CN1184036C - Prepn process of TbDyFe-base directionally solidified alloy crystal - Google Patents
Prepn process of TbDyFe-base directionally solidified alloy crystal Download PDFInfo
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- CN1184036C CN1184036C CN02110945.1A CN02110945A CN1184036C CN 1184036 C CN1184036 C CN 1184036C CN 02110945 A CN02110945 A CN 02110945A CN 1184036 C CN1184036 C CN 1184036C
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Abstract
The present invention discloses a preparation process of TbDyFe-base magnetostriction alloys suitable for production requirements. The process uses a cold crucible induction furnace to prepare master alloys to substantially raise the preparation efficiency and the quality of master rods and solves the difficult problem of directional solidification in melting with a resistance heater due to the design of a plurality of heating structures. The quality and the preparation efficiency of crystals are raised and a magnetic heat treatment method with high efficiency is developed by a method of conducting several times of directional solidification in one operation cycle and a method of simultaneously conducting the directional solidification to a plurality of master rods by a technology of preparing crystals with various diameters. The present invention has no requirement that the processed alloys must be twin single crystals.
Description
Technical field:
The invention belongs to preparation directional freeze TbDyFe base magnetic striction alloy technology.
Background technology:
The rareearth super magnetostrictive alloy is a kind ofly can produce very big strained RFe in magnetic field
2Compound (R refers to rare earth element) mainly comprises (TbDy) Fe
2Alloy and SmFe
2Alloy two classes, that the most frequently used is Tb
0.3Dy
0.7Fe
1.95Alloy (Terfenol-D).The TbDyFe alloy is generally used the vacuum non-consumable arc furnace master alloy melting, handles in vacuum oriented solidification equipment, alloy is formed have＜tissue of 112〉orientation crystallographic orientation, heat-treats then.
Directional freeze about Terfenol-D is handled, and prepares monocrystalline with the Czochralski technology in early days.Savage in 1981 etc. have adopted the Bridgeman technology in U.S. Patent No. 4308474: with induction coil the female rod in the tubulose crucible is melted, crucible descends with certain speed.The U.S. Patent No. 4609402 that O.D.McMasters in 1986 delivers is used the floating region zone melting techniques: female rod is positioned the axle center of vertical tubular type quartz chamber, makes female clavate become the melting zone with induction coil, and along with inductor block moves from bottom to top, the melting zone moves upward.E.D.Gibson in 1988 etc. have delivered improved Bridgman technology in U.S. Patent No. 4770704.This technology is put into the crucible of upper of furnace body with some ingots, makes the furnace charge fusing evenly with medium frequency induction power supply, and alloy liquid injects the quartz molds pipe by the hole of crucible bottom.On this basis, U.S. ETREMA company has set up ETREMA Crystal Growth technology from nineteen ninety-five, is used for producing in batches.
Be equipped with other technology of major diameter crystalline with the MB legal system and also comprise K.Murakami resistance furnace melting batch, move down the method (U.S. Patent No. 5067551 of crucible then, 1991), Murakami is molten female excellent with the high-frequency induction coil district, the method that crucible and bar all move down (U.S. Patent No. 5063986,1991), the S.Okatomo molten induction coil of the outer high frequency region of quartz chamber that moves up, and (see Int.Symp.On GMSM and their Appl. with the method that thermal insulation element improves the directional freeze condition, Tokyo, 1992,175～180), and usefulness ion arc such as E.Nakamura dissolves the furnace charge in the water jacketed copper crucible, crucible bottom has and the cold long mould of water receiving, and the carriage in the mould is drop-down continuously, and alloy liquid progresses into the continuous processing technology that mould solidifies and (sees U.S. Patent No. 5114467,1992), or the like.
Above-mentioned review shows that the directional freeze of Terfenol-D is handled and adopted high-frequency induction coil as well heater mostly, and utilizes not appearing in the newspapers as yet of the molten formula directional freeze processing in resistive heating district.
Summary of the invention:
The technological method that the purpose of this invention is to provide preparation high-performance TbDyFe base directional solidificating alloy, it should have higher preparation efficiency, lower production cost, adapt to industrial scale.
1, the method for preparing the TbDyFe base alloy directionally solidified crystal provided by the present invention, its operation is mother alloy preparation, directional freeze, thermal treatment and thermomagnetic treatment, it is characterized in that:
A, mother alloy preparation section are: before melting, make the stopper rod head stop up the crucible orifice; When heat-processed generation frame material, move up and down the stopper rod head with loosening furnace charge; In changing the material process, rotate and move up and down the stopper rod head, stir the alloy liquation; Rising stopper rod head is raised the alloy pig that solidifies after the melting in crucible, and head upset alloy pig is controlled in operation, sends the alloy pig that is reversed back to the crucible remelting, makes the alloy liquation enter mould then and is frozen into the mother alloy rod;
B, directional freeze operation are: the internal diameter of earlier seed crystal and female rod being packed into is slightly larger than the crucible of female rod, then body of heater is vacuumized, and is higher than 10 in vacuum tightness
-1Behind the Pa, rapidly charged pressure be-0.09～+ rare gas element of 0.2MPa; Using then around the molten formula resistance heater of the pressure of female rod makes the upper end of seed crystal and the lower end of female rod form the melting zone, drop-down again and rotation melting zone is left the high-temperature zone and is moved to the water cooler direction, the melting zone is solidified from bottom to top, new melting zone is moved up along female rod, continue to carry out this process ,-process of setting molten up to the district finished at the excellent top of mother; In this process, the melting zone temperature should be controlled in 1260～1380 ℃ of scopes, the melting zone width should be controlled with female excellent diameter roughly the same, movement velocity of melting zone is in 0.5～30mm/min scope, speed of rotation is got 0.5～30rpm, and the alloy bar of this process of process has crystallographic orientation tissue or twin single crystal organization.
C, thermal treatment and thermomagnetic treatment operation are:
The directional solidificating alloy rod is carried out dynamic thermal treatment, and promptly treatment temp fluctuates near 800～1100 ℃ of eutectic temperatures, slowly cooling after 1～5 hour.Then alloy bar is put into the vertical silica tube of tubular axis and field direction, silica tube is vacuumized and charges into rare gas element, startup is around the process furnace of silica tube, make alloy bar 380～580 ℃ of scope internal heating 0.5～3 hour, after this reduce to 280～340 ℃ when temperature, start magnetic field, make the magnetic field temperature reach 240～960KA/m, silica tube is pivoted with 0.2～10rpm rotating speed, and keep slowly cooling after 0.5～3 hour.
In said process, by the stopper rod crown portion of drive control blade is housed, make it to pump simultaneously at the rotation whipping process.Resistance heater is made up of 2～3 heating zones, and the superiors are preheating section, and the middle level is a high temperature section, is preferably in lower floor holding-zone is set, and makes high temperature section formation temperature gradient up and down.The melting zone can be repeated repeatedly along the excellent moving process of mother.The temperature in melting zone is preferably in 1280～1330 ℃, and movement velocity of melting zone is preferably in 2～15mm/min, and speed of rotation is preferably got 2～15rpm.The alloy bar thermal treatment temp is preferably in fluctuation in 900～1000 ℃.The alloy bar that is arranged in silica tube is in the thermomagnetic treatment process, preferably make alloy bar 400～500 ℃ of temperature range internal heating 1～2 hour, starting magneticstrength when preferably cooling the temperature to 310～330 ℃ then is the magnetic field of 400～640KA/m, silica tube rotates with 0.5～2rpm rotating speed simultaneously, after heating 1～2 hour, keeping slowly cooling under magnetic field and the silica tube operating condition then.
The present invention proposes the technology of more complete preparation directional freeze TbDyFe base magnetic striction alloy, be suitable for that high-level efficiency prepares high performance product under working condition, the crystal that comprises all sizes such as microlite and coarse crystal has all been proposed rational preparation technology.
Aspect mother alloy prepared, present technique mainly adopted the cold crucible vacuum induction furnace as melting and casting equipment.Compare with vacuum non-consumable arc furnace, preparation efficiency of the present invention is much bigger, the requirement that is suitable for producing.Compare with the conventional vacuum induction furnace, alloy is remelting repeatedly, can adjust to ideal accuracy and homogeneity to composition, and the defective material that produces in melting-castingprocesses can melt down, and has reduced preparation cost.Use has the cold crucible vacuum melting furnace that stirs-turn over ingot-casting operation system and carries out melting and casting, has further improved preparation efficiency, female excellent quality and lumber recovery.
Compare with induction heater, be heated by resistive device and carry out directional freeze and handle that to have equipment cost low, temperature is measured easily and is controlled, and the heat penetration depth is big, helps preparing advantages such as coarse crystal.Method proposed by the invention has solved the difficulty that is heated by resistive the molten formula directional freeze in device district, has alleviated the pollution of crucible material to alloy; Utilize control to feed the technology of female rod, eliminated the disturbance to molten bath when molten of female rod district; By holding-zone being set at well heater, hot-fluid is prevented from along the radial transport of alloy bar, guaranteed the axial transmission of hot-fluid; Utilization is provided with several melting zones in a well heater, make can realize directional freeze several times in a cycle of operation; Utilize technology of the present invention, can also be implemented in a cycle of operation carries out directional freeze to many female rods simultaneously and handles.These technology provide assurance for effect and the raising processing efficiency that improves directional freeze.In addition, the present invention is the technology that the preparation microlite designs, and makes to utilize resistance heater to realize that it is possible that the floating region district is melt into.
Aspect thermal treatment, the present invention adopts the dynamichandling technology to shorten the treatment time.Aspect thermomagnetic treatment, the technology that the present invention proposes makes the directionally solidified crystal of non-twin monocrystalline also can carry out this processing, and does not need to carry out metallographicobservation, makes thermomagnetic treatment can be used for production process.
Description of drawings:
Fig. 1 has represented mother alloy rod preparation system synoptic diagram, wherein
The 1-induction power supply, 2-vacuum melting furnace, 3-vacuum-inert gas system, the 4-electrical control system, 5-crucible, 6-are annotated stopper rod mechanism (6-1-stopper rod head, the 6-2-driving stem, 6-3-power-transmission rig, the 6-4-blade), (7-1-controls head to 7-ingot tumbler structure, the 7-2-operating stick), 8-Casting Mechanism (8-1-mould, 8-2-die frame, 8-3-mold heated-attemperator).
Fig. 2 has represented the directional freeze system schematic, wherein
9-mother alloy rod, 10-body of heater, 11-vacuum-inert gas system, 12-power supply-heater system (12-1-power supply, 12-2-resistance heater, 12-3-temperature probe, the 12-4-temperature regulating device), 13-furnace charge treatment system (13-1-crystal pulling rod, 13-2-crystallizer, the 13-3-crucible, the 13-4-water cooler, 13-5-heat insulating mattress, 13-6-feeding rod), the 14-drive system, the 15-seed crystal.
Fig. 3 has represented that several districts melt formula resistive heating method synoptic diagram, wherein
A-simple heaters (12-2-well heater),
The B-multy-membered heating radiator (12-2 '-the 1-preheating section, 12-2 '-2-high temperature section, 12-2 '-3-holding-zone),
Many melting zones of C-well heater (12-2 " 1-preheating section, 12-2 " 2-high temperature section, 12-2 " 3-holding-zone, 12-2 " 4-interlude),
The double-deck well heater (12-2 -1-auxiliary heater, 12-2 -2-primary heater) of D-.9-mother alloy rod, the 9-1-melting zone.
Fig. 4 has represented vacuum oriented coagulation system drive pattern synoptic diagram, wherein
A-well heater move up (12-2-well heater),
B-does not move female rod and well heater (12-2-a ,-b ,-c ,-d, each section that-e well heater is bottom-up).9-mother alloy rod, 13-1-crystal pulling rod, 13-2-crystallizer, 13-3-crucible, 13-4-water cooler, 13-5-heat insulating mattress, 13-6-feeding rod, 15-seed crystal.
Fig. 5 has represented the excellent directional freeze pattern diagram of dissimilar mothers, wherein
The A-intermediate diameters is rod slightly, the thin rod of B-intermediate diameters, and C-major diameter rod, the D-small-diameter rods, how excellent E-is.
9-mother alloy rod, 12-2-well heater, 13-1-crystal pulling rod, 13-2-crystallizer, 13-3-crucible, 13-4-water cooler, 13-5-heat insulating mattress, 13-6-feeding rod, 15-seed crystal.
Fig. 6 has represented thermomagnetic treatment technology synoptic diagram
9-mother alloy rod, 16-Quartz stove tube, 17-electro-magnet, the rotatable vacuum-sealing of 18-, 19-vacuum-inert gas system, 20-process furnace.
Embodiment:
The equipment that ad hoc proposal of the present invention adopts my patent application (01274217.1) formerly to be proposed prepares mother alloy, as shown in Figure 1.This equipment is provided with a cover and stirs-turn over ingot-casting operation system, and it comprises annotates stopper rod mechanism (6), ingot tumbler structure (7) and several parts of Casting Mechanism (8).Annotating stopper rod mechanism is made up of stopper rod head (6-1), driving stem (6-2) and power-transmission rig (6-3).The stopper rod head is the element that can insert and stop up crucible bottom orifice (5-1), and upper surface can have short blade (6-4), and the lower end links to each other with driving stem.The dead in line of the axis of driving stem and crucible orifice, it stretches out body of heater (2) by vacuum-sealing downwards and combines with power-transmission rig.Power-transmission rig can move up and down the stopper rod head by driving stem and rotates around the crucible axis.Recirculated water is received the stopper rod head makes its refrigerative effect to driving stem in addition.Ingot tumbler structure (7) is positioned at crucible top, and it has the effect of the alloy pig that overturns by controlling controlling head (7-1) and handling the operating stick (7-2) of controlling head and form of alloy pig.Around driving stem (6-2), it mainly is made up of mould (8-1) and die frame (8-2) Casting Mechanism (8) below crucible.Mould has single tube mould and multitube mould two classes.This mechanism generally also need to be provided with mould heating or (with) attemperator (8-3).
There is loosening furnace charge in this system, stirs feed liquid, turns over the ingot remelting, directly multiple function such as casting.Before melting, should make stopper rod head (6-1) stop up crucible orifice (5-1); When in heat-processed, the frame material taking place, can become flexible furnace charge by moving up and down the stopper rod head; In changing the material process, rotate and move up and down the stopper rod head and can stir alloy liquid; Rising stopper rod head is raised the alloy pig that solidifies after the melting in crucible, and operation ingot tumbler structure upset alloy pig sends back to crucible with the alloy pig that is reversed then and accepts remelting.Drop-down stopper rod head (6-1) after fusion process is finished makes the stopper rod head move to mould (8-1) from crucible orifice (5-1), and alloy liquid just enters mould thereupon and solidifies.This system makes operations such as alloying, homogenizing and casting concentrate on a heat and finishes, and has improved preparation efficiency, has improved quality product, has reduced production cost.Utilize the Casting Mechanism of this system can many mother alloy rods of one-step casting, can improve the compactness of female rod, reduce metallurgical shortcoming, improve lumber recovery by pressure die casting or centrifugal casting technique.
Mother alloy rod (9) is in apparatus for directional solidification, as shown in Figure 2.Carry out directional freeze with the molten formula resistance heater in district and handle, this equipment mainly consists of the following components:
(1) system of bf body (10).The vertical metal body of heater of general use also can be used quartzy body of heater.They should have good vacuum leakproofness.
(2) vacuum-inert gas system (11).Effect is vacuum condition to be provided and to charge into the rare gas element (as Ar gas) of protectiveness for body of heater.Rare gas element preferably adopts high-purity gas.
(3) well heater-power-supply system (12).Power supply (12-1) provides stable interchange or galvanic current to annular resistance heater (12-2).Well heater generally is contained in body of heater inside, around female rod (9).When using quartzy body of heater, well heater also can be contained in the outside of body of heater, around body of heater.This system also comprises near temperature probe (12-3) and the control device (2-4) that is installed in the melting zone.The thermo electric material of well heater can be that high-quality NiCr is that alloy or high-quality FeCrAl are common electrical thermalloys such as alloy, also can be Pt, W, Mo, Ta, graphite, SiC or MoSi
2Deng the high-melting-point material.There is thermal insulation layer the outside of thermo electric material.
(4) furnace charge treatment system (13).Mainly be made up of the metal crystal pulling rod (13-1) of water-cooled, the water mold (13-2) of crystal pulling rod head and the tubulose crucible (13-3) that is contained on the crystallizer, the mother alloy rod is placed in the crucible.Crystal pulling rod straight down, crucible is generally made of the high-quality heat resisting ceramic materials, the dead in line of the two.Between female excellent bottom and crystallizer, seed crystal (15) is arranged preferably, preferably install the water cooler (13-4) of and crystal pulling rod excellent around mother in well heater (12-2) below, well heater is with the annular heat insulating mattress (13-5) that preferably has between the water cooler around the crystal pulling rod of female rod, and it uses heat-stable ceramic material.
(5) drive system (14).Act on and drive crystal pulling rod moving axially along female rod.This system preferably can drive the axis rotation of crystal pulling rod around female rod simultaneously, makes the temperature of female rod on same cross section even.
The internal diameter of being packed in seed crystal (15) and female excellent (9) earlier is slightly larger than the crucible (13-3) of female excellent diameter, then body of heater (10) is vacuumized, and is higher than 10 in vacuum tightness
-1Pa (is to be higher than 10
-2Pa) after, rapidly charged pressure be-0.09～+ 0.2Mpa (be preferably-0.06～+ 0.1MPa) rare gas element.For guaranteeing the atmosphere cleaning, the operation that vacuumizes-inflate can move for several times.If do not possess perfect vacuum system, also can not vacuumize or only take out elementary vacuum, wash body of heater with rare gas element then, atmosphere cleaning in body of heater.
In the directional freeze process, make the upper end of seed crystal (15) and the lower end fusing of female rod (9) form melting zone (9-1) with well heater (12-2) earlier, drop-down then crystal pulling rod (13-1) (preferably rotation simultaneously), make the melting zone that formed in the high-temperature zone of leaving well heater in the mobile process of water cooler (13-4) bottom-up solidifying, new melting zone is moved up along female rod.This process continues to carry out, and, process of setting molten until the district finished at the excellent top of mother.For in order to be effective, the directional freeze process can repeat 1 time or several.In this process, the melting zone temperature should be controlled at 1260～1380 ℃, preferably is controlled at 1280～1330 ℃, and the melting zone width should be controlled identically substantially with the diameter of female rod; Desirable 0.5～the 30mm/min of the translational speed of crystal pulling rod preferably gets 2～15mm/min; Speed of rotation is got 0.5～.0rpm, preferably gets 2～15rpm.The alloy bar of handling through directional freeze has the tissue of crystallographic orientation or the tissue of twin monocrystalline.
In order to shorten the duration of contact of the same sidewall of crucible of alloy liquid (13-3), use the resistance heater (12-2) that produces the molten heats in district.Molten bath (9-1) produced when molten in the district for fear of female rod and to impact and disturbance, be preferably in the top installing feeding rod (13-6) of female rod (9), the upper end of the female rod of clamping, its axis should with the dead in line of crystal pulling rod (13-1).Use another drive system (14 ') to move down feeding rod, in the process that the melting zone moves up along female rod,, guarantee the stability in melting zone in time with mother's rod feeding melting zone (13-3).Use the technology of feeding rod to be applicable to that also induction heater carries out the treating processes of directional freeze.
Translational speed (the V of feeding rod (13-6)
2) should with the translational speed (V of crystal pulling rod (3-1)
1) coupling: if the internal diameter of crucible (13-3) is D
1, the diameter of female rod (9) is D2, then V
1* D==V
2* D
2, i.e. V
2=V
1* D
1/ D
2Feeding rod in the process that moves down, preferably simultaneously around the curve rotation of female rod, turning direction preferably and the direction of rotation of crystal pulling rod, speed of rotation is close.
In order to realize distinguishing the directional freeze of molten formula, the present invention has proposed following several designs (Fig. 3) to resistance heater (12-2):
(1) simple heaters (12-2) (Fig. 3-A)
The height of this well heater is less, by limitation in height melting zone (9-1) width of well heater itself.The difficulty that produces local melting zone with little well heater in female rod is bigger, so the most handy materials with high melting point of this well heater is made.
(2) multy-membered heating radiator (12-2 ') (Fig. 3-B)
The height of this well heater is bigger, and it is made up of several heating zones, and the temperature of each section detects respectively and controls.The simplest situation is the two-part well heater, and the one section broad (12-2 '-1) above it is provided with the zero pour that temperature is lower than alloy, is used for the female rod of preheating (9); One section following (12-2 '-2) are narrower, and the fusing point that temperature is higher than alloy is set, and it makes female rod produce melting zone (9-1).Because high temperature section is the female excellent local heating to preheating, so be easier to form the melting zone, its role is to stop the radial heat flows of alloy liquid at process of setting, impel type of thermal communication to cross crystal pulling rod (13-1) and the concentrated axially transmission downwards of water cooler (13-4), guarantee the effect of directional freeze along crystal (9).In addition, preheating section and holding-zone can also comprise several sections respectively, make the temperature of close high temperature section higher, and be lower away from the temperature of high temperature section, and the heating and cooling speed of slowing down female rod prevents that female rod from ftractureing.
The thermo electric material of each section of well heater can be identical, also can be different, but the most handy materials with high melting point of high temperature section is made.
(3) many melting zones well heater (12-2 ") (Fig. 3-C)
This also is a kind of multy-membered heating radiator, but is provided with several high temperature section (12-2 " 2), can carry out the molten directional freeze in several district to female rod and handle in an operational process.Well heater has preheating section (12-2 " 1) topmost, and preferably there is holding-zone (12-2 " 3) bottom, and interlude (12-2 " 4) is arranged between the high temperature section.The most frequently used is two melting zones well heaters.High temperature section the fusing point that temperature is higher than alloy is set, preheating section, holding-zone and interlude the zero pour that temperature is lower than alloy is set.Similar to the multy-membered heating radiator of front, preheating section, holding-zone and interlude also can comprise several heating zones respectively.The material selection principle of each section of well heater is identical with multy-membered heating radiator.
(4) double-deck well heater (12-2 ) (Fig. 3-C)
This well heater comprises two-layer, and the temperature of each layer detects respectively and controls.The highly bigger auxiliary heater (12-2 -1) of outer use is provided with the zero pour that temperature is lower than alloy, produces the effect of preheating and insulation, can make of the common electrical hot material; Internal layer uses narrower primary heater (12-2 -2), and the fusing point that temperature is higher than alloy is set, and is used to produce the melting zone, and the most handy materials with high melting point is made.In auxiliary heater, primary heater preferably is positioned at its position on the lower side, middle part, preferably is provided with two or more along female rod (9) axle and the primary heater of arranging and have mutually certain intervals.When two primary heaters are set, can realize the molten directional process in district twice at an operational process.Auxiliary heater can be an one-part form, also can be multi-stage type.
4, the drive pattern of directional freeze
The front is all according to the drive pattern design directional solidification technique that moves down female rod.Except that this mode, can also use following drive pattern:
(1) drives the well heater (Fig. 4-A) that moves up
(14 ") drive well heater (12-2) and move up, and heat insulating mattress (13-5) and water cooler (13-4) should be followed mobile, and crystal pulling rod (13-1) does not move to use drive system.If feed female rod (9) with feeding rod (13-6), the speed that feeding rod moves down should be with the translational speed coupling of well heater.The structure of the well heater of this pattern and equipment other parts with move down the identical of female excellent pattern, the district is molten also similar with the process of directional freeze, comprises that crystal pulling rod and feeding rod preferably can pivot.
(2) do not move female rod and well heater (Fig. 4-B)
When adopting this drive pattern, the molten and directional freeze process in district relies on regulates well heater (12-2) temperature and realizes along the variation of female rod (9) axis direction.Crystal pulling rod (13-1) and well heater (12-2) all do not move.The structure of well heater is similar to multy-membered heating radiator (12-2 '), but height should should make whole female rod be positioned at the height of well heater greater than the length of female rod.The mode of regulating each section temperature is: make female rod form melting zone (9-1) in the bottom stage (12-2-a) of well heater earlier; Make the melting zone move to a section (12-2-b) upwards then, make the alloy graining of bottom stage; Again, a section (12-2-c) that the melting zone is moved to go up again makes the alloy graining of a section (12-2-b) below it.Regulate so successively, female rod of one section is distinguished molten and is solidified until the top.More than the molten section in district, the design temperature of each section should be lower than the zero pour of alloy.They can be identical, also can set the molten section rising piecemeal towards the district for; Below the molten section in district, the design temperature of each section also should be lower than the zero pour of alloy, and they can be identical, also can set for to leave Qu Rongduan and reduce piecemeal.The hop count of well heater is many more, and the effect of directional freeze is good more.If feed female rod with feeding rod (13-6), the speed that feeding rod moves down should be with the temperature regulation process coupling of well heater, and crystal pulling rod and feeding rod preferably can pivot.
5, the selection of directional solidification technique pattern
The device structure of the 2nd to 4 of front and technology are all applicable for various female rod (9) conditions (diameter, length and quantity) in principle, but select different technology modes can obtain the preparation efficiency of better directional solidification effect and Geng Gao according to physical condition.For example:
(1) the single female rod preparation of intermediate diameters
When the diameter of female rod (9) is big with use multy-membered heating radiator (12-2 ') particularly many melting zones well heater (12-2 ") is (Fig. 5-A) better; Because the individual layer resistance heater is difficult realizes narrow melting zone, thus when the diameter of female rod hour, better to use double-deck well heater (12-2 ), preferably install two primary heaters (12-2 -2), so that improve the effect (Fig. 5 B) of directional freeze.
Though use feeding rod (13-6) can produce better directional solidification effect, because female excellent diameter is less to the impact in molten bath to fusing when little, the control difficulty of feeding rod is bigger, so can not use feeding rod under this condition.
(2) the female rod preparation of large diameter single (Fig. 5-C)
When handling the female rod of major diameter (9), female rod can produce bigger impact to molten bath (9-1) when the district was molten, so preferably feeding rod (13-6) clamping and feed female excellent.During operation,, move female rod or crucible and make female rod, utilize well heater (12-2) to make the formation melting zone, zone of action of female rod and seed crystal with the seed crystal contact with pack into crucible (13-3) bottom of seed crystal (15).Then, same crystal pulling rod of feeding rod (13-1) or well heater move up the melting zone with the same moved further of the speed of accurate coupling.
The female rod of major diameter requires wide melting zone, so can adopt multy-membered heating radiator heating (12-2 ').Though simple heaters can be used, it does not have heat insulation effect for the alloy of below, melting zone, can not stop radial heat flows, and the alloy that solidifies is easy to cracking; Though double-deck well heater (12-2 ) also can use, its structure is complicated, and the control difficulty is bigger.
(3) the female rod preparation of minor diameter list (Fig. 5-D)
The female rod of minor diameter (9) is though can adopt and the identical directional solidification technique of the female rod of intermediate diameters, because the specific surface area of thin crucible is very big, the tendency that produces surface reaction and surface shortcoming is serious, so the most handy floating region zone melting technique is carried out directional freeze.At this moment must install feeding rod (13-6), but not use crucible (13-3), the upper/lower terminal of female rod is respectively by crystal pulling rod (13-1) and feeding rod (13-6) clamping.Well heater (12-2) produces melting zone (9-1) in the bottom of female rod earlier, and the melting zone relies on the surface tension of alloy liquid to keep stable.Then, crystal pulling rod moves down with identical speed with feeding rod, or traveling heater only, and the melting zone is moved up.Crystal pulling rod preferably also pivots with identical speed and direction with feeding rod.
When using seed crystal (15), the lower end of seed crystal is respectively by crystal pulling rod (13-1) clamping, and the upper end of female rod is by feeding rod (13-6) clamping, and mobile crystal pulling rod or feeding rod make the following end in contact of the upper end of seed crystal with female rod.Then, utilize well heater (12-2) to make in the zone of action of female rod and seed crystal and form the melting zone fusion, other operation is the same.
Must be very narrow in this pattern requirement melting zone, so the most handy double-deck well heater (12-2 ) heating.
(4) intermediate diameters/many female rod preparations (Fig. 5-E)
This pattern is used for an operational process many female rods is carried out the directional freeze processing, so that improve preparation efficiency, reduces energy consumption.The structure of this pattern and technology and intermediate diameters/excellent pattern of list basic identical, just well heater (12-2), water cooler (12-4), heat insulating mattress (12-5) and crystallizer (12-2) all should have bigger diameter.Should be vertical on the crystallizer load onto each crucible of manifold shape crucible (13-3) pack into seed crystal (15) and female rod (9).Then, carry out the directional freeze operation according to the technology of intermediate diameters/excellent pattern of list.This pattern can be used the well heater of various structures, but is best with double-deck well heater (12-2 ).When adopting double-deck well heater, outside each crucible, all should be around a primary heater (12-2 -2), or the primary heater of certain intervals is arranged around two female excellent directions in edge.The temperature of auxiliary heater (12-2 -1) and each primary heater should be measured respectively and control.Water cooler adopts liquid metal (as the In-Ga alloy etc.) better as heat-eliminating medium (13-4-1), and like this, each crucible can obtain similar cooling conditions after entering water cooler.
Under this pattern, to use feeding rod also can give birth to better directional solidification effect, but handle for many rods, its control difficulty is bigger.
6, thermal treatment and thermomagnetic treatment
In directionally solidified crystal, except principal phase RFe
2Outside, also exist in process of setting and form RFe
3And R non-equilibrium phases such as (R refer to Tb and Dy).By near eutectic temperature, heat-treating the RFe in the alloy
3Identical R phase reaction forms RFe
2, non-equilibrium phase is disappeared, performance improves.
Thermal treatment is carried out under the condition that vacuumizes back filling with inert gas (as Ar gas), and rare gas element should have higher purity, and temperature should be controlled at 800～1100 ℃ (being preferably in 900～1000 ℃).Because
Reaction slower, thermal treatment generally needed the long period, as 10 hours or longer.The dynamichandling technology that the present invention proposes fluctuates treatment temp in the temperature range that requires, energy accelerated reaction process shortens the treatment time like this.Utilize this technology, only need carry out thermal treatment in 1～5 hour and finish, obtain perfect performance with regard to reacting.Processing needs slow cooling after finishing, and prevents that alloy from forming crackle.
At bar-shaped (TbDy) Fe
2In the twin monocrystalline, one group parallel, and { the 111} twining plane is parallel to the rod axle,＜112〉direction also parallel and rod axles.Below Curie temperature (about 350 ℃), along perpendicular to twining plane＜111〉direction (easy magnetization axis) apply magnetic field, can make magnetic domain along arranging perpendicular to the direction of rod axle.Through the crystal of this thermomagnetic treatment, its magnetostriction performance can be greatly improved.The difficulty of thermomagnetic treatment is and need carries out metallographicobservation to each crystal, determine its vertical bars axle＜111〉direction, and have only twin monocrystalline just might carry out this observation.At general directional freeze (TbDy) Fe
2In the alloy bar, though＜112〉direction also approach the parallel bars axle, the vertical bars axle＜111〉direction be stochastic distribution.
Processed alloy can be twin monocrystalline, can not be twin monocrystalline also, and not need to carry out metallographicobservation that processing efficiency is higher.The foundation of this processing is: in the directional freeze quality preferably in the alloy bar, most of crystal grain＜112〉direction be parallel to the rod axle, in these crystal grain, just have＜111〉direction spool vertical with rod.So, if the alloy bar that makes directional freeze is perpendicular to magnetic field, and slowly rotate around excellent direction of principal axis, these crystal grain just have an opportunity to make its＜111〉direction be parallel to field direction, the magnetic domain that makes it is along the direction orientation perpendicular to the rod axle.After treatment, the most of magnetic domains in the alloy bar are just along the direction orientation perpendicular to the rod axle.
Treating processes comprises: will be through directional freeze and heat treated (TbDy) Fe
2Alloy bar (9) is placed in the silica tube (16), and makes the rod axle parallel with tubular axis.Silica tube is put into direct magnetic field (17), and is axially vertical with field direction, and is connected with vacuum-filling with inert gas system (19) by a rotary vacuum-sealing interface (18), and process furnace (20) is placed around silica tube.Through after vacuumizing and charge into rare gas element (as Ar gas), alloy bar is heated 0.5～3 hour (best 1～2 hour) at 380～580 ℃ (best 400～500 ℃).Then, cool the temperature to 280～340 ℃ (best 310～330 ℃), and start magnetic field.Make magneticstrength reach 240～960kA/m (best 400～640kA/m), simultaneously, silica tube is pivoted, rotating speed is got 0.2～10rpm (best 0.5～2rpm).When alloy bar is long, silica tube is moved along tube axial direction, make excellent each several part can accept the effect in magnetic field uniformly.After heating 0.5～3 hour (best 1～2 hour), keeping magnetic field and driving under the condition of silica tube, slowly cooling.Fig. 6 has represented the synoptic diagram of thermomagnetic treatment.
The another kind of method that vacuum or inert gas conditions are provided is alloy bar (9) to be put into the silica tube (16) of an end closure, under the condition that vacuumizes or vacuumize under the condition of back filling with inert gas, seals the other end of silica tube.Then, silica tube is put into magnetic field (17), use with the front similar methods and carry out thermomagnetic treatment.
Embodiment:
Stir-turn over the cold crucible vacuum induction melting alloy (Fig. 1) of ingot-casting operation system with band, power 200kw, frequency is 8kH.Crucible (5) is the distinguish water-cooled red copper crucible that the rising pouring mouth is arranged, internal diameter 80mm, and high 180mm, geat diameter are 25mm.The feed trumpet of Casting Mechanism (8) screws in geat, and the mould tube of different diameter is communicated with feed trumpet by the rising pouring dish, and well heater (8-3) is around mould.
Press Tb
0.29Dy
0.71Fe
1.95The proportioning prepared furnace charge, 3.5kg altogether.Vacuumize after the charging with charged pressure is-the 0.02MPa high-purity argon to start power supply heating furnace charge then.After furnace charge melts clearly, rotate stopper rod head (6-1) and stir feed liquid, close the melting power supply after 2～3 minutes.Rising stopper rod head lifting alloy pig behind the alloy graining.Use ingot tumbler structure (7) with the ingot upset then, reduce the stopper rod head again, ingot is sent add crucible.According to said method with twice of alloy remelting.Last remelting is after 1 minute, and under the condition that does not stop to heat, the velocity pull-down stopper rod head with 80mm/ minute enters mould tube (8-1) until whole liquid alloys.
After coming out of the stove, obtained the casting rod of 1 φ 20mm, 10 φ 10mm and 8 φ 8mm, all about 200mm of length, the about 2.9kg of gross weight, quality is good.From the rod difference sampling analysis composition of three kinds of specifications, the result shows, the composition of alloy even, correct (table 1), foreign matter content very low (table 2).The mother as crystallographic orientation after surface grinding is excellent for the casting rod.
Table 1, the alloying element analytical results of embodiment 1 alloy, %
| Tb | Dy | Fe | |
| Require composition | 17.71 | 42.25 | 40.04 |
| Analyze composition | 17.74±0.03 | 42.18±0.08 | 40.08±0.05 |
Table 2, the impurity analysis result of embodiment 1 alloy, %
| O | N | F | C | S | Al | Si | |
| Require composition | ≤0.03 | ≤0.01 | ≤0.02 | ≤0.02 | ≤0.01 | ≤0.01 | ≤0.02 |
| Analyze composition | 0.012 | 0.005 | 0.010 | 0.008 | 0.002 | 0.008 | 0.013 |
Use device for directionally solidifying shown in Figure 2,, handle feeding rod (13-6) clamping (Fig. 5-3) of the upper end of rod by large diameter single rod pattern female rod (9) of the long 195mm of φ 20mm of embodiment 1 preparation.Internal diameter 21mm, the quartz crucible of long 250mm (13-3) are clamped in above the crystallizer (13-2), highly are placed in the crucible for the φ 18mm seed crystal (15) of 15mm.Crucible by 3 segmentation well heaters (12-2) around, internal diameter 30mm, total power 20kw.The high 100mm of well heater epimere (12-2 '-1), the high 50mm of hypomere (12-2 '-3), all with the preparation of high temperature FeCrAl alloy, design temperature is 1000 ℃.The stage casing of well heater (12-2 '-2) makes of the Pt silk, and high 30mm, design temperature are 1290 ℃.Heater holder is on the ring-type corundum heat insulating mattress (13-5) of 20mm at thickness, and its below is the water-cooled annular water cooler (13-4) of red copper fixedly, internal diameter 30mm, high 50mm.
Rising crystal pulling rod (13-1), make the upper surface of seed crystal be positioned at the center in well heater stage casing after, reduce feeding rod (13-6), make female rod (9) enter crucible (13-3), the lower end just contacts with seed crystal (15).Directed stove (10) is evacuated to 5 * 10
-3Charged pressure is the high-purity Ar of 0.01Mpa behind the Pa, starts heater power source (12-1) then.After the temperature in stage casing reaches design temperature and is incubated 2 minutes, start drive system (14,14 ') up and down simultaneously, crystal pulling rod is descended with the speed of 6mm/min, speed with 3rpm clockwise rotates, and feeding rod is descended with the speed of 6.3mm/min, rotates counterclockwise with the speed of 3rpm.The well heater lower end is shifted out in upper end to female rod, when entering water cooler (13-4), stops heating and driving process.
Obtain the about 20.5mm of diameter after coming out of the stove, finished product rod, flawless and the hole of the about 200mm of length.Detection shows, at 40kAm
-1Axial magnetic field under, the rod axial strain be 520 * 10
-6
The alloy bar (9) that embodiment 2 obtains is put into vacuum heat treatment furnace, be evacuated to 5 * 10
-3Charged pressure is the high-purity Ar of 0.01Mpa behind the Pa.The temperature for the treatment of processes is 850～950 ℃ of fluctuations, and be 20min cycle of fluctuation, handles accumulative total cooling after 2 hours, the alloy furnace cooling.The result that the alloy bar of coming out of the stove is detected shows, at 40kAm
-1Axial magnetic field under, the rod axial strain be 610 * 10
-6Axial compression stress and 40kAm at 6Mpa
-1Magnetic field under, strain reaches 1230 * 10
-6
To put into long 250mm through heat treated rod (9), the silica tube (16) of internal diameter 30mm one end closure connects silica tube and vacuum system (19), and vacuum is evacuated to 2 * 10
-1During Pa, with the quartzy not sealing end that burns the lamp heating and seal silica tube.With the long 400mm that packs into of this silica tube man, the process furnace of internal diameter 40mm (20) is put into process furnace between the cartridge of electro-magnet (17) again, makes tubular axis parallel with the cartridge face (referring to Fig. 6).Heated quarty tube, rise to 480 ℃ to temperature after insulation 1 hour.Then, be cooled to 320 ℃, start magnetic field, make magneticstrength reach 480kA/m.Simultaneously, with the velocity of rotation of 1rpm and 50mm/min move back and forth the speed drive silica tube, make the each several part of the action of a magnetic field to the long alloy bar of 200mm.Be incubated after 0.5 hour slowly cooling under the condition that keeps magnetic field and driving silica tube.After coming out of the stove, the detected result of alloy bar is shown, at 40kAm
-1Strain under the axial magnetic field is 880 * 10
-6Axial compression stress and 40kAm at 2MPa
-1Magnetic field under, strain reaches 1260 * 10
-6
Claims (7)
1, a kind of method for preparing the TbDyFe base alloy directionally solidified crystal, its operation is mother alloy preparation, directional freeze, thermal treatment and thermomagnetic treatment, it is characterized in that:
A, mother alloy preparation section are: before melting, make stopper rod head (6-1) stop up crucible orifice (5-1); When heat-processed generation frame material, move up and down the stopper rod head with loosening furnace charge; In changing the material process, rotate and move up and down the stopper rod head, stir the alloy liquation; Rising stopper rod head is raised the alloy pig that solidifies after the melting in crucible, and head (7-1) upset alloy pig is controlled in operation, sends the alloy pig that is reversed back to the crucible remelting, makes the alloy liquation enter mould (8-1) then and is frozen into mother alloy rod (9);
B, directional freeze operation are: the internal diameter of earlier seed crystal (15) and female rod (9) being packed into is slightly larger than female excellent crucible (13-3), then body of heater (10) is vacuumized, and is higher than 10 in vacuum tightness
-1Behind the Pa, rapidly charged pressure be-0.09～+ rare gas element of 0.2MPa; Using then around the molten formula resistance heater (12-2) in the district of female rod makes the upper end of seed crystal and the lower end of female rod form the melting zone, and then drop-down and rotation melting zone is left the high-temperature zone and is moved to water cooler (13-4) direction, the melting zone is solidified from bottom to top, new melting zone is moved up along female rod, continue to carry out this process ,-process of setting molten up to the district finished at the excellent top of mother; In this process, the melting zone temperature should be controlled in 1260～1380 ℃ of scopes, the melting zone width should be controlled with female excellent diameter roughly the same, movement velocity of melting zone is in 0.5～30mm/min scope, speed of rotation is got 0.5～30rpm, and the alloy bar of this process of process has crystallographic orientation and is organized into twin single crystal organization;
C, thermal treatment and thermomagnetic treatment
The directional solidificating alloy rod is carried out dynamic thermal treatment, and promptly treatment temp fluctuates near 800～1100 ℃ of eutectic temperatures, slowly cooling after 1～5 hour; Then alloy bar (9) is put into tubular axis and the vertical silica tube of field direction (16), silica tube is vacuumized and charges into rare gas element, startup is around the process furnace (20) of silica tube, make alloy bar 380～580 ℃ of scope internal heating 0.5～3 hour, after this reduce to 280～340 ℃ when temperature, start magnetic field, make magneticstrength reach 240～960KA/m, silica tube is pivoted with 0.2～10rpm rotating speed, and keep slowly cooling after 0.5～3 hour.
2, the method for preparing the TbDyFe base alloy directionally solidified crystal according to claim 1 is characterized in that by stopper rod head (6-1) top of drive control blade (6-4) being housed, and makes it to pump simultaneously at the rotation whipping process.
3, the method for preparing the TbDyFe base alloy directionally solidified crystal according to claim 1, it is characterized in that resistance heater is made up of 2～3 heating zones, the superiors are preheating section, and the middle level is a high temperature section, in lower floor holding-zone is set, makes high temperature section formation temperature gradient up and down.
4, the method for preparing the TbDyFe base alloy directionally solidified crystal according to claim 1 is characterized in that the melting zone can repeat repeatedly along female rod (9) moving process.
5, the method for preparing the TbDyFe base alloy directionally solidified crystal according to claim 4, the temperature that it is characterized in that the melting zone is in 1280～1330 ℃, and movement velocity of melting zone is at 2～15mm/min, and speed of rotation is got 2～15rpm.
6, the method for preparing the TbDyFe base alloy directionally solidified crystal according to claim 1 is characterized in that the alloy bar thermal treatment temp fluctuates in 900～1000 ℃.
7, the method for preparing the TbDyFe base alloy directionally solidified crystal according to claim 1, the alloy bar (9) that it is characterized in that being arranged in silica tube (16) is in the thermomagnetic treatment process, make alloy bar 400～500 ℃ of temperature range internal heating 1～2 hour, starting magneticstrength when cooling the temperature to 310～330 ℃ then is the magnetic field of 400～640KA/m, silica tube rotates with 0.5～2rpm rotating speed simultaneously, after heating 1～2 hour, keeping slowly cooling under magnetic field and the silica tube operating condition then.
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| CN100392777C (en) * | 2004-12-14 | 2008-06-04 | 宁波大学 | Method for preparing aeolotropic R-Fe-B-M permanent magnet material |
| CN100393893C (en) * | 2005-11-03 | 2008-06-11 | 徐宝田 | Heat treatment method and equipment through rotating magnetic field generated from magnetic parts of an apparatus |
| JP5213594B2 (en) * | 2008-09-04 | 2013-06-19 | 東京エレクトロン株式会社 | Heat treatment equipment |
| CN101775565B (en) * | 2009-11-30 | 2011-09-28 | 浙江大学 | Heat treatment method for improving magnetostrictive property of Tb<x>Dy<1-x>Fe<y> alloy bars with <112> axial alignment |
| EP2581151B1 (en) * | 2010-06-11 | 2015-05-06 | Diavac Limited | Arc melting furnace device |
| CN102491622A (en) * | 2011-12-15 | 2012-06-13 | 西南技术物理研究所 | Atmosphere melting and forming method for terbium-activated silicate glass |
| CN102814569B (en) * | 2012-08-06 | 2015-09-16 | 深圳市智讯达光电科技有限公司 | Eutectic furnace |
| CN103555903B (en) * | 2013-11-13 | 2014-11-19 | 北京科技大学 | Preparation method for improving mechanical property of giant magnetostrictive material |
| CN104195635A (en) * | 2014-09-28 | 2014-12-10 | 哈尔滨工业大学 | Large-width columnar crystal silicon ingot preparation method by adopting seed crystal method |
| CN104947194B (en) * | 2015-05-04 | 2017-11-28 | 北京航空航天大学 | A kind of magnetostriction materials and preparation method thereof |
| CN105543952B (en) * | 2015-12-28 | 2017-11-24 | 北京航空航天大学 | A kind of Rapid Directional Solidification equipment and Rapid Directional Solidification method |
| CN107052282B (en) * | 2017-04-26 | 2018-12-04 | 郑州航空工业管理学院 | A kind of preparation method of the twin dendrite of Al-40%Zn alloy |
| CN107962169B (en) * | 2017-12-08 | 2019-07-23 | 山东森宇精工科技有限公司 | The preparation facilities and method of refractory metal base gradient composite material |
| CN109825881B (en) * | 2019-01-09 | 2020-12-01 | 江西嘉圆磁电科技有限公司 | Process for preparing magnetostrictive material by oriented crystal zone melting method |
| CN110592676A (en) * | 2019-10-18 | 2019-12-20 | 磐石创新(江苏)电子装备有限公司 | VTM furnace and tellurium-zinc-cadmium single crystal synthesis method |
| CN112458308A (en) * | 2020-11-25 | 2021-03-09 | 清远先导材料有限公司 | Method for preparing ultra-high pure cadmium |
| CN113073249B (en) * | 2021-02-26 | 2022-12-02 | 湖南大学 | Preparation method of <111> + <110> preferred orientation giant magnetostrictive material TbxDy1-xFey |
| CN113447153B (en) * | 2021-06-28 | 2024-04-19 | 哈尔滨工业大学 | Temperature measuring device and method in directional solidification process of cold crucible |
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