CN110523997A - A kind of subzero treatment aluminum matrix composite and preparation method thereof of high-entropy alloy particle enhancing - Google Patents
A kind of subzero treatment aluminum matrix composite and preparation method thereof of high-entropy alloy particle enhancing Download PDFInfo
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- CN110523997A CN110523997A CN201910764316.0A CN201910764316A CN110523997A CN 110523997 A CN110523997 A CN 110523997A CN 201910764316 A CN201910764316 A CN 201910764316A CN 110523997 A CN110523997 A CN 110523997A
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 127
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 127
- 239000000956 alloy Substances 0.000 title claims abstract description 107
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 105
- 239000002131 composite material Substances 0.000 title claims abstract description 97
- 239000011159 matrix material Substances 0.000 title claims abstract description 68
- 239000002245 particle Substances 0.000 title claims abstract description 45
- 230000002708 enhancing effect Effects 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 239000000843 powder Substances 0.000 claims abstract description 106
- 239000000758 substrate Substances 0.000 claims abstract description 38
- 230000005291 magnetic effect Effects 0.000 claims abstract description 32
- 239000011812 mixed powder Substances 0.000 claims abstract description 17
- 238000009768 microwave sintering Methods 0.000 claims abstract description 14
- 238000000498 ball milling Methods 0.000 claims description 39
- 238000000034 method Methods 0.000 claims description 28
- 239000004411 aluminium Substances 0.000 claims description 22
- 238000001238 wet grinding Methods 0.000 claims description 22
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 20
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 238000005275 alloying Methods 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 12
- 239000010935 stainless steel Substances 0.000 claims description 12
- 229910001220 stainless steel Inorganic materials 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 10
- 229910002065 alloy metal Inorganic materials 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 229910052796 boron Inorganic materials 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 229910052706 scandium Inorganic materials 0.000 claims description 8
- 239000000654 additive Substances 0.000 claims description 7
- 230000000996 additive effect Effects 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000009837 dry grinding Methods 0.000 claims description 6
- 210000001161 mammalian embryo Anatomy 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 230000002787 reinforcement Effects 0.000 claims description 6
- 229910052772 Samarium Inorganic materials 0.000 claims description 5
- 238000005056 compaction Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 229910052758 niobium Inorganic materials 0.000 claims description 4
- 238000004886 process control Methods 0.000 claims description 4
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 4
- 239000012300 argon atmosphere Substances 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 230000005415 magnetization Effects 0.000 claims description 3
- 230000010358 mechanical oscillation Effects 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000005057 refrigeration Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 229910002545 FeCoNi Inorganic materials 0.000 claims description 2
- 239000011324 bead Substances 0.000 claims description 2
- 238000005551 mechanical alloying Methods 0.000 claims description 2
- 239000008188 pellet Substances 0.000 claims description 2
- 239000006104 solid solution Substances 0.000 claims description 2
- 230000003068 static effect Effects 0.000 claims description 2
- 230000001629 suppression Effects 0.000 claims description 2
- 239000002023 wood Substances 0.000 claims description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 238000005538 encapsulation Methods 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 229910052726 zirconium Inorganic materials 0.000 claims 1
- 238000013461 design Methods 0.000 abstract description 6
- 239000004615 ingredient Substances 0.000 abstract description 6
- 238000003825 pressing Methods 0.000 abstract description 2
- 238000000748 compression moulding Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 230000005389 magnetism Effects 0.000 description 10
- 239000013078 crystal Substances 0.000 description 9
- 229910001172 neodymium magnet Inorganic materials 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 229910000838 Al alloy Inorganic materials 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 229910052779 Neodymium Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 2
- 229910000905 alloy phase Inorganic materials 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005294 ferromagnetic effect Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- NIBOOWWJLUHQPC-UHFFFAOYSA-N alumane;argon Chemical compound [AlH3].[Ar] NIBOOWWJLUHQPC-UHFFFAOYSA-N 0.000 description 1
- ZDVYABSQRRRIOJ-UHFFFAOYSA-N boron;iron Chemical compound [Fe]#B ZDVYABSQRRRIOJ-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000000320 mechanical mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000007780 powder milling Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
- B22F3/24—After-treatment of workpieces or articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0408—Light metal alloys
- C22C1/0416—Aluminium-based alloys
-
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1054—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by microwave
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/042—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling using a particular milling fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention belongs to technical field of composite preparation, and in particular to a kind of subzero treatment aluminum matrix composite and preparation method thereof of high-entropy alloy particle enhancing.The present invention is by preferred design high-entropy alloy ingredient, and then vacuum sphere mill prepares high-entropy alloy, the aluminum substrate powder of high-entropy alloy powder and microalloying mix in proportion it is dry after obtain mixed powder；Using isostatic cool pressing compression moulding, composite material billet is obtained；The aluminum matrix composite of high-entropy alloy particle enhancing is obtained using microwave sintering process；Aluminum matrix composite is finally subjected to subzero treatment.The present invention can make aluminum matrix composite have good magnetic property while high-entropy alloy particle enhanced aluminum-based composite material realizes aluminum matrix composite intensity and plasticity improves.
Description
Technical field
The present invention relates to technical field of composite preparation, and in particular to a kind of subzero treatment of high-entropy alloy particle enhancing
Aluminum matrix composite and preparation method thereof.
Background technique
As that studies aluminum matrix composite gos deep into, discovery has high than strong using particle enhanced aluminum-based composite material
The excellent properties such as degree, high ratio modulus, wearability and good stability of the dimension.Natural interface cohesion is special between metal and metal
Property, the boundary lubrication and interface compatibility between high-entropy alloy and aluminum-based matrix are good；Using specific high-entropy alloy particle as aluminium
The reinforced phase of sill can break through the bottleneck of traditional ceramic particle enhancing and toughening alumina-base material, it is multiple to can be realized aluminium base
The raising of condensation material intensity and plasticity.High-entropy alloy can have both higher intensity and good plasticity by ingredient design, still
The research of its magnetic property is very few, and existing high-entropy alloy system often contains ferromagnetic element Fe, Co, Ni, thus, research has
The magnetic high-entropy alloy reinforced aluminum matrix composites of good comprehensive performance are imperative.
When using high-entropy alloy particle enhanced aluminum-based composite material, preparing high-entropy alloy reinforcement, there are a variety of methods, mesh
Preceding comparative maturity and use scope it is most wide be using vacuum arc is molten plus the quick water cooling of copper mold；But the button of arc cast preparation
Ingot size is smaller, and the coarse as-cast structure of high-entropy alloy keeps alloy material performance poor, additionally as reinforced particulate, must also
The high-entropy alloy of as cast condition must be carried out being crushed can just be added in aluminum-based matrix；This conventional method efficiency is lower, higher cost,
And the performance of the aluminum matrix composite of enhancing is influenced to a certain extent.Microwave Sintering Techniques are a kind of the new of material sintering process
Method has many advantages, such as whole heating, low temperature fast firing, improves tissue and performance, safety non-pollution, can be realized the entirety of material
Heating；Under microwave field action, it can effectively accelerate densification process；The heating rate of microwave sintering method is fast, and crystal grain comes not
And grow up, it is easy to get to uniform fine grained texture, composite material can be made to obtain better toughness and ductility.
To the mechanism for the mechanical property for improving aluminium alloy at home and abroad there are no being formed to come to a conclusion, domestic is Central-South for subzero treatment
Chen Ding of university et al. has certain research to it, he points out aluminium and aluminium alloy after subzero treatment, and mechanical property can mention
Height finds that the intensity value of some diffraction maximums changes, to propose crystal grain rotation effect by observing X-ray diffraction analysis
Answer theory.Since crystal grain is in rotation, the direction for being conducive to hinder the movement of dislocation may be gone to, and then improve aluminium alloy material
The plasticity and toughness of material.Wang Qifan of domestic Institutes Of Technology Of Taiyuan etc. studies the discovery of subzero treatment sintered NdFeB, and subzero treatment can
The ratio of the increase and some non-magnetic phases that make the main magnetic phase proportion of neodymium iron boron sample reduce and the reduction of hole to
The consistency of magnet is improved, to improve remanent magnetism, and then improves maximum magnetic energy product.
Summary of the invention
Based on the deficiencies of the prior art, the present invention provides a kind of subzero treatment aluminum-base composite material of high-entropy alloy particle enhancing
Material, while providing preparation method, using high-entropy alloy particle enhanced aluminum-based composite material realize aluminum matrix composite intensity and
Plasticity improves, while subtle stress weight occurs by the aluminum matrix composite that cryogenic treatment process enhances high-entropy alloy particle
New distribution and tissue change, make aluminum matrix composite have good magnetic property, make aluminium while improving the plastic toughness of material
Based composites have more extensive use.
For achieving the above object, the technical solution adopted by the present invention are as follows:
A kind of subzero treatment aluminum matrix composite of high-entropy alloy particle enhancing, which is characterized in that the high-entropy alloy
Particle is reinforcement, and the high-entropy alloy component atoms are FeCoNi than expression formula1.5CrCuMx, wherein 0.5≤x≤1.5, x are
Molar ratio, M are Nb and B；Micro alloying element Ti, La, Sc and Sm are added in the aluminum substrate.
Further, the additive amount that rare earth element Sm is added in aluminum substrate is 0.6vol%~0.8vol%, Ti element
Additive amount is 0.04vol%~0.06vol%, and the additive amount of Sc element is 0.6vol%~0.8vol%, the addition of La element
Amount is 0.08vol%~0.12vol%, remaining is aluminium.
Further, the high-entropy alloy particle is face-centered cubic solid solution alloy system.
The preparation method of the subzero treatment aluminum matrix composite of the high-entropy alloy particle enhancing, which is characterized in that packet
Include following steps:
(1) high-entropy alloy powder is prepared, high-entropy alloy metal powder is weighed and is placed in stainless steel jar mill, in ball grinder
Zirconia ball is added, stainless steel jar mill is vacuumized to and is filled with argon gas, high-entropy alloy powder is subjected to mechanical alloying；First do
Wet-milling after mill, drum's speed of rotation of dry grinding when ball milling starts are 150-200r/min, Ball-milling Time 12-20h, and when wet-milling was added
Vacuumize and be filled with argon gas after program-controlled preparation n-hexane, drum's speed of rotation 260-300r/min, Ball-milling Time 36-40h are wet
Powder is taken out after mill, and the powder after ball milling is put into vacuum oven dry 20-30h and obtains high-entropy alloy powder；
(2) aluminum substrate powder is prepared, pure aluminium powder is weighed and micro alloying element is placed in stainless steel jar mill, in ball grinder
Stainless steel jar mill, is vacuumized and is filled with argon gas, by aluminum substrate by middle addition zirconia ball and wet-milling process control agent normal hexane
Powder carries out microalloying and refines pure aluminium powder simultaneously；Wet-milling drum's speed of rotation is 260-300r/min when ball milling, and Ball-milling Time is
24-30h takes out powder after wet-milling, the powder after ball milling is put into vacuum oven dry 20-30h obtains microalloying and receive
Meter level aluminum substrate powder；
(3) ultrasonic wave disperses mixed powder, and high-entropy alloy powder prepared by step (1) is added in ball grinder and is weighed in proportion
Normal hexane wet-milling is added using zirconia ball as ball-milling medium in the aluminum substrate powder of good step (2) preparation, carries out vacuum ball milling
Mixed powder, specific ball milling parameter are 180r/min × 3h+200r/min × 10h, obtain mixed-powder；Then mixed-powder is placed in
Ultrasonic wave dispersion is carried out by medium of normal hexane in container, drying and processing is carried out to mixed-powder in vacuum drying box later,
Temperature is 55 DEG C~65 DEG C, is uniformly mixed, the composite powder of soilless sticking；
(4) composite powder prepared by step (3) is placed in rubber mold by green compact, using the method for mechanical oscillation by rubber
The abundant jolt ramming of powder in sealing rubber die after vacuumizing rubber mold, is pressed into base with cold isostatic compaction method, obtains fine and close answer
Condensation material billet；
(5) the composite material billet for obtaining step (4) carries out microwave sintering, by composite material obtained in step (4)
It is placed in the microwave agglomerating furnace that microwave power is 4kW, is sintered under an argon atmosphere, first with the heating rate of 100 DEG C/min
From room temperature to 200 DEG C, the pre-sintering of 200 DEG C × 20min is carried out, removes the gas inside composite material billet, then again
500 DEG C -550 DEG C are warming up to the heating rate of 50 DEG C/min, carries out the microwave sintering of 500 DEG C -550 DEG C × 45min；Final
The aluminum matrix composite enhanced to high-entropy alloy particle；
(7) aluminum matrix composite that high-entropy alloy particle enhances is put into deep freeze refrigeration plant, with the speed of 8 DEG C/min from room
25 DEG C of temperature drops to -175 DEG C, and in -175 DEG C of heat preservation 4h；Sample restores with deep cooling box to room temperature after subzero treatment；It will be through too deep
The aluminum matrix composite of the high-entropy alloy particle enhancing of cold treatment is in high-intensity magnetic field after impulse magnetization.
Further, 99.9% or more the metal powder purity of the raw material use of high-entropy alloy powder, aluminum substrate powder,
Powder size is not more than 45 μm；99.9% or more pure aluminium powder powder purity, granularity is less than 300 μm；The high-entropy alloy powder of preparation
Last grain graininess range is 30~50nm.
Further, in step (3), when high-entropy alloy powder is mixed with aluminum substrate powder, the total matter of high-entropy alloy powder Zhan
35~40wt% of amount, the mass content of aluminum substrate powder are as follows: 60wt%~65wt%.
Further, after the cold isostatic compaction method is the mixed-powder drying that will be prepared, it is loaded into rubber package set,
It is pressed into raw embryo, between 75-85%, gained raw embryo Vacuum Package saves raw embryo consistency；The medium static pressure suppression of forming process
When, using the oil pressure load of 250-300Mpa, and the dwell time is 1-2min.
Further, 8. the preparation method according to claim 4, which is characterized in that in step (2), the ball of ball milling
Material mass ratio is 10:1~15:1；Normal hexane additional amount is 35-45ml.
Further, when the high-entropy alloy metal powder ball milling, zirconium oxide balls diameter is respectively 15,10 and 6mm,
Big ball: middle ball: the mass ratio of bead is 1:2:4, and ball material mass ratio is 8:1~10:1.
Further, when high-entropy alloy metal powder dry grinding, 5min is shut down after every rotation 30min；When wet-milling, just
Hexane additional amount is 35-45ml.
Compared with prior art, beneficial effects of the present invention embody as follows:
(1) the subzero treatment aluminum matrix composite of high-entropy alloy particle enhancing provided by the invention, the high-entropy alloy
Particle is reinforcement, and alloying component atomic ratio expression formula is FeCoNi1.5CrCuMx, wherein 0.5≤x≤1.5, x are mole
Than M is Nb and B.The aluminum substrate is to add the aluminum substrate that micro alloying element is Ti, La, Sc and Sm.In aluminum-base composite material
In material, the generation of the rare earth elements such as boron element, ferro element and neodymium element is also easy to produce the ferromagnetic neodymium of low temperature in high-entropy alloy system
Iron boron phase, while the neodymium iron boron is mutually Nd2Fe14B is substrate, Nd-rich phase and boron-rich phase and the three-phase structure deposited, and Nd-rich phase is main
It is distributed in around main magnetic phase crystal boundary, there is higher magnetic energy product and reliable coercivity.In addition, the main magnetic after subzero treatment
The diffraction peak intensity of property phase is enhanced；And in some non-magnetic phases and soft magnetism phase, then after subzero treatment, diffraction maximum
Intensity weakened.Last composite material carries out Metallographic Analysis discovery, the rich neodymium in the aluminum matrix composite after subzero treatment
The distribution of phase is more uniform, and grain boundary is more round and smooth；In addition, observation crystal grain can see, the black after subzero treatment
Graininess dot becomes more；Additionally, due to the principle expanded with heat and contract with cold, the hole inside magnet is slightly reduced.Thus it is seen that at deep cooling
The increase of the main magnetic phase proportion of the aluminum matrix composite that reason can be such that high-entropy alloy particle enhances and some non-magnetic phases
Ratio is reduced and the reduction of hole is to improve the consistency of aluminum matrix composite, so that it is surplus to improve aluminum matrix composite
Magnetic, and then improve maximum magnetic energy product；Simultaneously because subzero treatment reduces the spin-exchange-coupled of aluminum matrix composite main phase grain
Effect, is improved the coercivity of aluminum matrix composite.
(2) high-entropy alloy particle enhanced aluminum-based composite material of the invention, designs and prepares process optimization by ingredient, makes
The alloy structure that there is aluminum matrix composite reinforcement particle face-centred cubic structure to mix with a variety of magnetic phase structures, by high energy
The high-entropy alloy that ball milling obtains is nanocrystalline segregation on aluminum substrate crystal boundary, high-entropy alloy particle after vacuum ball milling mixes powder,
Disperse is evenly distributed in aluminum substrate, can be generated metal phase enhancing and be strengthened；In microwave sintering densification process, high entropy is closed
For metallographic with aluminum substrate phase while keeping respective crystal structure, being formed has the Interface bonding mechanism centainly spread, thus real
The strong plasticity of the aluminum matrix composite of existing high-entropy alloy particle enhancing combines, and prepares the high-entropy alloy particle enhancing of high-strength and high ductility
Aluminum matrix composite.
(3) preparation method of the invention, when carrying out mixing high-entropy alloy powder and aluminum substrate powder, using work
Skill optimization mechanical attrition method+ultrasonic wave disperse blending processes of powders, can be uniformly mixed, the composite powder of soilless sticking it is same
Shi Jinliang reduces ball milling and mixes powder energy, effectively avoids influence of the high energy to the high-entropy alloy particle of alloying.
(4) present invention has been made full use of using combined microalloying principle using micro alloying element Ti, Sm, La, Sc
The compound action of beneficial element improves the interface cohesion between high-entropy alloy particle and Al matrix, refines crystal grain, improves aluminum-base composite
Plasticity and toughness, hardness, tensile strength, wearability of material etc..
(5) preparation method of the invention prepares composite material using microwave sintering method using nano particle matrix, utilizes
Microwave sintering method can be realized whole heating, low temperature fast firing, the characteristic that alternative heats, improvement tissue and performance are excellent, be made
High-entropy alloy distribution of particles disperse, crystal grain refinement, consistency is 98% or more, and porosity is in 3% aluminum matrix composite below；
And have the characteristics of low temperature fast firing to material under microwave field action using microwave sintering method, it can effectively avoid sintering aluminium base
Expect that hot-spot causes aluminium base body portion to melt when block.
Detailed description of the invention
Fig. 1 is that the subzero treatment aluminum matrix composite of high-entropy alloy particle enhancing of the present invention prepares preparation method stream
Cheng Tu.
Fig. 2 is that high-entropy alloy granule content is the aluminum matrix composite of 35wt% before and after subzero treatment in embodiment 1
XRD compares map.
Fig. 3 is that high-entropy alloy granule content is the aluminum matrix composite of 40wt% before and after subzero treatment in embodiment 2
XRD compares map.
Fig. 4 is the micro-organization chart of the aluminum matrix composite prepared in embodiment 1.
Fig. 5 is the micro-organization chart of the aluminum matrix composite prepared in embodiment 2.
Specific embodiment
The present invention provides following case study on implementation, but is not the application range and condition for limiting the invention in any way.
Embodiment 1:
The present embodiment prepares aluminum matrix composite according to process flow shown in FIG. 1, specific:
(1) raw material selects, and prepares the purity of high-entropy alloy metal powder 99.9% or more, powder size is not more than 45
μm, ingredient is carried out according to molar ratio with high-entropy alloy ingredient；Prepare the purity of pure aluminium powder powder in 99.9wt% or more, fine aluminium
Powder powder size is not more than 300 μm, uses precision for the electronic balance weighing metal powder of 0.01g.The high-entropy alloy
Grain is reinforcement, and selecting the high-entropy alloy component atoms of preparation than expression formula is FeCoNi1.5CrCuM, M are Nb and B；
Aluminum substrate is the aluminium alloy for being added to micro alloying element Ti, La, Sc and Sm.The microalloying member added in fine aluminium
Element is Ti, La, Sc and Sm；Weighed with volume fraction and add micro alloying element: rare earth element Sm optimum addition is
0.6vol%~0.8vol%, Ti element optimum addition are 0.04vol%~0.06vol%, and Sc element optimum addition is
0.6vol%~0.8vol%, La element optimum addition are 0.08vol%~0.12vol%.
(2) prepared by high-entropy alloy powder, and the high-entropy alloy metal powder that step (1) weighs is placed in stainless steel jar mill
In, zirconia ball is added in ball grinder, stainless steel jar mill is vacuumized to and is filled with argon gas, high-entropy alloy powder is subjected to machine
Tool alloying；Wet-milling after first dry grinding, drum's speed of rotation of dry grinding when ball milling starts is 150-200r/min, Ball-milling Time 12-
20h vacuumizes and is filled with argon gas, drum's speed of rotation 260-300r/min, ball after adition process controlling agent n-hexane when wet-milling
Time consuming is 36-40h, takes out powder after wet-milling, and the powder after ball milling is put into vacuum oven dry 20-30h and obtains height
Entropy alloy powder.
(3) prepared by aluminum substrate powder, and pure aluminium powder and micro alloying element that step (1) weighs are placed in stainless steel jar mill
In, zirconia ball and wet-milling process control agent normal hexane are added in ball grinder, stainless steel jar mill is vacuumized and is filled with argon
Aluminum substrate powder is carried out microalloying and refines pure aluminium powder simultaneously by gas；Wet-milling drum's speed of rotation is 260-300r/min when ball milling,
Ball-milling Time is 24-30h, takes out powder after wet-milling, and the powder after ball milling is put into vacuum oven dry 20-30h and is obtained
Microalloying nanometer aluminum matrix powder；
(4) ultrasonic wave disperses mixed powder, and high-entropy alloy powder prepared by step (2) is added in ball grinder and is weighed in proportion
Normal hexane wet-milling is added using zirconia ball as ball-milling medium in the aluminum substrate powder of good step (3) preparation, carries out vacuum ball milling
Mixed powder, specific ball milling parameter are 180r/min × 3h+200r/min × 10h, obtain mixed-powder；Then mixed-powder is placed in
Ultrasonic wave dispersion is carried out by medium of normal hexane in container, drying and processing is carried out to mixed-powder in vacuum drying box later,
Temperature is 55 DEG C~65 DEG C, is uniformly mixed, the composite powder of soilless sticking；The mass content of high-entropy alloy powder is when mixed powder
35wt%, the mass content of aluminium substrate alloy powder are 65wt%.
(5) composite powder prepared by step (4) is placed in rubber mold by green compact, using the method for mechanical oscillation by powder
The abundant jolt ramming in end, after rubber mold is vacuumized, is pressed into base with cold isostatic compaction method, obtains fine and close composite wood material base
Ingot.
(6) the composite material billet for obtaining step (5) carries out microwave sintering, by composite material obtained in step (5)
It is placed in the microwave agglomerating furnace that microwave power is 4kW, is sintered under an argon atmosphere, first carry out the pre-burning of 200 DEG C × 20min
Knot removes the gas inside composite material billet, then carries out the microwave sintering of 500-550 DEG C × 45min again；Finally obtain height
The aluminum matrix composite of entropy alloying pellet enhancing.
(7) the aluminum matrix composite sample that high-entropy alloy particle enhances is put into the deep freeze refrigeration plant of SLX-30, with 8 DEG C/
The speed of min drops to -175 DEG C from 25 DEG C of room temperature, and in -175 DEG C of heat preservation 4h.After subzero treatment sample with deep cooling box restore to
Room temperature.The aluminum matrix composite sample that high-entropy alloy particle Jing Guo subzero treatment is enhanced impulse magnetization in high-intensity magnetic field
Afterwards, with NIM-1000 type permanent-magnet material analyzer to its magnetism testing, the magnetic parameters such as available Br, Hci, (BH) max,
To the aluminum matrix composite of the high-entropy alloy particle of preparation enhancing using the analyses such as XRD, testing machine for mechanical properties carry out structure and
Performance characterization.
It is as follows to test and analyze result:
A. Fig. 2 show in the present embodiment the XRD before and after subzero treatment, XRD analysis discovery, aluminum substrate and high-entropy alloy
Respective crystallographic structure is kept, the main magnetic phase Nd of some diffraction maximum variations is labelled with2Fe14B and non-master magnetic phase, pass through ratio
To PDF card it can be found that mass content is the aluminum matrix composite of 35wt% high-entropy alloy enhancing after subzero treatment, main magnetic
Property phase Nd2Fe14The diffraction peak intensity of B phase enhances, and the diffracted intensity of the phases such as soft magnetism phase and boron-rich phase, which then has, slightly to be declined.Main magnetic
Property phase Nd2Fe14B content is moderate, is evenly distributed, and is conducive to improve material hardness and toughness, main magnetism phase Nd2Fe14B, which increases, to be helped
In the aluminum matrix composite magnetic property of enhancing.As shown in Figure 4, see from micro-organization chart, obtained according to 1 preparation method of embodiment
To mass content be 35wt% high-entropy alloy enhancing subzero treatment aluminum matrix composite in high-entropy alloy phase content it is moderate.
B. the microhardness that reset condition pure aluminum substrate is tested is 81.2HV, utilizes high-entropy alloy in the present embodiment
The aluminum matrix composite microhardness of grain enhancing is 148.9HV.
C. the elasticity modulus that reset condition pure aluminum substrate is tested is 71.2GPa, utilizes high-entropy alloy in the present embodiment
The aluminum matrix composite elasticity modulus of particle enhancing is 83.9GPa, and Modulus of Composites is improved compared to pure aluminum substrate
17.84%.
D. magnetic property analysis result is as follows: remanent magnetism (Br) reaches 0.28T, and coercivity (Hcj) reaches 450kAm-1, magnetic energy product (BH) max reaches 82k Jm-3。
Embodiment 2:
High-entropy alloy powder preparation: the mass content of high-entropy alloy powder is 40wt%, aluminum substrate when experimental design mixes powder
The mass content of alloyed powder is 60wt%；Remaining preparation method is same as Example 1.
A. see from micro-organization chart Fig. 5, be 40wt% high entropy according to the mass content that 1 preparation method of embodiment obtains
The subzero treatment aluminum matrix composite of alloy enhancing is compared to sample in embodiment 1, hence it is evident that sees high entropy in aluminum matrix composite
Alloy phase content increases.Fig. 3 show in the present embodiment the XRD before and after subzero treatment, and XRD analysis discovery is labelled with
The main magnetic phase Nd of diffraction maximum variation2Fe14B and non-master magnetic phase, by comparing PDF card it can be found that mass content is
The aluminum matrix composite of 40wt% high-entropy alloy enhancing is after subzero treatment, main magnetism phase Nd2Fe14The diffraction peak intensity of B phase is bright
Aobvious enhancing, the diffracted intensity of the phases such as soft magnetism phase and boron-rich phase, which then has, slightly to be declined.Main magnetism phase Nd2Fe14B content is more, point
Cloth is uniform, moderate dimensions, is conducive to improve material hardness and toughness, highly beneficial to the aluminum matrix composite magnetic property of enhancing.
B. the microhardness that reset condition pure aluminum substrate is tested is 81.2HV, utilizes high-entropy alloy in the present embodiment
The aluminum matrix composite microhardness of grain enhancing is 159.8HV.
C. the elasticity modulus that reset condition pure aluminum substrate is tested is 71.2GPa, utilizes high-entropy alloy in the present embodiment
The aluminum matrix composite elasticity modulus of particle enhancing is 79.9GPa, and Modulus of Composites is improved compared to pure aluminum substrate
14.84%.
D. magnetic property analysis result is as follows: remanent magnetism (Br) will reach 0.34T, and coercivity (Hcj) reaches 490kA
m-1, magnetic energy product (BH) max reach 89k Jm-3。
The high-entropy alloy reinforced aluminum matrix composites of subzero treatment of the invention, using high-entropy alloy particle as reinforced phase.
It is the design principle according to high-entropy alloy first, designs the hard high-entropy alloy system of high-strength height；It is matched according to design ingredient
Alloy, using Mechanic Alloying Technology, vacuum sphere, which is ground, takes high-entropy alloy powder；The high-entropy alloy powder and ball milling that will be prepared
The fine aluminium powder for refining microalloying carries out sufficient mechanical mixture；Using isostatic cool pressing in advance at the technique of base microwave sintering again,
The aluminum matrix composite of high-entropy alloy enhancing is prepared, cryogenic treatment process then is carried out to aluminum matrix composite again and obtains performance
The high-entropy alloy reinforced aluminum matrix composites of excellent subzero treatment.
The above is only a preferred embodiment of the present invention, it should be pointed out that: for the ordinary skill people of the art
For member, without departing from the principle of the present invention, the replacement of several improvement and equivalent form can also be made, these improvement
The technical solution obtained with equivalent replacement also should belong to protection scope of the present invention.
Claims (10)
1. a kind of subzero treatment aluminum matrix composite of high-entropy alloy particle enhancing, which is characterized in that the high-entropy alloy
Grain is reinforcement, and the high-entropy alloy component atoms are FeCoNi than expression formula1.5CrCuMx, wherein 0.5≤x≤1.5, x are to rub
That ratio, M are Nb and B；Micro alloying element Ti, La, Sc and Sm are added in the aluminum substrate.
2. the subzero treatment aluminum matrix composite of high-entropy alloy particle enhancing according to claim 1, which is characterized in that aluminium
The additive amount that rare earth element Sm is added in matrix is 0.6vol%~0.8vol%, the additive amount of Ti element be 0.04vol%~
The additive amount of 0.06vol%, Sc element is 0.6vol%~0.8vol%, the additive amount of La element be 0.08vol%~
0.12vol%, remaining is aluminium.
3. the subzero treatment aluminum matrix composite of high-entropy alloy particle enhancing according to claim 1, which is characterized in that institute
The high-entropy alloy particle stated is face-centered cubic solid solution alloy system.
4. the preparation method of the subzero treatment aluminum matrix composite of high-entropy alloy particle enhancing described in claim 1, feature
It is, includes the following steps:
(1) high-entropy alloy powder is prepared, high-entropy alloy metal powder is weighed and is placed in stainless steel jar mill, be added in ball grinder
Stainless steel jar mill is vacuumized and is filled with argon gas by zirconia ball, and high-entropy alloy powder is carried out mechanical alloying；After first dry grinding
Wet-milling, dry grinding drum's speed of rotation are 150-200r/min, Ball-milling Time 12-20h, the adition process control in ball grinder when wet-milling
Argon gas, drum's speed of rotation 260-300r/min, Ball-milling Time 36-40h, after wet-milling are vacuumized and are filled with after preparation n-hexane
Powder is taken out, the powder after ball milling is put into vacuum oven dry 20-30h and obtains high-entropy alloy powder；
(2) aluminum substrate powder is prepared, pure aluminium powder is weighed and micro alloying element is placed in stainless steel jar mill, add in ball grinder
Enter zirconia ball and wet-milling process control agent normal hexane, stainless steel jar mill is vacuumized to and is filled with argon gas, by aluminum substrate powder
It carries out microalloying and refines pure aluminium powder simultaneously；Wet-milling drum's speed of rotation is 260-300r/min, Ball-milling Time 24- when ball milling
30h takes out powder after wet-milling, and the powder after ball milling is put into vacuum oven dry 20-30h and obtains microalloying nanoscale
Aluminum substrate powder；
(3) ultrasonic wave disperses mixed powder, high-entropy alloy powder prepared by step (1) is added in ball grinder load weighted in proportion
Normal hexane wet-milling is added using zirconia ball as ball-milling medium in the aluminum substrate powder of step (2) preparation, carries out vacuum ball milling and mixes powder,
Specific ball milling parameter is 180r/min × 3h+200r/min × 10h, obtains mixed-powder；Then mixed-powder is placed in container
It is interior to carry out ultrasonic wave dispersion by medium of normal hexane, drying and processing, temperature are carried out to mixed-powder in vacuum drying box later
It is 55 DEG C~65 DEG C, is uniformly mixed, the composite powder of soilless sticking；
(4) composite powder prepared by step (3) is placed in rubber mold by green compact, using the method for mechanical oscillation by rubber pattern
The abundant jolt ramming of powder in tool after vacuumizing rubber mold, is pressed into base with cold isostatic compaction method, obtains fine and close composite wood
Material base ingot；
(5) the composite material billet for obtaining step (4) carries out microwave sintering, and composite material obtained in step (4) is placed in
Microwave power is to be sintered under an argon atmosphere in the microwave agglomerating furnace of 4kW, first with the heating rate of 100 DEG C/min from room
Temperature is warming up to 200 DEG C, carries out the pre-sintering of 200 DEG C × 20min, the gas inside composite material billet is removed, then again with 50
DEG C/heating rate of min is warming up to 500 DEG C -550 DEG C, carry out the microwave sintering of 500 DEG C -550 DEG C × 45min；Finally obtain height
The aluminum matrix composite of entropy alloying pellet enhancing；
(7) aluminum matrix composite that high-entropy alloy particle enhances is put into deep freeze refrigeration plant, with the speed of 8 DEG C/min from room temperature 25
DEG C -175 DEG C are dropped to, and in -175 DEG C of heat preservation 4h；Sample restores with deep cooling box to room temperature after subzero treatment；It will be by deep cooling
The aluminum matrix composite for the high-entropy alloy particle enhancing managed is in high-intensity magnetic field after impulse magnetization.
5. the preparation method according to claim 4, which is characterized in that high-entropy alloy powder, aluminum substrate powder raw material adopt
99.9% or more metal powder purity, powder size are not more than 45 μm；99.9% or more pure aluminium powder powder purity, grain
Degree is less than 300 μm；The high-entropy alloy powder grain graininess range of preparation is 30~50nm.
6. the preparation method according to claim 4, which is characterized in that in step (3), high-entropy alloy powder and aluminum substrate powder
When the mixing of end, high-entropy alloy powder accounts for 35~40wt% of gross mass, the mass content of aluminum substrate powder are as follows: and 60wt%~
65wt%.
7. the preparation method according to claim 4, which is characterized in that the cold isostatic compaction method be will prepare it is mixed
After closing powder drying, it is loaded into rubber package set, is pressed into raw embryo, raw embryo consistency is between 75-85%, gained raw embryo vacuum
Encapsulation saves；When the medium static pressure suppression of forming process, using the oil pressure load of 250-300Mpa, and the dwell time is 1-
2min。
8. the preparation method according to claim 4, which is characterized in that in step (2), the ball material mass ratio of ball milling is 10:1
~15:1；Normal hexane additional amount is 35-45ml.
9. the preparation method according to claim 4, which is characterized in that when the described high-entropy alloy metal powder ball milling, oxygen
Changing zirconium ball radius is respectively 15,10 and 6mm, big ball: middle ball: the mass ratio of bead is 1:2:4, ball material mass ratio be 8:1~
10:1。
10. the preparation method according to claim 4, which is characterized in that when the high-entropy alloy metal powder is dry grinded, often
5min is shut down after rotation 30min；When wet-milling, normal hexane additional amount is 35-45ml.
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