CN109554572A - A kind of multiple dimensioned ceramic particle mixes high elastic modulus high-strength aluminum alloy and preparation method thereof - Google Patents
A kind of multiple dimensioned ceramic particle mixes high elastic modulus high-strength aluminum alloy and preparation method thereof Download PDFInfo
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- 239000002245 particle Substances 0.000 title claims abstract description 177
- 239000000919 ceramic Substances 0.000 title claims abstract description 125
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 121
- 238000002360 preparation method Methods 0.000 title claims abstract description 42
- 239000000843 powder Substances 0.000 claims abstract description 207
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 64
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 64
- 229910033181 TiB2 Inorganic materials 0.000 claims abstract description 25
- 239000000203 mixture Substances 0.000 claims abstract description 12
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 4
- 239000000956 alloy Substances 0.000 claims description 79
- 229910045601 alloy Inorganic materials 0.000 claims description 68
- 229910018566 Al—Si—Mg Inorganic materials 0.000 claims description 59
- 230000032683 aging Effects 0.000 claims description 56
- 239000002131 composite material Substances 0.000 claims description 45
- 239000004411 aluminium Substances 0.000 claims description 43
- 238000000034 method Methods 0.000 claims description 40
- 238000007254 oxidation reaction Methods 0.000 claims description 32
- 230000003647 oxidation Effects 0.000 claims description 31
- 238000010792 warming Methods 0.000 claims description 25
- 238000012545 processing Methods 0.000 claims description 23
- 238000000498 ball milling Methods 0.000 claims description 22
- 238000010907 mechanical stirring Methods 0.000 claims description 22
- 239000012459 cleaning agent Substances 0.000 claims description 18
- 239000002893 slag Substances 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 17
- 239000005030 aluminium foil Substances 0.000 claims description 16
- 238000007670 refining Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000004615 ingredient Substances 0.000 claims description 10
- 238000010791 quenching Methods 0.000 claims description 9
- 230000000171 quenching effect Effects 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminium flouride Chemical compound F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 claims description 6
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 6
- 239000010931 gold Substances 0.000 claims description 6
- 229910052737 gold Inorganic materials 0.000 claims description 6
- 238000005266 casting Methods 0.000 claims description 4
- 229910020056 Mg3N2 Inorganic materials 0.000 claims description 3
- 229910001610 cryolite Inorganic materials 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 3
- VHHHONWQHHHLTI-UHFFFAOYSA-N hexachloroethane Chemical compound ClC(Cl)(Cl)C(Cl)(Cl)Cl VHHHONWQHHHLTI-UHFFFAOYSA-N 0.000 claims description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims 3
- 239000006104 solid solution Substances 0.000 claims 1
- 238000011065 in-situ storage Methods 0.000 abstract description 19
- 239000000758 substrate Substances 0.000 abstract description 6
- 239000002105 nanoparticle Substances 0.000 abstract description 4
- 230000002195 synergetic effect Effects 0.000 abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 18
- 239000003795 chemical substances by application Substances 0.000 description 18
- 229910002804 graphite Inorganic materials 0.000 description 18
- 239000010439 graphite Substances 0.000 description 18
- 239000011812 mixed powder Substances 0.000 description 18
- 239000000463 material Substances 0.000 description 17
- 238000006243 chemical reaction Methods 0.000 description 14
- 229910052751 metal Inorganic materials 0.000 description 13
- 239000002184 metal Substances 0.000 description 13
- 229910052593 corundum Inorganic materials 0.000 description 12
- 239000010431 corundum Substances 0.000 description 12
- 238000003825 pressing Methods 0.000 description 12
- 239000000523 sample Substances 0.000 description 12
- 238000005728 strengthening Methods 0.000 description 12
- 239000008187 granular material Substances 0.000 description 11
- 238000004321 preservation Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 9
- 230000003014 reinforcing effect Effects 0.000 description 8
- 238000001035 drying Methods 0.000 description 7
- 238000002844 melting Methods 0.000 description 7
- 230000008018 melting Effects 0.000 description 7
- 238000004880 explosion Methods 0.000 description 6
- 238000000227 grinding Methods 0.000 description 6
- 238000000875 high-speed ball milling Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 229910001928 zirconium oxide Inorganic materials 0.000 description 6
- 238000007792 addition Methods 0.000 description 5
- -1 and optimizes TiCN Inorganic materials 0.000 description 5
- 238000000280 densification Methods 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 238000002604 ultrasonography Methods 0.000 description 5
- 235000013339 cereals Nutrition 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 230000000630 rising effect Effects 0.000 description 4
- 229910000905 alloy phase Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 229910000861 Mg alloy Inorganic materials 0.000 description 2
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 229910052571 earthenware Inorganic materials 0.000 description 2
- 238000010406 interfacial reaction Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910021364 Al-Si alloy Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- KMWBBMXGHHLDKL-UHFFFAOYSA-N [AlH3].[Si] Chemical compound [AlH3].[Si] KMWBBMXGHHLDKL-UHFFFAOYSA-N 0.000 description 1
- 239000011195 cermet Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/1015—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
- C22C1/1052—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites by mixing and casting metal matrix composites with reaction
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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- 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
- C22C21/02—Alloys based on aluminium with silicon as the next major constituent
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- 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
- C22C32/0047—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 carbides, nitrides, borides or silicides as the main non-metallic constituents
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
- C22F1/043—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys with silicon as the next major constituent
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- Crystallography & Structural Chemistry (AREA)
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Abstract
The present invention discloses a kind of multiple dimensioned ceramic particle and mixes high elastic modulus high-strength aluminum alloy, and the multiple dimensioned ceramic particle mixes the chemical composition and its mass percent of high elastic modulus high-strength aluminum alloy are as follows: Si:6.5%-10wt.%；Mg:0.3-0.7wt.%；SiC:2-8wt.%；TiCN, AlN and TiB2: 0.1-0.6wt.%；Surplus is Al.The present invention also provides the preparation methods that a kind of multiple dimensioned ceramic particle mixes high elastic modulus high-strength aluminum alloy, by Al powder, Ti powder and BN and B4The TiB of the TiCN particle of C powder sintering in-situ endogenic nano-scale, submicron-scale2High elastic modulus high-strength aluminum alloy is prepared with AlN particle and micron SiC ceramic particle, and optimizes TiCN, AlN and TiB2The content of particle and SiC particulate realizes the synergistic effect of nano-sized ceramic particles and micron-sized ceramic particles in aluminum substrate, improves the mechanical property of aluminium alloy.
Description
Technical field
The present invention relates to high-performance aluminium alloy processing and its preparation fields, and more particularly, the present invention relates to a kind of more rulers
Degree ceramic particle mixes high elastic modulus high-strength aluminum alloy and preparation method thereof.
Background technique
Hypoeutectic Al-Si-Mg alloy is as a kind of heat-treatable strengthened alloy, with natrual ageing ability, intensity compared with
Height, plasticity are preferable.In addition, the casting character of the alloy is excellent, good fluidity, linear shrinkage are small, hot cracking tendency is low, air-tightness is high,
Corrosion resistance is good.But with the continuous development of automobile, rail traffic and aerospace, military field in recent years, for required
The requirement of material property is also higher and higher.While the requirement light for material, it is also necessary to which alloy material keeps higher
Mechanical property.The means of usual reinforced alloys have heat treatment reinforcement or a particle strengthening agent, but conventionally used reinforced aluminium alloy
Hardening agent often damages the plasticity of material while improving intensity, therefore develops a kind of while improving hypoeutectic Al-Si-
The hardening agent of the strong moulding of Mg alloy becomes current key.Cermet containing interior raw ceramic particle is compound to carry out aluminium alloy
Say it is a kind of ideal hardening agent.The particle strengthening agent for mixing size is added into aluminium alloy, passes through various sizes of
It is a kind of reinforcing means with bright prospects that cooperating between grain, which further increases the performance of alloy,.Mix the pottery of scale
Porcelain particle can pass through the further reinforced aluminium alloy of modes such as grain refining strengthening, Ao Luowan reinforcing, precipitation hardened.This technology
In invention, SiC used is micron-scale, can dramatically increase the rigidity and elasticity modulus of aluminium alloy；But early-stage study table
Bright, low-alloyed plasticity can drop in the particle of a large amount of micron-scales；And by the way that Al-Ti-B is added4In-situ endogenic in C-BN system
TiCN-TiB containing nanometer and submicron-scale2- AlN particle strengthening agent, can be further improved the plasticity of alloy.By more
The compound addition of kind ceramic particle ensure that it is preferable while the rigidity and elasticity modulus for further increasing aluminium alloy
Plasticity.Al-Si-Mg alloy according to the present invention, as a kind of heat-treatable strengthened alloy, with natrual ageing ability,
Casting character is excellent, and good fluidity, air-tightness are high, corrosion resistance is good.So further increasing Al-Si-Mg alloy by the means
Comprehensive performance, the application field of the alloy can be widened, and step is relatively simple, it is easily operated, be suitable for industrial production, have
There is important practical application value.The elasticity modulus and rigidity of aluminium alloy further increase, can be to avoid the lower of aluminium alloy
The shortcomings that elasticity modulus, substitutes steel in wider range, realizes the exploitation of high-performance high rigidity lightweighting materials, have important
Application prospect.
Summary of the invention
It is an object of the invention to design and develop a kind of multiple dimensioned ceramic particle to mix high elastic modulus high intensity aluminium
Alloy passes through the TiCN particle of in-situ endogenic nano-scale, the TiB of submicron-scale2With AlN particle and additional micron SiC
Ceramic particle prepares high elastic modulus high-strength aluminum alloy, and optimizes TiCN, AlN and TiB2Particle and SiC particulate contain
Amount, improves the mechanical property of aluminium alloy.
Another object of the present invention is to have designed and developed a kind of multiple dimensioned ceramic particle to mix high elastic modulus high intensity
The preparation method of aluminium alloy, by Al powder, Ti powder and BN and B4TiCN particle, the sub-micro of C powder sintering in-situ endogenic nano-scale
The TiB of meter ruler cun2High elastic modulus high-strength aluminum alloy is prepared with AlN particle and micron SiC ceramic particle, and is optimized
TiCN, AlN and TiB2The content of particle and SiC particulate realizes nano-sized ceramic particles and micron-scale in aluminum substrate
The synergistic effect of ceramic particle improves the mechanical property of aluminium alloy.
Technical solution provided by the invention are as follows:
A kind of multiple dimensioned ceramic particle mixes high elastic modulus high-strength aluminum alloy, and the multiple dimensioned ceramic particle mixes height
The chemical composition and its mass percent of elasticity modulus high-strength aluminum alloy are as follows: Si:6.5%-10wt.%；Mg:0.3-
0.7wt.%；SiC:2-8wt.%；TiCN, AlN and TiB2: 0.1-0.6wt.%；Surplus is Al.
A kind of multiple dimensioned ceramic particle mixes the preparation method of high elastic modulus high-strength aluminum alloy, includes the following steps:
Step 1: by the SiC powder of high temperature oxidation process and Al-Si-Mg alloyed powder ball milling mixing, wrapping up aluminium foil and cylinder is made
Shape pottery aluminium composite green compact；
Wherein, the mass ratio of the SiC powder and Al-Si-Mg alloyed powder is 1:20-1:1.5, and the cylindrical pottery aluminium is compound
The consistency of green compact is 60-75%；
Step 2: by Al powder, Ti powder, BN powder and B4Cylindrical green compact is made in C powder ball milling mixing, package aluminium foil, and carries out true
Sky sintering, specifically includes:
It is warming up to 773K with the rate of 25-60K/min, keeps the temperature 15-25min；
It is continuously heating to 1173-1193K, keeps the temperature 10min, be cooled to 1073K, to the cylindrical green compact in insulating process
Apply the pressure of axial direction 25-55MPa, pressure maintaining 20-90s, vacuum cooled to room temperature；
Wherein, the consistency of the cylindrical green compact is 60-75%, the BN powder and B4The molar ratio of C powder is 1:1, institute
State Ti powder, B4The molar ratio of C powder and BN powder is 9:2.8:2.8, TiCN, AlN and TiB in the cylindrical green compact after vacuum-sintering2
The mass fraction of particle is 20-40wt.%；
Step 3: by Al-Si-Mg alloy, molten refined obtains Al-Si-Mg aluminium alloy at 1073-1123K；
The cylindrical green compact is placed in Al-Si-Mg aluminium alloy, mechanical stirring 60-180s；
The cylindrical pottery aluminium composite green compact is placed in Al-Si-Mg aluminium alloy again, mechanical stirring 120-300s, heat preservation
After 3-5min, it is ultrasonically treated 3-8min, continues to keep the temperature 3-5min, except casting obtains the conjunction of composite ceramic particle reinforced aluminum after Slag treatment
Gold；
Wherein, TiCN, AlN and TiB in the composite ceramic particle reinforced aluminium alloy2The mass fraction of particle is 0.1-
The mass fraction of 0.52wt.%, SiC are 3-8wt.%；
Preferably, in step 1, the high temperature oxidation process of SiC powder carries out high-temperature oxydation to SiC using staged oxidation mode
Processing:
It is warming up to 573K with the rate of 20-100K/min, keeps the temperature 10-20min；
Continue to be warming up to 973K with the rate of 20-100K/min, keeps the temperature 5-10min；
It is heated to predetermined temperature 973-1373K, keeps the temperature 1-12h.
It preferably, further include that solution treatment, solid solubility temperature 803- are carried out to composite ceramic particle reinforced aluminium alloy
823K, solution time 6-15h carry out cold water quenching after solution treatment.
It preferably, further include that natural aging treatment, aging time are carried out in air to the aluminium alloy after solution treatment
For 6-15h.
It preferably, further include that artificial aging processing is carried out to the aluminium alloy after natural aging treatment, aging temp is
428-438K, aging time 6-15h.
Preferably, described except Slag treatment includes: that the slag-cleaning agent of 0.05-0.10wt.% is added to aluminium alloy in step 3
Carry out refining slagging-off, the ingredient and mass percent of the slag-cleaning agent are as follows: KCl:35wt.%；MgCl2: 30wt.%；AlF3:
5wt.%；Na3AlF6: 15wt.%；Mg3N2: 5wt.%；Na2CO3: 5wt.%；C2Cl6: 5wt.%.
Preferably, the pressure for preparing the cylindrical pottery aluminium composite green compact is 60-100MPa；Prepare the cylindrical pressure
The pressure of base is 60-100MPa.
Preferably, when the cylindrical green compact carries out vacuum-sintering, vacuum pressure is less than or equal to 10Pa.
Preferably, the partial size of the SiC powder is 5-20 μm, and the partial size of Al-Si-Mg alloyed powder is 15-40 μm, Al powder
Partial size be 13-48 μm, the partial size of Ti powder is 13-45 μm, and the partial size of BN powder is 0.5-1.3 μm, B4The partial size of C powder is 0.5-
6.5μm。
It is of the present invention the utility model has the advantages that
(1) present invention has designed and developed a kind of multiple dimensioned ceramic particle and mixes high elastic modulus high-strength aluminum alloy, leads to
Cross the TiCN particle of in-situ endogenic nano-scale, the TiB of submicron-scale2With AlN particle and additional micron SiC ceramic particle system
Standby high elastic modulus high-strength aluminum alloy, and optimize TiCN, AlN and TiB2The content of particle and SiC particulate, nano ceramics
Particle is stabilized in aluminum substrate, and interface cohesion is good, is uniformly dispersed, and each size granule is good in realization aluminum alloy materials
Distribution.
(2) present invention has designed and developed the preparation that a kind of multiple dimensioned ceramic particle mixes high elastic modulus high-strength aluminum alloy
Method, by Al powder, Ti powder and BN and B4The TiB of the TiCN particle of C powder sintering in-situ endogenic nano-scale, submicron-scale2With
AlN particle and micron SiC ceramic particle prepare high elastic modulus high-strength aluminum alloy, and optimize TiCN, AlN and TiB2
The content of particle and SiC particulate realizes that micro-nano granules are uniformly distributed in pottery aluminium composite material, cooperate micron-scale
SiC particulate realizes the synergistic effect of nano-sized ceramic particles and micron-sized ceramic particles in aluminum substrate, multiphase ceramic
Grain is stabilized in aluminum substrate, and interface cohesion is good, is uniformly dispersed, and realizes that the multiphase of particle in pottery aluminium composite material is multiple dimensioned
Interfacial reaction, particle ruler will not occur for distribution, and the multiple dimensioned particle stabilized presence of multiphase, interior raw ceramic particle and alloy matrix aluminum
It is very little to mix for nanometer, micron, the plasticity of composite material will not be reduced, there is important application value.Integrated operation is simple, saves
Cost has important economic benefit.
Detailed description of the invention
Fig. 1 is raw multiphase TiCN-AlN-TiB in the 20wt.% prepared in the embodiment of the present invention 12The X of/Al intermediate alloy
X ray diffration pattern x.
Fig. 2 is raw multiphase TiCN-AlN-TiB in the 20wt.% prepared in the embodiment of the present invention 12It is more in/Al intermediate alloy
Phase TiCN-AlN-TiB2Hybrid ceramic granule-morphology figure.
Fig. 3 is micron SiC granule-morphology figure used in the embodiment of the present invention 1.
Fig. 4 is raw multiphase TiCN-AlN-TiB in the 30wt.% prepared in the embodiment of the present invention 22The X of/Al intermediate alloy
X ray diffration pattern x.
Fig. 5 is raw multiphase TiCN-AlN-TiB in the 30wt.% prepared in the embodiment of the present invention 22It is more in/Al intermediate alloy
Phase TiCN-AlN-TiB2Hybrid ceramic granule-morphology figure.
Fig. 6 is micron SiC granule-morphology figure used in the embodiment of the present invention 2.
Fig. 7 is raw multiphase TiCN-AlN-TiB in the 40wt.% prepared in the embodiment of the present invention 32The X of/Al intermediate alloy
X ray diffration pattern x.
Fig. 8 is raw multiphase TiCN-AlN-TiB in the 40wt.% prepared in the embodiment of the present invention 32It is more in/Al intermediate alloy
Phase TiCN-AlN-TiB2Hybrid ceramic granule-morphology figure.
Fig. 9 is micron SiC granule-morphology figure used in the embodiment of the present invention 3.
Specific embodiment
Present invention will be described in further detail below with reference to the accompanying drawings, to enable those skilled in the art referring to specification text
Word can be implemented accordingly.
The present invention provides a kind of multiple dimensioned ceramic particle and mixes high elastic modulus high-strength aluminum alloy, the multiple dimensioned ceramics
The chemical composition and its mass percent of confusion high elastic modulus high-strength aluminum alloy are as follows: Si:6.5%-10wt.%；Mg:
0.3-0.7wt.%；SiC:2-8wt.%；TiCN, AlN and TiB2: 0.1-0.6wt.%；Surplus is Al.
The multiple dimensioned ceramic particle that the present invention designs and develops mixes high elastic modulus high-strength aluminum alloy, by original position
Give birth to the TiCN particle of nano-scale, the TiB of submicron-scale2High resiliency is prepared with AlN particle and additional micron SiC ceramic particle
Modulus high strength aluminium alloy, and optimize TiCN, AlN and TiB2The content of particle and SiC particulate, nano-ceramic particle is in aluminium
It is stabilized in matrix, interface cohesion is good, is uniformly dispersed, and realizes the good distribution of each size granule in aluminum alloy materials.
The present invention also provides the preparation method that a kind of multiple dimensioned ceramic particle mixes high elastic modulus high-strength aluminum alloy, packets
Include following steps:
Step 1: the pretreatment of SiC ceramic particle
(1) surface of SiC oxidation processes:
I. by SiC powder be laid in diameter be 100mm, highly be 20mm high-purity corundum crucible on, thickness is about 0.3-
Then corundum crucible is put into high temperature box type resistance furnace and is calcined by 0.8mm.
High temperature oxidation process is carried out to SiC using staged oxidation mode, specific staged oxidation technique is as follows: being with rate
20-100K/min is warming up to 573K, keeps the temperature 10-20min, continues to be warming up to 973K with rate 20-100K/min, keeps the temperature 5-
10min is then heated to predetermined temperature 973K-1373K, keeps the temperature 1-12h.
(2) the pre-dispersed processing of ball milling:
I. take Al-Si-Mg that SiC powder, granularity that granularity is 5-20 μm are 15-40 μm (Si:6.5%-10wt.%,
Mg:0.3-0.7wt.%, surplus are aluminium) alloy powder matches according to SiC and Al-Si-Mg alloyed powder mass ratio 1:20-1:1.5
Mixed-powder is made；
Ii. prepared mixed powder is put into ball grinder.The ZrO of Φ 4.5- Φ 20mm is filled in tank2Ceramic Balls, ball
Material mass ratio is 10:1, and ball material total volume is the 2/3 of spherical tank volume, and revolving speed is 20-90rpm (positive and negative rotation alternately, when interval
Between 30min), Ball-milling Time 12-96h.
Filled in advance in the ball grinder filled in planetary ball mill diameter be respectively 5mm, 7mm, 11mm, 15mm, 20mm,
The ZrO of 22mm2Ball, 10 every kind, ZrO2The total 800g of ball quality.
(3) preparation containing SiC particulate green compact:
The powder of ball mill mixing is taken out, is wrapped with aluminium foil, the axis that diameter is Φ 30- Φ 45 is made in cold pressing on a hydraulic press
The cylindrical pottery aluminium composite green compact densified to pressure, pressure 60-100MPa；Consistency is 60-75%.
Step 2: Al-Ti-B4The preparation of ceramics particle strengthened dose of C-BN system in-situ endogenic, specific as follows:
(1)Al-Ti-B4The preparation of C-BN system reaction green compact:
I weighs the Al powder of about 13-48 μm of a certain amount of required granularity, the Ti powder that granularity is about 13-45 μm, granularity
0.5-6.5 μm of B4C powder, the BN powder that granularity is 0.5~1.3 μm are spare；
II is first by BN powder, B4C powder is put into ball grinder, wherein BN powder, B4The molar ratio of C powder is 1:1.With planetary ball
Powder is activated 1.5~3h with the speed high speed ball milling of 200~300r/min by grinding machine.
III is estimated in Al-Ti-B4C-BN system generates TiCN, TiB2, AlN particle total content be 20wt.%-
40wt.%, by Ti powder, B4The molar ratio of C powder and BN powder is the BN powder and B that 9:2.8:2.8 weighs Ti powder and mixes4C powder, it is remaining
Amount is Al powder.
Prepared powder and zirconium oxide balls are put into batch mixer, batch mixer mixes 8- with the speed of 30-60r/min
32h；Finally the powder of ball mill mixing is taken out, the mixed powder of ball milling is wrapped with aluminium foil, Φ is made in cold pressing on a hydraulic press
30 cylindrical green compacts, pressure 60-100MPa；High 35-45mm；Consistency is 60-75%.
(2) green compact is sintered reaction in-situ:
30 cylindrical green compact of Φ obtained is put into the cylindrical graphite mold with inner cavity by I, intracavity diameter Φ
32mm。
Graphite jig and 30 cylindrical green compact of Φ are put into vacuum thermal explosion furnace by II, close fire door, after be evacuated to furnace
Interior pressure is lower than 10Pa；
III is started to warm up with the speed of 25-60K/min；When temperature is increased to 773K, in order to make graphite jig temperature with
The lesser temperature difference is kept in furnace, keeps the temperature 15-25min.
IV is heated to 1173K-1193K to after observing that air pressure has apparent rise in furnace, keeps the temperature 10min, then
Stop heating.1073K is dropped to temperature, axial direction 25-55MPa pressure, pressure maintaining are applied to cylindrical green compact simultaneously in insulating process
Time 20-90s；The cylindrical green compact densified after reaction and through axial compressive force is cooled to room temperature in a vacuum with furnace.
Step 3: multiple dimensioned Particles dispersed strengthens Al-Si-Mg alloy:
(1) preparatory load weighted aluminium alloy is placed in crucible and is put into togerther crucible type melting resistance furnace with crucible
It is interior, it is warming up to 1073K；The ingredient of aluminium alloy are as follows: Si:6.5%-10wt.%, Mg:0.3-0.7wt.%, surplus are aluminium；
(2) it after alloy is completely melt and keeps the temperature 30min, slag-cleaning agent is added, refining slagging-off carried out to aluminium alloy, at slag hitting
10min is kept the temperature after reason.Al-Si-Mg alloy is not strengthened.
The ingredient and mass percent of the slag-cleaning agent are as follows: KCl:35wt.%；MgCl2: 30wt.%；AlF3: 5wt.%；
Na3AlF6: 15wt.%；Mg3N2: 5wt.%；Na2CO3: 5wt.%；C2Cl6: 5wt.%.
(3) adjustment furnace temperature is to 1073-1123K, hardening agent (the i.e. cylindrical shape containing multiphase ceramic particle that will be prepared
Green compact) it is added in crucible, so that TiCN, AlN and TiB in composite ceramic particle reinforced aluminium alloy2The mass fraction of particle is
0.1-0.52wt.%, immediately mechanical stirring melt 60-180s；
(4) hardening agent (i.e. cylindrical pottery aluminium composite green compact) containing micron SiC ceramic particle is added in crucible, is made
The mass fraction for obtaining SiC in composite ceramic particle reinforced aluminium alloy is 3-8wt.%, handles melt 120- using mechanical stirring
300s then keeps the temperature 3-5min；
(6) ultrasonic probe uses the aluminium alloy in crucible after alloy liquid level 60-120mm heat preservation 10-20min
It is ultrasonically treated 3-8min.After ultrasonic wave added disperses, ultrasonic device is removed, keeps the temperature 3-5min.
(7) the aluminium alloy slag-cleaning agent of 0.05~0.10wt.% of aluminium alloy addition after being ultrasonically treated, mechanical stirring 2min,
It carries out refinery by de-gassing, skim；Molten aluminum by finally removing Slag treatment can directly cast；
(8) by the molten metal after stir process be cast to metal type dies (45# steel, having a size of 200mm × 150mm ×
In 20mm), the plate tensile sample of composite ceramic particle reinforced aluminium alloy is obtained.
Step 4: the heat treatment of the Al-Si-Mg alloy after strengthening:
(1) aluminium alloy after reinforcing solution treatment: is subjected to solution treatment, solid solubility temperature 803- in high temperature oven
823K, solution time 6-15h carry out cold water quenching after solution treatment；
(2) natural aging treatment: natural aging treatment, aging time 6-15h are carried out in air；
(3) artificial aging is handled: the progress artificial aging processing in electric drying oven with forced convection, aging temp 428-438K,
Aging time is 6-15h.
Embodiment 1
This example preparation method the following steps are included:
Step 1: the pretreatment of SiC ceramic particle, specific as follows:
(1) surface of SiC oxidation processes:
I. by SiC powder be laid in diameter be 100mm, highly be 20mm high-purity corundum crucible on, thickness is about
Then corundum crucible is put into high temperature box type resistance furnace and is calcined by 0.3mm.
High temperature oxidation process is carried out to SiC using staged oxidation mode, specific staged oxidation technique is as follows: being with rate
20K/min is warming up to 573K, and 573K keeps the temperature 20min, continues to be that 30K/min is warming up to 973K with rate, keeps the temperature 10min, then
It is heated to predetermined temperature 973K, keeps the temperature 12h.
(2) the pre-dispersed processing of ball milling:
I. SiC powder that granularity is 6 μm is taken, (Si:7%, Mg:0.3wt.%, surplus are by Al-Si-Mg that granularity is 40 μm
Aluminium) alloy powder according to SiC and Al-Si-Mg alloyed powder mass ratio 1:2 is configured to mixed-powder；
Ii. prepared mixed powder is put into ball grinder.The ZrO of Φ 4.5mm is filled in tank2Ceramic Balls, ball material matter
Amount is than being 10:1, and ball material total volume is the 2/3 of spherical tank volume, and revolving speed is 20rpm (positive and negative rotation alternately, interval time
30min), Ball-milling Time 12h.
(3) preparation containing SiC particulate green compact:
The powder of ball mill mixing is taken out, is wrapped with aluminium foil, the axial pressure that diameter is Φ 30 is made in cold pressing on a hydraulic press
The cylindrical pottery aluminium composite green compact of power densification, pressure 60MPa；Consistency is 60%.
Step 2: Al-Ti-B4The preparation of ceramics particle strengthened dose of C-BN system in-situ endogenic, specific as follows:
(1)Al-Ti-B4The preparation of C-BN system reaction green compact:
It is 0.5 μm that I, which weighs the Al powder of about 13 μm of a certain amount of required granularity, the Ti powder that granularity is about 13 μm, granularity,
B4C powder, the BN powder that granularity is 0.5 μm are spare；
II is first by BN powder, B4C powder is put into ball grinder, wherein BN powder, B4The molar ratio of C powder is 1:1.With planetary ball
Powder is activated 1.5h with the speed high speed ball milling of 200r/min by grinding machine.
III is estimated in Al-Ti-B4C-BN system generates TiCN, TiB2, AlN particle total content be 20wt.%, by Ti
Powder, B4The molar ratio of C powder and BN powder is the BN powder and B that 9:2.8:2.8 weighs Ti powder and mixes4C powder, surplus are Al powder, are prepared
At 100g powder.Multiphase TiCN-AlN-TiB2The mass fraction of ceramics is 20wt.%: wherein Al-Ti-B4In C-BN system, Ti:
B4The molar ratio of C:BN is 9:2.8:2.8；Wherein Al powder: 80g, Ti powder: 13.16g, B4C powder: 4.72g, BN powder: 2.12g.
Prepared powder and zirconium oxide balls are put into batch mixer, batch mixer mixes 8h with the speed of 60r/min；Most
The powder of ball mill mixing is taken out afterwards, the mixed powder of ball milling is wrapped with aluminium foil, 30 cylinder of Φ is made in cold pressing on a hydraulic press
Shape green compact, pressure 100MPa；High 35mm；Consistency is 75%.
(2) green compact is sintered reaction in-situ:
30 cylindrical green compact of Φ obtained is put into the cylindrical graphite mold with inner cavity by I, intracavity diameter Φ
32mm。
Graphite jig and 30 cylindrical green compact of Φ are put into vacuum thermal explosion furnace by II, close fire door, after be evacuated to furnace
Interior pressure is lower than 10Pa；
III is started to warm up with the speed of 25K/min；When temperature is increased to 773K, in order to make graphite jig temperature and furnace
It is interior to keep the lesser temperature difference, keep the temperature 15min.
IV is heated to 1193K to after observing that air pressure has significantly rising in furnace, keeps the temperature 10min, then stops adding
Heat.1073K is dropped to temperature, axial direction 55MPa pressure, dwell time 20s are applied to cylindrical green compact simultaneously in insulating process；Instead
The cylindrical green compact densified after answering and through axial compressive force is cooled to room temperature in a vacuum with furnace.
Step 3: multiple dimensioned Particles dispersed strengthens Al-Si-Mg alloy:
(1) preparatory load weighted aluminium alloy is placed in crucible and is put into togerther crucible type melting resistance furnace with crucible
It is interior, it is warming up to 1073K；The ingredient of aluminium alloy are as follows: Si:7wt.%, Mg:0.3wt.%, surplus are aluminium；
(2) it after alloy is completely melt and keeps the temperature 30min, slag-cleaning agent is added, refining slagging-off carried out to aluminium alloy, at slag hitting
10min is kept the temperature after reason.Al-Si-Mg alloy is not strengthened.
(3) by adjustment furnace temperature to 1073K, hardening agent (the i.e. cylinder containing multiphase ceramic particle that step 2 is prepared
Shape green compact) it is added in crucible, so that TiCN, AlN and TiB in composite ceramic particle reinforced aluminium alloy2The mass fraction of particle
For 0.1wt.%, immediately mechanical stirring melt 60s；
(4) hardening agent (i.e. cylindrical pottery aluminium composite green compact) containing micron SiC ceramic particle is added in crucible, is made
The mass fraction for obtaining SiC in composite ceramic particle reinforced aluminium alloy is 3wt.%, handles melt 120s using mechanical stirring.Then
Keep the temperature 3min；
(6) ultrasonic probe uses at ultrasound the aluminium alloy in crucible after alloy liquid level 60mm heat preservation 10min
The reason processing time is 3min.After ultrasonic wave added disperses, ultrasonic device is removed, keeps the temperature 5min.
(7) the aluminium alloy slag-cleaning agent of 0.05wt.% is added in the aluminium alloy after being ultrasonically treated, and mechanical stirring 2min is removed
Gas refining is skimmed；Molten aluminum by finally removing Slag treatment can directly cast；
(8) molten metal after stir process is cast in metal type dies, obtains composite ceramic particle reinforced aluminium alloy
Plate tensile sample.
Step 4: the heat treatment of the Al-Si-Mg alloy after strengthening:
(1) solution treatment: carrying out solution treatment for the aluminium alloy after reinforcing in high temperature oven, solid solubility temperature 803K, Gu
The molten time is 15h, and cold water quenching is carried out after solution treatment；
(2) natural aging treatment: natural aging treatment, aging time 15h are carried out in air；
(3) artificial aging is handled: artificial aging processing, aging temp 438K, timeliness are carried out in electric drying oven with forced convection
Time is 6h.
0.1wt.% endogenetic particle (the TiB of the TiCN particle of nano-scale, submicron-scale2With AlN blend of granules)
The bullet of the compound hardening treatment Al-Si-Mg alloy of (as depicted in figs. 1 and 2) and 3wt.%SiC ceramic particle (as shown in Figure 3)
Property modulus, tensile strength and breaking strain are respectively as follows: 79.2GPa, 335MPa, 8.3%, than the Al-Si-Mg alloy that do not strengthen
The performance of (elasticity modulus: 70.5GPa, tensile strength: 282MPa, breaking strain are respectively as follows: 7.6%) is respectively increased
12.3%, 18.7%, 9.2%.Elasticity modulus and intensity improve significantly, and improve the plasticity of material.
Embodiment 2:
Step 1, the pretreatment of micron SiC ceramic particle are specific as follows:
(1) surface of SiC oxidation processes:
I. by SiC powder be laid in diameter be 100mm, highly be 20mm high-purity corundum crucible on, thickness is about
Then corundum crucible is put into high temperature box type resistance furnace and is calcined by 0.6mm.
High temperature oxidation process is carried out to SiC using staged oxidation mode, specific staged oxidation technique is as follows: being with rate
50K/min is warming up to 573K, and 573K keeps the temperature 15min, continues to be that 80K/min is warming up to 973K with rate, keeps the temperature 8min, then plus
Heat arrives predetermined temperature 1373K, keeps the temperature 2h.
(2) the pre-dispersed processing of ball milling:
I. the SiC powder that granularity is 10 μm, Al-Si-Mg (Si:8%, Mg:0.5wt.%, surplus that granularity is 15 μm are taken
For aluminium) alloy powder according to SiC and Al-Si-Mg alloyed powder mass ratio 1:3 is configured to mixed-powder；
Ii. prepared mixed powder is put into ball grinder.The ZrO of Φ 10mm is filled in tank2Ceramic Balls, ball material quality
Than for 10:1, ball material total volume is the 2/3 of spherical tank volume, revolving speed be 50rpm (positive and negative rotation alternately, interval time 30min),
Ball-milling Time 36h.
(3) preparation containing SiC particulate green compact:
The powder of ball mill mixing is taken out, is wrapped with aluminium foil, the axial pressure that diameter is Φ 45 is made in cold pressing on a hydraulic press
The cylindrical pottery aluminium composite green compact of power densification, pressure 100MPa；Consistency is 75%.
Step 2: Al-Ti-B4The preparation of ceramics particle strengthened dose of C-BN system in-situ endogenic, specific as follows:
(1)Al-Ti-B4The preparation of C-BN system reaction green compact:
It is 6.5 μm that I, which weighs the Al powder of about 48 μm of a certain amount of required granularity, the Ti powder that granularity is about 45 μm, granularity,
B4C powder, the BN powder that granularity is 1.3 μm are spare；
II is first by BN powder, B4C powder is put into ball grinder, wherein BN powder, B4The molar ratio of C powder is 1:1.With planetary ball
Powder is activated 2h with the speed high speed ball milling of 260r/min by grinding machine.
III is estimated in Al-Ti-B4C-BN system generates TiCN, TiB2, AlN particle total content be 30wt.%, by Ti
Powder, B4C powder, BN powder molar ratio are the BN powder and B that 9:2.8:2.8 weighs Ti powder and mixes4C powder, surplus are Al powder, are configured to
100g powder.Multiphase TiCN-AlN-TiB2The mass fraction of ceramics is 30wt.%, wherein Al-Ti-B4In C-BN system, Ti:
B4The molar ratio of C:BN is 9:2.8:2.8；Wherein Al powder: 70g, Ti powder: 19.73g, B4C powder: 7.09g, BN powder: 3.18g.
Prepared powder and zirconium oxide balls are put into batch mixer, batch mixer mixes 32h with the speed of 30r/min；
Finally the powder of ball mill mixing is taken out, the mixed powder of ball milling is wrapped with aluminium foil, the circle of Φ 30 is made in cold pressing on a hydraulic press
Cylindricality green compact, pressure 60MPa；High 45mm；Consistency is 60%.
(2) green compact is sintered reaction in-situ:
30 cylindrical green compact of Φ obtained is put into the cylindrical graphite mold with inner cavity by I, intracavity diameter Φ
32mm。
Graphite jig and 30 cylindrical green compact of Φ are put into vacuum thermal explosion furnace by II, close fire door, after be evacuated to furnace
Interior pressure is lower than 10Pa；
III is started to warm up with the speed of 60K/min；When temperature is increased to 773K, in order to make graphite jig temperature and furnace
It is interior to keep the lesser temperature difference, keep the temperature 25min.
IV is heated to 1173KK to after observing that air pressure has apparent rise in furnace, keeps the temperature 10min, then stops
Heating.1073K is dropped to temperature, axial direction 25MPa pressure, dwell time 90s are applied to cylindrical green compact simultaneously in insulating process；
The cylindrical green compact densified after reaction and through axial compressive force is cooled to room temperature in a vacuum with furnace.
Step 3: multiple dimensioned Particles dispersed strengthens Al-Si-Mg alloy:
(1) preparatory load weighted aluminium alloy is placed in crucible and is put into togerther crucible type melting resistance furnace with crucible
It is interior, it is warming up to 1073K；The ingredient of aluminium alloy are as follows: Si:8wt.%, Mg:0.5wt.%, surplus are aluminium；
(2) it after alloy is completely melt and keeps the temperature 30min, slag-cleaning agent is added, refining slagging-off carried out to aluminium alloy, at slag hitting
10min is kept the temperature after reason.Al-Si-Mg alloy is not strengthened.
(3) furnace temperature will be adjusted to 1123K, the hardening agent containing multiphase ceramic particle that step 2 is prepared is added to earthenware
In crucible, so that TiCN, AlN and TiB in composite ceramic particle reinforced aluminium alloy2The mass fraction of particle is 0.3wt.%, then
Mechanical stirring melt 120s immediately；
(4) hardening agent containing micron SiC ceramic particle is added in crucible, so that composite ceramic particle reinforced aluminum closes
The mass fraction of SiC is 5wt.% in gold, handles melt 300s using mechanical stirring.Then heat preservation 5min；
(6) ultrasonic probe uses at ultrasound the aluminium alloy in crucible after alloy liquid level 120mm heat preservation 20min
The reason processing time is 5min.After ultrasonic wave added disperses, ultrasonic device is removed, keeps the temperature 4min.
(7) the aluminium alloy slag-cleaning agent of 0.10wt.% is added in the aluminium alloy after being ultrasonically treated, and mechanical stirring 2min is removed
Gas refining is skimmed；Molten aluminum by finally removing Slag treatment can directly cast；
(8) molten metal after stir process is cast in metal type dies, obtains composite ceramic particle reinforced aluminium alloy
Plate tensile sample.
Step 4: the heat treatment of the Al-Si-Mg alloy after strengthening:
(1) solution treatment: carrying out solution treatment for the aluminium alloy after reinforcing in high temperature oven, solid solubility temperature 823K, Gu
The molten time is 6h, and cold water quenching is carried out after solution treatment；
(2) natural aging treatment: natural aging treatment, aging time 15h are carried out in air；
(3) artificial aging is handled: artificial aging processing, aging temp 428K, timeliness are carried out in electric drying oven with forced convection
Time is 15h.
It is raw in 0.3wt.% to mix the size granule (TiB of the TiCN particle of nano-scale, submicron-scale2With AlN particle
Mixture) (such as Fig. 4 and Fig. 5) and 5wt.%SiC ceramic particle (such as Fig. 6) compound hardening treatment Al-Si-Mg alloy elasticity
Modulus, tensile strength and breaking strain are respectively as follows: 85.3GPa, 379MPa, 7.9%, than the Al-Si-Mg alloy (bullet that do not strengthen
Property modulus: 70.5GPa, tensile strength: 282MPa, breaking strain be respectively as follows: performance 7.6%) be respectively increased 20.9%,
34.3%, 3.9%.Elasticity modulus and intensity improve significant.
Embodiment 3
The preparation method of this example the following steps are included:
Step 1: the pretreatment of SiC ceramic particle, specific as follows:
(1) surface of SiC oxidation processes:
I. by SiC powder be laid in diameter be 100mm, highly be 20mm high-purity corundum crucible on, thickness is about
Then corundum crucible is put into high temperature box type resistance furnace and is calcined by 0.8mm.
High temperature oxidation process is carried out to SiC using staged oxidation mode, specific staged oxidation technique is as follows: being with rate
90K/min is warming up to 573K, and 573K keeps the temperature 15min, continues to be that 70K/min is warming up to 973K with rate, keeps the temperature 10min, then
It is heated to predetermined temperature 1273K, keeps the temperature 5h.
(2) the pre-dispersed processing of ball milling:
I. take SiC powder that granularity is 10 μm, Al-Si-Mg that granularity is 25 μm (Si:9.5wt.%, Mg:0.7wt.%,
Surplus is aluminium) alloy powder according to SiC and Al-Si-Mg alloyed powder mass ratio 1:4 is configured to mixed-powder；
Ii. prepared mixed powder is put into ball grinder.The ZrO of Φ 20mm is filled in tank2Ceramic Balls, ball material quality
Than for 10:1, ball material total volume is the 2/3 of spherical tank volume, revolving speed be 80rpm (positive and negative rotation alternately, interval time 30min),
Ball-milling Time 96h.
(3) preparation containing SiC particulate green compact:
The powder of ball mill mixing is taken out, is wrapped with aluminium foil, the axial pressure that diameter is Φ 38 is made in cold pressing on a hydraulic press
The cylindrical pottery aluminium composite green compact of power densification, pressure 80MPa；Consistency is 68%.
Step 2: Al-Ti-B4The preparation of ceramics particle strengthened dose of C-BN system in-situ endogenic, specific as follows:
(1)Al-Ti-B4The preparation of C-BN system reaction green compact:
I weighs the Al powder of about 25 μm of a certain amount of required granularity, the Ti powder that granularity is about 25 μm, the B that granularity is 3 μm4C
Powder, the BN powder that granularity is 1 μm are spare；
II is first by BN powder, B4C powder is put into ball grinder, wherein BN powder, B4The molar ratio of C powder is 1:1.With planetary ball
Powder is activated 3h with the speed high speed ball milling of 300r/min by grinding machine.
III is estimated in Al-Ti-B4C-BN system generates TiCN, TiB2, AlN particle total content be 40wt.%, by Ti
Powder, B4C powder, BN powder molar ratio are the BN powder and B that 9:2.8:2.8 weighs Ti powder and mixes4C powder, surplus are Al powder, are configured to
100g powder.Multiphase TiCN-AlN-TiB2The mass fraction of ceramics is 40wt.%, wherein Al-Ti-B4In C-BN system, Ti:
B4The molar ratio of C:BN is 9:2.8:2.8；Wherein Al powder: 60g, Ti powder: 26.31g, B4C powder: 9.45g, BN powder: 4.24g.
Prepared powder and zirconium oxide balls are put into batch mixer, batch mixer mixes 20h with the speed of 40r/min；
Finally the powder of ball mill mixing is taken out, the mixed powder of ball milling is wrapped with aluminium foil, the circle of Φ 30 is made in cold pressing on a hydraulic press
Cylindricality green compact, pressure 80MPa；High 40mm；Consistency is 68%.
(2) green compact is sintered reaction in-situ:
30 cylindrical green compact of Φ obtained is put into the cylindrical graphite mold with inner cavity by I, intracavity diameter Φ
32mm。
Graphite jig and 30 cylindrical green compact of Φ are put into vacuum thermal explosion furnace by II, close fire door, after be evacuated to furnace
Interior pressure is lower than 10Pa；
III is started to warm up with the speed of 50K/min；When temperature is increased to 773K, in order to make graphite jig temperature and furnace
It is interior to keep the lesser temperature difference, keep the temperature 20min.
IV is heated to 1183K to after observing that air pressure has significantly rising in furnace, keeps the temperature 10min, then stops adding
Heat.1073K is dropped to temperature, axial direction 40MPa pressure, dwell time 60s are applied to cylindrical green compact simultaneously in insulating process；Instead
The cylindrical green compact densified after answering and through axial compressive force is cooled to room temperature in a vacuum with furnace.
Step 3: multiple dimensioned Particles dispersed strengthens Al-Si-Mg alloy:
(1) preparatory load weighted aluminium alloy is placed in crucible and is put into togerther crucible type melting resistance furnace with crucible
It is interior, it is warming up to 1073K；The ingredient of aluminium alloy are as follows: Si:9.5%, Mg:0.7wt.%, surplus are aluminium；
(2) it after alloy is completely melt and keeps the temperature 30min, slag-cleaning agent is added, refining slagging-off carried out to aluminium alloy, at slag hitting
10min is kept the temperature after reason.Al-Si-Mg alloy is not strengthened.
(3) furnace temperature will be adjusted to 11103K, the hardening agent containing multiphase ceramic particle that step 2 is prepared is added to
In crucible, so that TiCN, AlN and TiB in composite ceramic particle reinforced aluminium alloy2The mass fraction of particle is 0.52wt.%, with
Mechanical stirring melt 180s immediately afterwards；
(4) hardening agent containing micron SiC ceramic particle is added in crucible, so that composite ceramic particle reinforced aluminum closes
The mass fraction of SiC is 8wt.% in gold, handles melt 300s using mechanical stirring.Then heat preservation 5min；
(6) ultrasonic probe uses at ultrasound the aluminium alloy in crucible after alloy liquid level 100mm heat preservation 15min
The reason processing time is 8min.After ultrasonic wave added disperses, ultrasonic device is removed, keeps the temperature 5min.
(7) the aluminium alloy slag-cleaning agent of 0.06wt.% is added in the aluminium alloy after being ultrasonically treated, and mechanical stirring 2min is removed
Gas refining is skimmed；Molten aluminum by finally removing Slag treatment can directly cast；
(8) molten metal after stir process is cast in metal type dies, obtains composite ceramic particle reinforced aluminium alloy
Plate tensile sample.
Step 4: the heat treatment of the Al-Si-Mg alloy after strengthening:
(1) solution treatment: carrying out solution treatment for the aluminium alloy after reinforcing in high temperature oven, solid solubility temperature 813K, Gu
The molten time is 10h, and cold water quenching is carried out after solution treatment；
(2) natural aging treatment: natural aging treatment, aging time 12h are carried out in air；
(3) artificial aging is handled: artificial aging processing, aging temp 433K, timeliness are carried out in electric drying oven with forced convection
Time is 11h.
It is raw in 0.52wt.% to mix the size granule (TiB of the TiCN particle of nano-scale, submicron-scale2With AlN
Grain mixture) (as shown in Figure 7 and Figure 8) and 8wt.%SiC ceramic particle (as shown in Figure 9) compound hardening treatment Al-Si-Mg
Elasticity modulus, tensile strength and the breaking strain of alloy are respectively as follows: 94.9GPa, 416MPa, 7.6%, than the Al-Si- not strengthened
The performance of Mg alloy (elasticity modulus: 70.5GPa, tensile strength: 282MPa, breaking strain are respectively as follows: 7.6%) is respectively increased
34.6%, 47.5%, 0%.Elasticity modulus and intensity improve significant.
Comparative example 1
The TiCN particle of nano-scale, the TiB of submicron-scale is not added in this comparative example2With AlN particle and micron SiC
When ceramic particle, matrix hypoeutectic al-si alloy AlSi8Mg0.5The preparation process of alloy, specific as follows:
(1) preparatory load weighted aluminium alloy is placed in crucible and is put into togerther crucible type melting resistance furnace with crucible
It is interior, it is warming up to 1073K；The ingredient of Al-Si-Mg alloy is Si:8wt.%, Mg:0.5wt.%, and surplus is aluminium；
(2) after alloy is completely melt and 30min is kept the temperature, the slag-cleaning agent that 0.05wt.% is added refines aluminium alloy
Slagging-off keeps the temperature 10min after slag hitting processing.Do not strengthened Al-Si-Mg alloy, carries out refinery by de-gassing, skims；By finally removing
The molten aluminum of Slag treatment directly carries out being cast in metal type dies into plate aluminium alloy slab, plate slab with a thickness of 20mm；
(3) solution treatment: aluminium alloy is subjected to solution treatment, solid solubility temperature 813K in high temperature oven, solution time is
6h carries out cold water quenching after solution treatment；
(4) natural aging treatment: natural aging treatment, aging time 8h are carried out in air；
(5) artificial aging is handled: artificial aging processing, aging temp 438K, timeliness are carried out in electric drying oven with forced convection
Time is 10h.
What is prepared in this comparative example a nanometer TiB is not added2The matrix hypoeutectic aluminium silicon of particle and micron SiC ceramic particle closes
Golden AlSi8Mg0.5Elasticity modulus, tensile strength and the breaking strain of alloy are respectively as follows: 70.5GPa, 282MPa, 7.6%.
Comparative example 2
This comparative example (interior raw nanometer TiB of a small amount of addition of comparison2Aluminium alloy in the case where particle and micron SiC ceramic particle
Strengthening effect) preparation method the following steps are included:
Step 1: the pretreatment of SiC ceramic particle, specific as follows:
(1) surface of SiC oxidation processes:
I. by SiC powder be laid in diameter be 100mm, highly be 20mm high-purity corundum crucible on, thickness is about
Then corundum crucible is put into high temperature box type resistance furnace and is calcined by 0.3mm.
High temperature oxidation process is carried out to SiC using staged oxidation mode, specific staged oxidation technique is as follows: being with rate
20K/min is warming up to 573K, and 573K keeps the temperature 20min, continues to be that 30K/min is warming up to 973K with rate, keeps the temperature 10min, then
It is heated to predetermined temperature 973K, keeps the temperature 12h.
(2) the pre-dispersed processing of ball milling:
I. SiC powder that granularity is 6 μm is taken, (Si:7%, Mg:0.3wt.%, surplus are by Al-Si-Mg that granularity is 40 μm
Aluminium) alloy powder according to SiC and Al-Si-Mg alloyed powder mass ratio 1:2 is configured to mixed-powder；
Ii. prepared mixed powder is put into ball grinder.The ZrO of Φ 4.5mm is filled in tank2Ceramic Balls, ball material matter
Amount is than being 10:1, and ball material total volume is the 2/3 of spherical tank volume, and revolving speed is 20rpm (positive and negative rotation alternately, interval time
30min), Ball-milling Time 12h.
(3) preparation containing SiC particulate green compact:
The powder of ball mill mixing is taken out, is wrapped with aluminium foil, the axial pressure that diameter is Φ 30 is made in cold pressing on a hydraulic press
The cylindrical pottery aluminium composite green compact of power densification, pressure 60MPa；Consistency is 60%.
Step 2: Al-Ti-B4The preparation of ceramics particle strengthened dose of C-BN system in-situ endogenic, specific as follows:
(1)Al-Ti-B4The preparation of C-BN system reaction green compact:
It is 0.5 μm that I, which weighs the Al powder of about 13 μm of a certain amount of required granularity, the Ti powder that granularity is about 13 μm, granularity,
B4C powder, the BN powder that granularity is 0.5 μm are spare；
II is first by BN powder, B4C powder is put into ball grinder, wherein BN powder, B4The molar ratio of C powder is 1:1.With planetary ball
Powder is activated 1.5h with the speed high speed ball milling of 200r/min by grinding machine.
III is estimated in Al-Ti-B4C-BN system generates TiCN, TiB2, AlN particle total content be 20wt.%, by Ti
Powder, B4C powder, BN powder molar ratio are the BN powder and B that 9:2.8:2.8 weighs Ti powder and mixes4C powder, surplus are Al powder, are configured to
100g powder.Multiphase TiCN-AlN-TiB2The mass fraction of ceramics is 20wt.%: wherein Al-Ti-B4In C-BN system, Ti:
B4The molar ratio of C:BN is 9:2.8:2.8；Wherein Al powder: 80g, Ti powder: 13.16g, B4C powder: 4.72g, BN powder: 2.12g.
Prepared powder and zirconium oxide balls are put into batch mixer, batch mixer mixes 8h with the speed of 60r/min；Most
The powder of ball mill mixing is taken out afterwards, the mixed powder of ball milling is wrapped with aluminium foil, 30 cylinder of Φ is made in cold pressing on a hydraulic press
Shape green compact, pressure 100MPa；High 35mm；Consistency is 75%.
(2) green compact is sintered reaction in-situ:
30 cylindrical green compact of Φ obtained is put into the cylindrical graphite mold with inner cavity by I, intracavity diameter Φ
32mm。
Graphite jig and 30 cylindrical green compact of Φ are put into vacuum thermal explosion furnace by II, close fire door, after be evacuated to furnace
Interior pressure is lower than 10Pa；
III is started to warm up with the speed of 25K/min；When temperature is increased to 773K, in order to make graphite jig temperature and furnace
It is interior to keep the lesser temperature difference, keep the temperature 15min.
IV is heated to 1193K to after observing that air pressure has significantly rising in furnace, keeps the temperature 10min, then stops adding
Heat.1073K is dropped to temperature, axial direction 55MPa pressure, dwell time 20s are applied to cylindrical green compact simultaneously in insulating process；Instead
The cylindrical green compact densified after answering and through axial compressive force is cooled to room temperature in a vacuum with furnace.
Step 3: multiple dimensioned Particles dispersed strengthens Al-Si-Mg alloy:
(1) preparatory load weighted aluminium alloy is placed in crucible and is put into togerther crucible type melting resistance furnace with crucible
It is interior, it is warming up to 1073K；The ingredient of aluminium alloy are as follows: Si:7wt.%, Mg:0.3wt.%, surplus are aluminium；
(2) it after alloy is completely melt and keeps the temperature 30min, slag-cleaning agent is added, refining slagging-off carried out to aluminium alloy, at slag hitting
10min is kept the temperature after reason.Al-Si-Mg alloy is not strengthened.
(3) furnace temperature will be adjusted to 1073K, the hardening agent containing multiphase ceramic particle that step 2 is prepared is added to earthenware
In crucible, so that TiCN, AlN and TiB in composite ceramic particle reinforced aluminium alloy2The mass fraction of particle is 0.05wt.%, then
Mechanical stirring melt 60s immediately；
(4) hardening agent containing micron SiC ceramic particle is added in crucible, so that composite ceramic particle reinforced aluminum closes
The mass fraction of SiC is 1.5wt.% in gold, handles melt 120s using mechanical stirring.Then heat preservation 3min；
(6) ultrasonic probe uses at ultrasound the aluminium alloy in crucible after alloy liquid level 60mm heat preservation 10min
The reason processing time is 3min.After ultrasonic wave added disperses, ultrasonic device is removed, keeps the temperature 5min.
(7) the aluminium alloy slag-cleaning agent of 0.05wt.% is added in the aluminium alloy after being ultrasonically treated, and mechanical stirring 2min is removed
Gas refining is skimmed；Molten aluminum by finally removing Slag treatment can directly cast；
(8) molten metal after stir process is cast in metal type dies, obtains composite ceramic particle reinforced aluminium alloy
Plate tensile sample.
Step 4: the heat treatment of the Al-Si-Mg alloy after strengthening:
(1) solution treatment: carrying out solution treatment for the aluminium alloy after reinforcing in high temperature oven, solid solubility temperature 803K, Gu
The molten time is 15h, and cold water quenching is carried out after solution treatment；
(2) natural aging treatment: natural aging treatment, aging time 15h are carried out in air；
(3) artificial aging is handled: artificial aging processing, aging temp 438K, timeliness are carried out in electric drying oven with forced convection
Time is 6h.
0.05wt.% endogenetic particle (the TiB of the TiCN particle of nano-scale, submicron-scale2With AlN blend of granules)
With elasticity modulus, tensile strength and the breaking strain of the compound hardening treatment Al-Si-Mg alloy of 1.5wt.%SiC ceramic particle
Be respectively as follows: 75.4GPa, 305MPa, 7.7%, than do not strengthen Al-Si-Mg alloy (elasticity modulus: 70.5GPa, tensile strength:
282MPa, breaking strain are respectively as follows: performance 7.6%) and have been respectively increased 6.9%, 8.1%, 1.3%.Elasticity modulus, intensity,
Breaking strain does not all significantly improve, it is clear that the addition of a small amount of ceramic particle is not enough to significantly improve the performance of aluminium alloy.
Comparative example 3
This comparative example (interior raw nanometer TiB of a large amount of additions of comparison2Aluminium alloy in the case where particle and micron SiC ceramic particle
Strengthening effect) preparation method the following steps are included:
Step 1: the pretreatment of SiC ceramic particle, specific as follows:
(1) surface of SiC oxidation processes:
I. by SiC powder be laid in diameter be 100mm, highly be 20mm high-purity corundum crucible on, thickness is about
Then corundum crucible is put into high temperature box type resistance furnace and is calcined by 0.8mm.
High temperature oxidation process is carried out to SiC using staged oxidation mode, specific staged oxidation technique is as follows: being with rate
90K/min is warming up to 573K, and 573K keeps the temperature 15min, continues to be that 70K/min is warming up to 973K with rate, keeps the temperature 10min, then
It is heated to predetermined temperature 1273K, keeps the temperature 5h.
(2) the pre-dispersed processing of ball milling:
I. take SiC powder that granularity is 10 μm, Al-Si-Mg that granularity is 25 μm (Si:9.5wt.%, Mg:0.7wt.%,
Surplus is aluminium) alloy powder according to SiC and Al-Si-Mg alloyed powder mass ratio 1:4 is configured to mixed-powder；
Ii. prepared mixed powder is put into ball grinder.The ZrO of Φ 20mm is filled in tank2Ceramic Balls, ball material quality
Than for 10:1, ball material total volume is the 2/3 of spherical tank volume, revolving speed be 80rpm (positive and negative rotation alternately, interval time 30min),
Ball-milling Time 96h.
(3) preparation containing SiC particulate green compact:
The powder of ball mill mixing is taken out, is wrapped with aluminium foil, the axial pressure that diameter is Φ 38 is made in cold pressing on a hydraulic press
The cylindrical pottery aluminium composite green compact of power densification, pressure 80MPa；Consistency is 68%.
Step 2: Al-Ti-B4The preparation of ceramics particle strengthened dose of C-BN system in-situ endogenic, specific as follows:
(1)Al-Ti-B4The preparation of C-BN system reaction green compact:
I weighs the Al powder of about 25 μm of a certain amount of required granularity, the Ti powder that granularity is about 25 μm, the B that granularity is 3 μm4C
Powder, the BN powder that granularity is 1 μm are spare；
II is first by BN powder, B4C powder is put into ball grinder, wherein BN powder, B4The molar ratio of C powder is 1:1.With planetary ball
Powder is activated 3h with the speed high speed ball milling of 300r/min by grinding machine.
III is estimated in Al-Ti-B4C-BN system generates TiCN, TiB2, AlN particle total content be 40wt.%, by Ti
Powder, B4C powder, BN powder molar ratio are the BN powder and B that 9:2.8:2.8 weighs Ti powder and mixes4C powder, surplus are Al powder, are configured to
100g powder.Multiphase TiCN-AlN-TiB2The mass fraction of ceramics is 40wt.%, wherein Al-Ti-B4In C-BN system, Ti:
B4The molar ratio of C:BN is 9:2.8:2.8；Wherein Al powder: 60g, Ti powder: 26.31g, B4C powder: 9.45g, BN powder: 4.24g.
Prepared powder and zirconium oxide balls are put into batch mixer, batch mixer mixes 20h with the speed of 40r/min；
Finally the powder of ball mill mixing is taken out, the mixed powder of ball milling is wrapped with aluminium foil, the circle of Φ 30 is made in cold pressing on a hydraulic press
Cylindricality green compact, pressure 80MPa；High 40mm；Consistency is 68%.
(2) green compact is sintered reaction in-situ:
30 cylindrical green compact of Φ obtained in step 2 (1) is put into the cylindrical graphite mold with inner cavity by I,
Intracavity diameter is Φ 32mm.
Graphite jig and 30 cylindrical green compact of Φ are put into vacuum thermal explosion furnace by II, close fire door, after be evacuated to furnace
Interior pressure is lower than 10Pa；
III is started to warm up with the speed of 50K/min；When temperature is increased to 773K, in order to make graphite jig temperature and furnace
It is interior to keep the lesser temperature difference, keep the temperature 20min.
IV is heated to 1183K to after observing that air pressure has significantly rising in furnace, keeps the temperature 10min, then stops adding
Heat.1073K is dropped to temperature, axial direction 40MPa pressure, dwell time 60s are applied to cylindrical green compact simultaneously in insulating process；Instead
The cylindrical green compact densified after answering and through axial compressive force is cooled to room temperature in a vacuum with furnace.
Step 3: multiple dimensioned Particles dispersed strengthens Al-Si-Mg alloy:
(1) preparatory load weighted aluminium alloy is placed in crucible and is put into togerther crucible type melting resistance furnace with crucible
It is interior, it is warming up to 1073K；The ingredient of aluminium alloy are as follows: Si:9.5%, Mg:0.7wt.%, surplus are aluminium；
(2) it after alloy is completely melt and keeps the temperature 30min, slag-cleaning agent is added, refining slagging-off carried out to aluminium alloy, at slag hitting
10min is kept the temperature after reason.Al-Si-Mg alloy is not strengthened.
(3) furnace temperature will be adjusted to 11103K, the hardening agent containing multiphase ceramic particle that step 2 is prepared is added to
In crucible, so that TiCN, AlN and TiB in composite ceramic particle reinforced aluminium alloy2The mass fraction of particle is 0.7wt.%, with
Mechanical stirring melt 180s immediately afterwards；
(4) hardening agent containing micron SiC ceramic particle is added in crucible, so that composite ceramic particle reinforced aluminum closes
The mass fraction of SiC is 8.5wt.% in gold, handles melt 300s using mechanical stirring.Then heat preservation 5min；
(6) ultrasonic probe uses at ultrasound the aluminium alloy in crucible after alloy liquid level 100mm heat preservation 15min
The reason processing time is 8min.After ultrasonic wave added disperses, ultrasonic device is removed, keeps the temperature 5min.
(7) the aluminium alloy slag-cleaning agent of 0.06wt.% is added in the aluminium alloy after being ultrasonically treated, and mechanical stirring 2min is removed
Gas refining is skimmed；Molten aluminum by finally removing Slag treatment can directly cast；
(8) molten metal after stir process is cast in metal type dies, obtains composite ceramic particle reinforced aluminium alloy
Plate tensile sample.
Step 4: the heat treatment of the Al-Si-Mg alloy after strengthening:
(1) solution treatment: carrying out solution treatment for the aluminium alloy after reinforcing in high temperature oven, solid solubility temperature 813K, Gu
The molten time is 10h, and cold water quenching is carried out after solution treatment；
(2) natural aging treatment: natural aging treatment, aging time 12h are carried out in air；
(3) artificial aging is handled: artificial aging processing, aging temp 433K, timeliness are carried out in electric drying oven with forced convection
Time is 11h.
0.7wt.% endogenetic particle (the TiB of the TiCN particle of nano-scale, submicron-scale2With AlN blend of granules)
With elasticity modulus, tensile strength and the breaking strain of the compound hardening treatment Al-Si-Mg alloy of 8.5wt.%SiC ceramic particle
Be respectively as follows: 97.6GPa, 385MPa, 2.7%, than do not strengthen Al-Si-Mg alloy (elasticity modulus: 70.5GPa, tensile strength:
282MPa, breaking strain are respectively as follows: performance 7.6%) and 38.4%, 36.5%, -64.4% have been respectively increased.Although springform
Amount and intensity improve, but intensity mixes size granule (the TiCN particle of nano-scale, sub-micron not as good as life in 0.52wt.%
The TiB of size2With AlN blend of granules) and 8.5wt.%SiC ceramic particle compound hardening treatment Al-Si-Mg alloy it is strong
Degree, and breaking strain is greatly reduced.
The mechanical experimental results of embodiment 1-3 and comparative example 1-3 are as shown in table 1.
The mechanical experimental results of table 1 embodiment 1-3 and comparative example 1-3
The multiple dimensioned ceramic particle that the present invention designs and develops mixes the preparation method of high elastic modulus high-strength aluminum alloy, will
Al powder, Ti powder and BN and B4The TiB of the TiCN particle of C powder sintering in-situ endogenic nano-scale, submicron-scale2With AlN particle
And micron SiC ceramic particle prepares high elastic modulus high-strength aluminum alloy, and optimizes TiCN, AlN and TiB2Particle with
And the content of SiC particulate, realize that micro-nano granules are uniformly distributed in pottery aluminium composite material, cooperate the SiC particulate of micron-scale,
Realize the synergistic effect of nano-sized ceramic particles and micron-sized ceramic particles in aluminum substrate, multiphase ceramic particle is in aluminium base
It being stabilized in vivo, interface cohesion is good, is uniformly dispersed, realize the multiple dimensioned distribution of multiphase of particle in pottery aluminium composite material, and
Interfacial reaction will not occur for the multiple dimensioned particle stabilized presence of multiphase, interior raw ceramic particle and alloy matrix aluminum, and particle size is to receive
Rice, micron mix, and will not reduce the plasticity of composite material, have important application value.Integrated operation is simple, save the cost,
With important economic benefit.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and legend shown and described herein.
Claims (10)
1. a kind of multiple dimensioned ceramic particle mixes high elastic modulus high-strength aluminum alloy, which is characterized in that the multiple dimensioned ceramics
The chemical composition and its mass percent of confusion high elastic modulus high-strength aluminum alloy are as follows: Si:6.5%-10wt.%；Mg:
0.3-0.7wt.%；SiC:2-8wt.%；TiCN, AlN and TiB2: 0.1-0.6wt.%；Surplus is Al.
2. the preparation method that a kind of multiple dimensioned ceramic particle mixes high elastic modulus high-strength aluminum alloy, which is characterized in that including
Following steps:
Step 1: by the SiC powder of high temperature oxidation process and Al-Si-Mg alloyed powder ball milling mixing, wrapping up aluminium foil and cylindrical pottery is made
Aluminium composite green compact；
Wherein, the mass ratio of the SiC powder and Al-Si-Mg alloyed powder is 1:20-1:1.5, the cylindrical pottery aluminium composite green compact
Consistency be 60-75%；
Step 2: by Al powder, Ti powder, BN powder and B4C powder ball milling mixing, cylindrical green compact is made in package aluminium foil, and carries out vacuum burning
Knot, specifically includes:
It is warming up to 773K with the rate of 25-60K/min, keeps the temperature 15-25min；
It is continuously heating to 1173-1193K, keeps the temperature 10min, 1073K is cooled to, the cylindrical green compact is applied in insulating process
The pressure of axial 25-55MPa, pressure maintaining 20-90s, vacuum cooled to room temperature；
Wherein, the consistency of the cylindrical green compact is 60-75%, the BN powder and B4The molar ratio of C powder is 1:1, the Ti
Powder, B4The molar ratio of C powder and BN powder is 9:2.8:2.8, TiCN, AlN and TiB in the cylindrical green compact after vacuum-sintering2Particle
Mass fraction be 20-40wt.%；
Step 3: by Al-Si-Mg alloy, molten refined obtains Al-Si-Mg aluminium alloy at 1073-1123K；
The cylindrical green compact is placed in Al-Si-Mg aluminium alloy, mechanical stirring 60-180s；
The cylindrical pottery aluminium composite green compact is placed in Al-Si-Mg aluminium alloy again, mechanical stirring 120-300s keeps the temperature 3-
After 5min, it is ultrasonically treated 3-8min, continues to keep the temperature 3-5min, except casting obtains the conjunction of composite ceramic particle reinforced aluminum after Slag treatment
Gold；
Wherein, TiCN, AlN and TiB in the composite ceramic particle reinforced aluminium alloy2The mass fraction of particle is 0.1-
The mass fraction of 0.52wt.%, SiC are 3-8wt.%.
3. multiple dimensioned ceramic particle as claimed in claim 2 mixes the preparation method of high elastic modulus high-strength aluminum alloy,
It is characterized in that, in step 1, the high temperature oxidation process of SiC powder carries out high temperature oxidation process to SiC using staged oxidation mode:
It is warming up to 573K with the rate of 20-100K/min, keeps the temperature 10-20min；
Continue to be warming up to 973K with the rate of 20-100K/min, keeps the temperature 5-10min；
It is heated to predetermined temperature 973-1373K, keeps the temperature 1-12h.
4. multiple dimensioned ceramic particle as claimed in claim 2 or claim 3 mixes the preparation method of high elastic modulus high-strength aluminum alloy,
It is characterized in that, further including carrying out solution treatment, solid solubility temperature 803-823K, solid solution to composite ceramic particle reinforced aluminium alloy
Time is 6-15h, and cold water quenching is carried out after solution treatment.
5. multiple dimensioned ceramic particle as claimed in claim 4 mixes the preparation method of high elastic modulus high-strength aluminum alloy,
It is characterized in that, further includes carrying out natural aging treatment, aging time 6-15h in air to the aluminium alloy after solution treatment.
6. multiple dimensioned ceramic particle as claimed in claim 5 mixes the preparation method of high elastic modulus high-strength aluminum alloy,
It is characterized in that, further includes carrying out artificial aging processing to the aluminium alloy after natural aging treatment, aging temp 428-438K, when
The effect time is 6-15h.
7. multiple dimensioned ceramic particle as claimed in claim 2 or claim 3 mixes the preparation method of high elastic modulus high-strength aluminum alloy,
It is characterized in that, in step 3, it is described except Slag treatment includes: that the slag-cleaning agent of 0.05-0.10wt.% is added to aluminium alloy progress essence
Refining slagging-off, the ingredient and mass percent of the slag-cleaning agent are as follows: KCl:35wt.%；MgCl2: 30wt.%；AlF3: 5wt.%；
Na3AlF6: 15wt.%；Mg3N2: 5wt.%；Na2CO3: 5wt.%；C2Cl6: 5wt.%.
8. multiple dimensioned ceramic particle as claimed in claim 7 mixes the preparation method of high elastic modulus high-strength aluminum alloy,
It is characterized in that, the pressure for preparing the cylindrical pottery aluminium composite green compact is 60-100MPa；Prepare the pressure of the cylindrical green compact
For 60-100MPa.
9. the preparation that the multiple dimensioned ceramic particle as described in claim 2,3,5 or 6 mixes high elastic modulus high-strength aluminum alloy
Method, which is characterized in that when the cylindrical green compact carries out vacuum-sintering, vacuum pressure is less than or equal to 10Pa.
10. multiple dimensioned ceramic particle as claimed in claim 9 mixes the preparation method of high elastic modulus high-strength aluminum alloy,
It is characterized in that, the partial size of the SiC powder is 5-20 μm, and the partial size of Al-Si-Mg alloyed powder is 15-40 μm, and the partial size of Al powder is
13-48 μm, the partial size of Ti powder is 13-45 μm, and the partial size of BN powder is 0.5-1.3 μm, B4The partial size of C powder is 0.5-6.5 μm.
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