CN105543952A - Rapid directional solidification equipment and rapid directional solidification method - Google Patents
Rapid directional solidification equipment and rapid directional solidification method Download PDFInfo
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- CN105543952A CN105543952A CN201511001423.6A CN201511001423A CN105543952A CN 105543952 A CN105543952 A CN 105543952A CN 201511001423 A CN201511001423 A CN 201511001423A CN 105543952 A CN105543952 A CN 105543952A
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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
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- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides rapid directional solidification equipment and a rapid directional solidification method. The rapid directional solidification equipment comprises a vacuum chamber, an electron beam emission device, a first drawing system, a first cooling system, a second drawing system and a second cooling system, wherein the first drawing system comprises a first hollow drawing rod capable of ascending, descending and rotating and a cooling pipe arranged in the first drawing rod; the first cooling system comprises an internal cavity and an external cavity; the internal cavity is formed outside the first drawing rod in an enclosing manner, and the external cavity is formed outside the internal cavity in the enclosing manner; the second drawing system comprises a second drawing rod capable of ascending, descending and rotating; the second cooling system is arranged above the first cooling system, and forms a gap with the first cooling system; electron beams emitted by the electron beam emission device can penetrate through the gap. The rapid directional solidification equipment can reach the cooling speed of 5x10<5>K/s, and can be used for preparing mono-crystalline and oriented polycrystalline materials with rapidly and directionally solidified structures.
Description
Technical field
The present invention relates to a kind of apparatus for directional solidification, be specifically related to a kind of Rapid Directional Solidification equipment and Rapid Directional Solidification method.
Background technology
Solidifying is that nature material becomes the most general solid-state phenomenon from liquid state, be also primary process prepared by material, particularly metallic substance, and the progress of solidifying science and solidification technology promotes human material's science and advances.Traditional solidification theory and the research of technology are mainly carried out around the castingprocesses of common foundry goods and ingot casting, along with the proposition of modern solidification theory, the science of solidifying obtains impressive progress: as appearance and application etc. of perfect, the flash set technology of the generation of continuous casting technology, directional freeze and Crystal Growth Technique.Make a general survey of solidify the reach of science be not difficult find, so-called modern solidification theory, be exactly research " people is for the process control of material solidification behavior " and " nonequilibrium solidification process and nonequilibrium effect ".
For many years, about modern solidification theory, researchist makes a large amount of work, obtain many fruitful achievements in research, mainly comprise: 1. in control solidi fication process, researchist proposes the theoretical model of directional freeze, namely in equilibrium freezing process, compulsive means are adopted, in frozen metal and molten metal, set up the thermograde of specific direction, thus melt is solidified along the direction contrary with hot-fluid, finally obtain column crystal, the monocrystal material with specific orientation.Directional freeze is a kind of important material preparation technology, is widely used in obtaining in the type material with particular orientation tissue and excellent properties.2., in nonequilibrium solidification process and nonequilibrium effect, researchist proposes multiple theoretical model to predict that multiple when far from equilibrium state of material solidifies behavior, and this field becomes the academic focus of science of solidifying in recent years.Along with the increasing of solidification cooling rate and condensate depression, process of setting departs from the degree aggravation of balance.Physical parameter and the forming cores such as alloy melt viscosity, spread coefficient, solid-liquid interface solute distribution coefficient, grow up, Interface morphology evolution process etc. all departs from balance, and then impact selection, organizational choice, structure choice mutually, cause structure refinement, formation crystallite, nanocrystalline, metastable phase, accurate crystalline substance, amorphous etc.
With the development of nonequilibrium freezing theory, researchist develops various nonequilibrium freezing technology and prepares many type materials.So-called non-equilibrium material, namely material structure is under conditions of use away from thermodynamic equilibrium state; Be exactly depart from thermodynamic(al)equilibrium point viewed from thermodynamics, be in a kind of unsure state; This kind of material generally has the unexistent metastable organization of balancing material and many excellent properties.Nonequilibrium freezing technology mainly contains two large classes: one is kinetics rapid cooling, forming core is suppressed by chilling, represent technique and have that gas atomization, aluminium alloy stream inject cooling fluid method, single roller revolves pure method etc., due to the restriction of being conducted heat, these class methods cannot obtain rapid solidification structure in large volume liquid metal, can only prepare the low-dimensional materials such as powdery, filament and band.Two is thermodynamics rapid cooling, suppress forming core by improving condensate depression, representing technique has drop dispersion method, cyclical superheating method, glass melt method etc., because condensate depression lifting is limited, solid-liquid interface fltting speed is slow, material rapid solidification structure prepared by these class methods is uneven, and performance is not good.
In order to solve simultaneously directional solidification processes under equilibrium conditions can not prepare the high-performance metastable phase material and non-equilibrium condition with rapid solidification structure under fast solidification technology can not prepare the high-performance block materials contradiction therebetween with specific orientation, inventors herein propose the concept of Rapid Directional Solidification, namely under the nonequilibrium freezing condition of rapid solidification, the oriented growth of material is realized, to preparing the block materials with rapid solidification structure and specific orientation.
It is 10 that Chinese patent CN102051668A discloses a kind of thermograde
5the device for directionally solidifying of K/cm and directional solidification process, this patent uses laser as heating source, gallium-indium-tin alloy as heat-eliminating medium, achieves material magnetostrictive properties under 200-1400W power, 1-300 μm/s speed of growth.This device and method can reach 10
5the thermograde of K/cm, but growth velocity lower (only up to 0.3mm/s), cause this device and method to be different from device and the Rapid Directional Solidification method of contriver's proposition.
The people such as Zhang Jun, Cui Chunjuan of solidification technology National Key Laboratory of Northwestern Polytechnical University utilize electron-beam floating zone melting directional freeze to prepare Si/TaSi
2the spontaneous Composite Field emissive material of eutectic, this electron-beam floating zone melting apparatus for directional solidification is produced by German Leybold – Heraeus company, working current is 0-500mA, operating voltage is 0-20kV, being mainly used in processing diameter is 2-10mm, length is not more than the metal bar of 200mm, achieved thermograde is only 350-500K/cm, drawing velocity (speed of growth) is up to 0.38mm/s, and zone length reaches 8-10mm, whole directional freeze process is the nearly balance directional freeze of carrying out under lower thermograde and the lower speed of growth, therefore these apparatus and method are also different from balance Rapid Directional Solidification device far away and the Rapid Directional Solidification method of contriver's proposition completely.
Summary of the invention
The invention provides a kind of Rapid Directional Solidification equipment and Rapid Directional Solidification method, for solve existing directional solidification technique irrealizable ultra high temperature gradient and the quick problem that grows of the irrealizable slewing of growth and rapid solidification institute, the material obtained is monocrystalline and the orientation polycrystalline material with Rapid Directional Solidification tissue.
The invention provides a kind of Rapid Directional Solidification equipment, comprise vacuum chamber, electron beam launcher, the first pull system, the first cooling system, the second pull system and the second cooling system,
Relatively with top in the bottom of described vacuum chamber offer bottom through-hole and top through hole, the middle part sidewall of described vacuum chamber offers electron beam window;
Described electron beam launcher is arranged on the outside of described vacuum chamber, and described electron beam launcher ejected electron bundle can enter described vacuum chamber by described electron beam window;
Described first pull system comprises the first pumping rod and cooling tube, described first pumping rod hollow and vertically plug in described vacuum chamber by described bottom through-hole, described first pumping rod is driven by motor and can be elevated and spinning motion, and it is inner that described cooling tube is arranged on described first pumping rod;
Described first cooling system is positioned at described internal vacuum chamber, and it comprises inner chamber and exocoel, and it is outside that described inner chamber is around in described first pumping rod, and described exocoel is around in described lumen outer;
Described second pull system comprises the second pumping rod, described second pumping rod vertically plugs in described vacuum chamber by described top through hole, and described second pumping rod is driven by motor and can be elevated and the spinning motion identical or contrary with described first pumping rod spinning motion direction;
Described the second cooling system is arranged on above described first cooling system and also and between described first cooling system forms gap, described the second cooling system has the through hole that coaxially arranges with described first pumping rod and can cool the material being positioned at described through hole, and described electron beam launcher ejected electron bundle can pass from described gap.
Rapid Directional Solidification equipment of the present invention is by arranging electron beam launcher, thus carry out directional freeze using electron beam as heating source, beam energy density is large, heating efficiency is high, utilize the beam bombardment metal material surface focused on through multistage magnetic lens, instantaneously kinetic energy can be passed to metallic substance, this kinetic transformation is that the interior metal that can make melts rapidly; Simultaneously, electronics incident is at a high speed after making a part of material of metal material surface melt rapidly, reactive force is utilized to be arranged to surrounding by molten metal liquid, thus expose new material surface, electron beam continues to act on new material surface, thus be conducive to forming narrow and dark melting zone, melting zone width can be less than 1mm, and heating efficiency reaches more than 95%.
And, in order to adapt to the larger electron beam heating of energy density, Rapid Directional Solidification equipment of the present invention arranges the first cooling system and the second cooling system, and in the first pumping rod of the first pull system, cooling tube is set, when carrying out directional freeze, inner chamber to the first cooling system loads liquid metal, loads cooling fluid, and utilize cooling tube inject high pressure cooling fluid to exocoel; Simultaneously, the second cooling system cools synchronous material, improve the cooling performance of apparatus for directional solidification, melting zone is controlled the gap location at the first cooling system and the second cooling system, make still can keep higher and stable thermograde in high speed draw process.
In addition, Rapid Directional Solidification equipment of the present invention arranges and can be elevated respectively and the first pull system of rotation and the second pull system, it is respectively used to the material (such as mother alloy rod) clamping seed crystal respectively and treat directional freeze, first pull system and the second pull system are independently arranged, thus the material treating directional freeze is separated with seed crystal, be convenient to utilize seed crystal to grow monocrystalline and orientation polycrystalline material fast; Rotation solute can be made in directional freeze process to distribute evenly, material microsegregation reduces, and quality is higher.
In the present invention, the voltage of described electron beam launcher can be 80kV, and power can be 10kW, and sweep rate can be 0-10000Hz; In addition, the working vacuum degree (such as 3 × 10 that electron beam launcher can be made to reach predetermined by mechanical pump
-2pa).In one embodiment, described electron beam launcher is high pressure Pierce electron gun.Further, the angle between described electron beam launcher ejected electron bundle and horizontal plane can be-5 °-5 °; Wherein, turned clockwise along the horizontal plane by electron beam and be set to "-", that is: "-5 ° " represent that the incident direction of electron beam is the direction of 5 ° of turning clockwise along the horizontal plane.
Above-mentioned electron beam launcher is in the oriented growth process of material, by electron beam incident direction along sample axial deflection, by adjusting the incident angle of electron beam, the control to convex, flat, recessed three kinds of interfacial configurations of material solid-liquid interface in oriented growth process can be realized, thus adapt to various different demand.Preferably, the angle between described electron beam launcher ejected electron bundle and horizontal plane is 3 °, even if electron beam is incident obliquely, it is easy to obtain monocrystal material and orientation polycrystalline material more.
In the present invention, the velocity range of the up-and-down movement done by motor-driven first pumping rod can be 0-100mm/s, and the velocity range of spinning motion can be 0-6000r/min; The velocity range of the up-and-down movement done by motor-driven second pumping rod can be 0-100mm/s, and the velocity range of spinning motion can be 0-6000r/min; Further, described gap can be 1-5mm.
Zone length can control at 1-2mm by controlling the power of electron beam launcher and the rising or falling speed of each pumping rod and rotational velocity by the present invention, preferred about 1mm, and in directional freeze process, the melting zone that electron beam heating material is formed is strict controlled in this gap location, by control material solid liquid interface morphology thus obtain needed for particular organization's structure.Particularly, the speed of the up-and-down movement that the first pumping rod and the second pumping rod are done is preferably 1-10mm/s, and the speed of spinning motion is preferably 60-6000r/min, and this scope is conducive to being uniformly distributed of solute in material, reduces microsegregation.
In one embodiment, described the second cooling system comprises metal tube and is around in the cooling chamber of described metal tube outside, and through hole and described first pumping rod of described metal tube are coaxially arranged, and described cooling chamber and described exocoel are equipped with import and outlet.When embody rule, the heat-eliminating mediums such as liquid nitrogen can be loaded in cooling chamber; Further, can also arrange black coating at the inwall of described cooling chamber, it is high temperature resistant, and is conducive to improving heat transfer efficiency.The second cooling system can adopt usual manner to fix, such as, on the inwall of described vacuum chamber, arrange back up pad, and utilizes this back up pad to support described the second cooling system.
In one embodiment, chuck is equipped with at described first pumping rod and described second pumping rod towards one end of described internal vacuum chamber.Chuck is used for Gripping material, and it can be connected to one end (being such as threaded) of pumping rod in a usual manner, and material can (such as high-speed coupling) be held on chuck by conventional methods; Further, suitable chuck can be selected according to actual needs, thus preparation size, the material that comes in every shape.Further, the chuck corresponding to the first pumping rod can be copper, and it is conducive to the conduction of heat.
In the present invention, described vacuum chamber for the formation of vacuum environment needed for Rapid Directional Solidification, the working vacuum degree that vacuum chamber can be made to reach predetermined by mechanical pump and molecular pump; Meanwhile, owing to can produce X-ray while high-pressure electronic rifle divergent bundle, therefore vacuum chamber need through special radioprotective process.
Further, the top board of described first cooling system inner chamber can be molybdenum plate, and it can effectively completely cut off the liquid metal radiative transfer loaded in inner chamber in melting zone, and the liquid level of Simultaneous Stabilization liquid metal is close to edge under melting zone all the time.
Above-mentioned Rapid Directional Solidification equipment of the present invention can realize 1 × 10
5-5 × 10
5the thermograde of K/cm and the speed of growth of 1-100mm/s.The material structure utilizing this Rapid Directional Solidification equipment to prepare evenly, grain refining, orientation be obvious, and properties is excellent.
The present invention also provides a kind of Rapid Directional Solidification method, comprises the steps:
1) mother alloy rod is prepared:
After being equipped with raw material according to the component requirements of unidirectional solidification material, the raw material of outfit being smelted into mother alloy ingot, melting described mother alloy ingot, and make mother alloy rod by vacuum casting;
2) above-mentioned arbitrary described Rapid Directional Solidification equipment is used to carry out directional freeze:
Described mother alloy rod and seed crystal are separately fixed at the second pumping rod and the first pumping rod end of described Rapid Directional Solidification equipment, alloy cooling fluid and circulating cooling liquid is loaded respectively in described inner chamber and exocoel, and make described seed crystal bottom immerse alloy cooling fluid, make described first pumping rod and described second pumping rod reverse rotation, and after starting described the second cooling system, shielding gas is filled with to described vacuum chamber, start electron beam launcher subsequently to heat the mother alloy rod and seed crystal that are positioned at described gap, first pumping rod described in pull and the second pumping rod carry out directional freeze in the same way, and the thermograde controlling described directional freeze is 1 × 10
5-5 × 10
5k/cm, the speed of growth (drawing velocity) is 1-100mm/s, obtained unidirectional solidification material.
Further, the drawing velocity controlling described first pumping rod is 1-10mm/s, and the speed of spinning motion is 60-6000r/min; And the drawing velocity controlling described second pumping rod is 1-10mm/s, the speed of spinning motion is 60-6000r/min.
Enforcement of the present invention, at least has following advantage:
1, Rapid Directional Solidification equipment of the present invention adopts electron beam as heating source, and adopt two cooling system, it can set up a fixing unidirectional thermograde between solid liquid phase, and realized the Rapid Directional Solidification of material by the quick propelling of solid-liquid interface, wherein thermograde can reach 1 × 10
5-5 × 10
5k/cm, the speed of growth can reach 1-100mm/s, and zone length can be less than the Rapid Directional Solidification of 1mm, finally can realize the change of material character.
2, simple to operate, the strong adaptability of Rapid Directional Solidification method of the present invention, it can prepare the non-equilibrium Nonequilibrium Materials of the three-dimensional bits height orientation with Rapid Directional Solidification tissue, the crystalline structure of this material arranges along specific crystallographic direction, thermodynamically be in metastable state, therefore there is the characteristic not available for balancing material.
Accompanying drawing explanation
The structural representation of the apparatus for directional solidification that Fig. 1 provides for the embodiment of the present invention 1;
The XRD diffracting spectrum of the mother alloy rod that Fig. 2 provides for the embodiment of the present invention 2;
(the Fe that Fig. 3 provides for the embodiment of the present invention 2
0.83ga
0.17)
99.9la
0.1the vertical profile melting zone fast quenching metallograph of material;
Unidirectional solidification material (the Fe that Fig. 4 provides for the embodiment of the present invention 2
0.83ga
0.17)
99.9la
0.1xRD diffracting spectrum;
Unidirectional solidification material (the Fe that Fig. 5 provides for the embodiment of the present invention 2
0.83ga
0.17)
99.9la
0.1bSE photo;
The Magnetostriction curve of the material that Fig. 6 provides for the embodiment of the present invention 2 and reference examples 1;
Unidirectional solidification material (the Mn that Fig. 7 provides for the embodiment of the present invention 3
54al
46)
0.97c
0.03vertical profile melting zone fast quenching metallograph;
Unidirectional solidification material (the Mn that Fig. 8 provides for the embodiment of the present invention 3
54al
46)
0.97c
0.03vertical profile metallograph;
Unidirectional solidification material (the Mn that Fig. 9 provides for the embodiment of the present invention 3
54al
46)
0.97c
0.03xRD diffracting spectrum;
Unidirectional solidification material (the Mn that Figure 10 provides for the embodiment of the present invention 3
54al
46)
0.97c
0.03m-H curve;
Figure 11 is the (Fe of reference examples 1 of the present invention preparation
0.83ga
0.17)
99.9la
0.1the BSE photo of material;
Figure 12 is the (Mn of reference examples 2 of the present invention preparation
54al
46)
0.97c
0.03the XRD diffracting spectrum of material.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly, below in conjunction with drawings and Examples of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
As shown in Figure 1, Rapid Directional Solidification equipment of the present invention comprises vacuum chamber 1, electron beam launcher 2, first pull system, first cooling system, (namely the second pull system and the second cooling system 6, offer bottom through-hole and top through hole relatively with top in the bottom of vacuum chamber 1, bottom through-hole and top through hole are coaxially arranged), the middle part sidewall of vacuum chamber 1 offers electron beam window 11; Electron beam launcher 2 is arranged on the outside of vacuum chamber 1, and electron beam launcher 2 ejected electron bundle can enter vacuum chamber 1 by electron beam window 11; First pull system comprises the first pumping rod 31 and cooling tube 32, first pumping rod 31 hollow and vertically plug in vacuum chamber 1 by bottom through-hole, first pumping rod 31 is driven by motor and can be elevated and spinning motion, and it is inner that cooling tube 32 is arranged on the first pumping rod 31; It is inner that first cooling system is positioned at vacuum chamber 1, and it comprises inner chamber 41 and exocoel 42, and it is outside that inner chamber 41 is around in the first pumping rod 31, and it is outside that exocoel 42 is around in inner chamber 41; Second pull system comprises the second pumping rod 51, second pumping rod 51 vertically plugs to (namely the second pumping rod 51 and the first pumping rod 31 are coaxially arranged) in vacuum chamber 1 by top through hole, and the second pumping rod 51 is driven by motor and can be elevated and the spinning motion identical or contrary with the first pumping rod 31 spinning motion direction; The second cooling system 6 is arranged on above the first cooling system and also and between the first cooling system forms gap, the second cooling system 6 has the coaxial through hole that arranges with the first pumping rod 31 and can cool the material being positioned at through hole, and electron beam launcher 2 ejected electron bundle can pass from gap.
In above-mentioned Rapid Directional Solidification equipment, vacuum chamber 1 is for the formation of vacuum environment needed for directional freeze, bottom it, the bottom through-hole offered relative to top and top through hole are coaxially arranged, and the working vacuum degree that vacuum chamber 1 can be made to reach predetermined by mechanical pump and molecular pump.
Electron beam launcher 2 is for divergent bundle, and it is used as the heating source heated material, and the voltage of electron beam launcher 2 can be 80kV, and power can be 10kW, and sweep rate can be 0-10000Hz; Angle between electron beam launcher 2 ejected electron bundle and horizontal plane can be-5 °-5 ° (i.e. electron beam incident, glancing incidences or incident obliquely obliquely).Electron beam is utilized to carry out directional freeze as heating source, beam energy density is large, heating efficiency is high, utilize the beam bombardment metal material surface focused on through multistage magnetic lens, instantaneously kinetic energy can be passed to metallic substance, this kinetic transformation is that the interior metal that can make melts rapidly; Simultaneously, electronics incident is at a high speed after making a part of material of metal material surface melt rapidly, reactive force is utilized to be arranged to surrounding by molten metal liquid, thus expose new material surface, electron beam continues to act on new material surface, be conducive to forming narrow and dark melting zone, heating efficiency reaches more than 95%.Above-mentioned electron beam launcher 2 is in the oriented growth process of material, by electron beam incident direction along sample axial deflection, by adjusting the incident angle of electron beam, the control to convex, flat, recessed three kinds of interfacial configurations of material solid-liquid interface in oriented growth process can be realized, thus adapt to various different demand.
In one embodiment, electron beam launcher 2 is high pressure Pierce electron gun, and its voltage is 80kV, and power is 10kW, while providing very high energies density, carry out high frequency sweep, can be reached the frequency of the highest 10000Hz by the control of magnetic lens; Further, the angle between electron beam launcher 2 ejected electron bundle and horizontal plane is 0 °, i.e. electron beam glancing incidence, and it can make material solid-liquid interface maintain horizontality in oriented growth process, is conducive to material slewing growth.
First pull system is used for fixing seed crystal 8 and seed crystal 8 can be elevated and spinning motion, and the speed of wherein up-and-down movement can be 0-100mm/s, and the speed of spinning motion can be 0-6000r/min.When directional freeze, heated by electron beam launcher 2 ejected electron Shu Jinhang, seed crystal 8 is made to become partially molten state (i.e. top melting, bottom are solidified), in solid-liquid phase-change process, solid-liquid interface advances along seed crystal 8 bottom, the advantage orientation of seed crystal 8 is retained, thus the new crystal formed is along the lattice stacking of seed crystal 8, is easier to single crystal growing.In addition, the cooling tube 32 being arranged on hollow first pumping rod 31 inside can inject high pressure cooling fluid (such as water coolant), thus is conducive to seed crystal 8 bottom and maintains and solidify.Further, be provided with chuck 33 at the first pumping rod 31 towards one end of vacuum chamber 1 inside, it can be connected to one end of the first pumping rod 31 in a usual manner for clamping seed crystal 8, and seed crystal 8 can be held on chuck 33 by high-speed coupling; Chuck 33 can be copper, thus is conducive to the conduction of heat, and can select suitable chuck according to actual needs, thus preparation size, the material that comes in every shape.
First cooling system is used for cooling material, when carrying out directional freeze, liquid metal can be loaded in inner chamber 41, in exocoel 42, loading cooling fluid, it can adapt to the larger electron beam heating of energy density, is easy to realize high-temperature gradient and growth fast.Further, inner chamber 41 top board can be set to molybdenum plate 411, and it can effectively completely cut off the liquid metal radiative transfer loaded in inner chamber 41 in melting zone 7, and the liquid level of Simultaneous Stabilization liquid metal is close to edge, 7 times, melting zone all the time.
Second pull system is used for fixing mother alloy rod 9 and mother alloy rod 9 can be elevated and spinning motion, and the speed of wherein up-and-down movement can be 0-100mm/s, and the speed of spinning motion can be 0-6000r/min.Second pull system and the first pull system are independently arranged, thus make mother alloy rod 9 and seed crystal 8 relative separation, and which is convenient to utilize seed crystal 8 to grow monocrystalline and orientation polycrystalline material fast.In addition, the rotation of seed crystal 8 and mother alloy rod 9 solute in Rapid Directional Solidification process can be made to distribute evenly, material microsegregation reduces, and quality is higher.Further, be provided with chuck 52 at the second pumping rod 51 towards one end of vacuum chamber 1 inside, it is for clamping mother alloy rod.
The second cooling system 6 is for cooling material, and it can adopt usual manner to fix, such as, can arrange back up pad 12 on the inwall of vacuum chamber 1, and utilizes this back up pad 12 to support the second cooling system 6.In one embodiment, the second cooling system 6 comprises metal tube 61 and is around in the cooling chamber 62 of metal tube 61 outside, through hole and first pumping rod 31 of metal tube 61 are coaxially arranged, and cooling chamber 62 and exocoel 42 are equipped with import and outlet, and this import and outlet are used for the circulation of cooling fluid.Further, can also arrange high temperature resistant black coating (not shown) at the inwall of cooling chamber 62, it is conducive to improving heat transfer efficiency.When carrying out directional freeze, the heat-eliminating mediums such as liquid nitrogen can be loaded in cooling chamber 62.The second cooling system 6 pairs of synchronous material cool, drastically increase the cooling performance of Rapid Directional Solidification equipment, simultaneously by controlling the power of electron beam launcher 2 and the rising or falling speed of each pumping rod 31,51 and rotational velocity by the cut to lengthen in melting zone 7 at 0.5-2mm.
In addition, the gap formed between the first cooling system and the second cooling system 6 can be 1-5mm; And in directional freeze process, the melting zone 7 formed by electron beam heating material is strict controlled in this gap location, by controlling material microcosmic solidification path thus required particular organization's structure can being obtained.
Above-mentioned Rapid Directional Solidification equipment can realize 1 × 10
5-5 × 10
5the thermograde of K/cm and the speed of growth of 1-100mm/s.
Embodiment 2
Rapid Directional Solidification method of the present invention (i.e. electron-beam zone melting Rapid Directional Solidification technique) is adopted to prepare magnetostriction materials (Fe
0.83ga
0.17)
99.9la
0.1, comprise the steps:
1, prepare burden
The purity of raw material Fe, Ga and La of selecting all is greater than 99.99wt%, and in order to prevent melting loss of elements in fusion process, when being equipped with Fe, Ga and La raw material according to mentioned component, add Ga and La respectively according to the scaling loss amount of about 1wt%, for subsequent use after weighing good each raw material.
2, 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, when placing, the metallic element of easy scaling loss is placed in crucible bottom, and not easily the metallic element of scaling loss is placed in above crucible.
4.0 × 10 are evacuated to vacuum non-consumable arc-melting furnace
-3after Pa, in body of heater, be filled with high-purity argon gas, the volumn concentration (purity) of argon gas is more than 99.99%, treats that the vacuum tightness in stove rises to 1.0 × 10
-1pa stops inflation later, and repeatedly after this step operation three times, melting electric current is set to 150A, carries out melting to raw material, the time controlling each melting is about 4 minutes, melt back four times, obtained mother alloy ingot.
3, mother alloy rod is prepared
Above-mentioned obtained master alloy ingot is placed in vacuum non-consumable arc-melting furnace, 3.0 × 10 are evacuated to vacuum non-consumable arc-melting furnace
-3after Pa, in body of heater, be filled with the high-purity argon gas that volumn concentration is more than 99.99%, treat that in stove, vacuum tightness rises to 1.0 × 10
-1pa stops inflation later.
Melting electric current is set to 150A, master alloy melting ingot, when master alloy ingot soon melts rapidly by melting current setting to 300A, aim at master alloy ingot center, mould hole place arc blow-out, open vacuum casting valve simultaneously, utilize negative pressure to be cast in mould by the mother alloy liquid of instant melting and make mother alloy rod, its XRD diffracting spectrum as shown in Figure 2; Result shows: this mother alloy rod is polycrystalline tissue, and polycrystalline orientation is based on <110>, <100>.
4, (Fe is prepared
0.83ga
0.17)
99.9la
0.1rapid Directional Solidification orientation polycrystalline material
By above-mentioned obtained mother alloy rod outside surface grinding homogeneity, ultrasonic cleaning 10min under the frequency of 50KHz, is put in after cleaning in baking oven, dries 20min in 120 DEG C, obtains washed samples.
The Rapid Directional Solidification equipment of embodiment 1 is adopted to carry out directional freeze to material, first by mother alloy rod 9 and (Fe
0.83ga
0.17)
99.9la
0.1polycrystalline seed crystal 8 is separately fixed at the second pumping rod 51 of Rapid Directional Solidification equipment and the first pumping rod 31 end (such as respectively by chuck 52, chuck 33 is fixed), and respectively at inner chamber 41, exocoel 42, Ga-In alloy cooling fluid is loaded in cooling chamber 62, recirculated cooling water and liquid nitrogen, seed crystal 8 bottom is made to immerse Ga-In alloy cooling fluid, make the first pumping rod 31 and the second pumping rod 51 reverse rotation, and make mother alloy rod 9 lower ends and the gap location of seed crystal 8 upper end all between the first cooling system and the second cooling system 6, mother alloy rod 9 and the end of seed crystal 8 close to but do not contact, subsequently vacuum chamber 1 is evacuated to 3.0 × 10
-3after Pa, in vacuum chamber 1, be filled with the high-purity argon gas that volumn concentration is more than 99.99%, treat that in vacuum chamber 1, vacuum tightness rises to 1.0 × 10
-1pa stops inflation later, repeatedly after this step operation three times, start electron beam launcher 2 to heat the mother alloy rod 9 and seed crystal 8 that are positioned at gap location, arranging the first pumping rod 31 rotational velocity is 100r/min, second pumping rod 51 rotational velocity is 100r/min, and two bar senses of rotation are contrary, and arranging electron beam gun 2 incident current is 35mA, heating 2s makes seed crystal 8 and mother alloy rod 9 fuse into one and form about 0.6mm between two rods stablize melting zone, and the thermograde of control directional freeze is 3 × 10
5k/cm, the speed of growth is 10mm/s, make the material of melting along seed crystal 8 lower flat quietly downwards pull in Ga-In alloy cooling fluid, carry out Rapid Directional Solidification, during Rapid Directional Solidification, by Ga-In alloy cooling fluid, material lower end is cooled, utilize cooling tube 32 inject high pressure water coolant to cool material lower end, melting zone 7 length is about 1mm, and melting zone 7 is strict controlled in above-mentioned gap simultaneously, after growth terminates, be down to room temperature, take out the material after growth, obtained composition is (Fe
0.83ga
0.17)
99.9la
0.1bar-shaped magnetostriction materials (size Φ 7mm × 100mm).
(Fe
0.83ga
0.17)
99.9la
0.1as shown in Figure 3, wherein a place is the columanar structure in Rapid Directional Solidification stable growth stage to the vertical profile melting zone fast quenching metallograph of material, and the straight size of grain form is tiny; The melting zone pattern that b place is formed for electron beam heating alloys, melting zone form dimpling, zone length is about 1mm; C place is fast quenching terminal material casting rod polycrystalline tissue.Show thus: the inventive method is at preparation (Fe
0.83ga
0.17)
99.9la
0.1can obtain good column fine grained texture during bar, and for stablize dimpling solid-liquid interface in process of growth, zone length is about 1mm.
(the Fe of above-mentioned preparation
0.83ga
0.17)
99.9la
0.1as shown in Figure 4, result shows the XRD diffracting spectrum of material: material grain refining after Rapid Directional Solidification, [100] orientation obviously strengthen, and directional effect is good.(the Fe of above-mentioned preparation
0.83ga
0.17)
99.9la
0.1as shown in Figure 5, result shows the BSE photo of material: this material internal there is no obvious precipitated phase, and material is uniform single phase structure, and therefore obtained is a kind of non-equilibrium Nonequilibrium Materials.
In addition, magnetostriction measurement system (Beijing WuKe opto-electrical Technology Co., Ltd's production) is adopted to measure (Fe
0.83ga
0.17)
99.9la
0.1the magnetostrictive strain value of material, wherein foil gauge adopts Japanese republicanism KFG-1-120-C1-11L3M2R type resistance strain gage, and result as shown in Figure 6.Result shows: (Fe
0.83ga
0.17)
99.9la
0.1the saturation magnetostriction constant of material is 600ppm, and saturation magnetic field is only about 400Oe, Magnetostriction and comprehensive usability good.
Embodiment 3
Club-shaped material (Mn is prepared with reference to embodiment 2 method
54al
46)
0.97c
0.03, wherein adopt the Rapid Directional Solidification equipment of embodiment 1 to carry out directional freeze to material, and the thermograde controlling directional freeze is 3 × 10
5k/cm, the speed of growth is 10mm/s, and obtained composition is (Mn
54al
46)
0.97c
0.03club-shaped material.
(Mn
54al
46)
0.97c
0.03as shown in Figure 7, the wherein melting zone pattern that formed for electron beam heating alloys of Fig. 7 central part, melting zone form dimpling, zone length is about 1mm to the vertical profile melting zone fast quenching metallograph of material, shows that the inventive method is at preparation (Mn thus
54al
46)
0.97c
0.03the melting zone of stable about 1mm can be obtained during alloy material.
(the Mn of above-mentioned preparation
54al
46)
0.97c
0.03as shown in Figure 8, result shows the vertical profile metallograph of material: this material columnar grain is straight tiny, and directional effect is obvious, and grain refining is remarkable.(Mn
54al
46)
0.97c
0.03the XRD diffracting spectrum of material as shown in Figure 9, the characteristic peak of obvious τ phase has been there is in this collection of illustrative plates, and 41.3 ° and 45.6 ° of peaks strong higher, represent that this material has stronger [101] orientation and [110] orientation, the τ phase constitution of orientation that illustrative material has [101], namely forms a kind of non-equilibrium Nonequilibrium Materials.
In addition, (Mn
54al
46)
0.97c
0.03the M-H curve of material as shown in Figure 10.Result shows: use present invention process preparation (Mn
54al
46)
0.97c
0.03during alloy, can obtain the obvious τ phase of a large amount of orientations in the material, and column crystal refinement is remarkable, significantly improve coercive force and the remanent magnetism of alloy, this material has the coercive force of 1500Oe and the remanent magnetism of 30emu/g.(Mn
54al
46)
0.97c
0.03alloy is as the novel non-rare earth permanent-magnetic material of a class, and its τ phase has very large saturation magnetization, and τ phase content is more, material orientation is better, and material monolithic magnetic energy product is higher, has huge application prospect.
Reference examples 1
This reference examples adopts LMC laser zone remelting apparatus for directional solidification to carry out directional freeze to mother alloy rod prepared by embodiment 2, LMC laser zone remelting apparatus for directional solidification adopts superpower Nd:YAG solid statelaser as heating source, and only adopt Ga-In alloy cooling fluid as heat-eliminating medium, when utilizing this apparatus for directional solidification to carry out directional freeze, the thermograde of directional freeze is 1 × 10
5k/cm, the speed of growth is 0.3mm/s, the BSE photo of obtained material as shown in figure 11, result shows: the precipitated phase of the spherical shape of the obvious adularescent of this material internal, detecting the precipitate of this spherical shape known through EDS is Nd-rich phase, and what show prepared by this reference examples thus is a kind of balancing material.In addition, the Magnetostriction curve of this material as shown in Figure 6.Result shows: the saturation magnetostriction constant of material prepared by this reference examples is 250ppm, and saturation magnetic field is about 500Oe.
LMC laser zone remelting directional freeze is adopted to prepare (Fe in this reference examples
0.83ga
0.17)
99.9la
0.1material, can realize higher thermograde (1 × 10
5k/cm), but due to the speed of growth comparatively slow (0.3mm/s), therefore speed of cooling (R
c=G
l× V) be only 3 × 10
3k/s, lower than embodiment 2 technique used two orders of magnitude.(Fe
0.83ga
0.17)
99.9la
0.1when the Nonequilibrium Materials special as a class, need the speed of cooling be exceedingly fast could be solidly soluted in FeGa matrix by force by not solid solution thick atom La in preparation process, otherwise will separate out at intergranular and intracrystalline with the form of second-phase, the Nd-rich phase of separating out serves the effect of pinning magnetic domain in magnetic history, causes the Magnetostriction of material monolithic to decline.In above-described embodiment 2, high-temperature liquid-phase structure can be remained into room temperature by electron-beam zone melting Rapid Directional Solidification technique used well, La atom is made to be present in FeGa basal body structure in the mode of substitutional solid solution, this solid solution brings strong tetragonal distortion to matrix, and this distortion result in material macroscopic body and reveals big magnetostriction.
Reference examples 2
Club-shaped material (Mn is prepared with reference to reference examples 1 method
54al
46)
0.97c
0.03, wherein the thermograde of directional freeze is 1 × 10
5k/cm, the speed of growth is 0.3mm/s, and obtained composition is (Mn
54al
46)
0.97c
0.03material.
(the Mn of above-mentioned preparation
54al
46)
0.97c
0.03the XRD diffracting spectrum of material as shown in figure 12, there is the characteristic peak of ε phase the positions such as 38.4 °, 41.2 °, 43.7 °, 77.1 ° in it, peak is comparatively obvious by force, illustrates that this material is ε phase constitution, it is a kind of balancing material for non-ferromagnetic phase, does not possess magnetic property.
Last it is noted that above each embodiment is only in order to illustrate technical scheme of the present invention, be not intended to limit; Although with reference to foregoing embodiments to invention has been detailed description, those of ordinary skill in the art is to be understood that: it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein some or all of technical characteristic; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the scope of various embodiments of the present invention technical scheme.
Claims (10)
1. a Rapid Directional Solidification equipment, is characterized in that, comprises vacuum chamber, electron beam launcher, the first pull system, the first cooling system, the second pull system and the second cooling system,
Relatively with top in the bottom of described vacuum chamber offer bottom through-hole and top through hole, the middle part sidewall of described vacuum chamber offers electron beam window;
Described electron beam launcher is arranged on the outside of described vacuum chamber, and described electron beam launcher ejected electron bundle can enter described vacuum chamber by described electron beam window;
Described first pull system comprises the first pumping rod and cooling tube, described first pumping rod hollow and vertically plug in described vacuum chamber by described bottom through-hole, described first pumping rod is driven by motor and can be elevated and spinning motion, and it is inner that described cooling tube is arranged on described first pumping rod;
Described first cooling system is positioned at described internal vacuum chamber, and it comprises inner chamber and exocoel, and it is outside that described inner chamber is around in described first pumping rod, and described exocoel is around in described lumen outer;
Described second pull system comprises the second pumping rod, described second pumping rod vertically plugs in described vacuum chamber by described top through hole, and described second pumping rod is driven by motor and can be elevated and the spinning motion identical or contrary with described first pumping rod spinning motion direction;
Described the second cooling system is arranged on above described first cooling system and also and between described first cooling system forms gap, described the second cooling system has the through hole that coaxially arranges with described first pumping rod and can cool the material being positioned at described through hole, and described electron beam launcher ejected electron bundle can pass from described gap.
2. Rapid Directional Solidification equipment according to claim 1, is characterized in that, the voltage of described electron beam launcher is 80kV, and power is 10kW, and sweep rate is 0-10000Hz.
3. Rapid Directional Solidification equipment according to claim 1 and 2, is characterized in that, described electron beam launcher is high pressure Pierce electron gun.
4. Rapid Directional Solidification equipment according to claim 1, is characterized in that, the angle between described electron beam launcher ejected electron bundle and horizontal plane is-5 °-5 °.
5. Rapid Directional Solidification equipment according to claim 1, is characterized in that, the velocity range of the up-and-down movement done by motor-driven first pumping rod is 0-100mm/s, and the velocity range of spinning motion is 0-6000r/min; The velocity range of the up-and-down movement done by motor-driven second pumping rod is 0-100mm/s, and the velocity range of spinning motion is 0-6000r/min.
6. Rapid Directional Solidification equipment according to claim 1, is characterized in that, described gap is 1-5mm.
7. Rapid Directional Solidification equipment according to claim 1, it is characterized in that, described the second cooling system comprises metal tube and is around in the cooling chamber of described metal tube outside, through hole and described first pumping rod of described metal tube are coaxially arranged, and described cooling chamber and described exocoel are equipped with import and outlet.
8. Rapid Directional Solidification equipment according to claim 7, is characterized in that, arranges black coating at the inwall of described cooling chamber.
9. a Rapid Directional Solidification method, is characterized in that, comprises the steps:
1) mother alloy rod is prepared:
After being equipped with raw material according to the component requirements of unidirectional solidification material, the raw material of outfit being smelted into mother alloy ingot, melting described mother alloy ingot, and make mother alloy rod by vacuum casting;
2) the arbitrary described Rapid Directional Solidification equipment of claim 1 to 8 is used to carry out directional freeze:
Described mother alloy rod and seed crystal are separately fixed at the second pumping rod and the first pumping rod end of described Rapid Directional Solidification equipment, alloy cooling fluid and circulating cooling liquid is loaded respectively in described inner chamber and exocoel, and make described seed crystal bottom immerse alloy cooling fluid, make described first pumping rod and described second pumping rod reverse rotation, and after starting described the second cooling system, shielding gas is filled with to described vacuum chamber, start electron beam launcher subsequently to heat the mother alloy rod and seed crystal that are positioned at described gap, first pumping rod described in pull and the second pumping rod carry out directional freeze in the same way, and the thermograde controlling described directional freeze is 1 × 10
5-5 × 10
5k/cm, the speed of growth is 1-100mm/s, obtained unidirectional solidification material.
10. Rapid Directional Solidification method according to claim 9, is characterized in that, the drawing velocity controlling described first pumping rod is 1-10mm/s, and the speed of spinning motion is 60-6000r/min; And the drawing velocity controlling described second pumping rod is 1-10mm/s, the speed of spinning motion is 60-6000r/min.
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