CN107012354B - A kind of preparation method of Al-Si9Cu1 particulate reinforced composite - Google Patents
A kind of preparation method of Al-Si9Cu1 particulate reinforced composite Download PDFInfo
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- CN107012354B CN107012354B CN201710216302.6A CN201710216302A CN107012354B CN 107012354 B CN107012354 B CN 107012354B CN 201710216302 A CN201710216302 A CN 201710216302A CN 107012354 B CN107012354 B CN 107012354B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
- 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
- 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
- C22C32/0073—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 only borides
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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
Abstract
The present invention relates to the preparation technical field of particle enhanced aluminum-based composite material, refers in particular to a kind of original position (TiB2+ZrB2) particle REINFORCED Al-Si-Cu based composites preparation method.The present invention is a certain proportion of Al18Si, pure Al, Al50Cu alloy, which is put into certain temperature graphite crucible, to be melted, and a certain proportion of potassium fluotitanate, potassium fluorozirconate and borax mixed-powder is added at a certain temperature later, after powder is added completely into, it opens mechanical stirring and magnetic stirrer carries out the stirring of certain time, after stirring, the temperature in furnace is fallen to a certain temperature, it skims, the casting that certain way is carried out after skimming obtains required composite material.The crystal grain of obtained composite as-cast tissue crystal grain ratio Al-Si-Cu alloy is more tiny, rounding, and possesses the advantage that intensity is high, moulding is good.
Description
Technical field
The present invention relates to a kind of preparation methods of technical field of composite materials, specifically, utilize mechanical stirring and electromagnetism
It stirs the melting-reaction method combined and prepares original position (TiB2+ZrB2) particle REINFORCED Al-Si-Cu based composites.
Background technique
Particle enhanced aluminum-based composite material has many advantages, such as high specific strength, high elastic modulus, in aerospace, advanced manufacture
The fields such as industry and national defence hold out broad prospects.Compared to traditional plus particle aluminum matrix composite, in-situ particle enhances aluminium base
The particle of composite material is good with matrix wetability, and interface cohesion is secured, and impurity should not be introduced in reaction process, the material prepared
More pure, performance is more excellent.Al-Si-Cu alloy is important Al-Si alloy, and the addition of Cu element can improve alloy
Performance.Firstly, larger-size Cu atom dissolves in Al-Si alloy, Al solid solution is made to generate serious distortion of lattice, hindered
The movement of dislocation increases the shearing stress of sliding motion, forms solution strengthening, improves the intensity of alloy.Again, Cu is in Al-Si
In alloy, θ (CuAl is formed2) phase, in solution treatment, CuAl2It dissolves in αsolidsolution, θ ', θ " is precipitated in ag(e)ing process
(CuAl2) metastable phase or CuAl2Stable phase, these hardening constituents can hinder the movement of dislocation, improve tensile strength, hardness, fatigue
Intensity and elevated temperature strength.The Al-Si-Cu alloy haveing excellent performance is prepared into (TiB as matrix2+ZrB2) particle enhancing aluminium base
Composite material is a kind of combination of ceramic particle for haveing excellent performance matrix and haveing excellent performance, and is a kind of excellent combination, and is prepared
Composite property it is more excellent compared with Al-Si-Cu alloy.
Direct reaction method is that directly alloy matrix aluminum is melted, and reactant is added wherein, is carried out after sufficiently reacting
It casts, this method can directly obtain the composite material of casting, and the technological operation is simple, and production cost is low, and the period is short, easily
In industrial production.But direct reaction method, there is also deficiency, the composite material granular of the preparation under the technique is reunited,
Influence material property.During being applied to fusant reaction using the combination of mechanical stirring and electromagnetic agitation, during stirring
The particle for constantly smashing reunion, keeps distribution of particles more uniform, due to particle TiB2With Grain refinement, so this legal system
Standby matrices of composite material crystal grain is more tiny, to increase substantially the performance of material.
Through to existing technical literature exploration discovery, China Patent No. are as follows: 2015107658685, a kind of title are as follows: particle
The preparation method of reinforced aluminum matrix composites, using composite particles cladding is first rolled into prefabricated section, then will be prefabricated
Block is put into gate and is poured with molten aluminum, needs to use ball mill ball-milling particle in this method, spends the time long, before particle
Prefabricated section is made, so particle dispersion and bad, particles coat and rolling increase step of preparation process, not as this
Patent preparation method is simple and saves cost, while particle is additional entrance in the patent, and particle and basis material conjugation are not
The composite material being prepared in situ such as this patent.China Patent No. are as follows: 2015100957741, a kind of title are as follows: situ Al3Ti
Grain REINFORCED Al-Si-Cu composite material semi-solid state slurry preparation method, is added using in Al-Si-Cu melted alloy
K2TiF6Powder is stirred carrying out electromagnetic agitation, gradually cools down in whipping process.Temperature-fall period in this method preparation process
Bad control, rate of temperature fall also will affect material property, and the patent system it is standby be Al3The enhancing of Ti particle, the particle are not so good as TiB2
Particle is tiny, also without TiB2Particle refines the effect of crystal grain, so the material that the patent preparation method is prepared is special without this
Benefit prepares that material controllability is high, and the composite material base body tissue crystal grain also prepared without this patent is tiny.
Summary of the invention
The present invention is that the fusant reaction preparation method using mechanical stirring in conjunction with electromagnetic agitation prepares (TiB in situ2
+ZrB2) particle enhancing Al-Si-Cu based composites.
Preparation process of the present invention are as follows:
(1) first by potassium fluotitanate (molecular formula K2TiF6), potassium fluorozirconate (molecular formula K2ZrF6), borax powder is put into
Drying box dries (175 DEG C of temperature, time 5h).After drying, example is weighed and is uniformly mixed according to a certain mass ratio, with spare.
(2) pure Al needed for calculating and weighing good a certain amount of Al-Si-Cu alloy of preparation, the matter of Al18Si and Al50Cu
Load weighted pure Al, Al18Si, are put into 400-450 DEG C of crucible of preheating melt later by amount, heat up after thawing to temperature
It is stirred to 720 DEG C of addition Al50Cu and with graphite rod.(3) it after Al50Cu melts completely, heats up 810 DEG C~860 DEG C, divides 3 batches
The potassium fluotitanate mixed, potassium fluorozirconate and borax mixed-powder is added, is stirred during the addition process and with graphite rod.
(4) it after being added completely into powder, opens simultaneously additional electromagnetic stirring device and mechanical agitator is stirred, mechanical stirring and electromagnetism
Mixing direction is on the contrary, mixing time is 15min.Stirring means are as follows: it is stirred together for 5min, stands 5min, point 3 stirrings are completed,
Entire whipping process is 25min.In whipping process, temperature is maintained between 810 DEG C~860 DEG C.(5) to be mixed to finish, it will
Melt is cooled to 705 DEG C~745 DEG C, and agent of skimming is added and skims.(6) it casts immediately after having taken off slag, casting die selects copper
Mould.(7) obtained composite material is heat-treated.
It is 1% that Si mass percent, which is 9%, Cu mass percent, in the Al-Si-Cu alloy substrate, surplus Al.
The voltage that the magnetic stirrer is stirred is 250V~380V, stirring frequency 10.1HZ.
The churned mechanically revolving speed is 200rpm.
The amount that the mixed-powder of enhancing particle reaction raw material is added accounts for the 10%~30% of alloy raw material quality, preferably
20%；The enhancing particle of generation is TiB2And ZrB2, mass ratio 1:1.
Original position (the TiB that the present invention is prepared using electromagnetic agitation and churned mechanically method2+ZrB2) particle REINFORCED Al-Si-
Matrix grain in Cu based composites tissue is tiny, organizes more pure, obtained TiB2And ZrB2Particle dispersion is more equal
It is even.The material mechanical performance prepared increases substantially, tensile strength also improves compared to for Al-Si-Cu alloy.
Detailed description of the invention
(the TiB that the nonheat-treated granular mass of Fig. 1 is 1.5%2+ZrB2) particle REINFORCED Al Si9Cu1 composite material gold
Phasor
(the TiB that the nonheat-treated granular mass of Fig. 2 is 3%2+ZrB2) particle REINFORCED Al Si9Cu1 composite material metallographic
Figure
(the TiB that the nonheat-treated granular mass of Fig. 3 is 6%2+ZrB2) particle REINFORCED Al Si9Cu1 composite material metallographic
Figure
Fig. 4 heat treatment after and nonheat-treated (TiB2+ZrB2) particle REINFORCED Al Si9Cu1 composite material metallographic microscope
Specific embodiment
Elaborate below to the embodiment of the present invention: the present embodiment carries out under the premise of the technical scheme of the present invention
Implement, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following implementation
Case.
It is prepared by the AlSi9Cu1 composite material that 1 granular mass score of case study on implementation is 1.5%
Material component and mass ratio of the invention are as follows: Si 9%, Cu 1%, (TiB2+ZrB2) particle 1.5%, surplus is pure
Al。
Preparation process is as follows:
(1) Al18Si, pure Al and Al50Cu have been configured into 500g alloy according to the mass ratio of 0.48:0.50:0.02, it will
Melt in the crucible that configured material is put into electromagnetic agitation furnace, after melting completely, heat up between 810 DEG C~860 DEG C,
Then the mixed-powder of dry potassium fluorozirconate, potassium fluotitanate and borax is added, powder quality accounts for the 10% of melt quality, mixing
Uniform 3 batches of additions of reaction powder point, and stirred during the addition process using graphite rod.
(2) after powder is added completely into, electromagnetic mixing apparatus is opened, stirring voltage is 250V~380V, and stirring frequency is
10.1HZ.It is opening electromagnetic mixing apparatus simultaneously, is opening the mechanical agitator above crucible and be stirred, mixing direction and electromagnetism
On the contrary, mechanical stirring revolving speed is 200rpm, electromagnetic agitation and stirring of unloading are stirred together for 5min, then stop mixing direction, quiet
5min is set, which is repeated 3 times.
(3) end to be mixed, turns down furnace temperature, cools the temperature to 705 DEG C~745 DEG C, and slagging agent is added, and graphite rod stirs,
And it skims.
(4) it casts immediately after skimming, cast temperature is 705 DEG C~745 DEG C, and the mold of casting is copper mold.
(5) composite material obtained successively carries out the heat treatment of the solid solution of 500 DEG C of 5h and the timeliness of 150 DEG C of 10h, leads to
Cross the material mechanical performance obtained after the heat treatment are as follows: σ b=230MPa, E=4.21GPa, elongation are as follows: 5.1%
(6) without the composite materials property of Overheating Treatment are as follows: σ b=210MPa, E=3.71GPa, elongation are as follows:
4.2%
As shown in Figure 1, a large amount of acicular structure, and branch are contained in the matrices of composite material that granular mass score is 1.5%
Brilliant distance is big, and crystal grain is more coarse.It is not heat-treated known to Fig. 4 and is compared with the composite material after heat treatment, after heat treatment
Si phase becomes corynebacterium or rodlike, wedge angle disappearance from needle-shaped in composite material, and is more uniformly dispersed on the crystal boundary of crystal grain.
It is prepared by the AlSi9Cu1 composite material that 2 granular mass score of case study on implementation is 3%
Material component and mass ratio of the invention are as follows: Si 9%, Cu 1%, (TiB2+ZrB2) particle 3%, surplus is pure
Al。
Preparation process is as follows:
(1) Al18Si, pure Al and Al50Cu have been configured into 500g alloy according to the mass ratio of 0.48:0.50:0.02, it will
Melt in the crucible that configured material is put into electromagnetic agitation furnace, after melting completely, heat up between 810 DEG C~860 DEG C,
Then the mixed-powder of dry potassium fluorozirconate, potassium fluotitanate and borax is added, powder quality accounts for the 20% of melt quality, mixing
Uniform 3 batches of additions of reaction powder point, and 2min is stirred using graphite rod during the addition process.
(2) after powder is added completely into, electromagnetic mixing apparatus is opened, stirring voltage is 250V~380V, and stirring frequency is
10.1HZ.It is opening electromagnetic mixing apparatus simultaneously, is opening the mechanical agitator above crucible and be stirred, mixing direction and electromagnetism
On the contrary, mechanical stirring revolving speed is 200rpm, electromagnetic agitation and stirring of unloading are stirred together for 5min, then stop mixing direction, quiet
5min is set, which is repeated 3 times.
(3) end to be mixed, turns down furnace temperature, cools the temperature to 705 DEG C~745 DEG C, and slagging agent is added, and graphite rod stirs,
And it skims.
(4) it casts immediately after skimming, cast temperature is 705 DEG C~745 DEG C, and the mold of casting is copper mold.
(5) composite material obtained successively carries out the heat treatment of the solid solution of 500 DEG C of 5h and the timeliness of 150 DEG C of 10h, leads to
Cross the material mechanical performance obtained after the heat treatment are as follows: σ b=290MPa, E=11.2GPa, elongation are as follows: 7.8%
(6) without the composite materials property of Overheating Treatment are as follows: σ b=250MPa, E=10.98GPa, elongation are as follows:
6.0%.
As shown in Figure 2, granular mass score be 3% matrices of composite material in acicular structure reduce, and interdendritic away from away from
From significantly reducing, crystal grain also becomes smaller and mellow and full.It is not heat-treated known to Fig. 4 and is compared with the composite material after heat treatment, heat
Si phase becomes corynebacterium or rodlike from needle-shaped in treated composite material, and wedge angle disappears, and is more uniformly dispersed in crystal grain
Crystal boundary on.
It is prepared by the AlSi9Cu1 composite material that 3 granular mass score of case study on implementation is 6%
Material component and mass ratio of the invention are as follows: Si 9%, Cu 1%, (TiB2+ZrB2) particle 6%, surplus is pure
Al。
Preparation process is as follows:
(1) Al18Si, pure Al and Al50Cu have been configured into 500g alloy according to the mass ratio of 0.48:0.50:0.02, it will
Melt in the crucible that configured material is put into electromagnetic agitation furnace, after melting completely, heat up between 810 DEG C~860 DEG C,
Then the mixed-powder of dry potassium fluorozirconate, potassium fluotitanate and borax is added, powder quality accounts for the 30% of melt quality, mixing
Uniform 3 batches of additions of reaction powder point, and 2min is stirred using graphite rod during the addition process.
(2) after powder is added completely into, electromagnetic mixing apparatus is opened, stirring voltage is 250V~380V, and stirring frequency is
10.1HZ.It is opening electromagnetic mixing apparatus simultaneously, is opening the mechanical agitator above crucible and be stirred, mixing direction and electromagnetism
On the contrary, mechanical stirring revolving speed is 200rpm, electromagnetic agitation and stirring of unloading are stirred together for 5min, then stop mixing direction, quiet
5min is set, which is repeated 3 times.
(3) end to be mixed, turns down furnace temperature, cools the temperature to 705 DEG C~745 DEG C, and slagging agent is added, and graphite rod stirs,
And it skims.
(4) it casts immediately after skimming, cast temperature is 705 DEG C~745 DEG C, and the mold of casting is copper mold.
(5) composite material obtained successively carries out the heat treatment of the solid solution of 500 DEG C of 5h and the timeliness of 150 DEG C of 10h, leads to
Cross the material mechanical performance obtained after the heat treatment are as follows: σ b=275MPa, E=9.16GPa, elongation are as follows: 6.8%
(6) without the composite materials property of Overheating Treatment are as follows: σ b=235MPa, E=6.06GPa, elongation are
4.1%
From the figure 3, it may be seen that containing a large amount of acicular structure in the matrices of composite material that granular mass score is 6%, and dendrite
Distance is smaller, and crystal grain also becomes smaller, but the particle being mingled between crystal grain is more more, particle agglomeration it is also more strict
Evil.It is not heat-treated known to Fig. 4 and is compared with the composite material after heat treatment, Si phase becomes from needle-shaped in the composite material after heat treatment
Corynebacterium is rodlike, and wedge angle disappears, and is more uniformly dispersed on the crystal boundary of crystal grain.Following table is composite material and basis material
Performance table.
1. composite material of table and its substrate performance table
As seen from table, (TiB2+ZrB2) particle REINFORCED Al Si9Cu1 composite material basis material performance more corresponding than its is more
Excellent, the more nonheat-treated material property of composite property after heat treatment has huge promotion.
Claims (9)
1. a kind of preparation method of Al-Si9Cu1 particulate reinforced composite, which is characterized in that, will in situ in reaction process
After the mixed-powder of enhancing particle reaction raw material is added in the alloy raw material for preparing matrix alloy Al-Si9Cu1 of melting, together
When open additional electromagnetic stirring device and mechanical agitator and be stirred, mechanical stirring is contrary with electromagnetic agitation, mixing time
For 15min；Stirring means are as follows: be first stirred together for 5min, then stand 5min, then be stirred together for 5min, then stand 5min, finally again
It is stirred together for 5min, entire whipping process is 25min；The specific steps of preparation method are as follows:
(1) pure Al needed for calculating and weighing good a certain amount of Al-Si9Cu1 alloy of preparation, the quality of Al18Si and Al50Cu,
Later by load weighted pure Al, Al18Si, which is put into the crucible of preheating, to be melted, and is warming up to 720 DEG C of additions to temperature after thawing
Al50Cu is simultaneously stirred with graphite rod；
(2) it after Al50Cu melts completely, heats up 810 DEG C~860 DEG C, the potassium fluotitanate that point 3 batches of additions mix, potassium fluorozirconate
And the mixed-powder of the enhancing particle reaction raw material of borax, it is stirred during the addition process and with graphite rod；
(3) after being added completely into powder, open simultaneously additional electromagnetic stirring device and mechanical agitator be stirred, mechanical stirring with
Electromagnetic agitation is contrary, and in whipping process, temperature is maintained between 810 DEG C~860 DEG C；
(4) to be mixed to finish, 705 DEG C~745 DEG C are cooled the melt to, agent of skimming is added and skims；
(5) it casts immediately after having taken off slag, casting die selects copper mold；
(6) obtained composite material is heat-treated.
2. a kind of preparation method of Al-Si9Cu1 particulate reinforced composite as described in claim 1, which is characterized in that institute
Stating the voltage that magnetic stirrer is stirred is 250V~380V, stirring frequency 10.1Hz.
3. a kind of preparation method of Al-Si9Cu1 particulate reinforced composite as described in claim 1, which is characterized in that institute
Stating churned mechanically revolving speed is 200rpm.
4. a kind of preparation method of Al-Si9Cu1 particulate reinforced composite as described in claim 1, which is characterized in that
The mass ratio of Al18Si, pure Al and Al50Cu are 0.48:0.50:0.02；The temperature of crucible preheating is 400~450 DEG C.
5. a kind of preparation method of Al-Si9Cu1 particulate reinforced composite as described in claim 1, which is characterized in that increase
The amount that the mixed-powder of strong particle reaction raw material is added accounts for the 10%~30% of alloy raw material quality；The enhancing particle of generation is
TiB2And ZrB2, mass ratio 1:1.
6. a kind of preparation method of Al-Si9Cu1 particulate reinforced composite as claimed in claim 5, which is characterized in that increase
The amount that the mixed-powder of strong particle reaction raw material is added accounts for the 20% of alloy raw material quality.
7. a kind of preparation method of Al-Si9Cu1 particulate reinforced composite as described in claim 1, which is characterized in that will
Obtained composite material carry out heat treatment refer to: obtained composite material successively carry out 500 DEG C of 5h solid solution and 150 DEG C of 10h
Timeliness heat treatment.
8. a kind of preparation method of Al-Si9Cu1 particulate reinforced composite as described in claim 1, which is characterized in that institute
State the mixed-powder of enhancing particle reaction raw material the preparation method is as follows: first by potassium fluotitanate, potassium fluorozirconate, borax powder is put into
After drying box drying, example is weighed and is uniformly mixed according to a certain mass ratio, with spare.
9. a kind of preparation method of Al-Si9Cu1 particulate reinforced composite as claimed in claim 8, which is characterized in that institute
Stating drying temperature is 175 DEG C, drying time 5h.
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