CN114959340B - Multi-principal-element oxide dispersion-strengthened superfine-crystal aluminum-based composite material and preparation method thereof - Google Patents

Multi-principal-element oxide dispersion-strengthened superfine-crystal aluminum-based composite material and preparation method thereof Download PDF

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CN114959340B
CN114959340B CN202210544292.XA CN202210544292A CN114959340B CN 114959340 B CN114959340 B CN 114959340B CN 202210544292 A CN202210544292 A CN 202210544292A CN 114959340 B CN114959340 B CN 114959340B
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CN114959340A (en
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谢聿铭
黄永宪
孟祥晨
冒冬鑫
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Harbin Institute of Technology
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
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    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C21/00—Alloys based on aluminium
    • C22C21/02—Alloys based on aluminium with silicon as the next major constituent
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C21/00—Alloys based on aluminium
    • C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
    • C22C21/08—Alloys based on aluminium with magnesium as the next major constituent with silicon
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C21/00—Alloys based on aluminium
    • C22C21/12—Alloys based on aluminium with copper as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
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    • 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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Abstract

The invention discloses a multi-principal element oxide dispersion strengthening ultra-fine grain aluminum-based composite material and a preparation method thereof, relating to the technical field of composite material preparation, wherein the preparation method comprises the following steps: step S1: mixing and ball-milling at least 5 kinds of metal oxide powder with equal molar ratio to obtain high-entropy multi-principal-element oxide mixture nano powder; step S2: mixing and ball-milling high-entropy multi-principal-element oxide mixture nano powder, aluminum powder and a process control agent in an argon protective atmosphere, heating and preserving heat to obtain aluminum-based composite material powder; and step S3: and carrying out rotary extrusion and load retention on the aluminum-based composite material powder by a large plastic deformation solid-phase sintering one-step method to obtain the multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material. According to the preparation method, the sharp characteristic appearance and stress concentration of the metal oxide particles are changed, the pinning effect on dislocation motion is enhanced, and the grain structure is refined.

Description

Multi-principal-element oxide dispersion-strengthened superfine-crystal aluminum-based composite material and preparation method thereof
Technical Field
The invention relates to the technical field of composite material preparation, in particular to a multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material and a preparation method thereof.
Background
The rapid development of technology-intensive industries such as aerospace science and technology, military engineering and the like brings the requirement of rapid iterative development of metal structural materials, which requires that the materials have high strength and high plasticity and also need to have low density and high rigidity. Although steel materials and the like have excellent obdurability, the excessive density of the steel materials seriously restricts the thrust-weight ratio performance of the carrier structure for aerospace. As a material with the density of only one third of that of steel materials, aluminum and aluminum alloy have good machinability and huge application value and potential. However, the absolute strength of aluminum alloys is still significantly different from that of steel materials, and the rigidity thereof is also low. Therefore, in order to further meet the requirements of a series of structural materials with light weight, high strength and toughness, aluminum-based composite materials are produced.
The particle reinforced aluminum-based composite material has been widely researched and applied because of higher specific strength and specific stiffness than aluminum alloy itself. The currently commonly used particle reinforced phase comprises SiC and Al 2 O 3 When the ceramic phase is adopted, the particle materials generally show good metallurgical compatibility with a matrix, and can play a role in pinning dislocation under the action of external loading, so that the structural strength of the composite material is improved. However, siC has a tendency to crack near the sharp edge during loading, especially under tension, due to the sharp edge of the SiC particles, which leads to premature failure of the material and leads to less than ideal elongation of the aluminum matrix composite. And Al 2 O 3 The pinning effect on dislocation is weaker due to the overhigh matrix compatibility and lower modulus, and the strengthening efficiency is lower than that of SiC and other particles with the same volume fraction. Therefore, a single particle reinforced aluminum matrix composite material often meets certain essential defects, and the application of the particle reinforced aluminum matrix composite material under complex working conditions is severely limited.
Disclosure of Invention
The problem solved by the invention is the essential insufficiency of the single-particle reinforced aluminum matrix composite material.
In order to solve the problems, the invention provides a preparation method of a multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material, which comprises the following steps:
step S1: mixing and ball-milling at least 5 kinds of metal oxide powder with equal molar ratio to obtain high-entropy multi-principal-element oxide mixture nano powder;
step S2: mixing and ball-milling the high-entropy multi-principal-element oxide mixture nano powder, aluminum powder and a process control agent in an argon protective atmosphere, heating and preserving heat to obtain aluminum-based composite material powder;
and step S3: and carrying out rotary extrusion and load retention on the aluminum-based composite material powder by a large plastic deformation solid-phase sintering one-step method to obtain the multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material.
Further, in step S1, the metal oxide includes one of lithium oxide, magnesium oxide, aluminum oxide, calcium oxide, scandium oxide, titanium oxide, vanadium oxide, chromium oxide, manganese oxide, iron oxide, cobalt oxide, nickel oxide, copper oxide, zinc oxide, yttrium oxide, zirconium oxide, niobium oxide, molybdenum oxide, cerium oxide, tantalum oxide, and tungsten oxide.
Further, in step S1, the ball milling process includes: carrying out ball milling by adopting a stainless steel ball milling tank and yttrium-stabilized zirconium dioxide ball milling balls; the diameter of the grinding ball is 4-10mm, and the ball-to-material ratio of the ball mill is (20-100): 1, the ball milling speed is 200-500rpm, and the ball milling time is 10-100h.
Further, in step S2, the ball-milling has a ball-to-material ratio of (5-50): 1, the ball milling speed is 200-500rpm, and the ball milling time is 2-50h.
Further, in step S2, the aluminum powder includes at least one of a pure aluminum powder, a 2 xxx-based Al-Cu or Al-Cu-Li-based powder, a 5 xxx-based Al-Mg-based powder, a 6 xxx-based Al-Mg-Si-based powder, and a 7 xxx-based Al-Zn-Mg-Cu-based powder, and has an average particle diameter of 1 μm to 200 μm.
Further, in the step S2, the heating temperature is 400-450 ℃, and the heat preservation time is 0.5-1h.
Further, in the step S2, the mass fraction of the high-entropy multi-principal-element oxide mixture nano powder in the aluminum-based composite material powder is 1% to 95%.
Further, in step S3, the rotating extrusion and load holding of the aluminum-based composite material powder by the large plastic deformation solid-phase sintering process includes:
and placing the aluminum-based composite material powder in a flat-bottom round groove die of a large plastic deformation solid-phase sintering process, and rotationally extruding and carrying the aluminum-based composite material powder through a pressure rod corresponding to the diameter of the flat-bottom round groove die.
Further, in step S3, the rotating speed is 500-8000rpm, and the guarantee time is 3-180S.
Compared with the prior art, the preparation method of the multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material has the beneficial effects that:
1. the invention mixes and ball-mills at least 5 kinds of metal oxide powder with equal molar ratio to obtain the high-entropy multi-principal-element oxide mixture nano powder, realizes the direct regulation and control of the reinforced phase lattice type and lattice constant, changes the lattice matching degree of the reinforced phase lattice type and lattice constant with an aluminum matrix, strengthens the pinning effect of dislocation movement in the bearing process, and greatly improves the strengthening efficiency. Meanwhile, the high-entropy multi-principal-element oxide mixture nano powder can change the sharp characteristic appearance of partial oxide particles, reduce the stress concentration of a phase interface in the bearing process and improve the toughness of the material.
2. According to the invention, through the ball milling process, the nanocrystallization of the strengthening phase is realized, the dispersion degree of the strengthening phase in the aluminum matrix is improved, and the subsequent large plastic deformation solid phase sintering process is combined, so that the agglomeration of the nanophase in the matrix is avoided, and the high strengthening and toughening level of the composite material is ensured.
3. The aluminum-based composite material powder is subjected to rotary extrusion through a large plastic deformation solid-phase sintering one-step method, so that the solid-phase sintering and densification of the aluminum-based composite material powder are realized while the large plastic deformation is realized, the dynamic recovery and recrystallization of an aluminum matrix are promoted, the ultra-fine crystallization of a grain structure is realized, and a high-quality ultra-fine grain composite material with extremely low porosity is formed.
The invention also provides a multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material which is prepared by the preparation method of the multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material.
Compared with the prior art, the beneficial effects of the multi-principal element oxide dispersion-strengthened ultrafine crystal aluminum-based composite material are the same as the preparation method of the multi-principal element oxide dispersion-strengthened ultrafine crystal aluminum-based composite material, and the details are not repeated here.
Drawings
FIG. 1 is a flow chart of the preparation of the multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material according to the embodiment of the present invention.
Detailed Description
The invention will be described in further detail below with reference to the accompanying drawings: the present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation is given, but the scope of the present invention is not limited to the following embodiments.
As shown in fig. 1, an embodiment of the present invention provides a method for preparing a multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material, including the following steps:
step S1: mixing and ball-milling at least 5 kinds of metal oxide powder with equal molar ratio to obtain high-entropy multi-principal-element oxide mixture nano powder;
step S2: mixing and ball-milling high-entropy multi-principal-element oxide mixture nano powder, aluminum powder and a process control agent in an argon protective atmosphere, heating and preserving heat to obtain aluminum-based composite material powder;
and step S3: and carrying out rotary extrusion and load retention on the aluminum-based composite material powder by a large plastic deformation solid-phase sintering one-step method to obtain the multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material.
According to the embodiment of the invention, the high-entropy multi-principal-element oxide mixture nano powder is obtained by mixing and ball-milling at least 5 kinds of metal oxide powder with equal molar ratio, so that the regulation and control of the type and the lattice constant of the reinforced phase lattice are realized directly, the lattice matching degree of the reinforced phase lattice and the aluminum matrix is changed, the pinning effect of the reinforced phase lattice on dislocation motion in the bearing process is enhanced, and the reinforcing efficiency is greatly improved. Meanwhile, the high-entropy multi-principal-element oxide mixture nano powder can change the sharp characteristic appearance of partial oxide particles, reduce the stress concentration of a phase interface in the bearing process and improve the toughness of the material.
According to the embodiment of the invention, through the ball milling process, the nanocrystallization of the strengthening phase-high entropy multi-principal-element oxide mixture nano powder is realized, the dispersion degree of the strengthening phase-high entropy multi-principal-element oxide mixture nano powder in an aluminum matrix is improved, and the subsequent large plastic deformation solid phase sintering process is combined, so that the agglomeration of the nano phase in the matrix is avoided, and the high strengthening and toughening level of the composite material is ensured.
Specifically, at least 5 kinds of metal oxide powder with equal molar ratio are placed in a ball milling tank for grinding, under the argon protection atmosphere, a certain proportion of high-entropy multi-principal-element oxide mixture nano powder and aluminum powder are weighed in a glove box and added into a vacuum sealing type ball milling tank, polyethylene glycol (Mn 2000) with the mass fraction of 3% -5% is added as a process control agent, grinding balls are added, the ball milling tank is sealed in the glove box, and then the mixture is taken out for ball milling, so that premixed powder is obtained. And then, placing the premixed powder under the protection of high-purity argon, heating and preserving heat, and obtaining the aluminum matrix composite powder after the process control agent is completely volatilized.
According to the embodiment of the invention, the aluminum-based composite material powder is subjected to rotary extrusion through a large plastic deformation solid-phase sintering one-step method, so that the solid-phase sintering and densification of the aluminum-based composite material powder are realized while the large plastic deformation is realized, the dynamic recovery and recrystallization of an aluminum matrix are promoted, the ultra-fine crystallization of a grain structure is realized, and a high-quality ultra-fine grain composite material with extremely low porosity is formed. Compared with the problems that solid-phase sintering and large plastic deformation are respectively carried out, excessive reaction between a multi-principal-element oxide mixture which easily causes high entropy in aluminum matrix composite powder and an aluminum matrix causes deformation of the high entropy oxide, and further unpredictable change occurs in the degree of matching with the crystal boundary of the matrix, and the like, the embodiment adopts a large plastic deformation solid-phase sintering one-step method to obtain the high-quality ultra-fine crystal composite with extremely low porosity through one-step forming, heat completely comes from large plastic deformation friction heat generation, heat input from the outside is not needed, the temperature of the friction heat generation is low, the excessive reaction is avoided, regulation and control of the degree of matching with the crystal lattice of the aluminum matrix are facilitated, and meanwhile, the reinforced phase stable high entropy state of the composite is ensured.
Specifically, in this embodiment, while the powder is compressed by the frictional deformation between the mold rotating at a high speed and the powder, the densified and ultra-fine grain-refined multi-principal-element oxide dispersion-strengthened ultrafine-grain aluminum-based composite material is prepared by solid-phase sintering through the frictional heat generation between the mold rotating at a high speed and the powder. The high-entropy multi-principal-element oxide mixture nano powder and the aluminum-based composite material powder in the embodiment of the invention are metastable materials, and the high-entropy oxides of the metastable materials are easy to undergo phase decomposition in the cooling process after high temperature, so that the performance of the materials is influenced, therefore, the temperature control is particularly important, and the metastable state of the materials can be damaged by ultrahigh-temperature process methods, such as casting methods such as smelting and the like or hot-pressing sintering and the like, so that the performance of the finally obtained composite materials cannot be improved. Therefore, the embodiment of the invention considers the characteristic that the strengthening phase is the high-entropy oxide, and adopts the large plastic deformation solid phase sintering one-step method to be matched with the strengthening phase, so that the process is simplified and the preparation efficiency is improved while various advantages of the high-entropy oxide material are kept.
In some specific embodiments, in step S1, the metal oxide includes one of lithium oxide, magnesium oxide, aluminum oxide, calcium oxide, scandium oxide, titanium oxide, vanadium oxide, chromium oxide, manganese oxide, iron oxide, cobalt oxide, nickel oxide, copper oxide, zinc oxide, yttrium oxide, zirconium oxide, niobium oxide, molybdenum oxide, cerium oxide, tantalum oxide, and tungsten oxide. Oxides in other valence states which are the same as the kinds of elements in the above metal oxides are also included. Therefore, the lattice matching degree of the reinforced phase lattice and the aluminum matrix is changed by regulating and controlling the type and the lattice constant of the reinforced phase lattice, the pinning effect of the reinforced phase lattice on dislocation motion in the bearing process is enhanced, and the reinforcing efficiency is greatly improved. Meanwhile, the sharp characteristic appearance of the single oxide particles is changed, the stress concentration of the phase interface in the bearing process is reduced, and the toughness of the material is improved. Preferably, magnesium oxide, cobalt oxide, nickel oxide, copper oxide, zinc oxide, lithium oxide, and cerium oxide can achieve more excellent properties as a reinforcing phase of the aluminum-based composite material.
In some embodiments, in step S1, the ball milling process comprises: carrying out ball milling by adopting a stainless steel ball milling tank and yttrium-stabilized zirconium dioxide bead grinding balls; wherein, the diameter of the grinding ball is 4-10mm, the ball-milling ball-material ratio is (20-100): 1, the ball milling speed is 200-500rpm, and the ball milling time is 10-100h. Therefore, the metal oxide is highly entropic, and the polishing agent has a better polishing effect on metal oxides with different hardness.
Specifically, the grinding balls have a diameter of 4 to 10mm.
In some specific embodiments, in step S2, the ball-milling has a ball-to-material ratio of (5-50): 1, the ball milling speed is 200-500rpm, and the ball milling time is 2-50h. Therefore, various metal oxides are fully ground to obtain nano-scale powder, the dispersion degree of the nano-scale powder in the aluminum matrix is favorably improved, and the subsequent large plastic deformation solid phase sintering process is combined, so that the agglomeration of nano-phases in the matrix is avoided, and the high strengthening and toughening level of the composite material is ensured.
In some specific examples, the aluminum powder in step S2 includes at least one of a pure aluminum powder, a 2 xxx-based Al-Cu or Al-Cu-Li-based powder, a 5 xxx-based Al-Mg-based powder, a 6 xxx-based Al-Mg-Si-based powder, and a 7 xxx-based Al-Zn-Mg-Cu-based powder, and the aluminum powder has an average particle diameter of 1 μm to 200 μm.
Therefore, the selection range of the aluminum powder is wide, and the performance of the required multi-principal-element oxide dispersion strengthening ultrafine-grained aluminum matrix composite material can be regulated and controlled. For example, when the aluminum powder is a mixed powder of two types, i.e., a 2xxx type Al-Cu-Li type powder and a 7xxx type Al-Zn-Mg-Cu type powder, a composite material having a high strength can be obtained. The total amount of all alloying elements added in the aluminum powder accounts for 0.03 to 20 percent of the total amount of the aluminum powder.
In some specific embodiments, in step S2, the heating temperature is 400-450 ℃ and the holding time is 0.5-1h. Therefore, the process control agent used in the ball milling process is completely volatilized, and the influence on the performance of the subsequent composite material is avoided.
In some specific embodiments, in the step S2, the mass fraction of the high-entropy multi-principal-element oxide mixture nano powder in the aluminum-based composite material powder is 1% to 95%. The rest is aluminum powder, and the multi-principal-element oxide dispersion strengthening ultrafine-grained aluminum-based composite material can be obtained within the mass fraction range. The regulation and control range is wide, and the material performance is favorably improved.
In some specific embodiments, in step S3, the rotary extrusion and load holding of the aluminum-based composite powder by the large plastic deformation solid-phase sintering process includes:
and placing the aluminum-based composite material powder in a flat-bottom round groove die of a large plastic deformation solid-phase sintering process, and performing rotary extrusion and load retention on the aluminum-based composite material powder through a pressure rod corresponding to the diameter of the flat-bottom round groove die.
In the embodiment, 0.8-2.4g of premixed aluminum-based composite material powder is weighed and placed in a flat-bottom circular groove die with the diameter of 16mm and the depth of 5mm, a cylindrical large plastic deformation pressure rod with the diameter of 16mm rotates at a high speed and is pressed into the flat-bottom circular groove, the powder is rotationally extruded and is carried for a period of time while the pressure rod rotating at the high speed and the powder are in friction deformation, and the volume after rotational extrusion can be calculated according to theoretical density. Therefore, the densification and the ultrafine crystallization of the powder are realized through the direct friction deformation heat generation and the high accumulated plastic strain of the compression bar and the powder, and finally the multi-principal element oxide dispersion strengthening ultrafine crystal aluminum-based composite material is obtained.
In some specific embodiments, the spin speed is 500-8000rpm and the hold time is 3-180s. Therefore, the densification and the superfine crystallization of the aluminum-based composite material powder are accelerated.
The embodiment of the invention also provides a multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material which is prepared by the preparation method of the multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material.
Compared with the prior art, the beneficial effects of the multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material are the same as the preparation method of the multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material, and the details are not repeated here.
Example 1:
the preparation method of the multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material in the embodiment specifically comprises the following steps:
step S1: weighing five metal oxide powders of magnesium oxide, copper oxide, cobalt oxide, nickel oxide and zinc oxide according to an equimolar ratio, placing the powders in a stainless steel ball-milling tank, adding yttrium-stabilized zirconium dioxide beads with the diameter of 6mm as grinding balls, wherein the ball-to-material ratio is 50:1, obtaining high-entropy multi-principal-element oxide mixture nano powder with the rotation speed of 500rpm and the ball milling time of 30 h;
step S2: in a high-purity argon-shielded glove box (water oxygen < 0.01 ppm), 1g of multi-principal-component oxide mixture nano powder and 9g of 2195Al-Cu-Li aluminum alloy powder are weighed and placed in a vacuum seal type stainless steel ball mill tank, 0.3g of polyethylene glycol (Mn 2000) is added as a process control agent, yttrium-stabilized zirconium dioxide beads with the diameter of 6mm are added as grinding balls, and the ball-to-material ratio is 10:1, sealing a stainless steel ball milling tank in a glove box, taking out and carrying out ball milling at the rotating speed of 200rpm for 10 hours to obtain premixed powder. Then placing the premixed powder in a high-purity argon protective atmosphere, heating to 450 ℃, preserving heat for 0.5h, and completely volatilizing the process control agent to obtain aluminum-based composite material powder;
and step S3: weighing 0.85g of aluminum-based composite material powder, placing the powder into a flat-bottom circular groove die with the diameter of 16mm and the depth of 5mm, rotating a cylindrical large plastic deformation pressing rod with the diameter of 16mm at a high speed and pressing the cylindrical large plastic deformation pressing rod into the flat-bottom circular groove, wherein the rotating speed is 1000rpm, compressing the powder to the thickness of 1.0mm while performing friction deformation between the pressing rod and the powder which rotate at the high speed, and carrying for 60s. The densification and the superfine crystallization of the powder are realized through the direct frictional deformation heat generation and the high-amount accumulated plastic strain of the die and the powder, and finally the multi-principal-element oxide dispersion-strengthened superfine-crystal aluminum-based composite material is obtained.
Example 2
The preparation method of the multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material in the embodiment specifically comprises the following steps:
step S1: weighing five metal oxide powders of magnesium oxide, copper oxide, cobalt oxide, nickel oxide and zinc oxide according to an equimolar ratio, placing the powders in a stainless steel ball-milling tank, adding yttrium-stabilized zirconium dioxide beads with the diameter of 4mm as grinding balls, wherein the ball-to-material ratio is 20:1, obtaining high-entropy multi-principal-element oxide mixture nano powder with the rotating speed of 200rpm and the ball milling time of 100 hours;
step S2: in a high-purity argon-protected glove box (water oxygen < 0.01 ppm), weighing 1g of multi-principal-element oxide mixture nano powder and 9g of 1060 industrial pure aluminum alloy powder, placing the powder in a vacuum-sealed stainless steel ball milling tank, adding 0.5g of polyethylene glycol (Mn 2000) as a process control agent, adding yttrium-stabilized zirconia beads with the diameters of 4mm, 6mm and 10mm (mass ratio 5: sealing a stainless steel ball milling tank in a glove box, taking out and carrying out ball milling at the rotation speed of 200rpm for 10h to obtain premixed powder. Then placing the premixed powder in a high-purity argon protective atmosphere, heating to 450 ℃, preserving heat for 1h, and completely volatilizing the process control agent to obtain aluminum-based composite material powder;
and step S3: weighing 0.82g of aluminum-based composite material powder, placing the powder into a flat-bottom round groove die with the diameter of 16mm and the depth of 5mm, rotating a cylindrical large plastic deformation compression bar with the diameter of 16mm at a high speed and pressing the compression bar into the flat-bottom round groove, wherein the rotating speed is 500rpm, compressing the powder to the thickness of 1.0mm while performing friction deformation between the compression bar and the powder, and carrying for 180s. The densification and the ultrafine crystallization of the powder are realized through the direct friction deformation heat generation and the high accumulated plastic strain of the die and the powder, and finally the multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material is obtained.
Example 3
The preparation method of the multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material in the embodiment specifically comprises the following steps:
step S1: weighing seven metal oxide powders of aluminum oxide, cobalt oxide, chromium oxide, iron oxide, manganese oxide, nickel oxide and yttrium oxide according to an equimolar ratio, placing the powders in a stainless steel ball-milling tank, and adding yttrium-stabilized zirconium dioxide beads with the diameter of 4mm as grinding balls, wherein the ball-to-material ratio is 100:1, obtaining high-entropy multi-principal-element oxide mixture nano powder with the rotating speed of 500rpm and the ball milling time of 10 hours;
step S2: weighing 0.5g of multi-principal component oxide mixture nano powder and 9.5g of 6082Al-Mg-Si aluminum alloy powder in a glove box (water oxygen is less than 0.01 ppm) protected by high-purity argon, placing the powder in a vacuum sealing type stainless steel ball milling tank, adding 0.4g of polyethylene glycol (Mn 2000) as a process control agent, adding yttrium-stabilized zirconium dioxide beads with the diameter of 10mm as grinding balls, wherein the ball-to-material ratio is 50:1, sealing a stainless steel ball milling tank in a glove box, taking out and carrying out ball milling at the rotation speed of 400rpm for 2 hours to obtain premixed powder. Then placing the premixed powder in a high-purity argon protective atmosphere, heating to 450 ℃, preserving heat for 0.5h, and completely volatilizing the process control agent to obtain aluminum-based composite material powder;
and step S3: weighing 0.80g of aluminum-based composite material powder, placing the powder in a flat-bottom circular groove die with the diameter of 16mm and the depth of 5mm, rotating a cylindrical large plastic deformation compression bar with the diameter of 16mm at a high speed and pressing the compression bar into the flat-bottom circular groove, wherein the rotating speed is 8000rpm, compressing the powder to the thickness of 1.0mm while performing friction deformation between the compression bar and the powder which rotate at the high speed, and carrying for 3s. The densification and the ultrafine crystallization of the powder are realized through the direct friction deformation heat generation and the high accumulated plastic strain of the die and the powder, and finally the multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material is obtained.
While the invention has been described with reference to specific preferred embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but is intended to cover various modifications and alternative embodiments, which may be apparent to those skilled in the art, within the spirit and scope of the invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (8)

1. A preparation method of a multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material is characterized by comprising the following steps:
step S1: mixing and ball-milling at least 5 kinds of metal oxide powder with equal molar ratio to obtain high-entropy multi-principal-element oxide mixture nano powder;
step S2: mixing and ball-milling the high-entropy multi-principal-element oxide mixture nano powder, aluminum powder and a process control agent in an argon protective atmosphere, heating and preserving heat to obtain aluminum-based composite material powder;
and step S3: carrying out rotary extrusion and load retention on the aluminum-based composite material powder by a large plastic deformation solid-phase sintering one-step method to obtain a multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material;
the aluminum matrix composite powder is rotationally extruded and carried by a large plastic deformation solid phase sintering one-step method, and the method comprises the following steps: placing the aluminum-based composite material powder in a flat-bottom round groove die of a large plastic deformation solid-phase sintering one-step method, and rotationally extruding and load-retaining the aluminum-based composite material powder through a pressure bar corresponding to the diameter of the flat-bottom round groove die; the rotating speed is 500-8000rpm, and the load-holding time is 3-180s.
2. The method for preparing a multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material according to claim 1, wherein in step S1, the metal oxide comprises one of lithium oxide, magnesium oxide, aluminum oxide, calcium oxide, scandium oxide, titanium oxide, vanadium oxide, chromium oxide, manganese oxide, iron oxide, cobalt oxide, nickel oxide, copper oxide, zinc oxide, yttrium oxide, zirconium oxide, niobium oxide, molybdenum oxide, cerium oxide, tantalum oxide, and tungsten oxide.
3. The method for preparing the multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material according to claim 1, wherein in step S1, the ball milling process comprises: carrying out ball milling by adopting a stainless steel ball milling tank and yttrium-stabilized zirconium dioxide bead grinding balls; the diameter of the grinding ball is 4-10mm, and the ball-to-material ratio of the ball mill is (20-100): 1, the ball milling speed is 200-500rpm, and the ball milling time is 10-100h.
4. The method for preparing the multi-principal element oxide dispersion-strengthened ultra-fine grain aluminum-based composite material of claim 1, wherein in the step S2, the ball-milling has a ball-to-material ratio of (5-50): 1, the ball milling speed is 200-500rpm, and the ball milling time is 2-50h.
5. The method for producing a multi-host oxide dispersion-strengthened ultrafine-grained aluminum-based composite material according to claim 1, wherein in step S2, the aluminum powder comprises at least one of pure aluminum powder, 2 xxx-based Al-Cu or Al-Cu-Li-based powder, 5 xxx-based Al-Mg-based powder, 6 xxx-based Al-Mg-Si-based powder, and 7 xxx-based Al-Zn-Mg-Cu-based powder, and has an average particle diameter of 1 μm to 200 μm.
6. The method for preparing the multi-principal element oxide dispersion-strengthened ultrafine grained aluminum-based composite material according to claim 1, wherein in step S2, the heating temperature is 400 to 450 ℃, and the holding time is 0.5 to 1 hour.
7. The method for preparing the multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material according to claim 1, wherein in step S2, the mass fraction of the high-entropy multi-principal-element oxide mixture nanopowder in the aluminum-based composite material powder is 1-95%.
8. The multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material is characterized by being prepared by the preparation method of the multi-principal-element oxide dispersion-strengthened ultrafine-grained aluminum-based composite material according to any one of claims 1 to 7.
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