CN109346848B - SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material and preparation method thereof - Google Patents
SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material and preparation method thereof Download PDFInfo
- Publication number
- CN109346848B CN109346848B CN201811284361.8A CN201811284361A CN109346848B CN 109346848 B CN109346848 B CN 109346848B CN 201811284361 A CN201811284361 A CN 201811284361A CN 109346848 B CN109346848 B CN 109346848B
- Authority
- CN
- China
- Prior art keywords
- ferrite
- silicon carbide
- wave
- carbonaceous material
- sic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01Q—ANTENNAS, i.e. RADIO AERIALS
- H01Q17/00—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01Q—ANTENNAS, i.e. RADIO AERIALS
- H01Q17/00—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems
- H01Q17/004—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems using non-directional dissipative particles, e.g. ferrite powders
Landscapes
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
A SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material and a preparation method thereof relate to wave-absorbing composite materials and aim to solve the technical problems of complex processing, higher cost and poor wave-absorbing effect of the existing wave-absorbing materials. The wave-absorbing composite material consists of ferrite, silicon carbide and carbonaceous materials; the preparation method comprises the following steps: firstly, pretreating the surface of silicon carbide; uniformly mixing hydrophilic silicon carbide, soluble salt for preparing ferrite, fluoride, a precipitator, a carbonaceous material, a silane coupling agent, alcohol and water, and carrying out hydrothermal synthesis to obtain a precursor; and roasting the precursor to obtain the wave-absorbing composite material. It can reach 90% absorption in X wave band of 8-12GHz, its reflection loss is lower than-10 dB, and its maximum reflection loss is up to-28 dB. The method can be used in the fields of monitoring of ground nuclear reactor systems, crude oil exploration, environmental monitoring, aviation, aerospace, radar, communication systems, high-power electronic converters and automobile motors.
Description
Technical Field
The invention relates to a wave-absorbing composite material and a preparation method thereof, belonging to the field of high-temperature wave-absorbing composite materials.
Background
With the rapid development of information technology, microwave absorbing materials play more and more important roles in the aspects of electronic reliability, medical care, national defense safety and the like. For example, microwave absorbing materials used in emerging high-speed communication devices (e.g., satellites) can improve the signal quality of the receiver by suppressing noise. In addition, the wave-absorbing materials of the radar station and the relay station can protect internal workers from excessive radiation of high-power microwaves. Most importantly, with the gradual maturity of novel advanced anti-stealth radars such as ultra-wideband radars, phased array radars, multi-base radars, passive radars and the like, the high-performance anti-detection wave-absorbing material becomes an effective way for improving the viability of military units. An ideal absorbing material has both strong absorption capacity and a wide absorption band. In addition, the wave-absorbing material with ultra-light weight and thin thickness will have advantages in the fields of aerospace, aviation, ground vehicles and the rapidly growing next-generation green miniature electronic products.
In most cases, solid particle absorbents such as ferrite, metal powder, ceramic, carbon nano-particles and the like are widely used for preparing wave-absorbing composite materials. Although the wave-absorbing performance is general, most of the wave-absorbing materials have not been practically applied due to the defects of large density, poor stability, large loading capacity and the like. The Chinese patent 'millimeter wave broadband wave-absorbing coating' with the patent number of 93102922.8 reports that the wave-absorbing coating is formed by mixing silicon carbide, conductive carbon black, a binder and the like, is prepared by adopting different formulas in layers and is coated on a carrier, and the wave-absorbing effect of 11-16dB can be realized in the frequency band of 26-100 GHz. However, the material method has the disadvantages of complex processing, higher cost and poor wave-absorbing effect.
Disclosure of Invention
The invention provides a SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material and a preparation method thereof, aiming at solving the technical problems of complex processing, higher cost and poor wave-absorbing effect of the existing wave-absorbing material.
The SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material consists of ferrite, silicon carbide and carbonaceous materials, wherein the carbonaceous materials are graphene, reduced graphene, oxidized graphene, conductive carbon black or carbon nano tubes; when the carbonaceous material is graphene, reduced graphene or oxidized graphene, the ferrite and the silicon carbide are loaded on the graphene sheet layer; when the carbonaceous material is conductive carbon black, the conductive carbon black is uniformly mixed with the ferrite and the silicon carbide; when the carbonaceous material is carbon nanotubes, the ferrite, the silicon carbide and the carbon nanotubes are uniformly mixed.
The preparation method of the SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material comprises the following steps:
firstly, silicon carbide surface pretreatment:
a. adding silicon carbide with the particle size of 1-10 mu m into a silicon carbide ball mill for ball milling for 12-24 h; putting the mixture into a tube furnace, heating the mixture to 500-600 ℃ under the air or nitrogen, and carrying out oxidation treatment for 2-4 h to achieve the purpose of removing surface impurities;
b. dispersing silicon carbide in an acidic hydrophilic solution, stirring for 2-3 h, then ultrasonically dispersing for 1-2 h, and radiating for 1-2 h by microwave to improve the hydrophilicity; then washing with distilled water, filtering, and airing at 15-30 ℃ to obtain hydrophilic silicon carbide;
secondly, synthesizing the SiC-ferrite/carbonaceous material by a one-pot method:
a. weighing hydrophilic silicon carbide, soluble salt for preparing ferrite, fluoride, a precipitator, a carbonaceous material, a silane coupling agent, an alcohol solvent and deionized water, stirring for 1-2 hours, and performing ultrasonic dispersion for 30 min-1 hour to obtain a mixed solution;
b. transferring the mixed solution into a high-temperature reaction kettle, heating to 120-150 ℃ at the speed of 2-4 ℃/min, preserving heat for 4-6 h, exchanging water and an alcohol solution after the reaction is finished, centrifuging, cleaning, and then drying in a vacuum drying oven to obtain a precursor;
c. and roasting the precursor in a tubular furnace at 350-450 ℃ for 2-4 h under air or nitrogen, and cooling to room temperature to obtain the SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material.
The high-temperature wave-absorbing composite material is a composite body of silicon carbide/ferrite loaded on a carbonaceous material, SiC has the characteristics of high strength, high hardness, corrosion resistance, high temperature resistance and low density, meanwhile, the forbidden bandwidth of SiC is 2-3 times of Si, the heat conductivity is 4.4 times of Si, the critical breakdown electric field is 8 times of Si, and the saturation drift velocity of electrons is 2 times of Si, so that the high-temperature wave-absorbing composite material becomes a preferred material of a semiconductor device with high frequency, high power, high temperature resistance and radiation resistance; the carbon material can be used as an electromagnetic wave absorbent due to the high dielectric loss characteristic, the method loads the silicon carbide/ferrite on the carbon material to form the carbon-based high-temperature resistant wave-absorbing composite material with magnetic loss and electric loss, and the wave-absorbing performance of the composite material can be greatly improved due to the synergistic effect of the components. The composite material realizes 90 percent of absorption in an X wave band (8-12GHz), the reflection loss of the composite material is lower than-10 dB, and the maximum reflection loss of the composite material reaches-28 dB. The composite material has good high-temperature resistance and oxidation resistance, and can meet the high-temperature use requirement of the composite material; by controlling the raw material ratio and the high-temperature sintering condition, the graphitization of the graphene is avoided. The raw materials are simple and easy to obtain, the preparation process is simple, and the yield is high.
The material of the invention can be used in the fields of monitoring of ground nuclear reactor systems, crude oil exploration, environmental monitoring, aviation, aerospace, radar, communication systems, high-power electronic converters, automobile motors and the like.
Drawings
FIG. 1 is a scanning electron micrograph of the SiC-ferrite/carbonaceous material high temperature wave-absorbing composite material in example 1;
FIG. 2 is a transmission electron micrograph of the SiC-ferrite/carbonaceous material high temperature wave-absorbing composite material in example 1;
FIG. 3 is an XRD spectrum of the SiC-ferrite/carbonaceous material high temperature wave-absorbing composite material in example 1;
FIG. 4 is a graph of the absorption performance of the SiC-ferrite/carbonaceous material high temperature wave-absorbing composite material in example 1;
FIG. 5 is the absorption performance curve of the SiC-ferrite/carbonaceous material high temperature wave-absorbing composite material in example 1;
FIG. 6 is an absorption performance diagram of the SiC-ferrite/carbonaceous material high temperature wave-absorbing composite material prepared in example 2;
FIG. 7 is the absorption performance curve of the SiC-ferrite/carbonaceous material high temperature wave-absorbing composite material in example 2;
FIG. 8 is an absorption performance diagram of the SiC-ferrite/carbonaceous material high temperature wave-absorbing composite material prepared in example 3;
FIG. 9 is the absorption performance curve of the SiC-ferrite/carbonaceous material high temperature wave-absorbing composite material in example 3.
Detailed Description
The first embodiment is as follows: the SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material of the embodiment is composed of ferrite, silicon carbide and carbonaceous materials, wherein the carbonaceous materials are graphene, reduced graphene, oxidized graphene, conductive carbon black or carbon nano tubes; the carbonaceous material is graphene, reduced graphene or oxidized graphene, and the ferrite and the silicon carbide are loaded on the graphene sheet layer; the carbonaceous material is conductive carbon black, and the conductive carbon black is uniformly mixed with ferrite and silicon carbide; the carbon material is carbon nano tube, and ferrite, silicon carbide and the carbon nano tube are uniformly mixed.
The second embodiment is as follows: the present embodiment is different from the first embodiment in that the ferrite is nickel oxide, iron oxide, or cobalt oxide. The rest is the same as the first embodiment.
The third concrete implementation mode: the preparation method of the SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material in the specific embodiment comprises the following steps:
firstly, silicon carbide surface pretreatment:
a. adding silicon carbide with the particle size of 1-10 mu m into a silicon carbide ball mill for ball milling for 12-24 h; putting the mixture into a tube furnace, heating the mixture to 500-600 ℃ under the air or nitrogen, and carrying out oxidation treatment for 2-4 h to achieve the purpose of removing surface impurities;
b. dispersing silicon carbide in an acidic hydrophilic solution, stirring for 2-3 h, then ultrasonically dispersing for 1-2 h, and radiating for 1-2 h by microwave to improve the hydrophilicity; then washing with distilled water, filtering, and airing at 15-30 ℃ to obtain hydrophilic silicon carbide;
secondly, synthesizing the SiC-ferrite/carbonaceous material by a one-pot method:
a. weighing hydrophilic silicon carbide, soluble salt for preparing ferrite, fluoride, a precipitator, a carbonaceous material, a silane coupling agent, an alcohol solvent and deionized water, stirring for 1-2 hours, and performing ultrasonic dispersion for 30 min-1 hour to obtain a mixed solution;
b. transferring the mixed solution into a high-temperature reaction kettle, heating to 120-150 ℃ at the speed of 2-4 ℃/min, preserving heat for 4-6 h, exchanging water and an alcohol solution after the reaction is finished, centrifuging, cleaning, and then drying in a vacuum drying oven to obtain a precursor;
c. and roasting the precursor in a tubular furnace at 350-450 ℃ for 2-4 h under air or nitrogen, and cooling to room temperature to obtain the SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material.
The fourth concrete implementation mode: the third difference between the present embodiment and the specific embodiment is that the acidic hydrophilic solution in the first step b is one or a combination of several of hydrofluoric acid with a volume concentration of 10% to 20%, concentrated hydrochloric acid with a volume concentration of 10% to 20%, concentrated nitric acid with a volume concentration of 20% to 30%, concentrated sulfuric acid with a volume concentration of 40% to 50%, mellitic acid, azothiosquaric acid, trichloroacetic acid, trinitrobenzene sulfonic acid, trifluoromethanesulfonic acid and trifluoroacetic acid; the rest is the same as the third embodiment.
The fifth concrete implementation mode: the third or fourth embodiment is different from the third or fourth embodiment in that the soluble salt for preparing ferrite in the second step is nickel salt, iron salt or cobalt salt; the prepared ferrite is nickel oxide, iron oxide or cobalt oxide. The other is the same as the third or fourth embodiment.
The sixth specific implementation mode: the difference between the fifth embodiment and the fifth embodiment is that the nickel salt is one or more of nickel chloride hexahydrate, nickel sulfate hexahydrate and nickel nitrate hexahydrate; the ferric salt is one or more of ferric chloride hexahydrate, ferrous sulfate heptahydrate and ferric nitrate nonahydrate; the cobalt salt is one or more of cobalt chloride hexahydrate, cobalt sulfate heptahydrate and cobalt nitrate hexahydrate; the rest is the same as the fifth embodiment.
The seventh embodiment: the difference between the third embodiment and the sixth embodiment is that the nickel salt is one or more of nickel chloride hexahydrate, nickel sulfate hexahydrate and nickel nitrate hexahydrate; the ferric salt is one or more of ferric chloride hexahydrate, ferrous sulfate heptahydrate and ferric nitrate nonahydrate; the cobalt salt is one or more of cobalt chloride hexahydrate, cobalt sulfate heptahydrate and cobalt nitrate hexahydrate; the others are the same as in one of the third to sixth embodiments.
The specific implementation mode is eight: this embodiment is different from one of the third to seventh embodiments in that the fluoride is ammonia fluoride, sodium fluoride, potassium fluoride, silver fluoride, or aluminum fluoride; the others are the same as in one of the third to seventh embodiments.
The specific implementation method nine: the difference between this embodiment and one of the third to eighth embodiments is that the precipitant is urea, sodium hydroxide, ammonia water, sodium carbonate, potassium carbonate, sodium bicarbonate, disodium hydrogen phosphate, sodium citrate or potassium citrate; the others are the same as in one of the third to eighth embodiments.
The detailed implementation mode is ten: this embodiment is different from one of the third to ninth embodiments in that the carbonaceous material is graphene, reduced graphene, graphene oxide, conductive carbon black, or carbon nanotubes. The others are the same as in one of the third to ninth embodiments.
The concrete implementation mode eleven: this embodiment differs from one of the third to tenth embodiments in that the silane coupling agent is aminopropyltriethoxysilane (KH550), glycidoxypropyltrimethoxysilane (KH560), methacryloxypropyltrimethoxysilane (KH570), vinyltriethoxysilane (A151), vinyltriethoxysilane (A171), mercaptopropyltrimethoxysilane (KH580, KH590), ethylenediaminepropyltriethoxysilane (KH792) or ethylenediaminepropylmethyldimethoxysilane (KBM 602). The others are the same as in one of the third to tenth embodiments.
The specific implementation mode twelve: the difference between the third embodiment and the eleventh embodiment is that the alcohol solvent is one or more of ethanol, methanol, propanol, isopropanol, n-butanol, tert-butanol, benzyl alcohol, cyclobutanol, cyclohexanol, cyclopentanol, isobutanol, and isoamyl alcohol. The others are the same as in one of the third to eleventh embodiments.
The specific implementation mode is thirteen: the third to twelfth differences from the first embodiment are that in the second step a, the mass ratio of the hydrophilic silicon carbide to the graphene is 1 (0.25-0.5); the molar ratio of soluble salt, fluoride and precipitator for preparing ferrite is 1 (2-3): (5-8); the molar ratio of the hydrophilic silicon carbide to soluble salt for preparing ferrite is 1 (1-2); the volume percentage concentration of the silane coupling agent in the mixed solution is 0.25-0.5%; the ratio of the mass of the hydrophilic silicon carbide to the volume of the alcohol solvent is 1 g: (40-60) mL; the ratio of the mass of the hydrophilic silicon carbide to the volume of the deionized water is 1 g: (40-60) mL. The rest is the same as the third to twelfth embodiments.
The specific implementation mode is thirteen: the third to twelfth differences from the first to second embodiments are that in the second step, the temperature of vacuum drying is 60-80 ℃ and the time is 12-24 h. The rest is the same as the third to twelfth embodiments.
The following examples are used to demonstrate the beneficial effects of the present invention:
example 1: the preparation method of the SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material of the embodiment comprises the following steps:
firstly, silicon carbide surface pretreatment:
a. adding silicon carbide with the particle size of 0.8-2 mu m into a silicon carbide ball mill for ball milling for 12 hours; then putting the mixture into a tube furnace, and heating the mixture to 550 ℃ in air atmosphere for oxidation treatment for 2h to achieve the purpose of removing surface impurities;
b. dispersing silicon carbide in an HF aqueous solution with the volume percentage concentration of 10%, magnetically stirring for 2h, then ultrasonically dispersing for 1h, heating for 1h by 800W microwave radiation to improve the hydrophilicity, and obviously and uniformly dispersing the solution; then washing with distilled water, filtering, and airing the solid phase substance at room temperature to obtain hydrophilic silicon carbide;
secondly, synthesizing the SiC-ferrite/carbonaceous material by a one-pot method:
a. weighing 0.2g of hydrophilic silicon carbide, 0.05g of graphene oxide, 1.188g of nickel chloride hexahydrate, 0.370g of ammonium fluoride, 1.502g of urea, 0.25ml of aminopropyltriethoxysilane (KH550), 40ml of ethanol and 40ml of deionized water, stirring for 1h, and performing ultrasonic dispersion for 30min to obtain a mixed solution;
b. transferring the mixed solution into a high-temperature reaction kettle, heating to 120 ℃ at the speed of 3 ℃/min, preserving heat for 4 hours, after the reaction is finished, exchanging water and an alcohol solution, centrifuging, cleaning, and then drying in a vacuum drying oven at 70 ℃ for 20 hours to obtain a precursor;
c. and roasting the precursor in a 350 ℃ tubular furnace for 2h in an air atmosphere, and cooling to room temperature to obtain the SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material.
The scanning electron micrograph of the SiC-ferrite/carbonaceous material high temperature wave-absorbing composite material obtained in this example is shown in fig. 1, and it can be seen from fig. 1 that nickel oxide is loaded on graphene oxide in a petal shape, and silicon carbide is loaded on a graphene oxide lamella in a random shape.
The transmission electron microscope photo of the SiC-ferrite/carbonaceous material high temperature wave-absorbing composite material obtained in the embodiment is shown in fig. 2, and it can be seen from fig. 2 that a large number of irregular particles are loaded on the surface of graphene oxide.
The XRD spectrogram of the SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material obtained in the embodiment is shown in figure 3, and as can be seen from figure 3, peaks in the XRD energy spectrum respectively correspond to graphene oxide, alpha-SiC and nickel oxide, which indicates that the wave-absorbing composite material is compounded by the graphene oxide, the alpha-SiC and the nickel oxide.
The 2-18 GHz wave-absorbing performance analysis chart of the SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material obtained in the embodiment is shown in fig. 4 and fig. 5, wherein it can be seen from fig. 4 that the X wave band can be fully covered by adjusting the thickness within the thickness of 2-5 mm. When the thickness is 2mm, the strongest wave absorption value is-19.15 dB at 12.08 GHz; as can be seen from FIG. 5, the maximum absorption at 7.36GHz is-23.03 dB at a thickness of 3 mm; when the thickness is 4mm, the strongest wave absorption value is-26.33 dB at 5.20 GHz; the maximum wave absorption value at 4.00GHz is-28.53 dB when the thickness is 5 mm.
Example 2: the preparation method of the SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material of the embodiment comprises the following steps:
firstly, silicon carbide surface pretreatment:
a. adding silicon carbide with the particle size of 0.8-2 mu m into a silicon carbide ball mill for ball milling for 12 hours; then putting the mixture into a tube furnace, and heating the mixture to 550 ℃ in air atmosphere for oxidation treatment for 2h to achieve the purpose of removing surface impurities;
b. dispersing silicon carbide in an HF aqueous solution with the volume percentage concentration of 10%, magnetically stirring for 2h, then ultrasonically dispersing for 1h, heating for 1h by 800W microwave radiation to improve the hydrophilicity, and obviously and uniformly dispersing the solution; then washing with distilled water, filtering, and airing the solid phase substance at room temperature to obtain hydrophilic silicon carbide;
secondly, synthesizing the SiC-ferrite/carbonaceous material by a one-pot method:
a. weighing 0.2g of hydrophilic silicon carbide, 0.05g of conductive carbon black, 1.3515g of ferric chloride hexahydrate, 0.555g of ammonium fluoride, 2.4032g of urea, 0.25ml of aminopropyltriethoxysilane (KH550), 40ml of ethanol and 40ml of deionized water, stirring for 1h, and performing ultrasonic dispersion for 30min to obtain a mixed solution;
b. transferring the mixed solution into a high-temperature reaction kettle, heating to 120 ℃ at the speed of 3 ℃/min, preserving heat for 4 hours, exchanging water and an alcohol solution after the reaction is finished, centrifugally cleaning the mixture, and then drying the mixture in a vacuum drying oven at the temperature of 70 ℃ for 20 hours to obtain a precursor;
c. and roasting the precursor in a 350 ℃ tubular furnace for 2h in an air atmosphere, and cooling to room temperature to obtain the SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material.
The 2-18 GHz wave-absorbing performance analysis chart of the SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material obtained in the embodiment is shown in fig. 6 and 7, wherein as can be seen from fig. 6, the X wave band can be fully covered by adjusting the thickness within the thickness of 2-4 mm. As can be seen from FIG. 7, the maximum absorption at 17.90GHz is-15.79 dB at a thickness of 2 mm; when the thickness is 2.19mm, the strongest wave absorption value is-27.59 dB at 17.68 GHz; when the thickness is 3mm, the strongest wave absorption value at 11.20GHz is-14.24 dB; when the thickness is 4mm, the maximum wave absorption value at 8.00GHz is-10.58 dB.
Example 3: the preparation method of the SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material of the embodiment comprises the following steps:
firstly, silicon carbide surface pretreatment:
a. adding silicon carbide with the particle size of 0.8-2 mu m into a silicon carbide ball mill for ball milling for 12 hours; then putting the mixture into a tube furnace, and heating the mixture to 550 ℃ in air atmosphere for oxidation treatment for 2h to achieve the purpose of removing surface impurities;
b. dispersing silicon carbide in HF (hydrogen fluoride) and HCl (hydrochloric acid) aqueous solution with the volume percentage concentration of 10%, magnetically stirring for 2 hours, then ultrasonically dispersing for 1 hour, heating for 1 hour by 800W microwave radiation to improve the hydrophilicity, and obviously and uniformly dispersing the solution; then washing with distilled water, filtering, and airing the solid phase substance at room temperature to obtain hydrophilic silicon carbide;
secondly, synthesizing the SiC-ferrite/carbonaceous material by a one-pot method:
a. weighing 0.2g of hydrophilic silicon carbide, 0.05g of graphene, 1.190g of cobalt chloride hexahydrate, 0.555g of ammonium fluoride, 1.502g of urea, 0.25ml of aminopropyltriethoxysilane (KH550), 40ml of ethanol and 40ml of deionized water, stirring for 1h, and performing ultrasonic dispersion for 30min to obtain a mixed solution;
b. transferring the mixed solution into a high-temperature reaction kettle, heating to 120 ℃ at the speed of 3 ℃/min, preserving heat for 4 hours, exchanging water and an alcohol solution after the reaction is finished, centrifugally cleaning the mixture, and then drying the mixture in a vacuum drying oven at the temperature of 70 ℃ for 20 hours to obtain a precursor;
c. and roasting the precursor in a 350 ℃ tubular furnace for 2h in an air atmosphere, and cooling to room temperature to obtain the SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material.
The 2-18 GHz wave-absorbing performance analysis chart of the SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material obtained in the embodiment is shown in fig. 8 and fig. 9, wherein it can be seen from fig. 8 that the X wave band can be fully covered by adjusting the thickness within the thickness of 2-4 mm. As can be seen from FIG. 9, the maximum absorption at 16.64GHz is-7.47 dB at a thickness of 2 mm; when the thickness is 2.66mm, the strongest wave absorption value at 14.72GHz is-25.23 dB; when the thickness is 3mm, the strongest wave absorption value is-21.90 dB at 12.48 GHz; the maximum wave absorption value at 8.64GHz is-15.51 dB when the thickness is 4 mm.
Claims (7)
1. A preparation method of a SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material is characterized by comprising the following steps:
firstly, silicon carbide surface pretreatment:
a. adding silicon carbide with the particle size of 1-10 mu m into a silicon carbide ball mill for ball milling for 12-24 h; putting the mixture into a tube furnace, heating the mixture to 500-600 ℃ in air or nitrogen, and carrying out oxidation treatment for 2-4 h to remove surface impurities;
b. dispersing silicon carbide in an acidic hydrophilic solution, stirring for 2-3 h, then ultrasonically dispersing for 1-2 h, and radiating for 1-2 h by microwave to improve the hydrophilicity; then washing with distilled water, filtering, and airing at 15-30 ℃ to obtain hydrophilic silicon carbide;
secondly, synthesizing the SiC-ferrite/carbonaceous material by a one-pot method:
a. weighing hydrophilic silicon carbide, soluble salt for preparing ferrite, fluoride, a precipitator, a carbonaceous material, a silane coupling agent, an alcohol solvent and deionized water, stirring for 1-2 hours, and performing ultrasonic dispersion for 30 min-1 hour to obtain a mixed solution;
wherein the mass ratio of the hydrophilic silicon carbide to the carbonaceous material is 1 (0.25-0.5);
the molar ratio of soluble salt, fluoride and precipitator for preparing ferrite is 1 (2-3): (5-8);
the molar ratio of the hydrophilic silicon carbide to soluble salt for preparing ferrite is 1 (1-2);
the volume percentage concentration of the silane coupling agent in the mixed solution is 0.25-0.5%;
the ratio of the mass of the hydrophilic silicon carbide to the volume of the alcohol solvent is 1 g: (40-60) mL;
the ratio of the mass of the hydrophilic silicon carbide to the volume of the deionized water is 1 g: (40-60) mL;
b. transferring the mixed solution into a high-temperature reaction kettle, heating to 120-150 ℃ at the speed of 2-4 ℃/min, preserving heat for 4-6 h, exchanging water and an alcohol solution after the reaction is finished, centrifuging, cleaning, and then drying in a vacuum drying box to obtain a precursor;
c. and roasting the precursor in a tubular furnace at 350-450 ℃ for 2-4 h under air or nitrogen, and cooling to room temperature to obtain the SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material.
2. The method for preparing the SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material according to claim 1, wherein the acidic hydrophilic solution in the step one b is one of hydrofluoric acid with a volume concentration of 10-20%, concentrated hydrochloric acid with a volume concentration of 10-20%, concentrated nitric acid with a volume concentration of 20-30%, concentrated sulfuric acid with a volume concentration of 40-50%, mellitic acid, azothiosquaric acid, trichloroacetic acid, trinitrobenzenesulfonic acid, trifluoromethanesulfonic acid and trifluoroacetic acid.
3. The method for preparing the SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material according to claim 1 or 2, characterized in that the soluble salt for preparing ferrite in the step two a is nickel salt, iron salt or cobalt salt.
4. The method for preparing the SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material according to claim 3, wherein the nickel salt is one of nickel chloride hexahydrate, nickel sulfate hexahydrate and nickel nitrate hexahydrate; the ferric salt is one of ferric chloride hexahydrate, ferrous sulfate heptahydrate and ferric nitrate nonahydrate; the cobalt salt is one of cobalt chloride hexahydrate, cobalt sulfate heptahydrate and cobalt nitrate hexahydrate.
5. The preparation method of the SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material according to claim 1 or 2, characterized in that the fluoride is ammonia fluoride, sodium fluoride, potassium fluoride, silver fluoride or aluminum fluoride.
6. The preparation method of the SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material according to claim 1 or 2, characterized in that the precipitant is urea, sodium hydroxide, ammonia water, sodium carbonate, potassium carbonate, sodium bicarbonate, disodium hydrogen phosphate, sodium citrate or potassium citrate.
7. The method for preparing the SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material according to claim 1 or 2, wherein the carbonaceous material is graphene, reduced graphene, oxidized graphene, conductive carbon black or carbon nanotubes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811284361.8A CN109346848B (en) | 2018-10-31 | 2018-10-31 | SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811284361.8A CN109346848B (en) | 2018-10-31 | 2018-10-31 | SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109346848A CN109346848A (en) | 2019-02-15 |
| CN109346848B true CN109346848B (en) | 2021-03-12 |
Family
ID=65313145
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811284361.8A Active CN109346848B (en) | 2018-10-31 | 2018-10-31 | SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109346848B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111040729B (en) * | 2019-11-15 | 2022-07-26 | 中国人民解放军陆军工程大学 | Preparation method and application of silicon carbide-based nano composite wave-absorbing material |
| CN111099888A (en) * | 2019-12-31 | 2020-05-05 | 天长市中德电子有限公司 | Preparation method of wave-absorbing ferrite |
| CN111534279B (en) * | 2020-05-13 | 2022-11-29 | 中国电子科技集团公司第三十三研究所 | Preparation method of V-waveband wave-absorbing powder |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1793039A (en) * | 2005-11-07 | 2006-06-28 | 中国科学院上海硅酸盐研究所 | Microwave absorbing composite material with silicon carbide-carbon and preparation process thereof |
| CN102876288A (en) * | 2012-10-29 | 2013-01-16 | 哈尔滨工业大学 | Graphite/barium ferrite composite wave-absorbing material and preparation method thereof |
| CN103524125A (en) * | 2013-10-22 | 2014-01-22 | 沈阳理工大学 | Process method for preparing carbon-black-loaded cobalt zinc ferrite wave-absorbing material |
| CN104341156A (en) * | 2014-10-17 | 2015-02-11 | 西安科技大学 | Silicon carbide based composite microwave-absorbing heating body composition and preparation method thereof |
| CN105609305A (en) * | 2016-01-19 | 2016-05-25 | 吉林大学 | Preparation method of Fe<3>O<4>/graphene composite membrane |
| CN105753059A (en) * | 2016-03-23 | 2016-07-13 | 上海理工大学 | Preparation method of carbon-based magnesium ferrite composite membrane with wave absorbing function |
| CN106281218A (en) * | 2016-08-02 | 2017-01-04 | 哈尔滨工业大学 | Carbon back absorbing material prepared by a kind of aluminosilicate polymer and preparation method thereof |
| CN107365567A (en) * | 2017-06-15 | 2017-11-21 | 广东工业大学 | A kind of absorbing material of carbon fiber surface coated magnetic ferrite nano carbon pipe and its preparation method and application |
-
2018
- 2018-10-31 CN CN201811284361.8A patent/CN109346848B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1793039A (en) * | 2005-11-07 | 2006-06-28 | 中国科学院上海硅酸盐研究所 | Microwave absorbing composite material with silicon carbide-carbon and preparation process thereof |
| CN102876288A (en) * | 2012-10-29 | 2013-01-16 | 哈尔滨工业大学 | Graphite/barium ferrite composite wave-absorbing material and preparation method thereof |
| CN103524125A (en) * | 2013-10-22 | 2014-01-22 | 沈阳理工大学 | Process method for preparing carbon-black-loaded cobalt zinc ferrite wave-absorbing material |
| CN104341156A (en) * | 2014-10-17 | 2015-02-11 | 西安科技大学 | Silicon carbide based composite microwave-absorbing heating body composition and preparation method thereof |
| CN105609305A (en) * | 2016-01-19 | 2016-05-25 | 吉林大学 | Preparation method of Fe<3>O<4>/graphene composite membrane |
| CN105753059A (en) * | 2016-03-23 | 2016-07-13 | 上海理工大学 | Preparation method of carbon-based magnesium ferrite composite membrane with wave absorbing function |
| CN106281218A (en) * | 2016-08-02 | 2017-01-04 | 哈尔滨工业大学 | Carbon back absorbing material prepared by a kind of aluminosilicate polymer and preparation method thereof |
| CN107365567A (en) * | 2017-06-15 | 2017-11-21 | 广东工业大学 | A kind of absorbing material of carbon fiber surface coated magnetic ferrite nano carbon pipe and its preparation method and application |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109346848A (en) | 2019-02-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109705808B (en) | Cobalt-nickel alloy-porous carbon composite wave-absorbing material with MOF structure and preparation method thereof | |
| CN108330471B (en) | Preparation method of yolk type double-shell hollow composite wave-absorbing material | |
| CN109181639B (en) | SiC @ SiO2@ ferrite high-temperature wave-absorbing composite material and preparation method thereof | |
| CN109346848B (en) | SiC-ferrite/carbonaceous material high-temperature wave-absorbing composite material and preparation method thereof | |
| CN112961650A (en) | Tri-metal organic framework derived iron-nickel alloy/porous carbon ultrathin wave absorber and preparation method thereof | |
| CN108154984B (en) | Porous ferroferric oxide/carbon nano rod-shaped electromagnetic wave absorption material and preparation method and application thereof | |
| CN110342531B (en) | Iron powder coated silicon dioxide material and preparation method thereof | |
| CN113316379B (en) | Nano composite structure wave absorber material, preparation method and application | |
| CN105295832A (en) | Preparation method for reduced graphene oxide/Ni-Co ternary composite wave-absorbing material | |
| CN108521754A (en) | Porous carbon-based electromagnetic wave absorption agent of one kind and preparation method thereof | |
| CN114195197B (en) | Magnetic porous carbon compound and preparation method and application thereof | |
| CN112996375B (en) | Cu9S5/C composite material and preparation method and application thereof | |
| CN113413838B (en) | Magnetoelectric aerogel and preparation method thereof | |
| CN108024493B (en) | Lotus seedpod structure mesoporous carbon and nano cobalt compound and preparation method and application thereof | |
| CN112752496A (en) | Hollow nitrogen-doped nickel oxide/nickel/carbon composite material, preparation method and application | |
| CN110564366B (en) | Using NiCl 2 Preparation method for preparing high-temperature-resistant dielectric wave absorber C @ SiC whisker powder | |
| CN110028930B (en) | HalS-Fe3O4@ C composite material and preparation method and application thereof | |
| CN114071982A (en) | Honeycomb reduced graphene oxide foam/nickel nanoparticle wave absorbing agent and preparation method thereof | |
| CN113597247A (en) | Magnetic metal nanoparticle modified carbon hollow sphere wave-absorbing material and preparation method thereof | |
| CN111217342B (en) | Preparation method of porous niobium nitride powder microwave absorbing material | |
| CN110564365B (en) | Preparation method of graphene foam composite material loaded with magnetic hollow nanospheres | |
| CN115332821B (en) | Preparation method of CoNi/NC wave-absorbing material | |
| CN107541186B (en) | Carbon nanotube film and ferrite composite wave-absorbing material and preparation method thereof | |
| CN115745627A (en) | SiCN ceramic wave absorbing agent and preparation method thereof | |
| CN113277567B (en) | Preparation method and application of carbon-coated ferroferric oxide nanocomposite with ordered mesoscopic arrangement |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |