CN113046590B - High-entropy alloy/aluminum composite foam type wave-absorbing material and preparation method thereof - Google Patents
High-entropy alloy/aluminum composite foam type wave-absorbing material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-entropy alloy/aluminum composite foam type wave-absorbing material and a preparation method thereof, and belongs to the field of wave-absorbing materials. The high-entropy alloy is FeCoNiNd0.2B0.6The matrix is aluminum alloy; preparing high-entropy alloy powder by high-energy ball milling; mixing aluminum alloy powder with TiH2Fully mixing the foaming agent, obtaining a pressed blank through cold isostatic pressing, and heating the pressed blank in a microwave smelting furnace to a semi-solid molten state; uniformly spraying high-entropy alloy powder on the surface of a melt by a powder spraying technology, and mechanically stirring and ultrasonically vibrating during the spraying; discharging and casting the mixture into a low-temperature mold to obtain the high-entropy alloy/aluminum composite foam type wave-absorbing material; the material and the method are environment-friendly and pollution-free, the temperature rise and fall can be accurately controlled by microwave heating, the integrity of the reinforced particles is ensured by the semi-solid molten matrix, the interface is cleanly combined, and the foam type wave-absorbing material has the characteristics of light weight, high wave-absorbing performance, high strength and toughness and the like.
Description
Technical Field
The invention belongs to the field of wave-absorbing materials, and relates to a high-entropy alloy/aluminum composite foam wave-absorbing material and a preparation method thereof.
Background
With the development of electronic information technology, various electronic devices are continuously developed, so that the life of people is facilitated on one hand, and the health of people is influenced by electromagnetic pollution generated by the electronic devices on the other hand; in addition, the progress of military radar communication also puts higher requirements on the wave-absorbing stealth performance of the stealth aircraft; therefore, the electromagnetic wave absorbing material has wide application prospect in both life and military.
The wave-absorbing material on the market at present mainly comprises ferrite, and the ferrite is low in price, easy to obtain and good in wave-absorbing performance, so that the wave-absorbing material is widely applied; however, the defects of large specific gravity, low saturation magnetization and narrow absorption band are gradually exposed, and in order to improve the wave-absorbing performance of the ferrite, some researchers make the ferrite into hollow microspheres and the like to improve the specific surface area, make the ferrite into nano-powder or add radioactive elements into the nano-powder to improve the free electrons and the like of the ferrite; however, the preparation problems such as low efficiency, high operation difficulty, environmental and safety hazards and the like gradually appear, and the ferrite has the problems of hardness and brittleness, high-temperature easy demagnetization caused by low curie temperature, poor high-temperature mechanical property and the like, so that the search for alternative wave-absorbing materials with simple preparation process, light weight and excellent mechanical property is the key point of the current research.
The high-entropy alloy is a novel high-mixed-entropy alloy consisting of five or more elements in a molar ratio or a near molar ratio, the content of each metal element is 5-35%, the high entropy value can increase the mutual solubility of the elements, so that the generation of complex phases and a large amount of intermetallic compounds is inhibited, and the performance of the high-entropy alloy is acted by multiple elements; generally, FeCoNi series high-entropy alloy generally has the characteristics of higher saturation magnetization, low coercive force, high strength, high hardness, good high-temperature mechanical property and the like, and after being added, elements Nd and B are mutually combined with Fe on one hand to form a high-magnetism nano precipitated phase, so that the magnetization intensity of the material is improved; nd can improve the high-temperature performance of the alloy, and the element B is B12The regular icosahedron is a basic structural unit, usually exists in a form of interstitial atoms, increases lattice distortion of the high-entropy alloy, has high B ionization energy and large electronegativity, and often generates a metal boride with high melting point with metal, and the more complex the B atomic structure and the higher the chemical stability are along with the increase of the relative content of boron in the boride; in addition, the addition of boron can modify the grain boundary, which has double effects of strengthening the interface and reducing the grain size; the obtained high-entropy alloy has high strength and high temperature stability, the nano-sized particles provide unique wave-absorbing performance, the high-entropy alloy has good impedance matching characteristics, has high dielectric loss and magnetic loss, can absorb electromagnetic waves by means of electronic polarization or interface polarization attenuation of a medium, hysteresis loss, domain wall resonance, aftereffect loss and the like, and has a dispersion strengthening effect on the performance of the material.
The aluminum-based composite material taking the high-entropy alloy as the principal component reinforcing phase is provided, and the high-entropy alloy reinforced aluminum-based composite material obtained by reasonably designing the component components of the high-entropy alloy and adding the component components into the aluminum alloy matrix has the characteristics of high wave absorption, light weight, high strength and toughness and the like, and has important significance for radar stealth, civil electronic equipment, anti-electromagnetic interference equipment and the like.
Disclosure of Invention
The invention aims to provide a high-entropy alloy/aluminum composite foam type wave-absorbing material to overcome performance defects of ferrite materials, such as large specific gravity, narrow wave-absorbing frequency band and poor mechanical property.
The purpose of the invention is realized by the following scheme.
A high-entropy alloy/aluminum composite foam wave-absorbing material is characterized in that: the high-entropy alloy is FeCoNiNd0.2B0.6The matrix is aluminum alloy, and the weight part ratio of the high-entropy alloy to the aluminum alloy is as follows: 15:100, the foaming agent is Ni-coated TiH2And the addition amount of the foaming agent is 0.1-1 wt% of the weight fraction of the aluminum alloy.
Further, the high-entropy alloy powder is prepared from iron, cobalt, nickel, neodymium and boron powder according to a molar ratio of 5:5:5:1:3, wherein the purity of the iron, the cobalt, the nickel and the neodymium is more than or equal to 99.9%, the granularity of the iron, the cobalt, the nickel and the neodymium is 10-20 microns, the purity of the boron powder is more than or equal to 99.99%, and the granularity of the boron powder is 5-10 microns.
Further, the aluminum alloy matrix comprises the following components in percentage by mass: 3.8-4.1%, Mg: 1.3-1.7%, Mn: 0.48-0.52%, Cr: 0.09-0.11%, Zn: 0.24-0.26%, and the balance of Al.
The invention also provides a preparation method of the high-entropy alloy/aluminum composite foam type wave-absorbing material, which comprises the steps of preparing high-entropy alloy particles by using high-energy ball milling, adding the high-entropy alloy into a matrix, uniformly dispersing the high-entropy alloy material in the matrix through microwave smelting and ultrasonic oscillation, and rapidly solidifying the high-entropy alloy material into a wave-absorbing material which is metallurgically combined with the matrix and has low diffusivity of high-entropy alloy components; the method specifically comprises the following steps:
(1) preparing high-entropy alloy powder by high-energy ball milling: iron, cobalt, nickel, neodymium and boron powder are mixed according to the mol ratio of 5:5:5:1:3Mixing the powder, putting the powder into a stainless steel ball-milling tank, adding the stainless steel balls according to the weight ratio of the ball powder, vacuumizing the ball-milling tank, introducing argon, and performing mechanical alloying by adopting a planetary ball mill to obtain FeCoNiNd0.2B0.6High-entropy alloy powder with the average grain diameter of 5 mu m;
(2) and preparing a pressed compact: mixing 2024 aluminum alloy powder and TiH2Ball-milling a foaming agent for 6 hours in an argon atmosphere at the rotating speed of 120r/min to fully and uniformly mix the foaming agent, pouring the mixed powder into a mould, and carrying out static pressure forming, wherein the static pressure is 500MPa and the static pressure time is 10 s;
(3) microwave semi-solid smelting: placing the pressed compact in a microwave stirring smelting furnace, heating and melting the pressed compact under the action of microwaves until the pressed compact is in a semi-solid state, removing surface layer slag, adding high-entropy alloy powder in a powder spraying mode, starting a mechanical stirring arm and an ultrasonic oscillation device to uniformly mix the high-entropy alloy powder and a matrix, and introducing argon for protection in the smelting process;
(4) and casting: casting the melt in a mold after low-temperature treatment, and quickly forming;
(5) solid-state treatment: and (5) sequentially carrying out solid solution treatment and artificial aging treatment on the sample in the step (4), wherein the artificial aging treatment utilizes a microwave device.
Preferably, the mechanical alloying parameters in the step (1) are as follows: pre-ball milling for 6 hours at the rotating speed of 150 r/min; setting the ball milling time to be 72-96h and the rotating speed to be 300-500 r/min; the ball milling temperature in the period is 250-350 ℃, and the ball-material ratio is as follows: 5:1-30:1.
Preferably, in the step (3), the microwave heating rate is 100-150 ℃/min, the temperature is raised to 620-640 ℃, the temperature is melted to a semi-solid state with a solid phase fraction of 45% -60%, the time for stirring and ultrasonic oscillation of the mechanical arm is 10-15 min, the stirring rate is 10-15 r/min, the ultrasonic frequency is 700-1000 kHZ, the powder spraying rate of the high-entropy alloy is 50g/min, and the powder spraying direction is from top to bottom.
Preferably, the temperature of the casting melt in the step (4) is 620-640 ℃, the time is 20-40 s, the speed is 0.4m/min, a mold is soaked in liquid nitrogen before casting, and the temperature of the mold is-50 to-100 ℃.
Preferably, the solution treatment temperature in the step (5) is 480 to 550 ℃, and the solution treatment time is 30 to 45 min.
Preferably, the temperature of the artificial aging treatment in the step (5) is 120-200 ℃, and the time of the aging treatment is 2-8 h.
Preferably, the artificial aging treatment in the step (5) adopts microwave heating, and the microwave frequency is 500 MHZ-300 GHZ.
The principle of the invention is as follows: the selected matrix aluminum alloy belongs to Al-Cu series hard aluminum alloy, and has the advantages of high strength, good forming performance in a hot state and after annealing, and remarkable heat treatment strengthening effect.
The composite phase is selected from high-entropy alloy, because the high-entropy alloy has a high-entropy effect, a solid solution structure can be generated, a strong solid solution strengthening effect can be generated, and the mechanical properties such as strength, hardness and the like of the alloy are obviously improved; the lattice distortion effect hinders the movement of dislocation to further cause obvious solid solution strengthening, and the lattice distortion can increase electrons and phonons during scattering and propagation so as to reduce the electric conductivity and the thermal conductivity; because the high-entropy alloy elements are more in types, the atomic sizes of the high-entropy alloy elements are greatly different, the internal structure of the high-entropy alloy elements is relatively complex, atomic diffusion is hindered, a compact nano-scale precipitated phase is easy to generate, Orowan strengthening is generated, and the like.
The saturation magnetization (Ms) of the FeCoNi high-entropy alloy is high, and the saturation magnetization (Ms) is low, and the saturation magnetization of the FeCoNi high-entropy alloy is reduced by adding any other element; the neodymium element is one of more active rare earth metal elements, and the larger atom size of the neodymium element increases the diffusion difficulty of other elements of the high-entropy alloy; secondly, neodymium has stronger intrinsic magnetic moment and is suitable for being used as an additive of a magnetic material; the B element is a common alloy element, the atom size is small, and small-sized boron atoms can form a gap solid solution in the alloy to achieve the interface solid solution strengthening effect, so that the overall strength and hardness of the alloy are improved; nd, Fe and B elements form a trace amount of nano Nd-Fe-B phase in the alloy, so that the effect of improving the magnetic saturation intensity is achieved.
Microwave smelting is adopted, a stirring rod and ultrasonic waves are jointly stirred, and powder spraying is adopted to add high-entropy alloy powder; the selected high-entropy alloy preparation process is a ball milling process; the method adopts a mode of combining powder metallurgy and vacuum melting, selects the semisolid temperature heating of aluminum, and aims to avoid more impurity reaction generation, ensure smooth stirring in the melting process and avoid rapid sedimentation of high-entropy alloy powder; the powder spraying technology ensures the uniformity of the distribution of the high-entropy alloy, and the ultrasonic-assisted oscillation is adopted to increase the sedimentation rate of the high-entropy alloy powder and avoid the agglomeration phenomenon; the production efficiency is improved by microwave smelting, the preparation process is green, environment-friendly and pollution-free, safe and effective, the repeatability is high, electromagnetic particles existing in the microwave are coupled with the high-entropy alloy, and partial elements of the high-entropy alloy are diffused to an aluminum interface, so that the interface bonding of the material is effectively improved, and the compact and uniform tissue is ensured; the microwave smelting temperature rise is fast, the fast diffusion of elements can be well inhibited, and the integrity of the high-entropy alloy is ensured; in the casting process, the foaming agent escapes from the matrix, so that the surface area of the material is effectively increased, and the wave-absorbing performance of the material is improved.
The heat treatment process comprises solid solution aging and artificial aging treatment, has more obvious effect of improving the structure and the performance of the aluminum-based composite material compared with the conventional aging heat treatment process, and can effectively improve the strength and the plasticity of the aluminum alloy; the microwave field is added in the aging process, so that the movement of vacancies is effectively promoted, the precipitation of fine dispersed phases is accelerated, the strength of the material is improved, and meanwhile, the plasticity and the ductility of the material are improved due to fine particles precipitated by the grain boundary.
Countless bubbles are distributed in the foamed aluminum structure, the holes are formed in a controllable manner, the specific surface area of the material is effectively improved, the foamed aluminum structure is various and contains closed holes, through holes, micro-through holes and the like, the contact surface of electromagnetic waves of the material can be effectively improved, and the wave absorbing performance of the material is improved.
The invention has the beneficial effects that:
(1) the high-entropy alloy/aluminum composite wave-absorbing material has the characteristics of wide wave-absorbing frequency band and high wave-absorbing efficiency, and the maximum reflection loss is improved by nearly one time compared with the conventional ferrite.
(2) Compared with the traditional aluminum-based composite material,the wave absorbing performance is improved by about 1 to 1.5 times, and the density of the obtained composite material is only 2.7 to 2.8g/cm3About 1/2 of the prior stealth material, and the hardness is more than or equal to 125HV0.3The tensile strength is more than or equal to 450 percent, and the elongation is more than or equal to 10 percent.
(3) The high-entropy alloy particles of the high-entropy alloy/aluminum composite wave-absorbing material have dielectric loss and magnetic loss effects, and the obtained composite material has excellent wave-absorbing performance and mechanical properties of light weight, high strength and toughness and the like.
(4) The invention adopts a semi-solid state smelting technology, and can obtain the high-entropy alloy/aluminum composite wave-absorbing material with good particle/matrix metallurgical bonding and uniformly distributed particles along with stirring of a stirring rod and ultrasonic oscillation.
Drawings
FIG. 1 is an XRD pattern of the high-entropy alloy/aluminum composite wave-absorbing material in example 1.
FIG. 2 is an SEM image of the high-entropy alloy/aluminum composite wave-absorbing material in example 1.
FIG. 3 is a wave-absorbing performance diagram of the wave-absorbing material compounded by the high-entropy alloy and the aluminum in example 1.
FIG. 4 is an SEM image of the high-entropy alloy/aluminum composite wave-absorbing material in example 2.
FIG. 5 is a wave-absorbing performance diagram of the wave-absorbing material of example 2.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention is further described in detail below with reference to the accompanying drawings.
Example 1:
the aluminum alloy used in the present embodiment comprises, in mass percent, Cu: 3.8%, Mg: 1.3%, Mn: 0.48%, Cr: 0.09%, Zn: 0.24% and the balance of Al.
The purity of iron, cobalt, nickel and neodymium used in the embodiment is more than or equal to 99.9%, the granularity is 10-20 μm, the purity of boron is more than or equal to 99.99%, and the granularity is 5-10 μm.
The preparation method comprises the following steps:
step 1: iron, cobalt, nickel, neodymium, boron powder and stainless steel balls are mixed according to component design, and then a ball-milling tank is vacuumized and communicated with a vacuum pumpArgon is added, a planetary ball mill is adopted for mechanical alloying, and the ball milling is carried out for 6 hours in advance at the rotating speed of 150 r/min; setting the ball milling time to be 96h, the rotating speed to be 500r/min, the ball milling temperature in the period to be 350 ℃ and the ball-to-material ratio to be 10:1 to obtain FeCoNiNd0.2B0.6The average grain diameter of the high-entropy alloy powder is 5 mu m.
Step 2: mixing aluminum alloy powder and TiH2Ball-milling the foaming agent for 6 hours in argon atmosphere at the rotating speed of 120r/min to fully and uniformly mix the foaming agent; pouring the mixed powder into a mould, and carrying out static pressure forming; static pressure is 500MPa, and static pressure time is 10 s; wherein TiH2The foaming agent is Ni-coated, and the content is 0.5wt. -%)
And step 3: placing the pressed blank in a microwave stirring smelting furnace, heating and melting the pressed blank under the action of microwaves to a semi-solid state temperature to enable the solid phase fraction to be 55%, and removing surface layer slag; adding high-entropy alloy powder in a powder spraying manner, and starting a mechanical stirring arm and an ultrasonic oscillation device to uniformly mix the high-entropy alloy powder and the matrix; the microwave heating rate is 120 ℃/min, the semi-solid state temperature is 640 ℃, the mechanical arm stirring and ultrasonic wave oscillating time is 10min, the stirring rate is 10r/min, the ultrasonic frequency is 1000kHZ, the powder spraying rate is 50g/min, and the powder spraying direction of the high-entropy alloy is from top to bottom; argon is introduced for protection in the smelting process.
And 4, step 4: casting the melt, and casting the melt in a mold which is processed at low temperature in advance at a certain speed to form the melt; the temperature of the casting melt is 640 ℃, the time is 20s, the speed is 0.4m/min, a mould is soaked in liquid nitrogen before casting, and the temperature of the mould is-50 ℃.
And 5: sequentially carrying out solid solution treatment and artificial aging treatment on the sample in the step 4, wherein the artificial aging treatment utilizes a microwave device; the solution treatment temperature is 480 ℃, and the solution treatment time is 45 min; the temperature of the artificial aging treatment is 120 ℃, and the aging treatment time is 4 h; the microwave frequency was 2.45 GHZ.
And (3) detection results: the XRD and SEM of the high-entropy alloy/aluminum composite foam type wave-absorbing material prepared in the embodiment 1 are shown in figures 1 and 2, and it can be seen from the figures that particles of the obtained composite material are uniformly distributed at the interface of a matrix, the structure is compact, the pores and defects are extremely low, figure 3 is a wave-absorbing performance curve of the high-entropy alloy/aluminum composite wave-absorbing material, and it can be seen from the figures that by taking the composite material with the thickness of 1.5mm as an example, the wave-absorbing performance of the material prepared by the embodiment is excellent, the reflection loss is as low as-56 dB and is one time lower than that of ferrite, the wave-absorbing frequency band is 7-14 GHZ, the tensile strength is 543MPa, and the elongation is 11.2%.
Example 2:
the aluminum alloy used in the present example comprises, in mass percent, Cu: 4.1%, Mg: 1.7%, Mn: 0.52%, Cr: 0.11%, Zn: 0.26% and the balance of Al.
The purity of iron, cobalt, nickel and neodymium used in the embodiment is more than or equal to 99.9%, the granularity is 10-20 μm, the purity of boron is more than or equal to 99.99%, and the granularity is 5-10 μm.
The preparation method of the high-entropy alloy/aluminum composite foam wave-absorbing material comprises the following steps:
step 1: iron powder, cobalt powder, nickel powder, neodymium powder, boron powder and stainless steel balls are mixed according to component design, then a ball-milling tank is vacuumized, argon gas is introduced, a planetary ball mill is adopted for mechanical alloying, and ball-milling is carried out for 6 hours in advance at the rotating speed of 150 r/min; setting the ball milling time to be 96h, the rotating speed to be 500r/min, the ball milling temperature in the period to be 350 ℃ and the ball-to-material ratio to be 5:1 to obtain FeCoNiNd0.2B0.6The average grain diameter of the high-entropy alloy powder is 5 mu m.
Step 2: mixing aluminum alloy powder and TiH2Ball-milling the foaming agent for 6 hours in argon atmosphere at the rotating speed of 120r/min to fully and uniformly mix the foaming agent; pouring the mixed powder into a mould, and carrying out static pressure forming; static pressure is 500MPa, and static pressure time is 10 s; wherein TiH2The foaming agent is Ni-coated, and the content is 0.5wt. -%)
And step 3: placing the pressed blank in a microwave stirring smelting furnace, heating and melting the pressed blank under the action of microwaves to a semi-solid state temperature to enable the solid phase fraction to be 55%, and removing surface layer slag; adding high-entropy alloy powder in a powder spraying manner, and starting a mechanical stirring arm and an ultrasonic oscillation device to uniformly mix particles and a matrix; the microwave heating rate is 120 ℃/min, the semi-solid state temperature is 640 ℃, the mechanical arm stirring and ultrasonic wave oscillation time is 15min, the stirring rate is 10r/min, the ultrasonic frequency is 700kHZ, the powder spraying rate is 50g/min, and the powder spraying direction of the high-entropy alloy is from top to bottom; argon is introduced for protection in the smelting process.
And 4, step 4: casting the melt, and casting the melt in a mold which is processed at low temperature in advance at a certain speed to form the melt; the temperature of the casting melt is 640 ℃, the time is 20s, the speed is 0.4m/min, a mould is soaked in liquid nitrogen before casting, and the temperature of the mould is-50 ℃.
And 5: sequentially carrying out solid solution treatment and artificial aging treatment on the sample in the step 4, wherein the artificial aging treatment utilizes a microwave device; the solution treatment temperature is 550 ℃, and the solution treatment time is 30 min; the temperature of the artificial aging treatment is 160 ℃, and the aging treatment time is 4 h; the microwave frequency was 2.45 GHZ.
The embodiment 2 is basically the same as the embodiment 1, except that the ultrasonic frequency is 700kHZ, the solid solution temperature is increased to 550 ℃, the solid solution time is increased to 45min, the aging temperature is increased to 160 ℃, the obtained composite material structure is shown in figure 4, compared with the figure 2, the microstructure can be seen to be thick reinforced particles, but the structure is compact, the pores and the defects are low, the figure 5 is a wave absorbing performance curve of the high-entropy alloy/aluminum composite foam type wave absorbing material, the composite material with the thickness of 2.5mm is taken as an example, the reflection loss of the material prepared by the embodiment is not as that of the embodiment 1, the minimum reflection loss is-33 dB, the frequency band is 8-18 GHZ, the tensile strength is 498MPa, and the wave absorbing elongation is 9.1%.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. A high-entropy alloy/aluminum composite foam type wave-absorbing material is characterized in that: the high-entropy alloy in the material is FeCoNiNd0.2B0.6The matrix is an aluminum alloy, and the high-entropy alloy and the aluminum alloy have the following weight part ratio: 15:100, the foaming agent is Ni-coated TiH2Foaming agent, wherein the addition amount of the foaming agent is 0.1 to up to about 0 weight percent of the aluminum alloy1 wt.%; the aluminum alloy comprises the following components in percentage by mass: 3.8-4.1%, Mg: 1.3-1.7%, Mn: 0.48-0.52%, Cr: 0.09-0.11%, Zn: 0.24-0.26% and the balance of Al.
2. The high-entropy alloy/aluminum composite foam type wave-absorbing material of claim 1, wherein: the high-entropy alloy powder is prepared from iron powder, cobalt powder, nickel powder, neodymium powder and boron powder according to a molar ratio of 5:5:5:1:3, wherein the purity of the iron powder, the cobalt powder, the nickel powder and the neodymium powder is greater than or equal to 99.9%, the granularity of the iron powder, the cobalt powder, the nickel powder and the neodymium powder is 10-20 micrometers, and the purity of the boron powder is greater than or equal to 99.99%, and the granularity of the boron powder is 5-10 micrometers.
3. The preparation method of the high-entropy alloy/aluminum composite foam type wave-absorbing material of claim 1, which is characterized by comprising the following steps:
(1) preparing high-entropy alloy powder by high-energy ball milling: mixing iron powder, cobalt powder, nickel powder, neodymium powder and boron powder according to the molar ratio of 5:5:5:1:3, putting the mixed powder into a stainless steel ball milling tank, adding a stainless steel ball, vacuumizing the ball milling tank, introducing argon gas, and performing mechanical alloying by adopting a planetary ball mill to obtain FeCoNiNd0.2B0.6High-entropy alloy powder with the average grain diameter of 5 mu m;
(2) and preparing a pressed compact: mixing 2024 aluminum alloy powder and TiH2Ball-milling a foaming agent for 6 hours in an argon atmosphere at the rotating speed of 120r/min to fully and uniformly mix the foaming agent, pouring the mixed powder into a mould, and carrying out static pressure forming, wherein the static pressure is 500MPa and the static pressure time is 10 s;
(3) microwave semi-solid smelting: placing the pressed compact in a microwave stirring smelting furnace, heating and melting the pressed compact to a semi-solid state under the action of microwaves, removing surface layer slag, adding high-entropy alloy powder in a powder spraying mode, starting a mechanical stirring arm and an ultrasonic oscillation device to uniformly mix the high-entropy alloy powder and a matrix, and introducing argon for protection in the smelting process;
(4) and casting: casting the melt in a mold after low-temperature treatment, and quickly forming;
(5) solid-state treatment: and (4) sequentially carrying out solid solution treatment and artificial aging treatment on the sample in the step (4), wherein the artificial aging treatment utilizes a microwave device.
4. The preparation method of the high-entropy alloy/aluminum composite foam type wave-absorbing material according to claim 3, characterized in that: the mechanical alloying parameters in the step (1) are as follows: pre-ball milling for 6 hours at the rotating speed of 150 r/min; setting the ball milling time to be 72-96h and the rotating speed to be 300-500 r/min; the ball milling temperature in the period is 250-350 ℃, and the ball-material ratio is as follows: 5:1-30:1.
5. The preparation method of the high-entropy alloy/aluminum composite foam type wave-absorbing material according to claim 3, characterized in that: in the step (3), the microwave heating rate is 100-150 ℃/min, the temperature is raised to 620-640 ℃, the mixture is melted to a semi-solid state with the solid phase fraction of 45% -60%, the mechanical arm stirring and ultrasonic oscillation time is 10-15 min, the stirring rate is 10-15 r/min, the ultrasonic frequency is 700-1000 kHz, the high-entropy alloy powder spraying rate is 50g/min, and the powder spraying direction is from top to bottom.
6. The preparation method of the high-entropy alloy/aluminum composite foam type wave-absorbing material according to claim 3, characterized in that: in the step (4), the temperature of the casting melt is 620-640 ℃, the time is 20-40 s, the casting speed is 0.4m/min, a mould is soaked in liquid nitrogen before casting, and the temperature of the mould is-50 to-100 ℃.
7. A preparation method of the high-entropy alloy/aluminum composite foam type wave-absorbing material according to claim 3, characterized in that: in the step (5), the solution treatment temperature is 480-550 ℃, and the solution treatment time is 30-45 min.
8. The preparation method of the high-entropy alloy/aluminum composite foam type wave-absorbing material according to claim 3, characterized in that: in the step (5), the temperature of the artificial aging treatment is 120-200 ℃, and the time of the aging treatment is 2-8 h.
9. The preparation method of the high-entropy alloy/aluminum composite foam type wave-absorbing material according to claim 3, characterized in that: the artificial aging treatment in the step (5) adopts microwave heating, and the microwave frequency is 500 MHz-300 GHz.
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| CN113860911B (en) * | 2021-10-27 | 2022-08-09 | 江西科技师范大学 | High-entropy ferrite porous ceramic material and preparation method and application thereof |
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