CN105543952B - A kind of Rapid Directional Solidification equipment and Rapid Directional Solidification method - Google Patents
A kind of Rapid Directional Solidification equipment and Rapid Directional Solidification method Download PDFInfo
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- CN105543952B CN105543952B CN201511001423.6A CN201511001423A CN105543952B CN 105543952 B CN105543952 B CN 105543952B CN 201511001423 A CN201511001423 A CN 201511001423A CN 105543952 B CN105543952 B CN 105543952B
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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
- C30B29/52—Alloys
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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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
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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
Abstract
The present invention provides a kind of Rapid Directional Solidification equipment and Rapid Directional Solidification method.Rapid Directional Solidification equipment includes vacuum chamber, electron beam launcher, the first pull system, the first cooling system, second pull system and the second cooling system, wherein the first pull system includes hollow and can lifted and the first pumping rod of rotation and the cooling tube being arranged on inside the first pumping rod；First cooling system includes inner chamber and exocoel, and inner chamber, which is enclosed, to be located at outside the first pumping rod, and exocoel, which encloses, is located at lumen outer；Second pull system includes that the second pumping rod with rotation can be lifted；The second cooling system is arranged on above the first cooling system and gap is formed between the first cooling system, and the electron beam of electron beam launcher transmitting can pass through from the gap.The Rapid Directional Solidification equipment can realize up to 5 × 105K/s cooling velocity, monocrystalline and orientation polycrystalline material with Rapid Directional Solidification tissue can be prepared using the Rapid Directional Solidification equipment.
Description
Technical field
The present invention relates to a kind of apparatus for directional solidification, and in particular to a kind of Rapid Directional Solidification equipment and Rapid Directional Solidification
Method.
Background technology
Solidification is that nature material is changed into the most common phenomenon of solid-state, and material, particularly metal material system from liquid
Standby basic process, the progress of solidification science and solidification technology promote human material's science to advance.Traditional solidification reason
Mainly carried out by the research with technology around the casting process of common casting and ingot casting, with carrying for modern solidification theory
Go out, solidification science obtains impressive progress：As the generation of continuously casting technology, directional solidification and Crystal Growth Technique it is perfect,
Appearance and application of flash set technology etc..Make a general survey of solidification the reach of science it is seen that, so-called modern solidification theory, be exactly
Study " process control of the people for material solidification behavior " and " nonequilibrium solidification process and nonequilibrium effect ".
For many years, on modern solidification theory, researcher makes substantial amounts of work, obtains many fruitful researchs
Achievement, mainly include：1. in terms of process of setting is controlled, researcher proposes the theoretical model of directional solidification, that is, is balancing
Compulsive means are used in process of setting, the thermograde of specific direction is established in frozen metal and molten metal, so that molten
Body solidifies along the direction opposite with hot-fluid, finally gives the column crystal with specific orientation, monocrystal material.Directional solidification is one
The important material preparation technology of kind, it is widely used in obtaining in the new material with particular orientation tissue and excellent properties.
2. in terms of nonequilibrium solidification process and nonequilibrium effect, researcher proposes a variety of theoretical models to predict material remote
A variety of solidification behaviors during poised state, this field turn into the academic focus for solidifying science in recent years.With solidification cooling speed
The increasing of rate and degree of supercooling, process of setting deviate the degree aggravation of balance.Alloy melt viscosity, diffusion coefficient, solid liquid interface are molten
The physical parameters such as matter distribution coefficient and forming core, grow up, Interface morphology evolution process etc. deviates balance, and then influence mutually to select
Select, organizational choice, structure choice, cause structure refinement, form crystallite, nanocrystalline, metastable phase, quasi-crystalline substance, amorphous etc..
With the development that nonequilibrium freezing is theoretical, researcher develops various nonequilibrium freezing technologies and prepared
Go out many new materials.So-called non-equilibrium material, i.e., material structure is under conditions of use away from thermodynamic equilibrium state；From heating power
Learn angle and see and exactly deviate thermodynamic equilibrium point, in a kind of unsure state；This kind of material generally has balancing material institute
Without metastable organization and many excellent properties.Nonequilibrium freezing technology mainly has two major classes：First, dynamics rapid cooling, passes through urgency
Cold suppression forming core, representing technique has gas atomization, aluminium alloy stream injection coolant method, single roller to revolve pure method etc., due to being conducted heat
Limitation, such method can not obtain rapid solidification structure in large volume liquid metal, can only prepare powdery, filament and band
Deng low-dimensional materials.Second, thermodynamics rapid cooling, suppresses forming core, representing technique has droplet distribution method, is circulated throughout by improving degree of supercooling
Hot method, glass melt method etc., because degree of supercooling is lifted, limited, solid liquid interface fltting speed is slow, and material prepared by such method is fast
The solid uneven microstructure of rapid hardening, performance are bad.
The high-performance Asia with rapid solidification structure can not be prepared in order to solve directional solidification processes under equilibrium condition simultaneously
Under steady phase material and non-equilibrium condition fast solidification technology can not prepare both high-performance block materials with specific orientation it
Between contradiction, inventors herein propose the concept of Rapid Directional Solidification, i.e., realize material under the conditions of the nonequilibrium freezing quickly solidified
The oriented growth of material, to prepare the block materials with rapid solidification structure and specific orientation.
The A of Chinese patent CN 102051668 disclose a kind of thermograde as 105K/cm device for directionally solidifying and orientation
Clotting method, the patent use laser, as cooling medium, to realize material in 200- as heating source, gallium-indium-tin alloy
Magnetostrictive properties under 1400W power, the 1-300 μm/s speeds of growth.The device and method can reach 105K/cm temperature ladder
Degree, but growth rate is relatively low (only up to 0.3mm/s), the device and method is caused to be different from device that inventor proposes and fast
Fast directional freeze method.
Zhang Jun, Cui Chunjuan of solidification technology National Key Laboratory of Northwestern Polytechnical University et al. utilize electron-beam floating zone melting
Directional solidification is prepared for Si/TaSi2The spontaneous compound field emmision material of eutectic, the electron-beam floating zone melting apparatus for directional solidification is by moral
Leybold-Heraeus companies of state produce, operating current 0-500mA, operating voltage 0-20kV, are mainly used in processing diameter
For 2-10mm, length is not more than 200mm metal bar, and achieved thermograde is only 350-500K/cm, drawing velocity
(speed of growth) is up to 0.38mm/s, and zone length reaches 8-10mm, and whole directional solidification process is in relatively low temperature
The nearly balance directional solidification carried out under gradient and the relatively low speed of growth, therefore the apparatus and method are also differ completely from inventor
The remote balance Rapid Directional Solidification device and Rapid Directional Solidification method proposed.
The content of the invention
The present invention provides a kind of Rapid Directional Solidification equipment and Rapid Directional Solidification method, for solving existing directional solidification
Technology irrealizable ultra high temperature gradient and fast-growth and quick solidification institute irrealizable slewing grow
Problem, the material obtained are the monocrystalline and orientation polycrystalline material for having Rapid Directional Solidification tissue.
The present invention provides a kind of Rapid Directional Solidification equipment, including vacuum chamber, electron beam launcher, the first pull system
System, the first cooling system, the second pull system and the second cooling system,
Bottom through-hole and top through hole are offered relatively at the bottom of the vacuum chamber and top, in the vacuum chamber
Electron beam window is offered in portion's side wall；
The electron beam launcher is arranged on the outside of the vacuum chamber, and electron beam launcher transmitting
Electron beam can enter the vacuum chamber by the electron beam window；
The first pull system includes the first pumping rod and cooling tube, and first pumping rod is hollow and by described
Bottom through-hole plugs into the vacuum chamber vertically, and first pumping rod is driven by motor and can be lifted and transport certainly
Dynamic, the cooling tube is arranged on inside first pumping rod；
First cooling system is located at the internal vacuum chamber, and it includes inner chamber and exocoel, and the inner chamber, which is enclosed, is located at institute
State outside the first pumping rod, the exocoel, which encloses, is located at the lumen outer；
The second pull system includes the second pumping rod, and second pumping rod is plugged vertically by the top through hole
Into the vacuum chamber, second pumping rod is driven by motor and can be lifted and be transported certainly with first pumping rod
The identical or opposite spinning motion in dynamic direction；
The second cooling system is arranged on above first cooling system and the shape between first cooling system
Into gap, the second cooling system has the through hole being coaxially disposed with first pumping rod and can be pointed to described logical
Material in hole is cooled down, and the electron beam of the electron beam launcher transmitting can pass through from the gap.
The Rapid Directional Solidification equipment of the present invention is by setting electron beam launcher, so as to be used as heating source using electron beam
Solidification is oriented, beam energy density is big, the efficiency of heating surface is high, utilizes the beam bombardment metal focused on through multistage magnetic lenses
Material surface, moment kinetic energy can be passed into metal material, the kinetic energy, which is converted into interior energy, makes metal melt rapidly；It is meanwhile high
Fast incident electronics makes a part of material of metal material surface rapidly after fusing, using reaction force by molten metal liquid
Body arranges to surrounding, and so as to expose new material surface, electron beam continues to act on new material surface, so as to advantageously form
Narrow and deep melting zone, melting zone width are smaller than 1mm, and the efficiency of heating surface reaches more than 95%.
Also, in order to adapt to the larger electron beam heating of energy density, Rapid Directional Solidification equipment of the invention is set
First cooling system and the second cooling system, and cooling tube is set in the first pumping rod of the first pull system, carrying out
During directional solidification, liquid metal is loaded to the inner chamber of the first cooling system, loads coolant to exocoel, and spray using cooling tube
Penetrate high-pressure coolant；Meanwhile the second cooling system cools down to synchronous material, the cooling effect of apparatus for directional solidification is improved,
By melting zone control in the first cooling system and the gap location of the second cooling system, make can still to keep in high speed draw process compared with
High and stable thermograde.
It can be lifted respectively and the first pull system of rotation and the in addition, the Rapid Directional Solidification equipment of the present invention is set
Two pull systems, it is respectively used to clamp seed crystal respectively and treats the material (such as foundry alloy rod) of directional solidification, the first pull system
System and the second pull system are independently arranged, so that treating material and the seed crystal separation of directional solidification, are easy to utilize the fast fast-growing of seed crystal
Grow monocrystalline and orientation polycrystalline material；Rotation can be such that solute in directional solidification process distributes evenly, and material microsegregation subtracts
Small, quality is higher.
In the present invention, the voltage of the electron beam launcher can be 80kV, and power can be 10kW, scan frequency
Can be 0-10000Hz；Furthermore, it is possible to electron beam launcher is set to reach predetermined working vacuum degree (such as 3 by mechanical pump
×10-2Pa).In one embodiment, the electron beam launcher is high pressure Pierce electron gun.Further, the electricity
Angle between the electron beam and horizontal plane of the transmitting of beamlet emitter can be -5 ° -5 °；Wherein, by electron beam along the horizontal plane
Turn clockwise and be set to "-", i.e.,：The incident directions of " -5 ° " expression electron beams are 5 ° of the direction of turning clockwise along the horizontal plane.
Above-mentioned electron beam launcher is axially inclined along sample by electron beam incident direction during the oriented growth of material
Turn, by the incident angle for adjusting electron beam, it is possible to achieve to convex, flat, recessed the three of material solid liquid interface during oriented growth
The control of kind interface configuration, so as to adapt to various different demands.Preferably, the electron beam of electron beam launcher transmitting with
Angle between horizontal plane is 3 °, even if electron beam is incident obliquely, it more easily obtains monocrystal material and orientation polycrystalline material
Material.
In the present invention, the velocity interval for the elevating movement made by motor-driven first pumping rod can be 0-
100mm/s, the velocity interval of spinning motion can be 0-6000r/min；The lifting made by motor-driven second pumping rod
The velocity interval of motion can be 0-100mm/s, and the velocity interval of spinning motion can be 0-6000r/min；Further, institute
It can be 1-5mm to state gap.
The present invention can be by controlling the power of electron beam launcher and the lifting speed of each pumping rod and from rotating speed
Degree controls zone length in 1-2mm, preferably 1mm or so, and in directional solidification process, by electron beam heating material institute shape
Into melting zone be strict controlled in the gap location, by controlling material solid liquid interface morphology so as to obtaining required particular organization's knot
Structure.Particularly, the speed for the elevating movement that the first pumping rod and the second pumping rod are made is preferably 1-10mm/s, spinning motion
Speed is preferably 60-6000r/min, and the scope is advantageous to being uniformly distributed for solute in material, reduces microsegregation.
In one embodiment, the second cooling system includes metal tube and encloses the cooling being located at outside the metal tube
Chamber, the through hole of the metal tube are coaxially disposed with first pumping rod, the cooling chamber and the exocoel be equipped with import and
Outlet.In specific application, the cooling mediums such as liquid nitrogen can be loaded into cooling chamber；Further, can also be in the cooling chamber
Inwall set black coating, its high temperature resistant, and be advantageous to improve heat transfer efficiency.The second cooling system can use routine side
Formula is fixed, such as supporting plate is set on the inwall of the vacuum chamber, and supports the second cooling system using the supporting plate.
In one embodiment, in first pumping rod and second pumping rod towards the one of the internal vacuum chamber
End is equipped with chuck.Chuck is used to clamp material, and it can be connected to one end of pumping rod (such as threaded connection) in a usual manner,
Material (such as high-speed coupling) can be held on chuck by conventional methods；And it is possible to fitted according to being actually needed to select
Suitable chuck, so as to the material for preparing size, coming in every shape.Further, the chuck corresponding to the first pumping rod can be copper
Matter, it is advantageous to the conduction of heat.
In the present invention, the vacuum chamber is used to form vacuum environment needed for Rapid Directional Solidification, can pass through mechanical pump
Vacuum chamber is set to reach predetermined working vacuum degree with molecular pump；Simultaneously as it can be produced while high-pressure electronic rifle launching electronics beam
Raw X ray, therefore vacuum chamber need to pass through special radiation proof and handle.
Further, the top plate of the first cooling system inner chamber can be molybdenum plate, and it is inside that it can effectively completely cut off melting zone
The liquid metal radiant heat transfer loaded in chamber, the liquid level of Simultaneous Stabilization liquid metal are close to melting zone lower edge all the time.
The above-mentioned Rapid Directional Solidification equipment of the present invention can realize 1 × 105-5×105K/cm thermograde and 1-
The 100mm/s speed of growth.The material structure prepared using the Rapid Directional Solidification equipment uniformly, crystal grain refinement, orientation it is obvious,
Properties are excellent.
The present invention also provides a kind of Rapid Directional Solidification method, comprises the following steps：
1) foundry alloy rod is prepared：
After component requirements according to unidirectional solidification material are equipped with raw material, the raw material of outfit is smelted into mother alloy ingot, melted
Change the mother alloy ingot, and foundry alloy rod is made by vacuum casting；
2) it is oriented solidification using any of the above-described described Rapid Directional Solidification equipment：
The foundry alloy rod and seed crystal are separately fixed to the second pumping rod and first of the Rapid Directional Solidification equipment
Pull boom end, alloy coolant and circulating cooling liquid are loaded in the inner chamber and exocoel respectively, and make the seed crystal bottom
Alloy coolant is immersed, first pumping rod is reversely rotated with second pumping rod, and start second cooling system
After system, to the vacuum chamber and protective gas is filled with, subsequent start-up electron beam launcher is pointed to the gap
Foundry alloy rod and seed crystal are heated, and the first pumping rod described in pull in the same direction and the second pumping rod are oriented solidification, and control
The thermograde for making the directional solidification is 1 × 105-5×105K/cm, the speed of growth (drawing velocity) are 1-100mm/s, are made
Unidirectional solidification material.
Further, the drawing velocity for controlling first pumping rod is 1-10mm/s, and the speed of spinning motion is 60-
6000r/min；And the drawing velocity for controlling second pumping rod is 1-10mm/s, and the speed of spinning motion is 60-
6000r/min。
The implementation of the present invention, at least has the advantage that：
1st, Rapid Directional Solidification equipment of the invention uses electron beam as heating source, and uses double cooling systems, its energy
It is enough to establish a fixed unidirectional thermograde solid-liquid is alternate, the quick fixed of material is realized by quickly propelling for solid liquid interface
To solidification, wherein thermograde is up to 1 × 105-5×105K/cm, the speed of growth are smaller than up to 1-100mm/s, zone length
1mm Rapid Directional Solidification, it can finally realize the change of material character.
2nd, Rapid Directional Solidification method of the invention is simple to operate, strong adaptability, and it can be prepared coagulates with slewing
Gu the highly oriented non-equilibrium Nonequilibrium Materials of the three-dimensional block of tissue, the crystal structure of the material are arranged along specific crystallographic direction
Row, thermodynamically in metastable state, therefore with the characteristic not available for balancing material.
Brief description of the drawings
Fig. 1 is the structural representation for the apparatus for directional solidification that the embodiment of the present invention 1 provides；
Fig. 2 is the XRD diffracting spectrums for the foundry alloy rod that the embodiment of the present invention 2 provides；
Fig. 3 is the (Fe that the embodiment of the present invention 2 provides0.83Ga0.17)99.9La0.1The vertical profile melting zone fast quenching metallograph of material；
Fig. 4 is the unidirectional solidification material (Fe that the embodiment of the present invention 2 provides0.83Ga0.17)99.9La0.1XRD diffracting spectrums；
Fig. 5 is the unidirectional solidification material (Fe that the embodiment of the present invention 2 provides0.83Ga0.17)99.9La0.1BSE photos；
Fig. 6 is the Magnetostriction curve for the material that the embodiment of the present invention 2 and reference examples 1 provide；
Fig. 7 is the unidirectional solidification material (Mn that the embodiment of the present invention 3 provides54Al46)0.97C0.03Vertical profile melting zone fast quenching metallographic
Figure；
Fig. 8 is the unidirectional solidification material (Mn that the embodiment of the present invention 3 provides54Al46)0.97C0.03Vertical profile metallograph；
Fig. 9 is the unidirectional solidification material (Mn that the embodiment of the present invention 3 provides54Al46)0.97C0.03XRD diffracting spectrums；
Figure 10 is the unidirectional solidification material (Mn that the embodiment of the present invention 3 provides54Al46)0.97C0.03M-H curves；
Figure 11 is (Fe prepared by reference examples 1 of the present invention0.83Ga0.17)99.9La0.1The BSE photos of material；
Figure 12 is (Mn prepared by reference examples 2 of the present invention54Al46)0.97C0.03The XRD diffracting spectrums of material.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, accompanying drawing and implementation below in conjunction with the present invention
Example, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is the present invention
Part of the embodiment, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not having
The every other embodiment obtained under the premise of creative work is made, belongs to the scope of protection of the invention.
Embodiment 1
As shown in figure 1, the Rapid Directional Solidification equipment of the present invention includes vacuum chamber 1, electron beam launcher 2, first takes out
Pull system, the first cooling system, the second pull system and the second cooling system 6, opened up relatively in the bottom of vacuum chamber 1 and top
There are bottom through-hole and top through hole (that is, bottom through-hole is coaxially disposed with top through hole), opened up in the middle part of sliding channel of vacuum chamber 1
There is electron beam window 11；Electron beam launcher 2 is arranged on the outside of vacuum chamber 1, and the electricity that electron beam launcher 2 is launched
Beamlet can enter vacuum chamber 1 by electron beam window 11；First pull system includes the first pumping rod 31 and cooling tube 32, the
One pumping rod 31 is hollow and is plugged vertically into vacuum chamber 1 by bottom through-hole, the first pumping rod 31 driven by motor and
It can lift and spinning motion, cooling tube 32 are arranged on inside the first pumping rod 31；First cooling system is located in vacuum chamber 1
Portion, it includes inner chamber 41 and exocoel 42, and inner chamber 41, which is enclosed, to be located at outside the first pumping rod 31, and exocoel 42, which encloses, to be located at outside inner chamber 41；
Second pull system includes the second pumping rod 51, and the second pumping rod 51 plugs into vacuum chamber 1 (i.e. vertically by top through hole
Two pumping rods 51 and the first pumping rod 31 are coaxially disposed), the second pumping rod 51 is driven by motor and can lifted and with the
The identical or opposite spinning motion in the spinning motion direction of one pumping rod 31；The second cooling system 6 is arranged on the first cooling system
Gap is formed between the cooling systems of Fang Bingyu first, the second cooling system 6 has the through hole being coaxially disposed with the first pumping rod 31
And the material that can be pointed in through hole is cooled down, the electron beam that electron beam launcher 2 is launched can pass through from gap.
In above-mentioned Rapid Directional Solidification equipment, vacuum chamber 1 is used to form vacuum environment needed for directional solidification, its bottom and top
The relative bottom through-hole opened up in portion and top through hole are coaxially disposed, and can reach vacuum chamber 1 by mechanical pump and molecular pump
To predetermined working vacuum degree.
Electron beam launcher 2 is used for launching electronics beam, and it is used as the heating source heated to material, electron beam transmitting
The voltage of device 2 can be 80kV, and power can be 10kW, and scan frequency can be 0-10000Hz；Electron beam launcher 2
Angle between the electron beam and horizontal plane of transmitting (i.e. electron beam incidence, the glancing incidence or oblique obliquely that can be -5 ° -5 °
Lower incidence).Solidification is oriented by the use of electron beam as heating source, beam energy density is big, the efficiency of heating surface is high, more using passing through
The beam bombardment metal material surface that level magnetic lenses focuses on, can pass to metal material moment by kinetic energy, kinetic energy conversion
Metal is set to melt rapidly for interior energy；Meanwhile the electronics of incidence makes a part of material of metal material surface melt rapidly at a high speed
Afterwards, molten metal liquid is arranged to surrounding using reaction force, so as to expose new material surface, electron beam continues to act on
In new material surface, narrow and deep melting zone is advantageously formed, the efficiency of heating surface reaches more than 95%.Above-mentioned electron beam launcher
2 during the oriented growth of material, by electron beam incident direction along sample axial deflection, by the incidence angle for adjusting electron beam
Degree, it is possible to achieve to the control of convex, flat, recessed three kinds of interface configurations of material solid liquid interface during oriented growth, so as to adapt to
Various different demands.
In one embodiment, electron beam launcher 2 is high pressure Pierce electron gun, and its voltage is 80kV, and power is
10kW, high frequency sweep is carried out while very high energies density is provided, highest 10000Hz can be reached by the control of magnetic lenses
Frequency；Also, the angle between the electron beam and horizontal plane that electron beam launcher 2 is launched is 0 °, i.e. electron beam level enters
Penetrate, it can make material solid liquid interface maintain horizontality during oriented growth, be advantageous to material slewing growth.
First pull system is used to fix seed crystal 8 and seed crystal 8 is lifted and spinning motion, wherein elevating movement
Speed can be 0-100mm/s, and the speed of spinning motion can be 0-6000r/min.In directional solidification, launched by electron beam and filled
The electron beam for putting 2 transmittings is heated, and seed crystal 8 is turned into partially molten state (i.e. top melting, bottom solidification), solid-liquid phase change
During solid liquid interface promoted along the bottom of seed crystal 8, be orientated the advantage of seed crystal 8 and be retained, so as to the crystal that is newly formed along
The lattice stacking of seed crystal 8, it is easier to crystal growth.In addition, the cooling tube 32 being arranged on inside hollow first pumping rod 31 can
High-pressure coolant (such as cooling water) is sprayed, solidification is maintained so as to be advantageous to the bottom of seed crystal 8.Further, in the first pumping rod
31 are provided with chuck 33 towards one end inside vacuum chamber 1, and it is used to clamp seed crystal 8, can be connected to the first pull in a usual manner
One end of bar 31, and seed crystal 8 can be held on chuck 33 with high-speed coupling；Chuck 33 can be copper, so as to be advantageous to
The conduction of heat, and suitable chuck can be selected according to being actually needed, so as to the material for preparing size, coming in every shape.
First cooling system is used to cool down material, when being oriented solidification, can load liquid in inner chamber 41
State metal, coolant is loaded in exocoel 42, it can adapt to the larger electron beam heating of energy density, it is easy to accomplish high temperature
Spend gradient and fast-growth.Further, the top plate of inner chamber 41 may be configured as molybdenum plate 411, and it can effectively completely cut off melting zone 7 to inner chamber
The liquid metal radiant heat transfer loaded in 41, the liquid level of Simultaneous Stabilization liquid metal are close to the lower edge of melting zone 7 all the time.
Second pull system is used to fix foundry alloy rod 9 and foundry alloy rod 9 is lifted and spinning motion, wherein rising
The speed of drop motion can be 0-100mm/s, and the speed of spinning motion can be 0-6000r/min.Second pull system is taken out with first
Pull system is independently arranged, so that foundry alloy rod 9 and the relative separation of seed crystal 8, which is easy to go out list using the fast-growth of seed crystal 8
Brilliant and orientation polycrystalline material.In addition, solute distributes during the rotation of seed crystal 8 and foundry alloy rod 9 can make Rapid Directional Solidification
Evenly, material microsegregation reduces, and quality is higher.Further, in the second pumping rod 51 towards one end inside vacuum chamber 1
Provided with chuck 52, it is used to clamp foundry alloy rod.
The second cooling system 6 is used to cool down material, and it can be fixed using usual manner, such as can be in vacuum
Supporting plate 12 is set on the inwall of room 1, and utilizes the supporting plate 12 support the second cooling system 6.In one embodiment, second
Cooling system 6 includes metal tube 61 and encloses the cooling chamber 62 being located at outside metal tube 61, the through hole of metal tube 61 and the first pull
Bar 31 is coaxially disposed, and cooling chamber 62 and exocoel 42 are equipped with inlet and outlet, and the inlet and outlet is used for the circulation of coolant.Enter
One step, high temperature resistant black coating (not shown) can also be set in the inwall of cooling chamber 62, it is advantageous to improve heat transfer efficiency.
When being oriented solidification, the cooling mediums such as liquid nitrogen can be loaded in cooling chamber 62.The second cooling system 6 enters to synchronous material
Row cooling, the cooling effect of Rapid Directional Solidification equipment is drastically increased, while by controlling the work(of electron beam launcher 2
The lifting speed and rotational velocity of rate and each pumping rod 31,51 control the length in melting zone 7 in 0.5-2mm.
In addition, the gap formed between the first cooling system and the second cooling system 6 can be 1-5mm；And fixed
Into process of setting, the melting zone 7 that electron beam heating material is formed is strict controlled in the gap location, by controlling material microcosmic
Solidification path is it is hereby achieved that required particular organization's structure.
Above-mentioned Rapid Directional Solidification equipment can realize 1 × 105-5×105K/cm thermograde and 1-100mm/s life
Long speed.
Embodiment 2
Mangneto is prepared using the Rapid Directional Solidification method (i.e. electron-beam zone melting Rapid Directional Solidification technique) of the present invention to stretch
Compression material (Fe0.83Ga0.17)99.9La0.1, comprise the following steps：
1st, dispensing
Raw material Fe, Ga and La of selection purity are all higher than 99.99wt%, and in order to prevent first biscuiting in fusion process
Damage, when being equipped with Fe, Ga and La raw material according to mentioned component, Ga and La is added respectively according to about 1wt% scaling loss amount, is weighed
It is standby after each raw material.
2nd, mother alloy ingot is prepared
Raw material Fe, Ga and La of above-mentioned outfit are put into the crucible of vacuum non-consumable arc-melting furnace, will when placing
The metallic element of easy scaling loss is placed in crucible bottom, and the metallic element being unlikely to be burnt is placed in above crucible.
Vacuum non-consumable arc-melting furnace is carried out being evacuated to 4.0 × 10-3After Pa, high-purity argon gas is filled with into body of heater,
The volumn concentration (purity) of argon gas is more than 99.99%, treats that the vacuum in stove rises to 1.0 × 10-1Stop after Pa
Inflation, repeatedly this step operation three times after, melting electric current is arranged to 150A, to raw material carry out melting, control each melting when
Between be 4 minutes or so, melt back four times, be made mother alloy ingot.
3rd, foundry alloy rod is prepared
Master alloy ingot obtained above is placed in vacuum non-consumable arc-melting furnace, to vacuum non-consumable arc-melting furnace
It is evacuated to 3.0 × 10-3After Pa, the high-purity argon gas that volumn concentration is more than 99.99% is filled with into body of heater, is treated true in stove
Reciprocal of duty cycle rises to 1.0 × 10-1Pa stops inflating later.
Melting electric current is arranged to 150A, master alloy melting ingot, rapidly by melting electric current when master alloy ingot soon melts
Regulation is to 300A, arc blow-out at alignment master alloy ingot center, mould hole, while opens vacuum casting valve, using negative pressure by wink
Between the foundry alloy liquid that melts be cast in mould foundry alloy rod be made, its XRD diffracting spectrum is as shown in Figure 2；As a result show：The mother
Alloy bar is polycrystalline tissue, polycrystalline orientation with<110>、<100>Based on.
4th, (Fe is prepared0.83Ga0.17)99.9La0.1Rapid Directional Solidification is orientated polycrystalline material
By foundry alloy rod outer surface grinding homogeneity obtained above, 10min is cleaned by ultrasonic under 50KHz frequency, is cleaned
After be put in baking oven, in 120 DEG C dry 20min, obtain washed samples.
Solidification is oriented to material using the Rapid Directional Solidification equipment of embodiment 1, first by the He of foundry alloy rod 9
(Fe0.83Ga0.17)99.9La0.1Polycrystalline seed crystal 8 is separately fixed at the second pumping rod 51 and the first pull of Rapid Directional Solidification equipment
The end of bar 31 (such as being fixed respectively by chuck 52, chuck 33), and respectively in inner chamber 41, exocoel 42, cooling chamber 62
Middle filling Ga-In alloys coolant, recirculated cooling water and liquid nitrogen, the bottom of seed crystal 8 is immersed Ga-In alloy coolants, make first
Pumping rod 31 reversely rotates with the second pumping rod 51, and the lower end of foundry alloy rod 9 and the upper end of seed crystal 8 is respectively positioned on the first cooling system
The end of gap location between the second cooling system 6, foundry alloy rod 9 and seed crystal 8 is close but does not contact；Then by vacuum chamber 1
It is evacuated to 3.0 × 10-3After Pa, the high-purity argon gas that volumn concentration is more than 99.99% is filled with into vacuum chamber 1, is treated
Vacuum rises to 1.0 × 10 in vacuum chamber 1-1Pa stops inflating later, repeatedly after this step operation three times, starts electron beam transmitting
Device 2 is pointed to the foundry alloy rod 9 of gap location and seed crystal 8 is heated, and it is 100r/ to set the rotational velocity of the first pumping rod 31
Min, the rotational velocity of the second pumping rod 51 are 100r/min, and two bar senses of rotation are on the contrary, the setting incident current of electron gun 2 is
35mA, heating 2s make seed crystal 8 and foundry alloy rod 9 fuse into one and form the stable melting zones of 0.6mm or so between two rods, and control is fixed
It is 3 × 10 to the thermograde of solidification5K/cm, speed of growth 10mm/s, make the material of melting along the bottom of seed crystal 8 smoothly
Downward pull carries out Rapid Directional Solidification into Ga-In alloy coolants, during Rapid Directional Solidification, is cooled down by Ga-In alloys
Liquid cools down to material lower end, while sprays high-pressure cooling water using cooling tube 32 and material lower end is cooled down, and melting zone 7 is grown
Spend for 1mm or so, and melting zone 7 is strict controlled in above-mentioned gap；After end to be grown, room temperature is down to, after taking out growth
Material, it is (Fe that composition, which is made,0.83Ga0.17)99.9La0.1Bar-shaped magnetostriction materials (size Φ 7mm × 100mm).
(Fe0.83Ga0.17)99.9La0.1The vertical profile melting zone fast quenching metallograph of material is as shown in figure 3, be slewing wherein at a
The columanar structure of solidification-stable growth phase, the straight size of grain form are tiny；Formed at b by electron beam heating alloy
Melting zone pattern, melting zone form dimpling, zone length is about 1mm；It is fast quenching terminal material casting rod polycrystalline tissue at c.It is indicated above：
The inventive method is preparing (Fe0.83Ga0.17)99.9La0.1Good column fine grained texture, and growth course can be obtained during bar
In be to stablize dimpling solid liquid interface, zone length is about 1mm.
(the Fe of above-mentioned preparation0.83Ga0.17)99.9La0.1The XRD diffracting spectrums of material are as shown in Figure 4, the results showed that：Material
Crystal grain refinement, [100] orientation are remarkably reinforced after Rapid Directional Solidification, and directional effect is good.Above-mentioned preparation
(Fe0.83Ga0.17)99.9La0.1The BSE photos of material are as shown in Figure 5, the results showed that：The material internal has no obvious precipitated phase,
Material is uniform homogeneous structure, therefore obtained is a kind of non-equilibrium Nonequilibrium Materials.
In addition, measured using magnetostriction measurement system (Beijing WuKe opto-electrical Technology Co., Ltd's production)
(Fe0.83Ga0.17)99.9La0.1The magnetostrictive strain value of material, wherein foil gauge use Japanese republicanism KFG-1-120-C1-
11L3M2R type resistance strain gages, as a result as shown in Figure 6.As a result show：(Fe0.83Ga0.17)99.9La0.1The saturation mangneto of material is stretched
Contracting coefficient is 600ppm, and saturation magnetic field is only 400Oe or so, and Magnetostriction and comprehensive usability are good.
Embodiment 3
Club-shaped material (Mn is prepared with reference to the method for embodiment 254Al46)0.97C0.03, wherein the slewing using embodiment 1
Solidification equipment is oriented solidification to material, and control directional solidification thermograde be 3 × 105K/cm, the speed of growth are
10mm/s, it is (Mn that composition, which is made,54Al46)0.97C0.03Club-shaped material.
(Mn54Al46)0.97C0.03The vertical profile melting zone fast quenching metallograph of material is as shown in fig. 7, wherein Fig. 7 central parts are electronics
The melting zone pattern that Shu Jiare alloys are formed, melting zone form dimpling, zone length is about 1mm, is indicated above the inventive method and exists
Prepare (Mn54Al46)0.97C0.03Stable 1mm or so melting zone can be obtained during alloy material.
(the Mn of above-mentioned preparation54Al46)0.97C0.03The vertical profile metallograph of material is as shown in Figure 8, the results showed that：The column of material
Shape crystal grain is tiny straight, and directional effect is obvious, and crystal grain refinement is notable.(Mn54Al46)0.97C0.03The XRD diffracting spectrums of material are as schemed
Shown in 9, occur the characteristic peak of obvious τ phases in the collection of illustrative plates, and it is higher in 41.3 ° and 45.6 ° of peak intensities, represent that the material has
Stronger [101] orientation and [110] orientation, illustrates that material has the τ phase constitutions of [101] orientation, that is, forms a kind of non-equilibrium Asia
Steady material.
In addition, (Mn54Al46)0.97C0.03The M-H curves of material are as shown in Figure 10.As a result show：Use present invention process system
Standby (Mn54Al46)0.97C0.03During alloy, it can in the material obtain and largely be orientated obvious τ phases, and column crystal refinement is notable,
The coercivity and remanent magnetism of alloy are significantly improved, the material has 1500Oe coercivity and 30emu/g remanent magnetism.
(Mn54Al46)0.97C0.03Alloy has very big saturation magnetization as a kind of new non-rare earth permanent-magnetic material, its τ phase,
And τ phase contents are more, material orientation is better, material entirety magnetic energy product is higher, has huge application prospect.
Reference examples 1
The foundry alloy rod that this reference examples is prepared using LMC laser zone remeltings apparatus for directional solidification to embodiment 2 is oriented solidifying
Gu LMC laser zone remeltings apparatus for directional solidification uses high power Nd:YAG solid state lasers are as heating source, and only with Ga-
In alloys coolant is as cooling medium, when being oriented solidification using this apparatus for directional solidification, the thermograde of directional solidification
For 1 × 105K/cm, speed of growth 0.3mm/s, the BSE photos of obtained material are as shown in figure 11, the results showed that：The material
The internal obvious precipitated phase for having white spherical shape, understand that the precipitate of the spherical shape is Nd-rich phase by EDS detections, thus
Show the preparation of this reference examples is a kind of balancing material.In addition, the Magnetostriction curve of the material is as shown in Figure 6.As a result
Show：The saturation magnetostriction constant of material prepared by this reference examples is 250ppm, and saturation magnetic field is 500Oe or so.
(Fe is prepared using LMC laser zone remelting directional solidifications in this reference examples0.83Ga0.17)99.9La0.1Material, it is possible to achieve
Higher thermograde (1 × 105K/cm), but because the speed of growth is relatively slow (0.3mm/s), therefore cooling velocity (Rc=Gl×V)
Only 3 × 103K/s, lower than technique used in embodiment 2 two orders of magnitude.(Fe0.83Ga0.17)99.9La0.1As a kind of special
During different Nonequilibrium Materials, the cooling velocity that needs to be exceedingly fast in preparation process could will not be dissolved thick atom La and be dissolved into FeGa by force
In matrix, otherwise it will be played in the form of the second phase in intergranular and transgranular precipitation, the Nd-rich phase of precipitation in magnetic history
The effect of pinning magnetic domain, the overall Magnetostriction of material is caused to decline.Electron-beam zone melting used is fast in above-described embodiment 2
High-temperature liquid-phase structure can be remained into room temperature well by fast directional solidification processes, La atoms is deposited in a manner of substitution solid solution
In FeGa basal body structures, this be dissolved brings strong tetragonal distortion to matrix, and this distortion result in material macroscopic view
Embody big magnetostriction.
Reference examples 2
Club-shaped material (Mn is prepared with reference to the method for reference examples 154Al46)0.97C0.03, the wherein thermograde of directional solidification is 1
×105K/cm, speed of growth 0.3mm/s, it is (Mn that composition, which is made,54Al46)0.97C0.03Material.
(the Mn of above-mentioned preparation54Al46)0.97C0.03The XRD diffracting spectrums of material are as shown in figure 12, its 38.4 °, 41.2 °,
43.7 °, the positions such as 77.1 ° there is the characteristic peak of ε phases, peak intensity is more apparent, and it is ε phase constitutions to illustrate the material, and it is for one kind
The balancing material of non-ferromagnetic phase, does not possess magnetic property.
Finally it should be noted that：Various embodiments above is merely illustrative of the technical solution of the present invention, rather than its limitations；To the greatest extent
The present invention is described in detail with reference to foregoing embodiments for pipe, it will be understood by those within the art that：Its according to
The technical scheme described in foregoing embodiments can so be modified, either which part or all technical characteristic are entered
Row equivalent substitution；And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention technology
The scope of scheme.
Claims (10)
- A kind of 1. Rapid Directional Solidification equipment, it is characterised in that including vacuum chamber, electron beam launcher, the first pull system, First cooling system, the second pull system and the second cooling system,Bottom through-hole and top through hole are offered relatively at the bottom of the vacuum chamber and top, in the medial side of the vacuum chamber Electron beam window is offered on wall；The electron beam launcher is arranged on the outside of the vacuum chamber, and the electronics of electron beam launcher transmitting Beam can enter the vacuum chamber by the electron beam window；The first pull system includes the first pumping rod and cooling tube, and first pumping rod is hollow and passes through the bottom Through hole is plugged into the vacuum chamber vertically, and first pumping rod is driven and can lifted and spinning motion by motor, The cooling tube is arranged on inside first pumping rod；First cooling system is located at the internal vacuum chamber, and it includes inner chamber and exocoel, and the inner chamber, which is enclosed, is located at described Outside one pumping rod, the exocoel, which encloses, is located at the lumen outer；The second pull system includes the second pumping rod, and second pumping rod is plugged to institute vertically by the top through hole State in vacuum chamber, second pumping rod by motor drive and can lift and with the first pumping rod spinning motion side To identical or opposite spinning motion；Between the second cooling system is arranged on above first cooling system and formed between first cooling system Gap, the second cooling system have the through hole being coaxially disposed with first pumping rod and can be pointed in the through hole Material cooled down, the electron beam of electron beam launcher transmitting can pass through from the gap.
- 2. Rapid Directional Solidification equipment according to claim 1, it is characterised in that the voltage of the electron beam launcher For 80kV, power 10kW, scan frequency is 0~10000Hz.
- 3. Rapid Directional Solidification equipment according to claim 1 or 2, it is characterised in that the electron beam launcher is High pressure Pierce electron gun.
- 4. Rapid Directional Solidification equipment according to claim 1, it is characterised in that the electron beam launcher transmitting Angle between electron beam and horizontal plane is -5 °~5 °.
- 5. Rapid Directional Solidification equipment according to claim 1, it is characterised in that by motor-driven first pumping rod institute The velocity interval of the elevating movement of work is 0~100mm/s, and the velocity interval of spinning motion is 0~6000r/min；Driven by motor The velocity interval for the elevating movement that the second dynamic pumping rod is made is 0~100mm/s, the velocity interval of spinning motion for 0~ 6000r/min。
- 6. Rapid Directional Solidification equipment according to claim 1, it is characterised in that the gap is 1~5mm.
- 7. Rapid Directional Solidification equipment according to claim 1, it is characterised in that the second cooling system includes metal The cooling chamber being located at outside the metal tube is managed and encloses, the through hole of the metal tube is coaxially disposed with first pumping rod, institute State cooling chamber and the exocoel is equipped with inlet and outlet.
- 8. Rapid Directional Solidification equipment according to claim 7, it is characterised in that set in the inwall of the cooling chamber black Color coating.
- A kind of 9. Rapid Directional Solidification method, it is characterised in that comprise the following steps：1) foundry alloy rod is prepared：After component requirements according to unidirectional solidification material are equipped with raw material, the raw material of outfit is smelted into mother alloy ingot, melts institute Mother alloy ingot is stated, and foundry alloy rod is made by vacuum casting；2) 1 to 8 any described Rapid Directional Solidification equipment of usage right requirement is oriented solidification：The foundry alloy rod and seed crystal are separately fixed to the second pumping rod and the first pull of the Rapid Directional Solidification equipment Boom end, alloy coolant and circulating cooling liquid are loaded in the inner chamber and exocoel respectively, and immerse the seed crystal bottom Alloy coolant, reversely rotate first pumping rod and second pumping rod, and after starting the second cooling system, To the vacuum chamber and protective gas is filled with, subsequent start-up electron beam launcher is pointed to the foundry alloy in the gap Rod and seed crystal are heated, and the first pumping rod described in pull in the same direction and the second pumping rod are oriented solidification, and described in control The thermograde of directional solidification is 1 × 105~5 × 105K/cm, the speed of growth are 1~100mm/s, and unidirectional solidification material is made.
- 10. Rapid Directional Solidification method according to claim 9, it is characterised in that control taking out for first pumping rod Pulling rate degree is 1~10mm/s, and the speed of spinning motion is 60~6000r/min；And control the pull of second pumping rod Speed is 1~10mm/s, and the speed of spinning motion is 60~6000r/min.
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| RU2287023C1 (en) * | 2005-05-05 | 2006-11-10 | Вадим Георгиевич Глебовский | Method of electron-beam zone melting of metal and device for realization of this method |
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