CN110079751A - A kind of preparation method of made of Al-Cu alloy supersaturated solid solution - Google Patents
A kind of preparation method of made of Al-Cu alloy supersaturated solid solution Download PDFInfo
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- CN110079751A CN110079751A CN201910321909.XA CN201910321909A CN110079751A CN 110079751 A CN110079751 A CN 110079751A CN 201910321909 A CN201910321909 A CN 201910321909A CN 110079751 A CN110079751 A CN 110079751A
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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
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/026—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
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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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
- C22F1/057—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 copper as the next major constituent
Abstract
The invention discloses a kind of preparation methods of made of Al-Cu alloy supersaturated solid solution, comprising: (I) Al-Cu master alloy is molten to match；The solidification of Al-Cu master alloy super-pressure obtained by (II) step (I), obtains made of Al-Cu alloy supersaturated solid solution；Wherein: in step (I), the molten smelting temperature matched of the Al-Cu master alloy is 620-680 DEG C；In step (II), the pressure of the super-pressure solidification is 3GPa, and heating temperature is 887-897 DEG C.The method that the present invention uses super-pressure solidification, by reducing solutes accumulation coefficient in process of setting, Cu atom diffusivity weakens significantly, obtains Al-Cu supersaturated solid solution alloy.Furthermore by subsequent ageing treatment, fine and uniformly distributed Al is obtained2Cu precipitated phase makes it in the fields such as automobile, aerospace extensive application to improve the mechanical property of alloy.
Description
Technical field
The invention belongs to materials processing technology fields, and in particular to a kind of preparation side of made of Al-Cu alloy supersaturated solid solution
Method.
Background technique
The advantages that made of Al-Cu alloy is a kind of high strength alumin ium alloy, and density is small, plasticity is good and excellent machinability, quilt
It is widely used in the fields such as automobile, space flight and aviation.But the crystallization range of made of Al-Cu alloy is wide, is coagulated in a manner of volume solidification
Gu being easy to produce the casting flaws such as serious dendritic segregation, hot tearing, microporosity, shrinkage cavity.The casting character of difference and serious ingredient
Segregation largely reduces the mechanical property of casting, seriously constrains the application of made of Al-Cu alloy.
For this purpose, present invention proposition prepares made of Al-Cu alloy supersaturated solid solution using super-pressure solidification technology, solidifying
Apply super-pressure in journey, be conducive to the pressure feeding under high pressure and reduce interdendritic solute copper atom diffusivity, and combines
Subsequent ageing treatment makes the second phase Al2Cu even dispersion is precipitated, to reduce segregation, reduce hot cracking tendency, it is equal to obtain ingredient
Even, fine microstructures casting.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of made of Al-Cu alloy supersaturated solid solution, are solidified by super-pressure
Technology prepares Al-Cu supersaturated solid solution.
In order to achieve the above object, specific technical solution is as follows:
The preparation method of made of Al-Cu alloy supersaturated solid solution of the invention, specifically includes:
(I) Al-Cu master alloy is molten to match；With
The solidification of Al-Cu master alloy super-pressure obtained by (II) step (I), obtains made of Al-Cu alloy supersaturated solid solution.
Further, the operating process of step (I) includes: by rafifinal (99.9%Al) and high purity copper (99.9%Cu) by matter
Amount percentage is that 19:1 (Al-5Cu alloy) is weighed to be placed in silica crucible or high-frequency vacuum induction furnace and is in smelting temperature
Induction melting is carried out under conditions of 620-680 DEG C；Wherein, the operation order of the high-frequency vacuum induction furnace includes:
Bell is first closed, rear mechanical pump of opening vacuumizes, then opens molecular pump, and being extracted into pressure to molecular pump is 5 × 10-3Pa
Molecular pump is closed when pressure, pours a certain amount of high-purity argon gas, is then turned on mechanical pump and molecular pump is evacuated to setting value, close and divide
Son pump pours a certain amount of high-purity argon gas as protective gas, opens power supply, start to melt, pour after the degasification of gained aluminium alloy, slagging-off
It infuses in copper mould and is solidified, be cooled to room temperature, obtain Al-Cu master alloy.
Further, the Al-Cu master alloy has Al-5Cu As-cast Microstructure.
Further, the operating process of step (II) includes: that Al-Cu master alloy sample obtained by step (I) is cut into cylinder
BN powder is covered on above-mentioned cylindrical body alloy sample table after the pyrophillite component drying in extra-high tension unit by body alloy sample
Face is placed in pyrophillite component；Pyrophillite component comprising alloy sample is put into extra-high tension unit, predetermined pressure is
It is heated after 3GPa, heating temperature is 887-897 DEG C, while opening recirculated water；After being heated to alloy sample fusing, heat preservation
Pressure maintaining 3-5 minutes, stop heating and being cooled to 100-200 DEG C, release is taken out.
Further, graphite flake near the cylindrical body alloy sample upper and lower surface carries out conductive heater, the leaf
An aperture is respectively contained in cured stone two sides, and K-type thermocouple is placed in pyrophillite component and the alloy in alloy measurement heating process
Temperature.
The present invention prepares supersaturated solid solution made of Al-Cu alloy using super-pressure solidification technology for the first time, is made by ageing treatment
Second phase even dispersion is precipitated, and significantly reduces the casting flaws such as segregation.It is compared with conventional cast, which can be substantially reduced
Made of Al-Cu alloy segregation, obtains the casting of fine microstructures even dispersion distribution, so that mechanical castings are improved, in automobile and boat
Empty space industry application prospect is big.
Detailed description of the invention
Fig. 1 is the microscopic structure that normal pressure solidifies Al-5Cu alloy.
Fig. 2 is the microscopic structure that 3GPa solidifies Al-5Cu alloy.
Fig. 3 is the X ray diffracting spectrum that normal pressure solidifies Al-5Cu alloy.
Fig. 4 is the X-ray map that 3GPa solidifies Al-5Cu alloy.
Fig. 5 is the Vickers hardness curve that normal pressure solidifies Al-5Cu alloy.
Fig. 6 is the Vickers hardness curve that 3GPa solidifies Al-5Cu alloy.
Fig. 7 is that 3GPa solidifies the Vickers hardness curve after Al-5Cu alloy aging.
Specific embodiment
The invention will be further described by taking supersaturated solid solution made of Al-Cu alloy as an example.
Step 1: Al-Cu master alloy ingot preparation process, key step have:
Rafifinal (99.9%Al), high purity copper (99.9%Cu) is respectively adopted in step 1:Al-5Cu master alloy ingot raw material,
Ingredient is carried out for 95:5 (Al-5Cu alloy) by mass percentage, load weighted raw material metal is put into silica crucible and is felt
Answer melting.
Step 2: raw material metal load weighted in mass ratio in advance is put into progress alloy system in high-frequency vacuum induction furnace
It is standby.Al-5Cu alloy melting temp is controlled at 650 DEG C or so, and mold is put into smelting equipment, is first closed by equipment operation specification
Closed furnace lid, rear mechanical pump of opening vacuumize, and then open molecular pump, and being extracted into pressure to molecular pump is 5*10-3When Pa pressure, close
Molecular pump pours a certain amount of high-purity argon gas, is then turned on mechanical pump and molecular pump is evacuated to setting value, close molecular pump, pour
A certain amount of high-purity argon gas opens power supply, starts to melt as protective gas.
Step 3: it is poured into copper mould and is solidified after aluminium alloy degasification, slagging-off after fusing, it is to be cooled to after room temperature, most
The Al-5Cu master alloy ingot that diameter is 20mm is obtained eventually.Sample is cut from master alloy ingot carries out microstructure observation.To
To Al-5Cu As-cast Microstructure.
Fig. 1 is normal pressure solidification Al-5Cu alloy microstructure morphology, by nascent a-Al phase and eutectic structure (eutectic a-Al phase
And Al2Cu it) forms, eutectic Al2Cu phase exists in the form of strip and two kinds of graininess.
Step 2: super-pressure solidification made of Al-Cu alloy supersaturated solid solution preparation, key step have:
Step 1: as-cast specimen being first cut into the cylindrical body of diameter 20mm, high 9mm, by the equipment middle period before super-pressure solidification
Other assembling parts such as cured stone carry out drying and processing.
Step 2: BN powder being first covered on alloy sample surface, is then placed in pyrophillite assembly together, passes through conjunction
Graphite flake near golden sample upper and lower surface carries out conductive heater.In order to measure alloy sample in the change of heating process temperature
Change, therefore respectively bore an aperture in pyrophillite two sides, then K-type thermocouple is placed in pyrophillite assembly close to alloy sample
Position, the temperature of alloy in heating process is measured with this.
Step 3: the pyrophillite assembly comprising alloy sample being put into extra-high tension unit, extra-high tension unit is adjusted to pre-
Constant-pressure is 3GPa, then starts to heat alloy sample, and Al-5Cu alloy heating and temperature control is at 887-897 DEG C, together
Shi Kaiqi recirculated water.
Step 4: in alloy sample heating process, paying attention to observing K-type thermocouple registration, be melted when being heated to alloy sample
Afterwards, it in order to melt alloy sample sufficiently, needs heat-insulation pressure keeping about 5 minutes, then stops heating, when alloy is cooled to 100-
At 200 DEG C, removal pressure simultaneously closes off recirculated water, takes out super-pressure solidified superalloy sample and carries out test analysis to it.
Fig. 2 is the Al-5Cu alloy microstructure prepared under the conditions of pressure is 3GPa, it can be seen from the figure that and normal pressure
As-cast structure compare, strip, rodlike and granular Al2Cu has vanished from sight, and is all dissolved into a-Al matrix, says
Al-5Cu under bright super-pressure solidification is supersaturated solid solution alloy.
Fig. 3 is the X-ray diffractogram of the Al-5Cu alloy under normal pressure solidification, from map as can be seen that tissue is by a-Al base
Body phase and Al2Cu phase composition.
Fig. 4 is the X-ray diffractogram of 3GPa solidification Al-5Cu alloy, from map as can be seen that only a-Al phase, Al2Cu
Phase diffraction maximum does not occur.In process of setting, due to the effect of super-pressure, the diffusivity of Cu atom weakens, and Cu atom is complete
Portion is solid-solubilized in a-Al matrix.The constituent concentration of Cu does not reach eutectic point in liquid phase, and eutectic reaction cannot occur, so tissue
In there is no Al2Cu occurs.Therefore Al-5Cu alloy is supersaturated solid solution under 3GPa pressure solidification.
Fig. 5 is the Vickers hardness curve of normal pressure solidification Al-5Cu alloy sample, and Vickers hardness average value is 53.4HV0.2。
Fig. 6 is the Vickers hardness curve of 3GPa pressure solidification Al-5Cu alloy sample, and Vickers hardness average value is
94.4HV0.2, compared with normal pressure solidifies Vickers hardness, 3GPa High Pressure Solidification alloy Vickers hardness increases 76.8%.
Fig. 7 is that 3GPa pressure solidification Al-5Cu alloy Vickers hardness curve, Vickers after 175 DEG C/8h ageing treatment are hard
Degree average value is 127.4HV0.2.It is compared with normal pressure solidification Al-5Cu alloy, 3GPa High Pressure Solidification alloy Vickers hardness increases after timeliness
It is big by 138.6%；It is compared with 3GPa High Pressure Solidification alloy, 3GPa High Pressure Solidification alloy Vickers hardness increases 35% after timeliness.
According to above-mentioned hardness analysis it is found that with normal pressure solidifying phase ratio, 3GPa High Pressure Solidification Al-5Cu alloy rigidity obviously increases
Add.Microstructure is organized from SEM it is found that being dispersed with strip and irregular particle shape Al under normal pressure in a-Al matrix2Cu phase.And
3GPa High Pressure Solidification is dissolved into Cu atom all in a-Al matrix, plays solution strengthening in the base, so that high pressure is solidifying
Gu Al-5Cu alloy becomes supersaturated solid solution, therefore hardness increases.It is closed in the supersaturated solid solution after 175 DEG C/8h timeliness
Tiny Al is precipitated in gold2Cu phase is evenly distributed on matrix, plays dispersion-strengtherning to matrix, therefore hardness further increases.
In conclusion the present invention not only successfully prepares supersaturated solid solution made of Al-Cu alloy using super-pressure solidification technology, and
And be sufficiently dissolved into matrix by the second phase, rear even dispersion is precipitated, and can significantly reduce segregation, and the second phase is dissolved to matrix energy
Certain solution strengthening is played, to improve the comprehensive mechanical property of alloy.And it is alloy properties for fields such as automobile, aerospaces
Height can be required, the supersaturated solid solution alloy that High Pressure Solidification obtains passes through Precipitation, can be further improved alloy property.Therefore it is high
Pressure solidification obtains supersaturated solid solution and aging strengthening model, can effectively solve the fields such as automobile, aerospace to alloy superiority
The demand of energy.
Claims (5)
1. a kind of preparation method of made of Al-Cu alloy supersaturated solid solution characterized by comprising
(I) Al-Cu master alloy is molten to match；With
The solidification of Al-Cu master alloy super-pressure obtained by (II) step (I), obtains made of Al-Cu alloy supersaturated solid solution；Wherein:
In step (I), the molten smelting temperature matched of the Al-Cu master alloy is 620-680 DEG C；
In step (II), the pressure of the super-pressure solidification is 3GPa, and heating temperature is 887-897 DEG C.
2. the preparation method of made of Al-Cu alloy supersaturated solid solution according to claim 1, which is characterized in that step (I)
It is by mass percentage 19:1 (Al-5Cu conjunction that operating process, which includes: by rafifinal (99.9%Al) and high purity copper (99.9%Cu),
Gold) it weighs to be placed in silica crucible or high-frequency vacuum induction furnace and be felt under conditions of smelting temperature is 620-680 DEG C
Answer melting；Wherein:
The operation order of the high-frequency vacuum induction furnace includes: first to close bell, and rear mechanical pump of opening vacuumizes, then opens molecule
Pump, being extracted into pressure to molecular pump is 5 × 10-3Molecular pump is closed when Pa pressure, a certain amount of high-purity argon gas is poured, is then turned on mechanical pump
It is evacuated to setting value with molecular pump, closes molecular pump, a certain amount of high-purity argon gas is poured as protective gas, opens power supply, open
Begin to melt, be poured into copper mould and solidified after the degasification of gained aluminium alloy, slagging-off, be cooled to room temperature, obtains mother's Al-Cu conjunction
Gold.
3. the preparation method of made of Al-Cu alloy supersaturated solid solution according to claim 1 or 2, which is characterized in that described
Al-Cu master alloy has Al-5Cu As-cast Microstructure.
4. the preparation method of made of Al-Cu alloy supersaturated solid solution according to claim 1, which is characterized in that step (II)
Operating process include: that Al-Cu master alloy sample obtained by step (I) is cut into cylindrical body alloy sample, in extra-high tension unit
Pyrophillite component drying after, BN powder is covered on above-mentioned cylindrical body alloy sample surface and is placed in pyrophillite component；It will
Pyrophillite component comprising alloy sample is put into extra-high tension unit, and predetermined pressure is heated after being 3GPa, and heating temperature is
887-897 DEG C, while opening recirculated water；After being heated to alloy sample fusing, heat-insulation pressure keeping 3-5 minutes, stopping heating was simultaneously cold
But 100-200 DEG C is arrived, release is taken out.
5. the preparation method of made of Al-Cu alloy supersaturated solid solution according to claim 4, which is characterized in that the cylinder
Graphite flake near body alloy sample upper and lower surface carries out conductive heater, and an aperture, K-type are respectively contained in the pyrophillite two sides
Thermocouple is placed in pyrophillite component and the alloy temperature in alloy measurement heating process.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111496200A (en) * | 2020-04-24 | 2020-08-07 | 浙江大学 | Horizontal continuous casting method and application of high-strength and high-conductivity copper alloy |
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| CN101653825A (en) * | 2009-09-24 | 2010-02-24 | 哈尔滨工业大学 | High-pressure counter-pressure casting method of Al-5 percent Cu base alloy |
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Application publication date: 20190802 |