US20130062032A1 - Method for producing a monocrystalline body from a magnetic shape memory alloy - Google Patents

Method for producing a monocrystalline body from a magnetic shape memory alloy Download PDF

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Publication number
US20130062032A1
US20130062032A1 US13/643,485 US201113643485A US2013062032A1 US 20130062032 A1 US20130062032 A1 US 20130062032A1 US 201113643485 A US201113643485 A US 201113643485A US 2013062032 A1 US2013062032 A1 US 2013062032A1
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region
msm
crystal
solidification
alloying material
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US13/643,485
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Markus Laufenberg
Emmanouel Pagounis
Anne Drevermann
Laszlo Sturz
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ETO Magnetic GmbH
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ETO Magnetic GmbH
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Assigned to ETO MAGNETIC GMBH reassignment ETO MAGNETIC GMBH ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: STURZ, LASZLO, DREVERMANN, ANNE, LAUFENBERG, MARKUS, PAGOUNIS, EMMANOUEL
Publication of US20130062032A1 publication Critical patent/US20130062032A1/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D23/00—Casting processes not provided for in groups B22D1/00 - B22D21/00
    • 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
    • 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
    • C30B11/14—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method characterised by the seed, e.g. its crystallographic orientation
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/0302—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity characterised by unspecified or heterogeneous hardness or specially adapted for magnetic hardness transitions
    • H01F1/0306—Metals or alloys, e.g. LAVES phase alloys of the MgCu2-type
    • H01F1/0308—Metals or alloys, e.g. LAVES phase alloys of the MgCu2-type with magnetic shape memory [MSM], i.e. with lattice transformations driven by a magnetic field, e.g. Heusler alloys
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N35/00—Magnetostrictive devices
    • H10N35/01—Manufacture or treatment
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N35/00—Magnetostrictive devices
    • H10N35/80—Constructional details
    • H10N35/85—Magnetostrictive active materials

Definitions

  • the present invention relates to method for producing a monocrystalline MSM body for the production of an MSM actuator and such a monocrystalline MSM body, as is produced by the method.
  • MSM Magnetic Shape Memory
  • the crystal orientation in which the MSM element is present is critical for the effectiveness of such an MSM actuator or respectively MSM actuator element:
  • Methods to be assumed as being known from the prior art for the production of monocrystalline MSM material have the characteristic that a crystal orientation resulting by the introduction of a molten alloying material into a molding shell and subsequent cooling or respectively solidification of the alloying material is stochastic, with the result that an alignment of the crystal axes is not predeterminable and must then be developed by subsequent manufacturing steps of the MSM body.
  • An MSM monocrystal 10 which has been solidified and elongated in the previously described manner has a geometric longitudinal axis 12 determined by the molding shell. Largely in a stochastic manner during the solidification of the material, however, a crystal orientation has formed in the monocrystal 10 , which is described by way of example by a first crystal axis 14 and a second crystal axis 16 orthogonal thereto (wherein the third axis is then automatically fixed orthogonally to them both).
  • nucleation crystals seed crystals
  • seed crystals can influence a crystal orientation in a monocrystal production process.
  • substantially a suitable monocrystal, oriented in the desired manner is incorporated into the process at the start of the process, on which the crystal which is to be produced ideally nucleates in a monocrystalline manner.
  • this procedure is also problematic in many respects; not only are suitable nucleation crystals costly and difficult to handle in particular for industrial manufacturing processes outside a laboratory environment, also such nucleation crystals require a very precise process management, in order to achieve the correct nucleation behaviour (with further possible disadvantages to the MSM effect of a produced MSM element if the nucleation crystal has material which is foreign to the alloy). Therefore, in addition to the obvious need for an increase in efficiency according to the problem described above, the need also exists for procedural simplification, with the aim of enabling processes which are simple to operate and are potentially large-scale for the production of monocrystal MSM bodies.
  • K. ROLFS et al. “Double twinning in NiMnGaCo”, ACTA MATERIALIA, Vol. 58, No. 7, 1 Apr. 2010, pages 2646-2651;
  • M. LANDA et al. “Ultrasonic characterization of Cu—Al—Ni single crystals lattice stability in the vicinity of the phase transition”, ULTRASONICS, Vol. 42, No. 1-9, 1 Apr. 2004, pages 519-526; 8.
  • F. XIONG et al. “Fracture mechanism of a Ni—Mn—Ga ferromagnetic shape memory alloy single crystal” JOURNAL OF MAGNETISM and MAGNETIC MATERIALS, Vol. 285, No. 3, 1 Jan. 2005, pages 410-416.
  • the object is achieved by providing a method to provide a monocrystal MSM body, (preferably for use as an actuator or respectively actuator element), which proceeds from the fact that the divided body (and divided further into individual actuator elements) resulting from the method of the present invention is further treated with typical (and otherwise known) heat treatment steps and/or magnetomechanical training steps, in order to achieve or respectively optimize the magnetic shape memory behaviour.
  • the production of the monocrystal MSM body preferably on the basis of a NiMnGaX alloying material, wherein X has optionally one or more elements of the group Co, Fe and Cu—without the necessity to provide a (separated) nucleation crystal, rather solely from the introduction of the molten MSM alloying material into the especially configured molding shell according to the invention.
  • the latter has a longitudinal axis and is deflected in the region of the selector region from this longitudinal axis, according to the invention by a deflection which exceeds the maximum cross-sectional width in the selector region.
  • this deflection has in longitudinal section the form of at least one spike, alternatively a spiral, a helix or another angle configuration.
  • the crystal structure of the solidifying or respectively then solidified MSM material then undergoes in a manner according to the invention a crystal orientation which orients itself on the longitudinal axis, more precisely runs along the direction of the longitudinal axis of the molding shell (or respectively deviates therefrom by an angle deviation which according to the invention is ⁇ 10°, according to a further development is advantageously ⁇ 6°, again according to a further development and advantageously is less than 3°).
  • the molding shell (in particular in the selector or respectively crystal region) is configured so as to be rectangular in cross-section, in addition the crystal orientation of the solidifying or respectively solidified MSM material can be influenced along a second crystal axis running orthogonally to the first crystal axis (and hence automatically to the third orthogonal axis), so that as a result in this way then also the complete three-dimensional crystal orientation of a resulting crystal is determined in the space (again without the necessity of measuring).
  • the longitudinal axis in vertical direction, so as to provide it approximately perpendicularly to an (otherwise known) cold plate as cooling device in or at the nucleation region of the molding shell. If the molding shell is then (in an otherwise known manner) moved from a warmth or respectively heat environment, opposed to the longitudinal axis, with a drawing speed, alloying material which is introduced into this molding shell in liquid state solidifies owing to the temperature gradient then in an upward direction along a solidification path, which is able to be described through the longitudinal axis and, deviating therefrom, is deflected according to the invention in the selector region.
  • the solidification—or respectively cooling behaviour of the molding shell is arranged here so that in cross-section (radially) no significant temperature gradient is present from the interior outwards in the melt adjacent to the solidification front, and a temperature gradient of the melt close to the solidification front is set at values of between 0.3 K/mm and 20 K/mm, wherein a particularly preferred range of values for producing the desired crystal orientation lies in the range between 1 K/mm and 15 K/mm.
  • the cooling rate described by the speed of movement of the solidification front along the solidification path (or respectively a drawing speed of the molding shell relative to the temperature gradient), at a range of between 0.1 ram/min and 10 mm/min, wherein a particularly preferred range lies between 0.3 mm/min and 5 mm/min.
  • a monocrystalline solidification behaviour is then advantageously achieved, which forms the first crystal axis of the crystal structure at least along the longitudinal axis (or respectively shows between these axes a maximum angular deviation of less than 10°, typically less than 6° or even less than 3°).
  • the cross-section of selector region and/or crystal region i.e. the plane perpendicular to the longitudinal axis
  • an influencing (parameter) of the orthogonal second or respectively third crystal axis can be achieved in the direction of the rectangular longitudinal edges in cross-section, so that in the ideal case of an e.g.
  • this region determines the three-dimensional orientation of a monocrystal which is solidified therein.
  • the present invention not only enables a drastic reduction in manufacturing steps or respectively upstream testing steps (because ideally any measuring of the crystal orientation can be dispensed with), the invention also permits MSM elements to be produced which are optimized with regard to dimension from the restricted interior of a molding shell, because in particular already in the described molding process by solidification along a solidification direction corresponding to the longitudinal axis of the molding shell and a crystal alignment effected therewith, a maximum length dimension is able to be produced. It is then to be expected in particular that MSM elements can be produced efficiently and with small manufacturing expenditure (and hence potentially on a large scale) as the basis for the production of MSM actuators (also by further dividing, e.g. sawing), which reach length dimensions of more than 20 mm, in particular more than 40 mm and/or permit a cross-sectional area of 15 mm 2 or more.
  • FIG. 1 a geometric schematic diagram of a molding shell arrangement for carrying out the method according to a first example embodiment of the invention
  • FIG. 2 an illustration analogous to FIG. 1 , but with a different geometrical configuration in the form of a cross-sectionally rectangular crystal region of the molding shell;
  • FIG. 3 a diagrammatic illustration of a cylindrical MSM monocrystal and of a crystal orientation drawn therein diagrammatically on realization of the invention
  • FIG. 4 an illustration analogous to FIG. 3 , but with a monocrystal body in the shape of a rectangular block to illustrate the crystal orientation of an MSM actuator element (likewise in the shape of a rectangular block) provided diagrammically therein and
  • FIG. 5 a diagrammatic illustration of an MSM monocrystal realized according to a generic method from the prior art with crystal axes oriented therein stochastically, and with the limited cut possibilities resulting therefrom for an MSM actuator element.
  • FIG. 1 illustrates the principle by which the present invention can be realized according to a first example embodiment.
  • a so-called molding shell is shown for the production of monocrystalline bodies by the so-called Bridgman method, which, extending from a cold plate 20 perpendicularly along a longitudinal axis (dot-and-dashed line 22 ), forms a nucleation region 24 , subsequently a selector region 26 and a crystal region 28 .
  • molten alloying material is introduced into the device through an upper opening 30 , and the liquid alloying material then solidifies from below upwards (arrow direction 32 ) with the formation of a correspondingly upward moving solidification front, the speed of movement of which is predetermined by a suitable temperature influence.
  • FIG. 1 illustrate how according to the invention the solidification path takes place not perpendicularly and linearly along the longitudinal axis 22 , but rather has a linear course which is bent in longitudinal section from FIG. 1 or respectively FIG. 2 ; more precisely, in the selector region 26 the molding shell is configured so that its interior channel which is effective for the solidification (from the direction from below upwards) firstly is deflected by an angle ⁇ of approximately 40° and then has a further, but oppositely deflected section, until the channel at the upper end of the selector region is again in alignment cross-sectionally with the cross-section on the base side.
  • this deflection which in the illustrated example embodiment at its maximum lateral deflection transcends over the projection of the cross-section in the crystal region or respectively in the base region adjacent to the cold plate 20 , advantageously provides for a longitudinal orientation of the crystal structures in vertical direction, i.e. in the direction of the axis 22 . In the solidified state, this then leads in the region of the crystal region 28 to the monocrystal which is present there having an orientation which has at least a first crystal axis orientated in the direction of the longitudinal axis (wherein here according to the invention a maximum angle error of 10°, typically however of less than 6° or even less than 3° can be achieved).
  • FIG. 2 shows a variant of the example embodiment of FIG. 1 ; here in the crystal region 28 ′, the channel extending vertically along the longitudinal axis 22 is square in cross-section, so that, in addition to a crystal axis orientation in vertical direction, additionally the two crystal axes orthogonal thereto extend parallel to the edge courses of the crystal region.
  • FIG. 3 or respectively 4 illustrate these geometrical relationships, in this respect in accordance with the forms of realization of FIG. 1 or respectively FIG. 2 :
  • FIG. 3 shows the result of a monocrystal body solidified in a hollow cylindrical crystal region.
  • the direction of the longitudinal axis (here: z-axis) corresponds approximately to the alignment of the crystal longitudinal axis c with the described small possible angle error.
  • a monocrystal is achieved, which through its shape in the form of a rectangular block already to the greatest possible extent also describes its actual crystalline orientation and in this respect is potentially not (or only minimally) in need of further treatment.
  • the result of the production method according to FIG. 1 ( FIG. 3 ) is already advantageous in so far as here with the crystal axis (c), running in the direction of the longitudinal extent (z) of the molding shell and of the blank which is solidified therein, a relevant alignment is fixed for instance for the expansion behaviour of an MSM body, and also such a cylindrical body is then able to be used without further (or only with minimal) further treatment, if the precise alignment of the a- or respectively b-crystal axes is not concerned.
  • Primary alloying material is produced as so-called master alloy by induction melting from the materials NiMnGa, in accordance with composition for an MSM alloy, by induction melting.
  • a typical melting temperature is set at a range of between 50° and 400° above the liquefaction temperature of the respective alloy.
  • the melting takes place under an Ar atmosphere between 100 mbar and 1200 mbar.
  • the liquid master alloy is poured into a ceramic molding shell which has a geometry in accordance with FIG. 1 .
  • This molding shell is moved in the Bridgman method relative to a temperature gradient from a hot zone into a cold zone, so that the solidification front runs through the molding shell from bottom to top.
  • This speed of the movement of the solidification front typically lies at 0.3 mm/min; the temperature gradient in the melt close to the solidification front is set at a value of typically 3 K/mm.
  • the MSM material solidifies with a crystal axis aligned vertically, i.e.
  • the material is heat-treated (either as a whole body before the separation, alternatively by heat treatment of the divided individual actuator elements). It is also advantageous to train these elements after dividing in their movement—or respectively expansion behaviour, wherein for this purpose, typically over some strokes, in the provided expansion—or respectively movement direction a movement is imprinted into the material by corresponding input of tensile force or respectively pressure force.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Power Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
US13/643,485 2010-05-28 2011-05-26 Method for producing a monocrystalline body from a magnetic shape memory alloy Abandoned US20130062032A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE102010021856.1 2010-05-28
DE102010021856A DE102010021856A1 (de) 2010-05-28 2010-05-28 Verfahren zur Herstellung eines Einkristall-MSM-Körpers
PCT/EP2011/058695 WO2011147946A1 (de) 2010-05-28 2011-05-26 Verfahren zur herstellung eines einkristallinen körpers aus einer magnetischen formgedächtnis - legierung

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EP (1) EP2577761B1 (ja)
JP (1) JP2013527114A (ja)
CN (1) CN102918673B (ja)
DE (1) DE102010021856A1 (ja)
WO (1) WO2011147946A1 (ja)

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WO2016090347A1 (en) * 2014-12-05 2016-06-09 Immunext, Inc. Identification of vsig8 as the putative vista receptor and its use thereof to produce vista/vsig8 modulators

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US4450889A (en) * 1982-08-20 1984-05-29 United Technologies Corporation Mold having a helix for casting single crystal articles
US4548255A (en) * 1982-03-01 1985-10-22 United Technologies Corporation Mold with starter and selector sections for directional solidification casting
US6515382B1 (en) * 1998-03-03 2003-02-04 Kari M Ullakko Actuators and apparatus
CN1465736A (zh) * 2002-06-21 2004-01-07 北京航空航天大学 区熔定向凝固法制备磁驱动记忆合金单晶
US20070051623A1 (en) * 2005-09-07 2007-03-08 Howmet Corporation Method of making sputtering target and target
CN101020976A (zh) * 2007-03-30 2007-08-22 北京航空航天大学 一种镍锰铁镓形状记忆合金材料

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EP0092496B1 (en) * 1982-03-01 1986-10-01 United Technologies Corporation Mold with starter and selector sections for directional solidification casting
FR2734189B1 (fr) * 1989-05-24 1997-07-18 Snecma Dispositif de selection d'un grain de cristallisation pour pieces monocristallines en fonderie
US5062469A (en) * 1989-07-19 1991-11-05 Pcc Airfoils, Inc. Mold and method for casting a single crystal metal article
EP1076119A1 (en) * 1999-08-11 2001-02-14 ABB Alstom Power (Schweiz) AG Apparatus and method for manufacture a directionally solidified columnar grained article
JP4231188B2 (ja) * 2000-03-28 2009-02-25 Ｎｅｃトーキン株式会社 Ｎｉ−Ｍｎ−Ｇａ系形状記憶合金薄膜とその製造方法
WO2002014565A1 (fr) * 2000-08-14 2002-02-21 National Institue Of Advance Industrial Science And Technology Alliage ferromagnetique a memoire de forme
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Publication number Priority date Publication date Assignee Title
US3580324A (en) * 1969-03-13 1971-05-25 United Aircraft Corp Double-oriented single crystal castings
US4548255A (en) * 1982-03-01 1985-10-22 United Technologies Corporation Mold with starter and selector sections for directional solidification casting
US4450889A (en) * 1982-08-20 1984-05-29 United Technologies Corporation Mold having a helix for casting single crystal articles
US6515382B1 (en) * 1998-03-03 2003-02-04 Kari M Ullakko Actuators and apparatus
CN1465736A (zh) * 2002-06-21 2004-01-07 北京航空航天大学 区熔定向凝固法制备磁驱动记忆合金单晶
US20070051623A1 (en) * 2005-09-07 2007-03-08 Howmet Corporation Method of making sputtering target and target
CN101020976A (zh) * 2007-03-30 2007-08-22 北京航空航天大学 一种镍锰铁镓形状记忆合金材料

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EP2577761B1 (de) 2013-09-11
WO2011147946A1 (de) 2011-12-01
JP2013527114A (ja) 2013-06-27
CN102918673A (zh) 2013-02-06
EP2577761A1 (de) 2013-04-10
CN102918673B (zh) 2015-04-29
DE102010021856A1 (de) 2011-12-01

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