CN115161531A - High-entropy alloy/graphene composite material with wave absorption performance and preparation method thereof - Google Patents
High-entropy alloy/graphene composite material with wave absorption performance and preparation method thereof Download PDFInfo
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 56
- 239000010935 stainless steel Substances 0.000 claims description 43
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- 238000001291 vacuum drying Methods 0.000 claims description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 18
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 17
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/068—Flake-like particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/12—Metallic powder containing non-metallic particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Abstract
The invention discloses a high-entropy alloy/graphene composite material with wave absorption performance, and the molecular formula is (FeNiCrAl) 0.2 ) x @C y The invention also provides a method for preparing the high-entropy alloy/graphene composite material with wave absorption performance, wherein x is more than 92 and less than 98, and x + y is not less than 100. Fe and Ni in the high-entropy alloy/graphene composite material provided by the invention can enhance magnetic loss capacity and wave-absorbing energyThe high-temperature oxidation resistance and the corrosion resistance of Al and Cr are improved, the impedance matching and attenuation characteristics are improved by adding graphene, the magnetic loss is mainly contributed by high-entropy alloy, the dielectric loss is mainly contributed by graphene, multiple electromagnetic wave loss mechanisms act synergistically, the impedance matching is good, electromagnetic waves are absorbed to the maximum extent, and the effect of improving the reflection loss is achieved.
Description
Technical Field
The invention belongs to the technical field of composite wave-absorbing materials, and particularly relates to a high-entropy alloy/graphene composite material with wave-absorbing performance and a preparation method thereof.
Background
With the rapid development of the electronic industry, electromagnetic pollution also becomes the fourth largest pollution following atmospheric pollution, water pollution and noise pollution. Electromagnetic wave pollution not only interferes with the normal operation of electronic equipment, but also harms the physical and mental health of human beings. The wave-absorbing material is a material which reduces the interference of electromagnetic waves by absorbing the energy of received electromagnetic waves, and people and equipment can be prevented from being injured by the electromagnetic waves. Whether for the purpose of protecting the environment and the human health, or guaranteeing the information safety and the national defense safety, the research and the improvement of the wave-absorbing material are imperative, and the wave-absorbing performance is continuously improved and improved.
At present, the traditional wave-absorbing material is thick and poor in impedance matching, so that the absorption strength is low, and the equipment performance is directly influenced. The high-entropy alloy is a novel material, and has excellent performance in various aspects, particularly the electromagnetic wave absorption performance. The high-entropy alloy is prepared into the alloy with required mechanical and physicochemical properties by adjusting the proportion of each element. The high-entropy alloy supplements the existing alloy system by virtue of unique structural performance characteristics, expands the understanding of people on the middle area of a multi-element phase diagram, and theoretically enriches the cognition of classical physical metallurgy. With the deep research of the high-entropy alloy, the high-entropy alloy composite material provides a larger space for the selection of the components of the wave-absorbing material. The high-entropy alloy and the carbon material are compounded, and the component design combining magnetic loss and electric loss can provide more electromagnetic loss approaches for the wave-absorbing material, so that the wave-absorbing performance is effectively improved.
Therefore, the high-entropy alloy/graphene composite material with wave-absorbing performance and the preparation method thereof are needed to be provided, so that the high-entropy alloy/graphene composite material is suitable for the wave-absorbing field, and the wave-absorbing performance is effectively improved.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a high-entropy alloy/graphene composite material with wave absorption performance, aiming at the defects of the prior art. The high-entropy alloy/graphene composite material contains Fe and Ni ferromagnetic elements, so that the magnetic loss capacity and the wave absorbing capacity are enhanced, al and Cr elements can enhance the corrosion resistance of the alloy while improving the high-temperature oxidation resistance, the impedance matching and attenuation characteristics are improved by adding graphene, the magnetic loss is mainly contributed by the high-entropy alloy, the dielectric loss is mainly contributed by the graphene, multiple electromagnetic wave loss mechanisms have synergistic effect, the impedance matching is good, electromagnetic waves are absorbed to the maximum extent, and the effect of improving the reflection loss is achieved.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: the high-entropy alloy/graphene composite material with the wave absorption performance is characterized in that the molecular formula of the composite material is (FeNiCrAl) 0.2 ) x @C y Wherein x and y are high-entropy alloy FeNiCrAl 0.2 And graphene C, and 92 < x < 98, x + y =100.
The high-entropy alloy/graphene composite material disclosed by the invention contains Fe and Ni ferromagnetic elements, the magnetic loss capacity of the high-entropy alloy/graphene composite material is enhanced, the wave absorbing capacity of the high-entropy alloy/graphene composite material is improved, meanwhile, al and Cr elements improve the high-temperature oxidation resistance of the high-entropy alloy/graphene composite material and can enhance the corrosion resistance of the alloy.
The high-entropy alloy/graphene composite material with wave absorption performance is characterized in that the molecular formula of the composite material is (FeNiCrAl) 0.2 ) x @C y Wherein x and y are high-entropy alloy FeNiCrAl 0.2 And graphene C, and 92 < x < 94, x + y =100. According to the invention, the ratio of the high-entropy alloy and the graphene composite material is controlled, so that the high-entropy alloy and the graphene composite material have the optimal wave-absorbing performance.
In addition, the invention also provides a method for preparing the high-entropy alloy/graphene composite material with wave absorption performance, which is characterized by comprising the following steps:
step one, mixing and grinding aluminum powder, chromium powder, iron powder, nickel powder and graphene powder to obtain a mixture;
step two, drying the mixture obtained in the step one to obtain a dried mixture;
step three, adding the dried mixture, absolute ethyl alcohol and stainless steel grinding balls obtained in the step two into a stainless steel ball milling tank purified by absolute ethyl alcohol for stirring, then packaging the stainless steel ball milling tank, performing reciprocating vacuum pumping and argon filling for a plurality of times to obtain a sealed stainless steel ball milling tank with a vacuum state inside;
transferring the sealed stainless steel ball milling tank obtained in the step three to a high-speed ball mill for ball milling to obtain powder in the stainless steel ball milling tank;
step five, drying the powder obtained in the step four to obtain the high-entropy alloy/graphene composite material with wave absorption performance;
and step six, screening the high-entropy alloy/graphene composite material obtained in the step five to obtain the high-entropy alloy/graphene composite powdery material in the shape of multi-scale irregular flakes.
The method is characterized in that in the step one, the mass purity of the aluminum powder is more than 99.9%, the particle size of the aluminum powder is less than 5 μm, the mass purity of the chromium powder is more than 99.9%, the particle size of the chromium powder is less than 10 μm, the mass purity of the iron powder is more than 99.9%, the particle size of the iron powder is less than 10 μm, the mass purity of the nickel powder is more than 99.9%, the particle size of the nickel powder is less than 50 μm, and the mass purity of the graphene powder is more than 99.9%, and the particle size of the graphene powder is less than 20 μm. According to the invention, the purity and the particle size of the raw materials are limited, so that the influence of uncertain factors such as impurities on the material performance is prevented, and the uniformity of the alloy powder in the ball milling process is ensured.
The method is characterized in that in the step one, the mixing and grinding are carried out by using an agate mortar, and absolute ethyl alcohol with the mass purity of more than 99.95% is added for multiple times in the mixing and grinding. According to the invention, due to the fact that the density of the graphene is low, the component deviation caused by the reduction of the quality of the graphene in the grinding process is avoided by adding the absolute ethyl alcohol for many times, the agglomeration and wall adhesion of the powder are inhibited, and the surface activity of the powder is reduced.
The method is characterized in that the vacuum degree in the sealed stainless steel ball milling tank in the vacuum state in the step three is less than 0.1Pa. According to the invention, by controlling the vacuum degree in the sealed stainless steel ball milling tank, the temperature in the ball milling tank can rise in the ball milling process, so that the internal pressure is increased, if the ball milling tank is not vacuumized at the beginning of ball milling, the cover of the ball milling tank is pushed open due to overlarge internal pressure in the ball milling process, so that air enters, so that a sample is oxidized, and after the ball milling tank is vacuumized, the ball milling tank is always in a vacuum sealing state due to the action of atmospheric pressure which is greater than the pressure in the tank body, so that air is prevented from entering oxidized powder.
The method is characterized in that the ball milling parameters in the fourth step are as follows: the rotating speed of the ball mill is 300 r/min-400 r/min, the ball milling time is 60 h-90 h, and the ball material ratio is 15; the grain size of the powder is less than 50 mu m. According to the invention, by limiting ball milling conditions, the mechanical alloying effect of the grinding balls on the raw material powder is ensured, and the serious iron scrap pollution caused by the damage of the ball milling tank due to the overlarge impact force of the grinding balls and the influence on the component content of the high-entropy alloy wave-absorbing material are avoided; the particle size of the powder is controlled in order to obtain composite material powder with smaller particle size.
The method is characterized in that the drying process in the second step and the fifth step is as follows: heating to 60-80 ℃ in a vacuum drying oven under the condition that the vacuum degree is not more than 0.1Pa, and then preserving heat for more than 24h, introducing argon into the vacuum drying oven in the drying process, and keeping the flow rate of the argon to be more than 0.1L/min. In the invention, the drying in the second step is to ensure that the mass ratio of the ethanol added in the fifth step to the powder is consistent, the vacuum degree is not more than 0.1Pa for unifying the process, the ball milling tank is heated to 60-80 ℃ and is kept warm for more than 24 hours to completely volatilize the ethanol, and the argon is introduced and the flow rate of the argon is kept to be 0.1L/min to prevent the residual air from oxidizing the sample.
Compared with the prior art, the invention has the following advantages:
1. the high-entropy alloy/graphene composite material contains Fe and Ni ferromagnetic elements, so that the magnetic loss capacity and the wave absorption capacity are enhanced, al and Cr elements can enhance the corrosion resistance of the alloy while enhancing the high-temperature oxidation resistance, the graphene is added to improve the impedance matching and attenuation characteristics, so that incident electromagnetic waves can enter the high-entropy alloy/graphene composite material as much as possible, the minimum reflection is realized on the surface, the energy of the electromagnetic waves is strongly attenuated under the synergistic action of multiple loss mechanisms, namely, the electromagnetic loss is increased, the electromagnetic waves are absorbed to the maximum extent, the ductility of the alloy can be improved, the composite material is uniformly dispersed on a high-entropy alloy matrix to obtain a thinner lamellar shape, the magnetic loss is mainly contributed by the high-entropy alloy, the dielectric loss is mainly contributed by the graphene, the synergistic action of multiple electromagnetic wave loss mechanisms is good in impedance matching, the electromagnetic waves are absorbed to the maximum extent, and the effect of improving the reflection loss is achieved.
2. According to the invention, the high-entropy alloy/graphene composite material is prepared by using a mechanical alloying method, so that the high-entropy alloy and graphene are compounded, the absolute ethyl alcohol is added for multiple times in the ball milling process, the component deviation caused by the reduction of the quality of the graphene in the grinding process is avoided, the agglomeration and wall adhesion of powder are inhibited, the surface activity of the powder is reduced, and the high-entropy alloy/graphene composite material with magnetic loss and electric loss is prepared, so that the wave-absorbing performance of the high-entropy alloy/graphene composite material is improved.
3. The method for preparing the high-entropy alloy/graphene composite material has multiple polarizations, including space charge polarization, dipole polarization, surface polarization and interface polarization, and has magnetic loss and electric loss, so that the purpose of reducing the thickness of the material and realizing excellent wave absorption performance is achieved.
4. The maximum reflection loss value of the high-entropy alloy/graphene composite material prepared by the invention is-42.5 dB, the effective wave-absorbing bandwidth which is less than-10 dB can reach 4.9GHz as high as possible, the attenuation constant is increased along with the increase of the frequency, the wave-absorbing performance follows the quarter wavelength principle, and the high-entropy alloy/graphene composite material is suitable for complex and severe military operation environments and is subject to the gradual flooding of electromagnetic pollution.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
Fig. 1 is a morphology diagram of the high-entropy alloy/graphene composite material prepared in embodiment 1 of the present invention.
Fig. 2 is a wave-absorbing property curve of the high-entropy alloy/graphene composite material prepared in embodiment 2 of the present invention.
Fig. 3 is a wave-absorbing performance curve of the high-entropy alloy/graphene composite material prepared in embodiment 3 of the present invention.
Detailed Description
Example 1
The embodiment comprises the following steps:
step one, mixing and grinding aluminum powder, chromium powder, iron powder, nickel powder and graphene powder to obtain a mixture; the mass purity of the aluminum powder is more than 99.9%, the granularity is less than 5 microns, the mass purity of the chromium powder is more than 99.9%, the granularity is less than 10 microns, the mass purity of the iron powder is more than 99.9%, the granularity is less than 10 microns, the mass purity of the nickel powder is more than 99.9%, the granularity is less than 50 microns, the mass purity of the graphene powder is more than 99.9%, and the granularity is less than 20 microns; the mixing and grinding are carried out by using an agate mortar, and absolute ethyl alcohol with the mass purity of more than 99.95 percent is added for multiple times in the mixing and grinding;
step two, drying the mixture obtained in the step one to obtain a dried mixture; the drying process comprises the following steps: heating to 70 ℃ in a vacuum drying oven under the condition that the vacuum degree is not more than 0.1Pa, and then preserving heat for more than 24h, introducing argon into the vacuum drying oven in the drying process, and keeping the flow rate of the argon to be more than 0.1L/min;
step three, adding 30g of the dried mixture obtained in the step two, 20ml of absolute ethyl alcohol and 600g of stainless steel grinding balls into a stainless steel ball milling tank purified by the absolute ethyl alcohol for stirring, then packaging the stainless steel ball milling tank, and performing reciprocating vacuum pumping and argon filling for several times to obtain a sealed stainless steel ball milling tank with the interior in a vacuum state; the vacuum degree in the sealed stainless steel ball milling tank in the vacuum state is less than 0.1Pa;
transferring the sealed stainless steel ball milling tank obtained in the step three to a high-speed ball mill for ball milling to obtain powder in the stainless steel ball milling tank; the ball milling parameters are as follows: the rotating speed of the ball mill is 400r/min, and the ball milling time is 60h; the particle size of the powder is less than 50 mu m;
step five, drying the powder obtained in the step four to obtain the high-entropy alloy/graphene composite material with wave absorption performance; the drying process comprises the following steps: heating to 80 ℃ in a vacuum drying oven under the condition that the vacuum degree is not more than 0.1Pa, and then preserving heat for more than 24h, introducing argon into the vacuum drying oven in the drying process, and keeping the flow rate of the argon to be more than 0.1L/min;
and step six, screening the high-entropy alloy/graphene composite material obtained in the step five to obtain the high-entropy alloy/graphene composite material.
Through detection, the molecular formula of the high-entropy alloy/graphene composite material prepared by the embodiment is (FeNiCrAl) 0.2 ) 97.5 @C 2.5 The maximum reflection loss value of the high-entropy alloy/graphene composite material is-37.6 dB when the thickness is 2.5mm, the effective wave-absorbing bandwidth is 2.6GHz less than-10 dB, the attenuation constant is increased along with the increase of the frequency, and the wave-absorbing performance follows a quarter wavelength principle.
Fig. 1 is a morphology diagram of the high-entropy alloy/graphene composite material prepared in this embodiment, and as can be seen from fig. 1, the prepared high-entropy alloy/graphene composite material has a multi-scale irregular sheet structure.
Example 2
The embodiment comprises the following steps:
step one, mixing and grinding aluminum powder, chromium powder, iron powder, nickel powder and graphene powder to obtain a mixture with the total weight of 30 g; the mass purity of the aluminum powder is more than 99.9%, the particle size of the aluminum powder is less than 5 microns, the mass purity of the chromium powder is more than 99.9%, the particle size of the chromium powder is less than 10 microns, the mass purity of the iron powder is more than 99.9%, the particle size of the iron powder is less than 10 microns, the mass purity of the nickel powder is more than 99.9%, the particle size of the nickel powder is less than 50 microns, and the mass purity of the graphene powder is more than 99.9%, and the particle size of the graphene powder is less than 20 microns; the mixing and grinding are carried out by using an agate mortar, and absolute ethyl alcohol with the mass purity of more than 99.95 percent is added for multiple times in the mixing and grinding;
step two, drying the mixture obtained in the step one to obtain a dried mixture; the drying process comprises the following steps: heating to 60 ℃ in a vacuum drying oven under the condition that the vacuum degree is not more than 0.1Pa, and then preserving heat for more than 24h, introducing argon into the vacuum drying oven in the drying process, and keeping the flow rate of the argon to be more than 0.1L/min;
step three, adding 40g of the dried mixture obtained in the step two, 20ml of absolute ethyl alcohol and 600g of stainless steel grinding balls into a stainless steel ball milling tank purified by the absolute ethyl alcohol for stirring, then packaging the stainless steel ball milling tank, and performing reciprocating vacuum pumping and argon filling for a plurality of times to obtain a sealed stainless steel ball milling tank with a vacuum state inside; the vacuum degree in the sealed stainless steel ball milling tank in the vacuum state is less than 0.1Pa;
transferring the sealed stainless steel ball milling tank obtained in the step three to a high-speed ball mill for ball milling to obtain powder in the stainless steel ball milling tank; the ball milling parameters are as follows: the rotating speed of the ball mill is 350r/min, and the ball milling time is 80h; the particle size of the powder is less than 50 mu m;
step five, drying the powder obtained in the step four to obtain the high-entropy alloy/graphene composite material with wave absorption performance; the drying process comprises the following steps: heating to 60 ℃ in a vacuum drying oven under the condition that the vacuum degree is not more than 0.1Pa, and then preserving heat for more than 24h, introducing argon into the vacuum drying oven in the drying process, and keeping the flow rate of the argon to be more than 0.1L/min;
and step six, screening the high-entropy alloy/graphene composite material obtained in the step five to obtain the high-entropy alloy/graphene composite material.
Through detection, the molecular formula of the high-entropy alloy/graphene composite material prepared by the embodiment is (FeNiCrAl) 0.2 ) 96 @C 4 The high-entropy alloy/graphene composite material has a multi-scale irregular sheet structure, the maximum reflection loss value is-42.5 dB when the thickness is 2.5mm, the effective wave-absorbing bandwidth is 2.7GHz less than-10 dB, the attenuation constant is increased along with the increase of frequency, and the wave-absorbing performance follows a quarter wavelength principle.
Fig. 2 is a wave-absorbing performance curve of the high-entropy alloy/graphene composite material prepared in this embodiment, and it can be seen from fig. 2 that different curves represent wave-absorbing tests performed by using high-entropy alloy/graphene composite materials with different thicknesses, and it can be seen that the reflection loss increases first and then decreases with the increase of the thickness of the wave-absorbing layer, reaches a maximum value when the thickness is 2.5mm, and the maximum reflection loss value is-42.5 dB, that is, the wave-absorbing performance is the best at this time.
Example 3
The embodiment comprises the following steps:
step one, mixing and grinding aluminum powder, chromium powder, iron powder, nickel powder and graphene powder to obtain a mixture with the total weight of 30 g; the mass purity of the aluminum powder is more than 99.9%, the granularity is less than 5 microns, the mass purity of the chromium powder is more than 99.9%, the granularity is less than 10 microns, the mass purity of the iron powder is more than 99.9%, the granularity is less than 10 microns, the mass purity of the nickel powder is more than 99.9%, the granularity is less than 50 microns, the mass purity of the graphene powder is more than 99.9%, and the granularity is less than 20 microns; the mixing and grinding are carried out by using an agate mortar, and absolute ethyl alcohol with the mass purity of more than 99.95 percent is added for multiple times in the mixing and grinding;
step two, drying the mixture obtained in the step one to obtain a dried mixture; the drying process comprises the following steps: heating to 80 ℃ in a vacuum drying oven under the condition that the vacuum degree is not more than 0.1Pa, and then preserving heat for more than 24h, introducing argon into the vacuum drying oven in the drying process, and keeping the flow rate of the argon to be more than 0.1L/min;
step three, adding 35g of the dried mixture obtained in the step two, 20ml of absolute ethyl alcohol and 600g of stainless steel grinding balls into a stainless steel ball milling tank purified by the absolute ethyl alcohol for stirring, then packaging the stainless steel ball milling tank, and performing reciprocating vacuum pumping and argon filling for several times to obtain a sealed stainless steel ball milling tank with the interior in a vacuum state; the vacuum degree in the sealed stainless steel ball milling tank in the vacuum state is less than 0.1Pa;
transferring the sealed stainless steel ball milling tank obtained in the step three to a high-speed ball mill for ball milling to obtain powder in the stainless steel ball milling tank; the ball milling parameters are as follows: the rotating speed of the ball mill is 400r/min, and the ball milling time is 60 hours; the particle size of the powder is less than 50 mu m;
step five, drying the powder obtained in the step four to obtain the high-entropy alloy/graphene composite material with wave absorption performance; the drying process comprises the following steps: heating to 70 ℃ in a vacuum drying oven under the condition that the vacuum degree is not more than 0.1Pa, and then preserving heat for more than 24h, introducing argon into the vacuum drying oven in the drying process, and keeping the flow rate of the argon to be more than 0.1L/min;
and step six, screening the high-entropy alloy/graphene composite material obtained in the step five to obtain the high-entropy alloy/graphene composite material.
Upon detection, the product of this exampleThe molecular formula of the high-entropy alloy/graphene composite material is (FeNiCrAl) 0.2 ) 94 @C 6 The high-entropy alloy/graphene composite material has a multi-scale irregular sheet structure, the maximum reflection loss value of the high-entropy alloy/graphene composite material is-37.3 dB when the thickness is 2mm, the effective wave-absorbing bandwidth is less than-10 dB and is 4.9GHz, the attenuation constant is increased along with the increase of frequency, and the wave-absorbing performance follows a quarter-wavelength principle.
Fig. 3 is a wave-absorbing performance curve of the high-entropy alloy/graphene composite material prepared in this embodiment, and it can be seen from fig. 3 that different curves represent wave-absorbing tests performed by using high-entropy alloy/graphene composite materials with different thicknesses, and it can be seen that the reflection loss increases first and then decreases with the increase of the thickness of the wave-absorbing layer, and reaches a maximum value when the thickness is 2mm, and the maximum reflection loss value is-37.3 dB, that is, the wave-absorbing performance is the best at this time.
Example 4
The embodiment comprises the following steps:
step one, mixing and grinding aluminum powder, chromium powder, iron powder, nickel powder and graphene powder to obtain a mixture with the total weight of 30 g; the mass purity of the aluminum powder is more than 99.9%, the granularity is less than 5 microns, the mass purity of the chromium powder is more than 99.9%, the granularity is less than 10 microns, the mass purity of the iron powder is more than 99.9%, the granularity is less than 10 microns, the mass purity of the nickel powder is more than 99.9%, the granularity is less than 50 microns, the mass purity of the graphene powder is more than 99.9%, and the granularity is less than 20 microns; the mixing and grinding are carried out by adopting an agate mortar, and absolute ethyl alcohol with the mass purity of more than 99.95 percent is added for multiple times in the mixing and grinding;
step two, drying the mixture obtained in the step one to obtain a dried mixture; the drying process comprises the following steps: heating to 70 ℃ in a vacuum drying oven under the condition that the vacuum degree is not more than 0.1Pa, and then preserving heat for more than 24h, introducing argon into the vacuum drying oven in the drying process, and keeping the flow rate of the argon to be more than 0.1L/min;
step three, adding 30g of the dried mixture obtained in the step two, 20ml of absolute ethyl alcohol and 600g of stainless steel grinding balls into a stainless steel ball milling tank purified by the absolute ethyl alcohol for stirring, then packaging the stainless steel ball milling tank, and performing reciprocating vacuum pumping and argon filling for several times to obtain a sealed stainless steel ball milling tank with the interior in a vacuum state; the vacuum degree in the sealed stainless steel ball milling tank in the vacuum state is less than 0.1Pa;
transferring the sealed stainless steel ball milling tank obtained in the step three to a high-speed ball mill for ball milling to obtain powder in the stainless steel ball milling tank; the ball milling parameters are as follows: the rotating speed of the ball mill is 300r/min, and the ball milling time is 90h; the particle size of the powder is less than 50 mu m;
step five, drying the powder obtained in the step four to obtain the high-entropy alloy/graphene composite material with wave absorption performance; the drying process comprises the following steps: heating to 70 ℃ in a vacuum drying oven under the condition that the vacuum degree is not more than 0.1Pa, and then preserving heat for more than 24h, introducing argon into the vacuum drying oven in the drying process, and keeping the flow rate of the argon to be more than 0.1L/min;
and step six, screening the high-entropy alloy/graphene composite material obtained in the step five to obtain the high-entropy alloy/graphene composite powdery material in the shape of multi-scale irregular flakes.
Through detection, the molecular formula of the high-entropy alloy/graphene composite material prepared by the embodiment is (FeNiCrAl) 0.2 ) 92 @C 8 The high-entropy alloy/graphene composite material has a multi-scale irregular sheet structure, the maximum reflection loss value of-35.5 dB and an effective wave-absorbing bandwidth of 2.8GHz less than-10 dB when the thickness of the high-entropy alloy/graphene composite material is 2.5mm, the attenuation constant is increased along with the increase of frequency, and the wave-absorbing performance follows a quarter-wavelength principle.
The results of the saturation magnetization Ms and the coercive force Hc of the high-entropy alloy/graphene composite material prepared in the embodiments 1 to 4 of the present invention are shown in table 1, and it can be seen from table 1 that the saturation magnetization Ms of the high-entropy alloy/graphene composite material prepared in the present invention is up to 0.196emu/g, and the coercive force Hc is only 87.70Oe.
TABLE 1
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (8)
1. The high-entropy alloy/graphene composite material with the wave absorption performance is characterized in that the molecular formula of the composite material is (FeNiCrAl) 0.2 ) x @C y Wherein x and y are high-entropy alloy FeNiCrAl 0.2 And graphene C, and 92 < x < 98, x + y =100.
2. A high entropy alloy/graphene composite material with wave absorbing properties as claimed in claim 1, wherein the composite material has a molecular formula of (FeNiCrAl) 0.2 ) x @C y Wherein x and y are high-entropy alloy FeNiCrAl 0.2 And graphene C, and 92 < x < 94, x + y=100.
3. A method of preparing a high entropy alloy/graphene composite material having wave absorbing properties as claimed in claim 1 or claim 2, comprising the steps of:
step one, mixing and grinding aluminum powder, chromium powder, iron powder, nickel powder and graphene powder to obtain a mixture;
step two, drying the mixture obtained in the step one to obtain a dried mixture;
step three, adding the dried mixture obtained in the step two, absolute ethyl alcohol and stainless steel grinding balls into a stainless steel ball milling tank purified by the absolute ethyl alcohol for stirring, then packaging the stainless steel ball milling tank, and performing reciprocating vacuum pumping and argon filling for a plurality of times to obtain a sealed stainless steel ball milling tank with a vacuum state inside;
step four, transferring the sealed stainless steel ball milling tank obtained in the step three to a high-speed ball mill for ball milling to obtain powder in the stainless steel ball milling tank;
step five, drying the powder obtained in the step four to obtain the high-entropy alloy/graphene composite material with wave absorption performance;
and step six, screening the high-entropy alloy/graphene composite material obtained in the step five to obtain the high-entropy alloy/graphene composite powdery material in the shape of multi-scale irregular flakes.
4. The method according to claim 3, wherein in step one, the mass purity of the aluminum powder is more than 99.9%, the particle size is less than 5 μm, the mass purity of the chromium powder is more than 99.9%, the particle size is less than 10 μm, the mass purity of the iron powder is more than 99.9%, the particle size is less than 10 μm, the mass purity of the nickel powder is more than 99.9%, the particle size is less than 50 μm, and the mass purity of the graphene powder is more than 99.9%, and the particle size is less than 20 μm.
5. The method according to claim 3, wherein the mixing and grinding in the first step is carried out by using an agate mortar, and absolute ethyl alcohol with the mass purity of more than 99.95% is added in multiple times in the mixing and grinding.
6. The method of claim 3, wherein the vacuum inside the sealed stainless steel ball mill pot in the vacuum state in step three is less than 0.1Pa.
7. The method of claim 3, wherein the ball milling parameters in step four are: the rotating speed of the ball mill is 300 r/min-400 r/min, the ball milling time is 60 h-90 h, and the ball-material ratio is 15; the grain size of the powder is less than 50 mu m.
8. The method of claim 3, wherein the drying process in the second and fifth steps is: heating to 60-80 ℃ in a vacuum drying oven under the condition that the vacuum degree is not more than 0.1Pa, and then preserving heat for more than 24h, introducing argon into the vacuum drying oven in the drying process, and keeping the flow rate of the argon to be more than 0.1L/min.
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