CN108655375A - The method and its device for directionally solidifying of functionally graded material are prepared using axial homogeneous magnetic field - Google Patents
The method and its device for directionally solidifying of functionally graded material are prepared using axial homogeneous magnetic field Download PDFInfo
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- CN108655375A CN108655375A CN201810475102.7A CN201810475102A CN108655375A CN 108655375 A CN108655375 A CN 108655375A CN 201810475102 A CN201810475102 A CN 201810475102A CN 108655375 A CN108655375 A CN 108655375A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
- B22D27/04—Influencing the temperature of the metal, e.g. by heating or cooling the mould
- B22D27/045—Directionally solidified castings
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
- B22D27/02—Use of electric or magnetic effects
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B30/00—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions
- C30B30/04—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions using magnetic fields
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Abstract
The invention discloses a kind of methods and its device for directionally solidifying preparing functionally graded material using axial homogeneous magnetic field,The magnetic field intensity range of the axial magnetic field generated using superconduction gradient strong magnetic body is not more than 5T,Using the thermoelectricity magneticaction of Magnetic Field-Induced on alloy melt,It is dynamic to generate thermoelectricity magnetic current,Increase with the decline of temperature the presence with temperature gradient in directional solidification process due to the content of precipitated phase in alloy melt,When melt is by low temperature,The phase fast-growth for being conducive to the precipitation of precipitated phase and being precipitated,The volume fraction of precipitated phase when precipitate volume fraction being caused to be more than the alloy equilibrium freezing,With the progress of directional solidification,Solutes content is reduced in remainder melt,Even become lean solute melt,Finally solidified with the ingredient of eutectic alloy,It is eutectic to form a kind of top,Lower part is the functionally graded material of primary phase and eutectic phase,New process orientation is provided to carry out special material preparation using axial homogeneous magnetic field.
Description
Technical field
The present invention relates to a kind of method preparing functionally gradient material (FGM) and orientation casting apparatus, having gradient more particularly to one kind
The technique and coagulation system of the metal material of tissue are applied to metal solidification texture control technology field.
Background technology
Functionally graded material is a kind of tissue and performance is continuous or the heterogeneous functional composite material of quasi-continuous variation.Due to
The ingredient and institutional framework of material consecutive variations on geometric space, performance are also continuous variation on geometric space.It is this
New material can meet extreme demand, such as the parts needed for aerospace and nuclear energy power generation.
At present prepare function-graded material method mainly have powder metallurgy hair, plasma spraying method, gas phase product method and
Laser cladding etc., but there are a variety of different disadvantages for these techniques, as the functionally graded material size obtained is small, performance
It is poor or of high cost etc..
Invention content
In order to solve prior art problem, it is an object of the present invention to overcome the deficiencies of the prior art, and to provide one kind
The method and its device for directionally solidifying that functionally graded material is prepared using axial homogeneous magnetic field, can carry out in-situ metal functionally gradient
The preparation of composite material generates thermoelectricity magnetic current and moves, due to alloy using the thermoelectricity magneticaction of Magnetic Field-Induced on alloy melt
The content of precipitated phase increases the presence with temperature gradient in directional solidification process with the decline of temperature in melt, and melt is through too low
When at temperature, the phase fast-growth for being conducive to the precipitation of precipitated phase and being precipitated, it is more than the alloy to lead to precipitate volume fraction
The volume fraction of precipitated phase when equilibrium freezing, with the progress of directional solidification, solutes content is reduced in remainder melt, or even is become
Lean solute melt is finally solidified with the ingredient of eutectic alloy, forms that a kind of top is eutectic, lower part is primary phase and eutectic phase
Functionally graded material provides a kind of completely new technology to prepare functionally graded material, also to utilize axial homogeneous magnetic field progress
Special material preparation provides new process orientation.
In order to achieve the above objectives, the present invention adopts the following technical scheme that：
A method of functionally graded material being prepared using axial homogeneous magnetic field, is included the following steps：
A. prepared by raw material：
According to the alloying component of functionally graded material to be prepared, simple metal is chosen as raw material, is suspended in vacuum induction
Melt back is carried out in stove, makes its homogenization of composition, and alloy melt is then carried out negative pressure with quartz ampoule inhales casting, and it is equal to obtain ingredient
Even virgin alloy stick；
B. apparatus for directional solidification is installed：
Device for directionally solidifying is put into axial homogeneous magnetic field, the magnetic field intensity near magnetic field center is in the model no more than 5T
It encloses interior continuously adjustable, the virgin alloy stick prepared in step a is surface-treated clean, is packed into the corundum crucible of corresponding size
In, corundum crucible is fixed on to the pull rod upper end of directional solidification, corundum crucible moves up and down in heating furnace with pull rod, passes through control
The pull system of directional solidification processed is oriented solidification with the drawing velocity set, and directional solidification is oriented parallel to axial magnetic field
Direction, while adjusting position of the heating furnace in magnetic field, after alloy melts in corundum crucible, make alloy in corundum crucible
Freezing interface is maintained at homogeneous magnetic field area；
C. prepared by functionally graded material：
After fixing the apparatus for directional solidification being arranged in the step b, inert gas is passed through into heating furnace as guarantor
Gas is protected, then starts heating device, heats up according to the preset heating speed no more than 10 DEG C/min, be raised to and be not higher than
After 1600 DEG C of specified temperature, it is then turned on field generator for magnetic, under the influence of a magnetic field, and is made just after at least 30 minutes
Virgin alloy stick melts the metal bath for forming homogenization completely in beautiful crucible, is then turned on directional solidification pull system, according to
Withdrawing rate not higher than 20 μm/s is oriented solidification, until all pulls of the alloy melt in corundum crucible are situated between to equipped with cooling
In the quenching bath of matter, the alloy bar of directional solidification is then taken out from quenching bath to get to functionally graded material.
As currently preferred technical solution, prepared functionally graded material is aluminium alloy, and aluminium in aluminium alloy
Mass percentage content be not higher than 88wt.%.
As a kind of technical solution advanced optimized of above-mentioned technical proposal, Al-Ni alloy functionally gradient materials are being prepared
When material, which is characterized in that include the following steps：
A. prepared by raw material：
It selects purity for 99.99% high pure metal raw material, is configured to be divided into the alloy of Al-12wt.%Ni, it is outstanding in vacuum
Melt back in floating stove, after making Al-Ni alloy raw material full and uniformization, negative pressure suction is carried out by Al-Ni alloy melts with quartz ampoule
Casting, obtains the uniform Al-Ni alloy bars of ingredient, and obtained Al-Ni alloy bars are encapsulated in corundum crucible, spare；
B. apparatus for directional solidification is installed：
Device for directionally solidifying is put into axial homogeneous magnetic field, the magnetic field intensity near magnetic field center is in the model no more than 5T
It encloses interior continuously adjustable, the original Al-Ni alloy bars prepared in step a is surface-treated clean, is packed into the corundum of corresponding size
In crucible, corundum crucible is fixed on to the pull rod upper end of directional solidification, corundum crucible moves up and down in heating furnace with pull rod, leads to
The pull system for crossing control directional solidification is oriented solidification with the drawing velocity set, and directional solidification is oriented parallel to axial direction
The direction in magnetic field, while position of the heating furnace in magnetic field is adjusted, after alloy melts in corundum crucible, make in corundum crucible
The freezing interface of Al-Ni alloys is maintained at homogeneous magnetic field area；
C. prepared by functionally graded material：
After fixing the apparatus for directional solidification being arranged in the step b, inert gas is passed through into heating furnace as guarantor
Gas is protected, then starts heating device, heats up according to the preset heating speed no more than 10 DEG C/min, be raised to and be not less than
After 800 DEG C of specified temperature, it is then turned on field generator for magnetic, under the influence of a magnetic field, and is made just after at least 30 minutes
Virgin alloy stick melts the metal bath for forming homogenization completely in beautiful crucible, is then turned on directional solidification pull system, according to
Withdrawing rate not higher than 10 μm/s is oriented solidification, until all pulls of the alloy melt in corundum crucible are situated between to equipped with cooling
In the quenching bath of matter, the alloy bar of directional solidification is then taken out from quenching bath to get to Al-Ni alloy functionally graded material.
The technical solution that another kind as above-mentioned technical proposal advanced optimizes is preparing made of Al-Cu alloy functionally gradient
When material, which is characterized in that include the following steps：
A. prepared by raw material：
It selects purity for 99.99% high pure metal raw material, is configured to be divided into the alloy of Al-40wt.%Cu, it is outstanding in vacuum
Melt back in floating stove, makes made of Al-Cu alloy raw material full and uniformization, and made of Al-Cu alloy melt is carried out negative pressure with quartz ampoule inhales casting,
The uniform made of Al-Cu alloy stick of ingredient is obtained, and obtained made of Al-Cu alloy stick is encapsulated in corundum crucible, it is spare；
B. apparatus for directional solidification is installed：
Device for directionally solidifying is put into axial homogeneous magnetic field, the magnetic field intensity near magnetic field center is in the model no more than 5T
It encloses interior continuously adjustable, the original made of Al-Cu alloy stick prepared in step a is surface-treated clean, is packed into the corundum of corresponding size
In crucible, corundum crucible is fixed on to the pull rod upper end of directional solidification, corundum crucible moves up and down in heating furnace with pull rod, leads to
The pull system for crossing control directional solidification is oriented solidification with the drawing velocity set, and directional solidification is oriented parallel to axial direction
The direction in magnetic field, while position of the heating furnace in magnetic field is adjusted, after alloy melts in corundum crucible, make in corundum crucible
The freezing interface of made of Al-Cu alloy is maintained at homogeneous magnetic field area；
C. prepared by functionally graded material：
After fixing the apparatus for directional solidification being arranged in the step b, inert gas is passed through into heating furnace as guarantor
Gas is protected, then starts heating device, heats up according to the preset heating speed no more than 10 DEG C/min, be raised to and be not less than
After 800 DEG C of specified temperature, it is then turned on field generator for magnetic, under the influence of a magnetic field, and is made just after at least 30 minutes
Virgin alloy stick melts the metal bath for forming homogenization completely in beautiful crucible, is then turned on directional solidification pull system, according to
Withdrawing rate not higher than 10 μm/s is oriented solidification, until all pulls of the alloy melt in corundum crucible are situated between to equipped with cooling
In the quenching bath of matter, the alloy bar of directional solidification is then taken out from quenching bath to get to made of Al-Cu alloy functionally graded material.
When carrying out functionally graded material preparation in the step c, preferably by controlling the size of magnetic field intensity, to adjust
The gradient magnitude that is longitudinally formed gradient distribution of the nascent phase constitution of directional solidification along prepared material.
When carrying out functionally graded material preparation in the step c, argon gas is preferably passed through into heating furnace as protection gas
Body；Or the cooling medium in quenching bath preferably uses Ga-In-Sn.
When carrying out functionally graded material preparation in the step c, preferably prepared functionally graded material is in one kind
Portion is eutectic, lower part is primary phase and the rodlike functionally graded material of eutectic phase.
A kind of device for directionally solidifying implemented the present invention and prepare the method for functionally graded material using axial homogeneous magnetic field, by
Protective atmosphere input pipe, water cooled furnace body, heating furnace, temperature-detecting device, quenching bath, thermal insulation medium, thermal insulation layer, corundum crucible with
And pull rod composition, the quenching bath are set to the lower section of the heating furnace, and by the thermal insulation layer by heating furnace bottom and quenching bath
It is separated, the water cooled furnace body is mounted on the outside of the heating furnace, and the temperature-detecting device detects the heating in real time
Alloy bar is encapsulated in the corundum crucible by the temperature in stove, then the corundum crucible is fixedly connected on the drawing vertically
The upper end of bar, the protective atmosphere input pipe are passed through inert gas from the heating furnace bottom end, and the alloy bar is made to be in inertia
Under gas atmosphere；Device for directionally solidifying is put into axial permanent magnetic by the axial magnetic field generated using superconduction kicker magnet device
In, the magnetic field intensity near magnetic field center is continuously adjusted in the range of no more than 5T；In the initial strip for being oriented solidification
Under part, first the corundum crucible is set in heating furnace, the alloy bar in the corundum crucible is in the heating furnace
Heat effect under melt, formed metal bath, then by control directional solidification pull system, with the pull of setting
The downward vertical shift of speed drawing pull rod, to drive corundum crucible to enter quenching bath, make metal bath in corundum crucible from
Bottom starts to be oriented solidification upwards；Position of the heating furnace in magnetic field is adjusted simultaneously, makes the metal bath in corundum crucible
Freezing interface be maintained at homogeneous magnetic field area；By controlling drawing velocity of the pull rod to set of the pull system of directional solidification,
The corundum crucible is set to move straight down, the direction for the magnetic field intensity B that the superconduction kicker magnet device generates and directional solidification
Direction is parallel, and in directional solidification process, and the solid/liquid interfaces of the alloy bar are in the superconduction kicker magnet device and generate
Homogeneous magnetic field region.
The internal layer furnace wall of above-mentioned heating furnace is preferably made of nonmagnetic stainless steel, is preferably heated furnace chamber maximum temperature and is
1600℃。
Above-mentioned temperature-detecting device preferably uses double platinum rhodium type thermocouple, measures the heating-furnace intracavitary temperature in real time.
The principle of the present invention：
The principle of the method for the present invention is, due to Seebeck effects, the primary phase of directional solidification mushy zone and melt due to
Seebeck coefficients are different, generate thermocurrent, under the action of axial homogeneous magnetic field, generate thermoelectricity magnetic force, thermoelectricity magneticaction exists
On alloy melt, it is dynamic just to generate thermoelectricity magnetic current.
The thermoelectricity magnetic force that unit volume melt is born in axial homogeneous magnetic field is：
In formula, σSAnd σLIt is the conductivity in solid phase and liquid phase, S respectivelySAnd SLIt is the temperature-difference thermoelectric of solid phase and liquid phase respectively
Gesture, fSAnd fLIt is the volume fraction of solid phase and liquid phase respectively, G is the temperature gradient in solid/liquid interfaces forward position, and B is magnetic field intensity.
Under the action of axial homogeneous magnetic field, the thermoelectricity magnetic current of radial rotary is dynamic to cause circulation, as shown in Figure 2.Due to being analysed in alloy melt
The content for going out phase increases presence with temperature gradient in directional solidification process with the decline of temperature, when melt is by low temperature,
The phase fast-growth for being conducive to the precipitation of precipitated phase and being precipitated, it is more than the alloy equilibrium freezing to lead to precipitate volume fraction
When precipitated phase volume fraction, with the progress of directional solidification, solutes content is reduced in remainder melt, or even to become lean solute molten
Body is finally solidified with the ingredient of eutectic alloy, formed a kind of top be eutectic structure, the work(that lower part is primary phase and eutectic structure
It can functionally gradient material (FGM).Since thermoelectricity magnetic force includes the Lorentz force of the Lorentz force that thermocurrent generates and induced field current generation, after
Person plays a major role when melt flows intensity is larger, so the thermoelectricity magnetic current in melt is also first to increase to reduce afterwards, in axial direction
Under the action of homogeneous magnetic field, the thermoelectricity magnetic current of radial rotary is dynamic to cause circulation to be also first to increase to reduce afterwards, therefore can pass through tune
The size of magnetic field intensity is saved to control the gradient of functionally gradient material (FGM), prepares the functionally graded material with different gradients.
The present invention compared with prior art, has following obvious prominent substantive distinguishing features and remarkable advantage：
1. the present invention applies axial homogeneous magnetic field during alloy directionally solidified, primary phase is caused to be longitudinally formed along sample
Gradient is distributed, and forms functionally graded material, and adjust the size of nascent phase gradient by controlling the size in magnetic field；
2. the method that the method for the present invention prepares functionally graded material using axial homogeneous magnetic field, magnetic field and functionally graded material
Between it is contactless, do not increase secondary pollution；
3. the method for the present invention is simple for process, of low cost, easy to operate, industrial production and manufacturing can be widely applied to.
Description of the drawings
Fig. 1 is various embodiments of the present invention directional solidification equipment configuration schematic diagram.
Fig. 2 is the schematic diagram that the axial homogeneous magnetic field of the present invention causes nascent phase gradient distribution, wherein figure a, b and c are respectively
Solidify the schematic diagram that early period, mid-term and the axial homogeneous magnetic field in later stage cause nascent phase gradient distribution.
Fig. 3 has under axial homogeneous magnetic field with comparative example one for the embodiment of the present invention one without the Al-Ni under transverse magnetic field
The metallographic structure photo comparison of Solidification Structure schemes.Wherein figure a is comparative example one without the solidification under axial homogeneous magnetic field
The longitudinal section of tissue, figure b, c and d be respectively embodiment one in the axial homogeneous magnetic field of 0.5T, 1T and 3T solidified structure it is vertical
Section.
Fig. 4 has under axial homogeneous magnetic field with comparative example two for the embodiment of the present invention two without the Al-Cu under transverse magnetic field
The metallographic structure photo comparison of Solidification Structure schemes.Wherein figure a is comparative example two without the solidification under axial homogeneous magnetic field
The longitudinal section of tissue, figure b, c and d are that the vertical of solidified structure in 0.5T, 1T and 3T axial direction homogeneous magnetic field of embodiment two cuts respectively
Face.
Specific implementation mode
Said program is described further below in conjunction with specific examples of the implementation, the preferred embodiment of the present invention is described in detail such as
Under：
Embodiment one
In the present embodiment, referring to Fig.1, a kind of device for directionally solidifying prepares functionally gradient material using axial homogeneous magnetic field
Material, device for directionally solidifying are situated between by protective atmosphere input pipe, water cooled furnace body 1, heating furnace 2, temperature-detecting device, quenching bath 8, heat preservation
Matter 5, thermal insulation layer 6, corundum crucible 3 and pull rod 9 form, and the internal layer furnace wall of the heating furnace 2 is made of nonmagnetic stainless steel,
2 inner cavity maximum temperature of the heating furnace is 1600 DEG C；The temperature-detecting device uses double platinum rhodium type thermocouple, measures institute in real time
State 2 furnace chamber temperature of heating furnace；The quenching bath 8 is set to the lower section of the heating furnace 2, and will be heated by the thermal insulation layer 6
2 bottom of stove is separated with quenching bath 8, and the water cooled furnace body 1 is mounted on the outside of the heating furnace 2, the temperature-detecting device
The temperature in the heating furnace 2 is detected in real time, alloy bar 4 is encapsulated in the corundum crucible 3, then by the corundum crucible 3
It is fixedly connected on the upper end of the pull rod 9 vertically, the protective atmosphere input pipe is passed through indifferent gas from 2 bottom end of the heating furnace
Body makes the alloy bar 4 be under inert gas shielding atmosphere；The axial magnetic field generated using superconduction kicker magnet device 7, will determine
It is put into axial homogeneous magnetic field to coagulation system, the magnetic field intensity near magnetic field center continuously may be used in the range of no more than 5T
It adjusts；Under the primary condition for being oriented solidification, first the corundum crucible 3 is set in heating furnace 2, in the corundum crucible
The alloy bar 4 in 3 melts under the heat effect of the heating furnace 2, forms metal bath, then fixed by controlling
To the pull system of solidification, with the 9 downward vertical shift of drawing velocity drawing pull bar of setting, to drive corundum crucible 3 to enter
Quenching bath 8 makes the metal bath in corundum crucible 3 be oriented solidification upwards since bottom；Heating furnace 2 is adjusted in magnetic simultaneously
Position in, makes the freezing interface of the metal bath in corundum crucible 3 be maintained at homogeneous magnetic field area；By controlling directional solidification
Pull system pull rod 9 with the drawing velocity of setting, so that the corundum crucible 3 is moved straight down, the superconduction kicker magnet
The direction for the magnetic field intensity B that device 7 generates is parallel with directional solidification direction, and in directional solidification process, the alloy bar 4
Solid/liquid interfaces be in the homogeneous magnetic field region that the superconduction kicker magnet device 7 generates.
In the present embodiment, referring to Fig.1~Fig. 3, the method for preparing functionally graded material using axial homogeneous magnetic field, is making
When standby Al-Ni alloy functionally graded material, include the following steps：
A. prepared by raw material：
It selects purity for 99.99% high pure metal raw material, is configured to be divided into the alloy of Al-12wt.%Ni, it is outstanding in vacuum
Melt back in floating stove, after making Al-Ni alloy raw material full and uniformization, negative pressure suction is carried out by Al-Ni alloy melts with quartz ampoule
Casting, obtains the uniform Al-Ni alloy bars of ingredient, and obtained Al-Ni alloy bars are encapsulated in corundum crucible, spare；
B. apparatus for directional solidification is installed：
Device for directionally solidifying is put into axial homogeneous magnetic field, the magnetic field intensity near magnetic field center is in the model no more than 5T
It encloses interior continuously adjustable, the original Al-Ni alloy bars prepared in step a is surface-treated clean, is packed into the corundum of corresponding size
In crucible, corundum crucible is fixed on to the pull rod upper end of directional solidification, corundum crucible moves up and down in heating furnace with pull rod, leads to
The pull system for crossing control directional solidification is oriented solidification with the drawing velocity set, and directional solidification is oriented parallel to axial direction
The direction in magnetic field, while position of the heating furnace in magnetic field is adjusted, after alloy melts in corundum crucible, make in corundum crucible
The freezing interface of Al-Ni alloys is maintained at homogeneous magnetic field area；
C. prepared by functionally graded material：
After fixing the apparatus for directional solidification being arranged in the step b, inert gas argon gas work is passed through into heating furnace
For protective gas, then start heating device, heats up according to the preset heating speed of 10 DEG C/min, be raised to 800 DEG C
After specified temperature, it is then turned on field generator for magnetic, respectively under the action of the magnetic field in 0.5T, 1T and 3T, at 30 minutes
So that virgin alloy stick in corundum crucible is melted the metal bath for forming homogenization completely afterwards, is then turned on directional solidification pull system
System, solidification is oriented according to the withdrawing rate of 10 μm/s, until all pulls of the alloy melt in corundum crucible are to equipped with Ga-
In-Sn is cooled down in the quenching bath of medium, and the alloy bar of directional solidification is then taken out from quenching bath to get to Al-Ni alloy work(
It can functionally gradient material (FGM).Functionally graded material prepared by the present embodiment be a kind of top be eutectic, lower part is primary phase and eutectic phase
Rodlike functionally graded material, as shown in Figure 3.
Referring to Fig. 2, Fig. 2 is the schematic diagram that the axial homogeneous magnetic field of the embodiment of the present invention one causes nascent phase gradient distribution,
Middle figure a, b and c are respectively the schematic diagram for solidifying early period, mid-term and the axial homogeneous magnetic field in later stage and causing nascent phase gradient distribution.
For the present embodiment under the action of axial homogeneous magnetic field, the thermoelectricity magnetic current of radial rotary is dynamic to cause circulation, as shown in Figure 2.Due to closing
The content of precipitated phase increases the presence with temperature gradient in directional solidification process with the decline of temperature in golden melt, and melt passes through
When at low temperature, the phase fast-growth for being conducive to the precipitation of precipitated phase and being precipitated, it is more than the conjunction to lead to precipitate volume fraction
The volume fraction of precipitated phase when golden equilibrium freezing, with the progress of directional solidification, solutes content is reduced in remainder melt, or even is become
It at lean solute melt, is finally solidified with the ingredient of eutectic alloy, forms that a kind of top is eutectic structure, lower part is primary phase and altogether
The functionally graded material of crystalline substance tissue.Since thermoelectricity magnetic force includes the Lorentz force that thermocurrent generates and the Lip river that induced field current generates
Lun Zili, the latter play a major role when melt flows intensity is larger, so the thermoelectricity magnetic current in melt is also first to increase to subtract afterwards
Small, under the action of axial homogeneous magnetic field, the thermoelectricity magnetic current of radial rotary is dynamic to cause circulation to be also first to increase to reduce afterwards, therefore can
To control the gradient of functionally gradient material (FGM) by adjusting the size of magnetic field intensity, the functionally gradient material with different gradients is prepared
Material.
Embodiment two
The present embodiment and embodiment one are essentially identical, are particular in that：
In the present embodiment, a method of preparing functionally graded material using axial homogeneous magnetic field, the orientation of use is solidifying
It is fixedly mounted with and sets identical as embodiment one, when preparing made of Al-Cu alloy functionally graded material, include the following steps：
A. prepared by raw material：
It selects purity for 99.99% high pure metal raw material, is configured to be divided into the alloy of Al-40wt.%Cu, it is outstanding in vacuum
Melt back in floating stove, makes made of Al-Cu alloy raw material full and uniformization, and made of Al-Cu alloy melt is carried out negative pressure with quartz ampoule inhales casting,
The uniform made of Al-Cu alloy stick of ingredient is obtained, and obtained made of Al-Cu alloy stick is encapsulated in corundum crucible, it is spare；
B. apparatus for directional solidification is installed：
Device for directionally solidifying is put into axial homogeneous magnetic field, the magnetic field intensity near magnetic field center is in the model no more than 5T
It encloses interior continuously adjustable, the original made of Al-Cu alloy stick prepared in step a is surface-treated clean, is packed into the corundum of corresponding size
In crucible, corundum crucible is fixed on to the pull rod upper end of directional solidification, corundum crucible moves up and down in heating furnace with pull rod, leads to
The pull system for crossing control directional solidification is oriented solidification with the drawing velocity set, and directional solidification is oriented parallel to axial direction
The direction in magnetic field, while position of the heating furnace in magnetic field is adjusted, after alloy melts in corundum crucible, make in corundum crucible
The freezing interface of made of Al-Cu alloy is maintained at homogeneous magnetic field area；
C. prepared by functionally graded material：
After fixing the apparatus for directional solidification being arranged in the step b, inert gas argon gas work is passed through into heating furnace
For protective gas, then start heating device, heats up according to for the preset heating speed of 10 DEG C/min, be raised to 800 DEG C
Specified temperature after, field generator for magnetic is then turned on, respectively under the action of the magnetic field in 0.5T, 1T and 3T, at 30 points
So that virgin alloy stick in corundum crucible is melted the metal bath for forming homogenization completely after clock, is then turned on directional solidification pull system
System, solidification is oriented according to the withdrawing rate of 10 μm/s, until all pulls of the alloy melt in corundum crucible are to equipped with Ga-
In-Sn is cooled down in the quenching bath of medium, and the alloy bar of directional solidification is then taken out from quenching bath to get to made of Al-Cu alloy work(
Can functionally gradient material (FGM), the functionally graded material prepared by the present embodiment be a kind of top be eutectic, lower part is primary phase and eutectic phase
Rodlike functionally graded material, as shown in Figure 4.
Comparative example one：
Referring to Fig. 3, it is oriented solidification under without axial homogeneous magnetic field and prepares Al-Ni alloy materials, includes the following steps：
A. it selects purity for 99.99% high pure metal Al and Ni, is configured to be divided into the alloy of Al-12wt.%Ni, true
Melting in empty shower furnace prepares the Al-Ni raw materials for waiting for directional solidification；
B. device for directionally solidifying uses typical Bridgman devices, is oriented to the Al-Ni prepared in above-mentioned steps a solidifying
Guyuan material is oriented solidification, obtains the alloy directionally solidified tissues of Al-Ni.
Comparative example two：
Referring to Fig. 4, it is oriented solidification under without axial homogeneous magnetic field and prepares made of Al-Cu alloy material, includes the following steps：
A. it selects purity for 99.99% high pure metal Al and Cu, is configured to be divided into the alloy of Al-40wt.%Cu, true
Melting in empty shower furnace prepares the Al-Cu raw materials for waiting for directional solidification；
B. device for directionally solidifying uses typical Bridgman devices, is oriented to the Al-Cu prepared in above-mentioned steps a solidifying
Guyuan material is oriented solidification, obtains made of Al-Cu alloy oriented freezing organization.
Experimental test and analysis：
Referring to Fig. 3 and Fig. 4, Fig. 3 has under axial homogeneous magnetic field with comparative example one for the embodiment of the present invention one without transverse direction
The metallographic structure photo comparison of Al-Ni Solidification Structures under magnetic field schemes.Wherein figure a is comparative example one without axial permanent
The longitudinal section of solidified structure under magnetic field, figure b, c and d are embodiment one respectively in the axial homogeneous magnetic field of 0.5T, 1T and 3T
The longitudinal section of solidified structure.Fig. 4 has under axial homogeneous magnetic field with comparative example two for the embodiment of the present invention two without transverse magnetic field
Under made of Al-Cu alloy solidified structure metallographic structure photo comparison figure.Wherein figure a is comparative example two without axial homogeneous magnetic field
Under solidified structure longitudinal section, figure b, c and d be the solidification group in 0.5T, 1T and 3T axial direction homogeneous magnetic field of embodiment two respectively
The longitudinal section knitted.
The directional solidification sample obtained by above-described embodiment and comparative example is symmetrically cut along longitudinal direction respectively, obtains tissues observed
Longitudinal section sample, after inlaying samples, metallographic structure is observed by grinding, polishing post-etching.Fig. 3 and Fig. 4 is respectively above-mentioned two
The comparison of the oriented freezing organization of a embodiment and two comparative examples, reflects the solidified structure before and after applying axial homogeneous magnetic field
Pattern compares.B-0.5T, figure c-1T in figure and figure d-3T, it can be seen that with the increase of magnetic field intensity, functionally gradient material
The gradient of material first increases to be reduced afterwards.
The dynamic circulation (circulation) and paste induced of thermoelectricity magnetic current when applying axial homogeneous magnetic field is shown in Fig. 2
Section length and the temperature (T) and solute (C in solid/liquid interfaces forward positioni) variation.Due to precipitated phase in alloy melt content with
The decline of temperature and increase the presence with temperature gradient in directional solidification process, when melt is by low temperature, be conducive to precipitated phase
Precipitation and the phase fast-growth that has been precipitated, the body of precipitated phase when precipitate volume fraction being caused to be more than the alloy equilibrium freezing
Fraction, with the progress of directional solidification, solutes content is reduced in remainder melt, or even becomes lean solute melt, while paste
Section length is gradually shortened and is disappeared with directional solidification process, is finally solidified with the ingredient of eutectic alloy, is formed a kind of
The functionally graded material that top is eutectic structure, lower part is primary phase and eutectic structure.
Above-described embodiment is solidifying in orientation using the nascent Seebeck effects existing between solid phase and liquid phase of directional solidification process
Gu process applies axial homogeneous magnetic field, generate that thermoelectricity magnetic current is dynamic, due to precipitated phase in alloy melt content with temperature decline
And increase and directional solidification process in temperature gradient presence, when melt is by low temperature, be conducive to the precipitation and of precipitated phase
Phase fast-growth through precipitation, the volume fraction of precipitated phase when precipitate volume fraction being caused to be more than the alloy equilibrium freezing, with
The progress of directional solidification, solutes content is reduced in remainder melt, or even becomes lean solute melt, finally with eutectic alloy at
Fractional condensation is solid, formed a kind of top be eutectic structure, the functionally graded material that lower part is primary phase and eutectic structure.
Embodiment three
The present embodiment is substantially the same as in the previous example, and is particular in that：
In the present embodiment, by controlling the size of magnetic field intensity, phase constitution is come into being prepared by adjust directional solidification
Material be longitudinally formed gradient distribution gradient magnitude.
As embodiment one and embodiment two it is found that respectively by the directional solidification sample obtained by embodiment one and embodiment two
It is symmetrical along longitudinal direction to cut, the longitudinal section sample of tissues observed is obtained, after inlaying samples, by grinding, polishing post-etching observation gold
Phase constitution.Fig. 3 and Fig. 4 is respectively the oriented freezing organization comparison of embodiment one and embodiment two, is reflected axial equal in application
Solidification Microstructure Morphology comparison before and after Constant charge soil.B-0.5T, figure c-1T in figure and figure d-3T, it can be seen that with magnetic field
The increase of intensity, the gradient of functionally graded material first increases to be reduced afterwards.Thus, the present embodiment is by controlling the big of magnetic field intensity
It is small, phase constitution is come into being along the gradient magnitude for being longitudinally formed gradient distribution of prepared material to adjust directional solidification, prepares symbol
The functionally graded material of functional requirement is closed, realizes the diversification for preparing functionally graded material；It is real simultaneously by considering energy factor
The energy-saving functionally graded material for meeting functional requirement is prepared compared with the condition of low energy expenditure now.The present embodiment can be into row metal
Orientation metal solidification texture control can be better achieved in the preparation of functional gradient composite materials in situ.
Shown in sum up, the above embodiment of the present invention prepares the method and dress of functionally graded material using axial homogeneous magnetic field
It sets, device is by heating furnace, thermal insulation medium, thermal insulation layer, water cooled furnace body, pull rod, system for detecting temperature, superconduction gradient strong magnetic body and quenches
Fiery pond composition, the magnetic field intensity ranging from 0-5T for the axial magnetic field that superconduction gradient strong magnetic body generates.The above embodiment of the present invention profit
With the thermoelectricity magneticaction of Magnetic Field-Induced on alloy melt, generate that thermoelectricity magnetic current is dynamic, since precipitated phase contains in alloy melt
Amount increases the presence with temperature gradient in directional solidification process with the decline of temperature and is conducive to analyse when melt is by low temperature
The phase fast-growth for going out the precipitation of phase and being precipitated, precipitated phase when precipitate volume fraction being caused to be more than the alloy equilibrium freezing
Volume fraction, with the progress of directional solidification, solutes content is reduced in remainder melt, or even becomes lean solute melt, finally
It is solidified with the ingredient of eutectic alloy, forms that a kind of top is eutectic, lower part is primary phase and the functionally graded material of eutectic phase, be
It prepares functionally graded material and provides a kind of completely new technology, also provided to carry out special material preparation using axial homogeneous magnetic field
New process orientation.
Combination attached drawing of the embodiment of the present invention is illustrated above, but the present invention is not limited to the above embodiments, it can be with
The purpose of innovation and creation according to the present invention makes a variety of variations, under the Spirit Essence and principle of all technical solutions according to the present invention
Change, modification, replacement, combination or the simplification made, should be equivalent substitute mode, as long as meeting the goal of the invention of the present invention,
Without departing from the present invention method of functionally graded material and its technology of device for directionally solidifying are prepared using axial homogeneous magnetic field
Principle and inventive concept, belong to protection scope of the present invention.
Claims (10)
1. a kind of method preparing functionally graded material using axial homogeneous magnetic field, which is characterized in that include the following steps：
A. prepared by raw material：
According to the alloying component of functionally graded material to be prepared, simple metal is chosen as raw material, in vacuum induction shower furnace
Melt back is carried out, its homogenization of composition is made, alloy melt is then carried out negative pressure with quartz ampoule inhales casting, and it is uniform to obtain ingredient
Virgin alloy stick；
B. apparatus for directional solidification is installed：
Device for directionally solidifying is put into axial homogeneous magnetic field, the magnetic field intensity near magnetic field center is in the range of no more than 5T
It is continuously adjustable, the virgin alloy stick prepared in step a is surface-treated totally, is fitted into the corundum crucible of corresponding size, it will
Corundum crucible is fixed on the pull rod upper end of directional solidification, and corundum crucible moves up and down in heating furnace with pull rod, fixed by controlling
Solidification, the side for being oriented parallel to axial magnetic field of directional solidification are oriented with the drawing velocity set to the pull system of solidification
To, while position of the heating furnace in magnetic field is adjusted, after alloy melts in corundum crucible, make the solidification of alloy in corundum crucible
Interface is maintained at homogeneous magnetic field area；
C. prepared by functionally graded material：
After fixing the apparatus for directional solidification being arranged in the step b, inert gas is passed through into heating furnace as protection gas
Then body starts heating device, heat up, be raised to not higher than 1600 according to the preset heating speed no more than 10 DEG C/min
DEG C specified temperature after, be then turned on field generator for magnetic, under the influence of a magnetic field, and make corundum earthenware after at least 30 minutes
Virgin alloy stick melts the metal bath for forming homogenization completely in crucible, directional solidification pull system is then turned on, according to not high
It is oriented solidification in the withdrawing rate of 20 μm/s, until all pulls of the alloy melt in corundum crucible are to equipped with cooling medium
In quenching bath, the alloy bar of directional solidification is then taken out from quenching bath to get to functionally graded material.
2. the method for preparing functionally graded material using axial homogeneous magnetic field according to claim 1, it is characterised in that：It is made
Standby functionally graded material is aluminium alloy, and the mass percentage content of aluminium is not higher than 88wt.% in aluminium alloy.
3. the method for preparing functionally graded material using axial homogeneous magnetic field according to claim 2 is preparing Al-Ni alloys
When functionally graded material, which is characterized in that include the following steps：
A. prepared by raw material：
It selects purity for 99.99% high pure metal raw material, is configured to be divided into the alloy of Al-12wt.%Ni, in vacuum suspension stove
Al-Ni alloy melts after making Al-Ni alloy raw material full and uniformization, are carried out negative pressure with quartz ampoule and inhale casting, obtained by interior melt back
It is encapsulated in corundum crucible to the uniform Al-Ni alloy bars of ingredient, and by obtained Al-Ni alloy bars, it is spare；
B. apparatus for directional solidification is installed：
Device for directionally solidifying is put into axial homogeneous magnetic field, the magnetic field intensity near magnetic field center is in the range of no more than 5T
It is continuously adjustable, the original Al-Ni alloy bars prepared in step a are surface-treated totally, the corundum crucible of corresponding size is packed into
In, corundum crucible is fixed on to the pull rod upper end of directional solidification, corundum crucible moves up and down in heating furnace with pull rod, passes through control
The pull system of directional solidification processed is oriented solidification with the drawing velocity set, and directional solidification is oriented parallel to axial magnetic field
Direction, while adjusting position of the heating furnace in magnetic field, after alloy melts in corundum crucible, make Al-Ni in corundum crucible
The freezing interface of alloy is maintained at homogeneous magnetic field area；
C. prepared by functionally graded material：
After fixing the apparatus for directional solidification being arranged in the step b, inert gas is passed through into heating furnace as protection gas
Then body starts heating device, heat up, be raised to not less than 800 according to the preset heating speed no more than 10 DEG C/min
DEG C specified temperature after, be then turned on field generator for magnetic, under the influence of a magnetic field, and make corundum earthenware after at least 30 minutes
Virgin alloy stick melts the metal bath for forming homogenization completely in crucible, directional solidification pull system is then turned on, according to not high
It is oriented solidification in the withdrawing rate of 10 μm/s, until all pulls of the alloy melt in corundum crucible are to equipped with cooling medium
In quenching bath, the alloy bar of directional solidification is then taken out from quenching bath to get to Al-Ni alloy functionally graded material.
4. the method for preparing functionally graded material using axial homogeneous magnetic field according to claim 2 is preparing made of Al-Cu alloy
When functionally graded material, which is characterized in that include the following steps：
A. prepared by raw material：
It selects purity for 99.99% high pure metal raw material, is configured to be divided into the alloy of Al-40wt.%Cu, in vacuum suspension stove
Interior melt back makes made of Al-Cu alloy raw material full and uniformization, and made of Al-Cu alloy melt is carried out negative pressure with quartz ampoule inhales casting, obtains
The uniform made of Al-Cu alloy stick of ingredient, and obtained made of Al-Cu alloy stick is encapsulated in corundum crucible, it is spare；
B. apparatus for directional solidification is installed：
Device for directionally solidifying is put into axial homogeneous magnetic field, the magnetic field intensity near magnetic field center is in the range of no more than 5T
It is continuously adjustable, the original made of Al-Cu alloy stick prepared in step a is surface-treated totally, the corundum crucible of corresponding size is packed into
In, corundum crucible is fixed on to the pull rod upper end of directional solidification, corundum crucible moves up and down in heating furnace with pull rod, passes through control
The pull system of directional solidification processed is oriented solidification with the drawing velocity set, and directional solidification is oriented parallel to axial magnetic field
Direction, while adjusting position of the heating furnace in magnetic field, after alloy melts in corundum crucible, make Al-Cu in corundum crucible
The freezing interface of alloy is maintained at homogeneous magnetic field area；
C. prepared by functionally graded material：
After fixing the apparatus for directional solidification being arranged in the step b, inert gas is passed through into heating furnace as protection gas
Then body starts heating device, heat up, be raised to not less than 800 according to the preset heating speed no more than 10 DEG C/min
DEG C specified temperature after, be then turned on field generator for magnetic, under the influence of a magnetic field, and make corundum earthenware after at least 30 minutes
Virgin alloy stick melts the metal bath for forming homogenization completely in crucible, directional solidification pull system is then turned on, according to not high
It is oriented solidification in the withdrawing rate of 10 μm/s, until all pulls of the alloy melt in corundum crucible are to equipped with cooling medium
In quenching bath, the alloy bar of directional solidification is then taken out from quenching bath to get to made of Al-Cu alloy functionally graded material.
5. according to any one of Claims 1 to 4 method for preparing functionally graded material using axial homogeneous magnetic field,
It is characterized in that：In the step c, by controlling the size of magnetic field intensity, phase constitution is come into being along made to adjust directional solidification
The gradient magnitude for being longitudinally formed gradient distribution of standby material.
6. according to any one of Claims 1 to 4 method for preparing functionally graded material using axial homogeneous magnetic field,
It is characterized in that：In the step c, argon gas is passed through into heating furnace as protective gas；Or the cooling medium in quenching bath
Using Ga-In-Sn.
7. according to any one of Claims 1 to 4 method for preparing functionally graded material using axial homogeneous magnetic field,
It is characterized in that：In the step c, prepared functionally graded material be a kind of top be eutectic, lower part is primary phase and altogether
The rodlike functionally graded material of crystalline phase.
8. a kind of directional solidification for implementing to be prepared the method for functionally graded material using axial homogeneous magnetic field described in claim 1 is filled
Set, by protective atmosphere input pipe, water cooled furnace body (1), heating furnace (2), temperature-detecting device, quenching bath (8), thermal insulation medium (5),
Thermal insulation layer (6), corundum crucible (3) and pull rod (9) composition, the quenching bath (8) are set to the lower section of the heating furnace (2),
And separated heating furnace (2) bottom and quenching bath (8) by the thermal insulation layer (6), the water cooled furnace body (1) is mounted on described add
The outside of hot stove (2), the temperature-detecting device detect the temperature in the heating furnace (2) in real time, and alloy bar (4) is encapsulated in
The corundum crucible (3) is interior, then the corundum crucible (3) is fixedly connected on to the upper end of the pull rod (9), the protection vertically
Atmosphere input pipe is passed through inert gas from the heating furnace (2) bottom end, and the alloy bar (4) is made to be in inert gas shielding atmosphere
Under, it is characterised in that：
The axial magnetic field generated using superconduction kicker magnet device (7), device for directionally solidifying is put into axial homogeneous magnetic field, magnetic field
The magnetic field intensity of immediate vicinity is continuously adjusted in the range of no more than 5T；Under the primary condition for being oriented solidification, first will
The corundum crucible (3) is set in heating furnace (2), and the alloy bar (4) in the corundum crucible (3) is in the heating
It is melted under the heat effect of stove (2), forms metal bath, then by controlling the pull system of directional solidification, with setting
Drawing velocity drawing pull bar (9) downward vertical shift, to drive corundum crucible (3) enter quenching bath (8), make corundum crucible
(3) metal bath in is oriented solidification upwards since bottom；Position of the heating furnace (2) in magnetic field is adjusted simultaneously, is made
The freezing interface of metal bath in corundum crucible (3) is maintained at homogeneous magnetic field area；By the pull system for controlling directional solidification
Pull rod (9) with the drawing velocity of setting, so that the corundum crucible (3) is moved straight down, the superconduction kicker magnet device (7)
The direction of the magnetic field intensity B of generation is parallel with directional solidification direction, and in directional solidification process, the alloy bar (4)
Solid/liquid interfaces are in the homogeneous magnetic field region that the superconduction kicker magnet device (7) generates.
9. device for directionally solidifying according to claim 8, it is characterised in that：The internal layer furnace wall of the heating furnace (2) uses nothing
Magnetic stainless steel makes, and heating furnace (2) inner cavity maximum temperature is 1600 DEG C.
10. device for directionally solidifying according to claim 8, it is characterised in that：The temperature-detecting device uses double platinum rhodium type
Thermocouple measures the heating furnace (2) furnace chamber temperature in real time.
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