CN113088746B - High-entropy alloy particle refinement reinforced aluminum-based composite material and preparation method thereof - Google Patents
High-entropy alloy particle refinement reinforced aluminum-based composite material and preparation method thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 65
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 50
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910000838 Al alloy Inorganic materials 0.000 claims abstract description 83
- 239000011159 matrix material Substances 0.000 claims abstract description 78
- 238000003756 stirring Methods 0.000 claims abstract description 58
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- 229910052786 argon Inorganic materials 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 7
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- 229910018520 Al—Si Inorganic materials 0.000 claims description 2
- JFBZPFYRPYOZCQ-UHFFFAOYSA-N [Li].[Al] Chemical compound [Li].[Al] JFBZPFYRPYOZCQ-UHFFFAOYSA-N 0.000 claims description 2
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- 238000009749 continuous casting Methods 0.000 claims description 2
- 238000001125 extrusion Methods 0.000 claims description 2
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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Abstract
The invention discloses a high-entropy alloy grain refinement reinforced aluminum-based composite material and a preparation method thereof. The high-entropy alloy particles prepared after mechanical alloying are added into a molten aluminum alloy matrix through a gas dispersion stirring device, stirred and dispersed, then vibration degassing is carried out, and finally a casting process is adopted to prepare a formed part of the high-entropy alloy particle reinforced aluminum matrix composite material. The process disperses the high-entropy alloy particles added into the melt by a gas dispersing and stirring device, increases the contact area and wettability of the high-entropy alloy particles and the aluminum alloy, avoids agglomeration, ensures uniform macroscopic and microscopic dispersion, improves interface bonding property, greatly increases nucleation points in the whole matrix during solidification, refines grains, improves tissues and strengthens performance.
Description
Technical Field
The invention relates to a high-entropy alloy particle reinforced aluminum matrix composite material and a stirring casting preparation process thereof, belonging to the field of metal matrix composite material preparation.
Background
Most of the composite materials used as reinforcing phases are ceramic particles, fibers, metal particle fibers and the like, and the composite materials have better strength and toughness, but have various problems such as poor wettability between ceramic particles and fiber reinforcements and aluminum substrates, poor interface bonding, uneven particle distribution and the like, and seriously affect the mass production and popularization and application of the aluminum-based composite materials for structures.
The high-entropy alloy is a novel multi-principal element alloy composed of five or more elements, and the molar mass of each element is equal or nearly equal. Thus, high entropy alloys have many textures and properties that are different from conventional alloys, such as high strength, good thermal stability, wear and corrosion resistance, high thermal resistance, high electrical resistance, and the like. The interface wettability and the interface compatibility of the high-entropy alloy and the aluminum matrix are good due to the natural interface bonding characteristic before metal and metal, and the problems of poor wettability, poor interface bonding and the like between the ceramic particle reinforcement and the metal matrix can be solved. Reports on preparing high-entropy alloy particle reinforced aluminum-based composite materials by adopting powder metallurgy, hot extrusion, hot-pressed sintering and the like are adopted, but the processes have great difficulty in forming large-size composite material blocks and formed parts. The liquid stirring method has great advantages in the aspect of preparing and forming the large-size composite material, but the liquid stirring method has great difficulty in uniformly dispersing and mixing the high-entropy alloy particles into the matrix, the high-entropy alloy particles have large specific surface area, and the high-entropy alloy particles tend to float on the surface of the melt and cannot be well wetted and dispersed with the aluminum alloy matrix at high temperature by adopting the conventional stirring and powder adding mode. The patent CN2015188188. X seals the high-entropy alloy particles into an aluminum alloy tube, then adds the segmented aluminum alloy tube into a molten matrix, and then stirs and disperses, the patent adopts the method that the high-entropy alloy particles are wrapped and pressed into the aluminum alloy matrix to stir, so as to prevent the particles from drifting to the surface of the material, but the problem is that the high-entropy alloy particles still contact with the aluminum alloy matrix in the form of a large number of agglomerates when the aluminum alloy tube is melted, the problem of poor dispersion and poor wetting still exists when the single particles are insufficiently contacted with the aluminum alloy matrix, the pure mechanical stirring can only macroscopically disperse the high-entropy alloy particles, the microscopic dispersion is uneven, the phenomenon that a large number of particle agglomerates are wrapped and solidified still exists in the solidification structure, this has hindered the improvement of the micro-uniformity and the structural properties of the composite material, especially as the proportion of the added high-entropy alloy components increases, the probability and the area of contact between the individual particles and the aluminum alloy matrix are further reduced, the pure mechanical stirring can only macroscopically disperse the high-entropy alloy particles, the problems of poor local micro-part dispersion and poor wetting become serious, the micro-dispersion is uneven, a large number of particle aggregates exist in the solidification structure and are wrapped and solidified, a large number of black lamellar particles appear in fig. 3 of the patent CN2015188188. X, and the agglomerates are formed by the poor dispersion of the high-entropy alloy, in addition, the micro-part of the high-entropy alloy particles is very favorable for heterogeneous nucleation of the high-temperature aluminum alloy matrix if the micro-part can be sufficiently evenly dispersed, so that the grains are greatly refined.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: how to improve the wettability of the reinforced phase particles and the matrix melt, so that the high-entropy alloy particles are fully and uniformly distributed in the alloy matrix in a macroscopic and microscopic manner, the fine grain effect and the particle reinforcing effect are further improved, and the comprehensive performance of the aluminum-based material is improved.
In order to solve the technical problems, the invention provides a preparation method of a high-entropy alloy particle refinement reinforced aluminum-based composite material, which comprises the steps of adding high-entropy alloy particles prepared after mechanical alloying into a molten aluminum alloy matrix through a gas dispersion stirring device, stirring and dispersing, then carrying out vibration degassing, and finally adopting a casting process to prepare a formed part of the high-entropy alloy particle reinforced aluminum-based composite material. The gas dispersion stirring device divides the process of introducing the high-entropy alloy particles into the aluminum alloy matrix into two processes of blowing the high-entropy alloy particles into the aluminum alloy matrix and independently stirring.
Preferably, the gas dispersing and stirring device comprises a ventilation stirrer, the ventilation stirrer is driven by a motor through a transmission structure, the ventilation stirrer is sequentially communicated with a gas cylinder through a rotary joint and a hose, a particle dispersing chamber is connected between the gas cylinder and the hose, the bottom of the particle dispersing chamber is communicated with the thicker end of a variable-section through pipe, the thinner end of the variable-section through pipe is arranged in the hose, and the top of the particle dispersing chamber is connected with a particle chamber filled with high-entropy alloy particles; when in use, the aeration stirrer is arranged in the crucible provided with the aluminum alloy matrix. The outflow quantity of particles is limited at the finer end of the variable-section through pipe, the air pressure is further pressurized, the particles are sprayed out of the variable-section through pipe, so that agglomerated particles are scattered, the agglomerated particles are fully dispersed in air, inert gas uniformly mixes high-entropy alloy particles and blows the particles into a rotary joint, then the particles are blown into an aluminum alloy matrix through a ventilation stirrer, and meanwhile, a motor drives the ventilation stirrer to stir the aluminum alloy matrix, so that the combination of high-entropy alloy particles blowing and mechanical stirring is realized, and high-entropy alloy powder is uniformly distributed in the alloy matrix from microcosmic and macroscopic aspects as well as local and whole aspects.
More preferably, a particle flow control valve is arranged between the particle material chamber and the particle dispersion chamber; and a gas flow control valve is arranged between the gas cylinder and the particle dispersion chamber.
Preferably, the preparation method of the high-entropy alloy particle refinement reinforced aluminum matrix composite material comprises the following steps,
step 1): calculating the content of each component of the metal powder according to the mole atomic ratio and mass fraction of the required alloy, weighing, mixing the powder, uniformly mixing, vacuumizing, and mechanically alloying under the protection of argon for 10-72h, preferably 30-60h; the rotating speed is 150r/min-500r/min (preferably 250-350 r/min), the process control agent is absolute ethyl alcohol, the temperature is room temperature, and the high-entropy alloy particles are obtained by sieving after alloying, and the particle size distribution of the high-entropy alloy particles is 1-500 mu m, preferably 0.5-20 mu m;
step 2): preheating high-entropy alloy particles for 20-90min at 60-150 ℃, heating and melting aluminum alloy to 680-780 ℃ (preferably to 700-780 ℃), adding the preheated high-entropy alloy particles into an aluminum alloy matrix through a gas dispersion stirring device, stirring at a speed of 100-500r/min, continuing stirring for 5-30min (preferably for 5-15 min) after the high-entropy alloy particles are completely added to obtain a mixed melt, standing, and carrying out ultrasonic vibration or mechanical vibration dispersion degassing treatment at 620-720 ℃ for 3-20min, preferably for 5-15min to obtain a high-entropy alloy particle refinement reinforced aluminum matrix composite melt;
step 3): casting ingot casting or pouring the high-entropy alloy grain refined reinforced aluminum-based composite material melt into a forming die material chamber, and closing to obtain a forming part of the high-entropy alloy grain refined reinforced aluminum-based composite material, and then carrying out solid solution and aging heat treatment.
Preferably, the mass fraction of the high-entropy alloy particles in the high-entropy alloy particle refinement reinforced aluminum-based composite material is 0.1-20%, and the mass fraction of the aluminum alloy is 80-99.9%; the high-entropy alloy particles are at least one element of CoCrFe system, coCrFeNi system, alCoCrFe system, alCoCrNi system, coCrNiCu system alloy and Ti, mg, zn, si, mo, B, sc, V and Mn; the atomic percentage of each element in the high-entropy alloy particles ranges from 5% to 35%. Five or more metal elements are generally adopted to form the high-entropy alloy.
Preferably, the aluminum alloy matrix is at least one of deformed aluminum alloy, cast aluminum alloy and aluminum lithium alloy; the wrought aluminum alloy is at least one of a 1xxx, 2xxx, 3xxx, 4xxx, 5xxx, 6xxx, and 7xxx alloy; the cast aluminum alloy is at least one of Al-Si system, al-Cu system, al-Mg system, al-Zn system and Al-RE system.
More preferably, the frequency of the ultrasonic vibration in the step 2) is 20kHZ, the frequency of the mechanical vibration is 50Hz, and the treatment time is 3-20min.
More preferably, the molding process of the molded article in the step 3) employs semi-continuous casting, gravity casting, high pressure casting, low pressure casting, liquid die forging or squeeze casting.
The invention also provides the high-entropy alloy grain refinement reinforced aluminum-based composite material prepared by the preparation method of the high-entropy alloy grain refinement reinforced aluminum-based composite material.
The preparation process is a new process for preparing the high-entropy alloy particle reinforced aluminum-based composite material by adopting a liquid method, namely, the preparation of high-entropy alloy powder, the introduction of an aluminum alloy matrix by a gas dispersion stirring device, the casting of the composite material and other key steps, can solve the problems that the particles of the high-entropy alloy particle reinforced aluminum-based composite material are difficult to introduce into the aluminum alloy matrix, the micro-distribution of the particles cannot be uniform by mechanical stirring, the insufficient wetting of the particles and the matrix, the agglomeration and the like, and is used for preparing the aluminum-based composite material with excellent comprehensive performance.
The preparation method of the invention has the principle that: the high-entropy alloy particles have stable structure at high temperature, so that the occurrence of interfacial chemical reaction of a general reinforcing phase and the generation of brittle phases such as intermetallic compounds are avoided, and in addition, the high-entropy alloy powder and an aluminum alloy matrix in the composite material can form an atomic semi-coherent physical bonding interface, so that the interface bonding strength is high and the interface wettability is good. Compared with the traditional particle reinforced aluminum alloy, the solution loading capacity of the melt on the high-entropy alloy metal particles is improved, and the addition of more reinforcing phase particles is beneficial to improving the hardness and strength. But the high-entropy alloy particles have smaller particle size and higher surface energy, float on the surface of the aluminum alloy matrix and easily form agglomerates when added into the melt, and cannot be fused into the aluminum alloy matrix by adopting a common mechanical stirring mode, so that macro-dispersion cannot be performed. Even if the coating is pressed into the melt to ensure that the particles cannot float on the surface of the melt, the particles are barely added into the alloy, a large number of flaky and spherical aggregates exist, the high-entropy alloy cannot be uniformly distributed in the aluminum alloy matrix in a microscopic and macroscopic manner, the phenomenon is more serious along with the increase of the number of the high-entropy alloy particles, and the problem of microscopic dispersion among the high-entropy alloy particles cannot be fundamentally solved no matter common stirring or pressing into the melt stirring, the contact and wetting problems of single particles and the melt cannot be increased and ensured, and the problem of macroscopic and microscopic dispersion of a large number of high-entropy alloy particles in the melt cannot be solved. According to the invention, the gas dispersing and stirring device is adopted to disperse the high-entropy alloy powder, the gas pressure is increased through the variable cross-section necking, so that a small amount of high-entropy alloy powder is pressurized, rotated and sprayed at the long and narrow necking when passing through, agglomerated particles are fully dispersed and mixed into inert gas, when the inert gas is introduced into a melt along with the dispersing and stirring device, the gas is dispersed under the condition of rotating and stirring, the dispersed gas further disperses the high-entropy alloy particles, strong pressure is generated when bubbles enter the melt to break, the dispersion of the high-entropy alloy particles is further increased, meanwhile, the dispersion of the high-entropy alloy is realized by melt convection caused by mechanical stirring, the macro-and micro-mixing and uniform dispersion of the high-entropy alloy particles in the whole melt are realized on the basis of the multiple dispersion effects, the problem of agglomeration and uneven distribution is solved, and then the residual gas is removed during the gas dispersion by ultrasonic vibration or mechanical vibration on the melt treatment, so that the problem of air holes is avoided. Meanwhile, the high-entropy alloy has higher thermal stability, and has natural affinity with a metal melt, heterogeneous nucleation can be carried out in the melt as nucleation points in the subsequent solidification casting process of the melt, a large number of high-entropy alloy particles dispersed between aluminum alloy matrixes can be used as heterogeneous nucleation points for carrying out a large number of nucleation, the number of grain nucleation is far more than that of the traditional particle reinforced aluminum matrix composite material, the grain refinement effect is directly determined by the dispersed high-entropy alloy particles, the grain refinement effect is greatly enhanced by a large number of fully dispersed high-entropy alloy particles, and the hardness, strength and plasticity are greatly improved by combining the strengthening effect of hard high-entropy alloy particles.
Compared with the prior art, the invention has the following advantages and effects:
(1) The high-entropy alloy powder has good high-temperature stability and strong oxidation resistance, and does not need additional chemical treatment and cleaning compared with the surfaces of reinforced particles made of other materials.
(2) The invention belongs to a process for preparing a composite material by a liquid method, wherein high-entropy alloy particles and an aluminum alloy matrix have relatively good wettability, a smooth and clean interface, no obvious reaction layer and high interface bonding strength.
(3) Compared with the traditional particle reinforced aluminum alloy, ceramic particles such as SiC and the like are not well bonded with the metal melt interface, the number of the fused aluminum alloy matrixes is small, but the interface bonding compatibility of the high-entropy alloy and the metal melt is good, the capability of carrying the high-entropy alloy by the melt is very strong, and a large number of high-entropy alloy particles can be added, so that the hardness and the strength are improved.
(4) The high-entropy alloy particles have smaller particle size and higher surface energy, float on the surface of an aluminum alloy matrix and easily form agglomerates when the melt is added, the common adding stirring and coating and immersing manner is adopted, particles are not well dispersed and are difficult to infiltrate when the melt is introduced, the high-entropy alloy cannot be uniformly distributed in the aluminum alloy matrix in a microscopic and macroscopic manner, a large number of flaky and spherical agglomerates exist in the melt, the agglomeration phenomenon is more and more serious along with the increase of the number of the added high-entropy alloy particles, and the reason is that the problem of microscopic dispersion among the high-entropy alloy particles cannot be fundamentally solved no matter the common stirring or the pressing-in melt stirring is adopted, the contact and wetting problems of single particles and the melt cannot be increased and guaranteed, and the problem of macroscopic and microscopic dispersion of a large number of high-entropy alloy particles in the melt cannot be solved. The gas stirring dispersion mode can well uniformly disperse a large number of high-entropy alloy particles among aluminum alloy matrixes when the high-entropy alloy particles are introduced into a melt, the particles are fully contacted with the melt, the infiltration is easy, the agglomeration problem can not occur,
(5) According to the invention, the gas dispersion stirring device is adopted to disperse the high-entropy alloy powder, the gas pressure is increased through the variable cross-section necking, so that a small amount of high-entropy alloy powder is pressurized, rotated and sprayed at the long and narrow necking position when passing through, agglomerated particles are fully dispersed and mixed into inert gas, when the inert gas is introduced into a melt along with the inert gas, the gas is dispersed under the condition of rotation stirring, the dispersed gas further disperses the high-entropy alloy particles, strong pressure is generated when bubbles break when entering the interior of the melt, the dispersion of the high-entropy alloy particles is further increased, the interface contact diffusion area of the singly dispersed high-entropy alloy particles and an aluminum melt is large, the agglomeration is fully wetted, the melt convection caused by mechanical stirring is promoted, the dispersion of the high-entropy alloy is realized on the basis of the multiple dispersion, the problems of macro-mixing and micro mixing and uniform dispersion of the high-entropy alloy particles in the whole melt are solved, the problem of agglomeration and uneven distribution are then the melt is treated by ultrasonic vibration or mechanical vibration, and the residual gas during the gas dispersion is removed, and the problem of subsequent generation is avoided.
(6) The invention adopts ultrasonic vibration or mechanical vibration before pouring, thereby avoiding the problem of more air holes remained in the melt due to long-time stirring and ventilation.
(7) Meanwhile, the high-entropy alloy has higher thermal stability and natural affinity with a metal melt, heterogeneous nucleation can be carried out in the melt as nucleation points in the subsequent solidification casting process of the melt, a large number of tiny and uniformly distributed high-entropy alloy particles dispersed through gas stirring are dispersed in an aluminum alloy matrix, a large number of nucleation points can be carried out as heterogeneous nucleation points, the nucleation rate is greatly increased, the number of crystal grain nucleation is far more than that of the traditional particle reinforced aluminum-based composite material and the composite material prepared by the common dispersion stirring process, the grain refinement effect is directly determined by the number and the dispersion degree of the particles added by the high-entropy alloy, the grain refinement effect is greatly enhanced by a large number of fully dispersed high-entropy alloy particles, and the hardness, the strength and the plasticity are greatly improved by combining the strengthening effect of the hard high-entropy alloy particles.
Drawings
FIG. 1 is a schematic diagram of a gas stirring and dispersing device;
fig. 2 is a metallographic structure diagram of a die-casting thin-wall part of the high-entropy alloy reinforced a356 aluminum-based composite material prepared in example 1.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments accompanied with figures are described in detail below.
The gas stirring and dispersing device adopted by each embodiment is shown in fig. 1, and comprises a ventilation stirrer 14, wherein the ventilation stirrer 14 is driven by a motor 11 through a transmission structure 10, the ventilation stirrer 14 is communicated with a gas cylinder 3 through a rotary joint 9 and a hose 8 in sequence, a particle dispersing chamber 6 is connected between the gas cylinder 3 and the hose 8, the bottom of the particle dispersing chamber 6 is communicated with the thicker end of a variable cross-section through pipe 7, the thinner end of the variable cross-section through pipe 7 is arranged in the hose 8, and the top of the particle dispersing chamber 6 is connected with a particle material chamber 1 filled with high-entropy alloy particles 4; in use, the aeration agitator 14 is disposed within the crucible 13 containing the aluminum alloy substrate 12. A particle flow control valve 5 is arranged between the particle material chamber 1 and the particle dispersion chamber 6; a gas flow control valve 2 is arranged between the gas cylinder 3 and the particle dispersion chamber 6.
Example 1
A preparation method of a high-entropy alloy grain refinement reinforced aluminum-based composite material comprises the following steps:
step one, preparing high-entropy alloy powder:
firstly, the reinforcing phase is AlCoCrFeNi series high-entropy alloy particles, the proportion of each component is 1:1:1:1:1, the mass of each component is calculated according to the mole atomic ratio and mass fraction of each element, the components are weighed and then are filled into a stainless steel ball grinding tank, a process control agent is absolute ethyl alcohol, vacuumizing and argon filling are carried out, then mechanical alloying is carried out on the planetary ball grinding tank for 60 hours, the ball-material ratio is 8:1, the rotating speed is 250r/min, high-entropy alloy powder is prepared, and the grain size after sieving is 1-20 mu m.
Introducing high-entropy alloy powder into an aluminum alloy matrix by utilizing a gas stirring and dispersing device, and performing vibration treatment:
weighing the high-entropy alloy powder prepared in the first step, wherein the mass fraction of the high-entropy alloy powder is 5%, and the mass fraction of the aluminum alloy matrix is A356 aluminum alloy and is 95%; preheating high-entropy alloy powder at 150 ℃ for 60min, heating and melting aluminum alloy to 720 ℃, adding the preheated high-entropy alloy powder into an aluminum alloy matrix at a speed of 10g/min by using variable cross-section compressed blowing gas through gas dispersion stirring equipment, stirring at a speed of 300r/min, continuously rotating and blowing after complete blowing for 15min to obtain a mixed melt, standing for one session, and carrying out ultrasonic vibration dispersion degassing treatment at 680 ℃ at an ultrasonic frequency of 20KHZ for 3-20min to obtain the particle reinforced aluminum alloy matrix.
Step three, casting a composite material and a formed part:
and (3) carrying out extrusion casting molding pouring on the particle reinforced aluminum alloy matrix at 650 ℃, and carrying out molding demoulding at the die temperature of 200 ℃ to obtain the high-entropy alloy particle reinforced aluminum matrix composite material. The tensile test result shows that the tensile strength of the composite material is 280MPa, and the elongation is 8%. Metallographic and SEM and EDS analysis show that the particles are uniformly dispersed in the matrix and the boundary, no obvious reaction layer exists, and the interface combination is good.
Example 2
A preparation method of a high-entropy alloy grain refinement reinforced aluminum-based composite material comprises the following steps:
step one, preparing high-entropy alloy powder:
firstly, the reinforcing phase is AlCoCrFeCu high-entropy alloy particles, the proportion of each component is 1:1:1:1:1, the mass of each component is calculated according to the mole atomic ratio and mass fraction of each element, the components are weighed and then are filled into a stainless steel ball grinding tank, a process control agent is absolute ethyl alcohol, vacuumizing and argon filling are carried out, then mechanical alloying is carried out on the planetary ball grinding tank for 50 hours, the ball-material ratio is 8:1, the rotating speed is 280r/min, high-entropy alloy powder is prepared, and the grain size after sieving is 2-10 mu m.
Introducing high-entropy alloy powder into an aluminum alloy matrix by utilizing a gas stirring and dispersing device, and performing vibration treatment:
weighing the high-entropy alloy powder prepared in the first step, wherein the mass fraction of the high-entropy alloy powder is 7%, the aluminum alloy matrix is 7075 aluminum alloy, and the mass fraction of the high-entropy alloy powder is 96%; preheating high-entropy alloy powder for 50min at 150 ℃, heating and melting aluminum alloy to 720 ℃, adding the preheated high-entropy alloy powder into an aluminum alloy matrix by using variable cross-section compressed injection gas through gas dispersion stirring equipment, stirring at a speed of 100r/min, continuously rotating, injecting and stirring for 15min after complete injection to obtain a mixed melt, standing for one session, and carrying out ultrasonic vibration dispersion degassing treatment at 670 ℃, wherein the ultrasonic frequency is 20KHZ, and the treatment time is 3-20min to obtain the particle reinforced aluminum alloy matrix.
Step three, casting a composite material and a formed part:
and (3) casting the particle reinforced aluminum alloy matrix at 660 ℃, forming at the die temperature of 200 ℃, and demoulding to obtain the high-entropy alloy particle reinforced aluminum matrix composite material. The tensile strength of the composite material is 290MPa, and the elongation is 10%. Metallographic and SEM and EDS analysis show that the particles are uniformly dispersed in the matrix and the boundary, no obvious reaction layer exists, and the interface combination is good.
Example 3
A preparation method of a high-entropy alloy grain refinement reinforced aluminum-based composite material comprises the following steps:
step one, preparing high-entropy alloy powder:
firstly, selecting CoCrFeNiCu-series high-entropy alloy particles as a reinforcing phase, wherein the specific components are CoCrFeNiCu0.25Ti0.25Mn0.25, respectively calculating the mass of each component according to the mol atomic ratio and mass fraction of each element, weighing, then filling the mixture into a stainless steel ball milling tank, vacuumizing and filling argon into a process control agent which is absolute ethyl alcohol, then mechanically alloying the mixture on a planetary ball milling tank for 65 hours, wherein the ball material ratio is 8:1, the rotating speed is 300r/min, and preparing the high-entropy alloy powder with the particle size of 1-15 mu m after sieving.
Introducing high-entropy alloy powder into an aluminum alloy matrix by utilizing a gas stirring and dispersing device, and performing vibration treatment:
weighing the high-entropy alloy powder prepared in the first step, wherein the mass fraction of the high-entropy alloy powder is 4%, and the mass fraction of the high-entropy alloy powder is 93% because the aluminum alloy matrix is 2024 aluminum alloy; preheating high-entropy alloy powder at 180 ℃ for 70min, heating and melting aluminum alloy to 720 ℃, adding the preheated high-entropy alloy powder into an aluminum alloy matrix by using variable cross-section compressed injection gas through gas dispersion stirring equipment, stirring at the speed of 200r/min, continuously rotating, injecting and stirring for 20min after complete injection to obtain a mixed melt, standing for one time, carrying out ultrasonic vibration dispersion degassing treatment at 670 ℃, and carrying out mechanical vibration frequency of 50HZ for 15min to obtain the particle reinforced aluminum alloy matrix.
Step three, casting a composite material and a formed part:
and (3) casting and molding the particle reinforced aluminum alloy matrix at 670 ℃, and obtaining the high-entropy alloy particle reinforced aluminum matrix composite after molding and demolding at the mold temperature of 250 ℃. The tensile test result shows that the tensile strength of the composite material is 270MPa, and the elongation is 9%. Metallographic and SEM and EDS analysis show that the particles are uniformly dispersed in the matrix and the boundary, no obvious reaction layer exists, and the interface combination is good.
Example 4
A preparation method of a high-entropy alloy grain refinement reinforced aluminum-based composite material comprises the following steps:
step one, preparing high-entropy alloy powder:
firstly, the reinforcing phase is AlCoCrNi series high-entropy alloy particles, and the specific components are AlCoCrNiCu in a ratio of 1:1:1:1:1, respectively calculating the mass of each component according to the mole atomic ratio and mass fraction of each element, weighing, then loading into a stainless steel ball grinding tank, wherein a process control agent is absolute ethyl alcohol, vacuumizing, filling argon, then mechanically alloying on a planetary ball grinding tank for 65 hours, wherein the ball-to-material ratio is 8:1, the rotating speed is 290r/min, preparing the high-entropy alloy powder, and the particle size after sieving is 5-20 mu m.
Introducing high-entropy alloy powder into an aluminum alloy matrix by utilizing a gas stirring and dispersing device, and performing vibration treatment:
weighing the high-entropy alloy powder prepared in the first step, wherein the mass fraction of the high-entropy alloy powder is 1%, and the mass fraction of the high-entropy alloy powder is 99% while the aluminum alloy matrix is 5005 aluminum alloy; preheating high-entropy alloy powder at 180 ℃ for 70min, heating and melting aluminum alloy to 720 ℃, adding the preheated high-entropy alloy powder into an aluminum alloy matrix by using variable cross-section compressed injection gas through gas dispersion stirring equipment, stirring at the speed of 200r/min, continuously rotating, injecting and stirring for 20min after complete injection to obtain a mixed melt, standing for one time, carrying out ultrasonic vibration dispersion degassing treatment at 670 ℃, and carrying out mechanical vibration frequency of 50HZ for 15min to obtain the particle reinforced aluminum alloy matrix.
Step three, casting a composite material and a formed part:
and (3) casting and molding the particle reinforced aluminum alloy matrix at 670 ℃, and obtaining the high-entropy alloy particle reinforced aluminum matrix composite after molding and demolding at the mold temperature of 250 ℃. The tensile test result shows that the tensile strength of the composite material is 180MPa, and the elongation is 12%. Metallographic and SEM and EDS analysis show that the particles are uniformly dispersed in the matrix and the boundary, no obvious reaction layer exists, and the interface combination is good.
Example 5
A preparation method of a high-entropy alloy grain refinement reinforced aluminum-based composite material comprises the following steps:
step one, preparing high-entropy alloy powder:
firstly, the reinforcing phase is AlCoCrFeNiTi series high-entropy alloy particles, the component proportion is 1:1:1:1:1, the mass of each component is calculated according to the mol atomic ratio and mass fraction of each element, the components are weighed and then are filled into a stainless steel ball grinding tank, a process control agent is absolute ethyl alcohol, vacuumizing and argon filling are carried out, then mechanical alloying is carried out on the planetary ball grinding tank for 70 hours, the ball-material ratio is 8:1, the rotating speed is 300r/min, the high-entropy alloy powder is prepared, and the grain size after sieving is 50-150 mu m.
Introducing high-entropy alloy powder into an aluminum alloy matrix by utilizing a gas stirring and dispersing device, and performing vibration treatment:
weighing the high-entropy alloy powder prepared in the first step, wherein the mass fraction of the high-entropy alloy powder is 10%, and the aluminum alloy matrix is ZL201 aluminum alloy, and the mass fraction of the high-entropy alloy powder is 90%; preheating high-entropy alloy powder at 180 ℃ for 70min, heating and melting aluminum alloy to 720 ℃, adding the preheated high-entropy alloy powder into an aluminum alloy matrix by using variable cross-section compressed injection gas through gas dispersion stirring equipment, stirring at the speed of 200r/min, continuously rotating, injecting and stirring for 30min after complete injection to obtain a mixed melt, standing for one time, and carrying out ultrasonic vibration dispersion degassing treatment at 670 ℃ with the mechanical vibration frequency of 50HZ for 25min to obtain the particle reinforced aluminum alloy matrix.
Step three, casting a composite material and a formed part:
and (3) carrying out die casting molding on the particle reinforced aluminum alloy matrix at 680 ℃, and obtaining the high-entropy alloy particle reinforced aluminum matrix composite material after molding and demolding at the mold temperature of 300 ℃. The tensile test result shows that the tensile strength of the composite material is 310MPa, and the elongation is 7%. Metallographic and SEM and EDS analysis show that the particles are uniformly dispersed in the matrix and the boundary, no obvious reaction layer exists, and the interface combination is good.
Claims (9)
1. A preparation method of a high-entropy alloy particle refined reinforced aluminum-based composite material is characterized in that a gas dispersion stirring device is adopted to disperse high-entropy alloy particles prepared after mechanical alloying, variable-section necking is utilized to increase gas pressure, the high-entropy alloy particles with mass fraction of 0.1% -20% are sprayed and mixed with inert gas to be added into a molten aluminum alloy matrix to be stirred and dispersed, vibration degassing is carried out, and finally a casting process is adopted to prepare a formed piece of the high-entropy alloy particle reinforced aluminum-based composite material.
2. The method for preparing the high-entropy alloy particle refinement reinforced aluminum-based composite material according to claim 1, wherein the gas dispersion stirring device comprises a ventilation stirrer (14), the ventilation stirrer (14) is driven by a motor (11) through a transmission structure (10), the ventilation stirrer (14) is communicated with a gas cylinder (3) sequentially through a rotary joint (9) and a hose (8), a particle dispersion chamber (6) is connected between the gas cylinder (3) and the hose (8), the bottom of the particle dispersion chamber (6) is communicated with the thicker end of a variable-section through pipe (7), the thinner end of the variable-section through pipe (7) is arranged in the hose (8), and the top of the particle dispersion chamber (6) is connected with a particle chamber (1) filled with high-entropy alloy particles (4); in use, the aeration agitator (14) is disposed within a crucible (13) containing an aluminum alloy substrate (12).
3. The method for preparing the high-entropy alloy grain refinement reinforced aluminum-based composite material according to claim 2, wherein a grain flow control valve (5) is arranged between the grain material chamber (1) and the grain dispersion chamber (6); a gas flow control valve (2) is arranged between the gas cylinder (3) and the particle dispersion chamber (6).
4. The method for preparing the high-entropy alloy grain refinement reinforced aluminum-based composite material as claimed in claim 1, which comprises the following steps,
step 1): calculating the content of each component of the metal powder according to the mole atomic ratio and mass fraction of the required alloy, weighing, mixing the powder, uniformly mixing, vacuumizing, and mechanically alloying under the protection of argon for 10-72h; the rotating speed is 150r/min-500r/min, the process control agent is absolute ethyl alcohol, the temperature is room temperature, and after alloying is completed, high-entropy alloy particles are obtained through sieving, and the particle size distribution of the high-entropy alloy particles is 1-500 mu m;
step 2): preheating high-entropy alloy particles for 20-90min at 60-150 ℃, heating and melting aluminum alloy to 680-780 ℃, adding the preheated high-entropy alloy particles into an aluminum alloy matrix through a gas dispersion stirring device, stirring at a speed of 100-500r/min, continuously stirring for 5-30min after the high-entropy alloy particles are completely added to obtain a mixed melt, standing, and performing ultrasonic vibration or mechanical vibration dispersion degassing treatment at 620-720 ℃ to obtain a high-entropy alloy particle refinement reinforced aluminum matrix composite melt;
step 3): casting ingot casting or pouring the high-entropy alloy grain refined reinforced aluminum-based composite material melt into a forming die material chamber, and closing to obtain a forming part of the high-entropy alloy grain refined reinforced aluminum-based composite material, and then carrying out solid solution and aging heat treatment.
5. The method for producing a grain-refined reinforced aluminum-based composite material as claimed in any one of claims 1 to 4, wherein the grain of the high-entropy alloy is at least one element selected from the group consisting of CoCrFe-based, coCrFeNi-based, alCoCrFe-based, alCoCrNi-based, coCrNiCu-based alloys, and Ti, mg, zn, si, mo, B, sc, V and Mn; the atomic percentage of each element in the high-entropy alloy particles ranges from 5% to 35%.
6. The method for preparing the high-entropy alloy grain refinement reinforced aluminum-based composite material according to any one of claims 1 to 4, wherein the aluminum alloy matrix is at least one of a wrought aluminum alloy, a cast aluminum alloy and an aluminum lithium alloy; the wrought aluminum alloy is at least one of a 1xxx, 2xxx, 3xxx, 4xxx, 5xxx, 6xxx, and 7xxx alloy; the cast aluminum alloy is at least one of Al-Si system, al-Cu system, al-Mg system, al-Zn system and Al-RE system.
7. The method for preparing the high-entropy alloy grain refinement reinforced aluminum-based composite material according to claim 4, wherein the ultrasonic vibration frequency in the step 2) is 20kHZ, the mechanical vibration frequency is 50Hz, and the treatment time is 3-20min.
8. The method for preparing the high-entropy alloy grain-refined reinforced aluminum-based composite material according to claim 4, wherein the molding process of the molded part in the step 3) adopts semi-continuous casting, gravity casting, high-pressure casting, low-pressure casting, liquid die forging or extrusion casting.
9. A high-entropy alloy grain-refined reinforced aluminum-based composite material prepared by the method for preparing a high-entropy alloy grain-refined reinforced aluminum-based composite material according to any one of claims 1 to 8.
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| DE102019000361A1 (en) * | 2019-01-18 | 2020-07-23 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Wear-resistant lightweight construction alloy made of a metal-matrix composite material with a metallic matrix and a ceramic hard phase, method for producing such a wear-resistant lightweight construction alloy, and brake disc mating with such a wear-resistant lightweight construction alloy |
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