80 ℃, performing irradiation, stirring at a constant speed for reaction for 18 hours, cooling the solution to room temperature, and performing reduced pressure distillation to remove the solvent, so that a solid product is washed by ethanol and acetone, and is fully dried to prepare the polysiloxane-coated barium cobalt ferrite-carbon nanotube composite material 5.
(4) Preparing a high-thermal-conductivity modified silicone rubber composite wave-absorbing material 5: adding a tetrahydrofuran solvent into a reaction bottle, then adding 5 parts of polysiloxane-coated barium-cobalt ferrite-carbon nanotube composite material, 69 parts of hydroxy silicone oil and 6 parts of cross-linking agent ethyl orthosilicate, stirring uniformly, then adding 3 parts of catalyst dibutyltin dilaurate, placing the reaction bottle into an oil bath pot, heating to 100 ℃, stirring at a constant speed for reaction for 8 hours, pouring the solution into a mold, standing and curing at 50 ℃, and preparing the high-thermal-conductivity modified silicone rubber composite wave-absorbing material 5.
The ZNBT8 vector network analyzer is used for testing the wave absorbing performance of the modified silicon rubber composite wave absorbing material in the embodiments 1-5, and the test standard is GB/T36763-2018.
In summary, the modified silicone rubber composite wave-absorbing material with high thermal conductivity takes the carboxylated carbon nanotube as the substrate, the in-situ synthesis method uniformly forms a layer of lanthanum-doped barium-cobalt ferrite on the surface of the carbon nanotube, the lanthanum doping replaces part of the crystal lattice of barium, compared with the common ferroferric oxide and barium-cobalt ferrite, the lanthanum-doped barium-cobalt ferrite has larger dielectric constant and saturation magnetization intensity, effectively generates magnetic loss and dielectric loss to electromagnetic waves, has excellent conductivity of the carbon nanotube, forms a trace three-dimensional conductive network to generate leakage loss, converts electromagnetic energy of the electromagnetic waves into heat energy through resistance type loss to be emitted, greatly enhances the impedance matching performance of the material under the combined action of the magnetic loss and the dielectric loss of the lanthanum-doped barium-cobalt ferrite and the leakage loss generated by the carbon nanotube, and enables the electromagnetic waves to be more fully incident into the wave-absorbing material, and the continuous reflection and loss are carried out, so that the wave absorbing performance of the material is enhanced.
Vinyl triethoxysilane is used for reacting with active carboxyl on the surface of the carbon nano tube, the vinyl triethoxysilane forms polysiloxane-coated barium-cobalt ferrite-carbon nano tube through self-polymerization under the irradiation effect, the polysiloxane coating layer has good compatibility with hydroxyl silicone oil, the hydroxyl silicone oil is polymerized to generate silicon rubber, the dispersibility and the compatibility of the barium-cobalt ferrite-carbon nano tube composite material in the silicon rubber are greatly improved under the polysiloxane coating effect, the influence of uneven dispersion of the barium-cobalt ferrite-carbon nano tube on the wave absorbing performance and the mechanical performance of the silicon rubber material is avoided, meanwhile, the barium-cobalt ferrite and the carbon nano tube have high heat conductivity coefficients, and the uniformly dispersed barium-cobalt ferrite-carbon nano tube composite material improves the heat diffusion coefficient and the heat conductivity of the silicon rubber material.
Claims (9)
1. The high-thermal-conductivity modified silicone rubber composite wave-absorbing material comprises the following formula raw materials in parts by weight and components, and is characterized in that: 2-6 parts of barium-cobalt ferrite-carbon nanotube composite material, 6-16 parts of silane coupling agent, 69-86 parts of hydroxyl silicone oil, 4-6 parts of cross-linking agent and 2-3 parts of catalyst.
2. The modified silicone rubber composite wave-absorbing material with high thermal conductivity as claimed in claim 1, wherein: the silane coupling agent is vinyl triethoxysilane.
3. The modified silicone rubber composite wave-absorbing material with high thermal conductivity as claimed in claim 1, wherein: the cross-linking agent is tetraethoxysilane.
4. The modified silicone rubber composite wave-absorbing material with high thermal conductivity as claimed in claim 1, wherein: the catalyst is dibutyltin dilaurate.
5. The modified silicone rubber composite wave-absorbing material with high thermal conductivity as claimed in claim 1, wherein: the preparation method of the barium-cobalt ferrite-carbon nanotube composite material comprises the following steps:
(1) adding carboxylated carbon nano tube and Ba (NO) into a reaction bottle3)2、CoCl2、FeCl3And La (NO)3)3Placing the reaction bottle into an ultrasonic treatment instrument after uniformly stirring, carrying out ultrasonic dispersion treatment for 20-40min at 40-50 ℃, adding a dispersing agent citric acid, carrying out ultrasonic dispersion treatment for 1-2h, placing the reaction bottle into a constant-temperature water bath kettle, heating to 50-70 ℃, carrying out uniform stirring reaction for 4-8h, adding ammonia water to adjust the pH value of the solution to be neutral, carrying out uniform stirring to form sol, placing the reaction bottle into an oven, and drying water to prepare the gel precursor.
(2) Placing the gel precursor in a resistance furnace, heating the gel precursor at the rate of 5-10 ℃/min, carrying out heat treatment at the temperature of 520-550 ℃ for 1-2h, heating the gel precursor to 1260-1300 ℃, carrying out heat preservation and calcination for 6-8h, washing the calcination product with distilled water, drying, then placing the product in a planetary ball mill for ball milling, wherein the revolution speed of the ball mill is 600-1500-mesh sieve rpm, and the rotation speed is 300-325-mesh sieve until the material passes through 1000-1500-mesh sieve, thereby preparing the barium-cobalt-ferrite-carbon nanotube composite material.
6. The modified silicone rubber composite wave-absorbing material with high thermal conductivity as claimed in claim 5, wherein: the ultrasonic treatment instrument comprises a main machine (1), an ultrasonic generator (2) is installed on the main machine (1), an ultrasonic probe (3) is fixedly installed at the bottom of the ultrasonic generator (2), the ultrasonic generator (2) is placed on a clamping seat (5) of the main machine (1) through a buckle (4), a pushing hand (6) is arranged on the right side of the main machine (1), a top plate (7) is fixedly connected with the bottom of the main machine (1) and is uniformly distributed, a supporting plate (8) is movably hinged to the bottom of the top plate (7), a tension spring (9) is installed on the supporting plate (8), a pedal (10) is fixedly connected to the front of the supporting plate (8), and a roller component (11) is movably installed at the bottom of the main machine (1).
7. The modified silicone rubber composite wave-absorbing material with high thermal conductivity as claimed in claim 5, wherein: the length of the carboxylated carbon nanotube is 10-30um, the diameter is less than or equal to 8nm, the carboxyl content is 2-3.8 percent, and FeCl is added3And the mass ratio of the carboxylated carbon nano tube is 5-8: 1.
8. The modified silicone rubber composite wave-absorbing material with high thermal conductivity as claimed in claim 5, wherein: said Ba (NO)3)2、CoCl2、FeCl3And La (NO)3)3The mass ratio of the barium ferrite to the lanthanum-doped barium cobalt ferrite is 2.6-2.9:0.1-0.4:2:24, and the chemical expression is La0.1-0.4Ba2.6-2.9Co2Fe24O41。
9. The modified silicone rubber composite wave-absorbing material with high thermal conductivity as claimed in claim 1, wherein: the preparation method of the high-thermal-conductivity modified silicone rubber composite wave-absorbing material comprises the following steps:
(1) adding a tetrahydrofuran solvent and 2-6 parts of barium-cobalt-ferrite-carbon nanotube composite material into a reaction bottle, carrying out ultrasonic dispersion treatment for 1-2h at 40-50 ℃, adding 6-16 parts of silane coupling agent vinyl triethoxysilane, placing the reaction bottle into a constant-temperature water bath, heating to 70-80 ℃, carrying out irradiation, stirring at a constant speed for reaction for 10-18h, cooling the solution to room temperature, carrying out reduced pressure distillation to remove the solvent, washing the solid product with ethanol and acetone, and fully drying to prepare the polysiloxane-coated barium-cobalt-ferrite-carbon nanotube composite material.
(2) Adding a tetrahydrofuran solvent into a reaction bottle, then adding a polysiloxane-coated barium-cobalt ferrite-carbon nano tube composite material, 69-86 parts of hydroxyl silicone oil and 4-6 parts of cross-linking agent ethyl orthosilicate, stirring uniformly, then adding 2-3 parts of catalyst dibutyltin dilaurate, placing the reaction bottle into an oil bath pot, heating to 80-100 ℃, stirring at a constant speed for reaction for 4-8 hours, pouring the solution into a mold, standing and curing at 40-50 ℃, and thus obtaining the high-thermal-conductivity modified silicone rubber composite wave-absorbing material.
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| CN112315044A (en) * | 2020-10-16 | 2021-02-05 | 浙江义乌露炜针织内衣有限公司 | Radiation-proof health-care underwear |
| CN113214638A (en) * | 2021-05-27 | 2021-08-06 | 湖南飞鸿达新材料有限公司 | Wave-absorbing heat-conducting flexible composite material and preparation method thereof |
| CN113248810A (en) * | 2021-04-26 | 2021-08-13 | 中科院长春应化所黄埔先进材料研究院 | Light electromagnetic shielding polymer composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112315044A (en) * | 2020-10-16 | 2021-02-05 | 浙江义乌露炜针织内衣有限公司 | Radiation-proof health-care underwear |
| CN113248810A (en) * | 2021-04-26 | 2021-08-13 | 中科院长春应化所黄埔先进材料研究院 | Light electromagnetic shielding polymer composite material and preparation method thereof |
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| CN113214638A (en) * | 2021-05-27 | 2021-08-06 | 湖南飞鸿达新材料有限公司 | Wave-absorbing heat-conducting flexible composite material and preparation method thereof |
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