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WO2004113596A1 - Procede et dispositif de tirage de monocristaux par tirage par zone - Google Patents

Procede et dispositif de tirage de monocristaux par tirage par zone Download PDF

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Publication number
WO2004113596A1
WO2004113596A1 PCT/EP2004/051171 EP2004051171W WO2004113596A1 WO 2004113596 A1 WO2004113596 A1 WO 2004113596A1 EP 2004051171 W EP2004051171 W EP 2004051171W WO 2004113596 A1 WO2004113596 A1 WO 2004113596A1
Authority
WO
WIPO (PCT)
Prior art keywords
coils
flow
phase shift
secondary coil
pulling
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/EP2004/051171
Other languages
German (de)
English (en)
Inventor
Janis Priede
Gunter Gerbeth
Regina Hermann
Ludwig Schultz
Günter BEHR
Hans-Jörg UHLEMANN
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Leibniz Institut fuer Festkorper und Werkstofforschung Dresden eV
Helmholtz Zentrum Dresden Rossendorf eV
Original Assignee
Leibniz Institut fuer Festkorper und Werkstofforschung Dresden eV
Helmholtz Zentrum Dresden Rossendorf eV
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Leibniz Institut fuer Festkorper und Werkstofforschung Dresden eV, Helmholtz Zentrum Dresden Rossendorf eV filed Critical Leibniz Institut fuer Festkorper und Werkstofforschung Dresden eV
Priority to EP04741840A priority Critical patent/EP1641963A1/fr
Publication of WO2004113596A1 publication Critical patent/WO2004113596A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
    • C30B13/16—Heating of the molten zone
    • C30B13/20—Heating of the molten zone by induction, e.g. hot wire technique
    • 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
    • C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
    • C30B13/26—Stirring of the molten zone

Definitions

  • the invention relates to the field of materials science and relates to a method and an apparatus for pulling single crystals by pulling zones, which are used for example for intermetallic compounds or semiconductors.
  • FIG. 1 A basic diagram of zone melting is shown in Fig. 1.
  • An induction coil 4 in which a high-frequency current flows is used to melt the starting material 3 in zone 2, which then solidifies as a single crystal 1 when the material is pulled in the vertical direction, the resulting single crystal usually being rotated. Depending on the execution of the process, the single crystal can be pulled up or down.
  • the electromagnetic field of the induction coil produces a flow in the molten zone 2 with a double vortex structure, which is shown in FIG. 2.
  • This flow is always directed inwards in the middle of the zone, while in the vicinity of the two ends of the melting zone the flow is always directed radially outwards.
  • the resulting flow in the melting zone is next to electromagnetic forces are also generated by buoyancy and marangoni forces as well as by the rotation of rods or crystals.
  • the geometry of the solidifying phase boundary is adjusted according to the temperature distribution prevailing in the rod, which in turn is influenced by the flow conditions.
  • the heat radiation from the molten zone leads to a phase boundary that is always concave at the edge of the solidifying single crystal, which promotes polycrystalline growth. It prevents the cultivation of complex multicomponent intermetallic compounds across the entire cross-section in single-crystal form.
  • DE 197 04 075 C2 describes a combination of a rotating and static magnetic field for the production of single crystals in closed ampoules
  • DE 195 29 381 A1 describes the use of combined magnetic fields for Czochralski growth. Due to the free liquid surfaces that occur during zone pulling, these types of flow influencing cannot be used for zone pulling.
  • the application of a rotating magnetic field when pulling zones is described in DD 263 310 A1, but with the aim of completely eliminating forced convection in the melt.
  • DE 100 51 885 A1 describes a solution for flow control during zone pulling, in which the superposition of crystal rotation and rotating magnetic field is used, both being rotated in opposite directions of rotation.
  • the object of the present invention is to provide a method and a device for pulling single crystals by pulling zones, with which an improved stability of the growth process and an improved quality of the single crystal as well as a targeted, well controllable influencing of the shape of the solid-liquid phase boundary is achieved ,
  • the flow in the area of the melt is driven by an electromagnetically generated volume force to form a radial-meridional flow which can be controlled in direction and strength.
  • This electromagnetic volume force arises through the use of a second induction coil, which is arranged above or below the primary induction coil, and a phase shift between the electrical currents in the two induction coils.
  • the secondary coil can be connected to a power supply, including that of the primary coil, but it can also advantageously have no connection to a power source.
  • phase shift of the electrical currents is advantageously generated in the resonant circuits of the two induction coils, the phase shift of the electrical currents advantageously being realized by regulating the capacitive force in the secondary resonant circuit and particularly advantageously a phase shift of the electrical currents of 90 °.
  • a secondary coil is arranged above or below the primary coil.
  • the secondary coil advantageously has no connection to a current source.
  • the secondary coil is likewise advantageously integrated into a resonant circuit with adjustable capacitance and adjustable ohmic resistance.
  • a further advantageous embodiment of the invention is if the secondary coil is arranged above the primary coil for realizing a melt flow upward on the free surface of the melt zone or if the secondary coil is arranged under the primary coil for realizing a melt flow downward on the free surface of the melt zone ,
  • the solution according to the invention makes it possible to influence the geometry of the phase interface in a targeted manner and to improve the homogeneity of the dopant distribution when pulling zones of single crystals by influencing the flow.
  • the flow structure in the molten zone is changed from a double vortex structure to a predominant single vortex of adjustable strength and direction.
  • the flow conditions in the zone have a decisive influence on the distribution of dopants in the single crystal, which should be as homogeneous as possible.
  • the distribution of the dopants and the shape of the solid-liquid phase boundary on solidifying single crystals are both dependent on the flow conditions in the zone. A targeted influencing of these variables is consequently possible through a targeted control of the flow.
  • the flow in the area of the melt is driven by an electromagnetically generated volume force to form a radial-meridional flow.
  • the volume force is generated by the phase shift of the currents flowing through the two induction coils.
  • the secondary coil is not connected to a power supply and this circuit of the secondary coil has a capacitor with adjustable capacitance and an adjustable ohmic resistance.
  • the current in the secondary coil is then induced solely by the primary current in the primary coil.
  • a phase shift is generated between the two resonant circuits, which leads to a flow-driving volume force in the molten zone.
  • Figures 1 and 2 show the principle of zone pulling according to the prior art and the dominant, electromagnetically driven flow in the molten zone with the associated shape of the resulting phase boundaries liquid-solid.
  • the solution according to the invention is shown schematically in principle in FIG. 3.
  • a secondary coil 5 is added to the primary coil 4.
  • An advantageous electrical scheme for the method according to the invention is shown in FIG. 4.
  • the electrical current in the secondary coil is only generated inductively between the primary coil Li and the secondary coil L 2 ; the secondary circuit has no direct connection to a power supply.
  • the secondary circuit contains a controllable ohmic resistor R 2 and a controllable capacitor C 2 .
  • the phase shift of the currents can advantageously be adjusted by regulating the capacitance C 2 of the secondary circuit.
  • the or the ohmic resistors Ri, R 2 only have the function of limiting the currents in their amplitude.
  • the resulting flow in the melting zone as a result of the device according to the invention essentially consists of a toroidal single vortex.
  • Figure 5 shows this single vortex structure of the electromagnetically driven flow as The result of a numerical simulation for the growth parameters specified in embodiment example 1.
  • the change in the shape of the phase boundary from a shape that is predominantly concave over the radius of the crystal to a predominantly convex geometry can be clearly seen, thereby considerably reducing the occurrence of polycrystalline growth.
  • the method according to the invention permits flexible and controllable influencing of the flow in the melt in a wide range.
  • Variables and parameters to be optimized for the respective breeding arrangement are frequency and current strength of the primary circuit, the vertical distance between the two coils, the inner diameter of the coils and capacitance C 2 and ohmic resistance R 2 of the secondary circuit. If the secondary coil is arranged above the primary coil, the direction of flow of the individual vortex on the free surface of the melting zone is directed upwards. The opposite flow direction results when the primary coil is located above the secondary coil.
  • the flow drive as a result of the device according to the invention is strongest when the vertical distance between the two coils corresponds to the radius of the crystal.
  • a nickel single crystal with a diameter of 6 mm is produced by zone pulling with the device according to the invention.
  • the secondary coil is arranged above the primary coil.
  • the design of the electromagnetic parameters was based on numerical simulations.
  • the frequency of the primary current is 250 kHz, its amplitude is 130 A.
  • the vertical distance between the two coils is 3 mm.
  • the capacitance of the secondary circuit is 446 nF, its ohmic resistance is 51.2 m ⁇ .
  • phase boundary of the melt single crystal predominantly has concave edge regions, an almost flat, slightly convex phase boundary is achieved by means of the solution according to the invention.
  • the stability of the breeding process was significantly increased compared to conventional technology.
  • Example 1 In accordance with the conditions in Example 1, a Ce-Pd-Co-Si single crystal of 6 mm in diameter was produced by zone pulling with the device according to the invention. Until now, single crystals could not be produced from these materials by means of zone pulling according to the prior art method. A stable breeding regime was achieved with the solution according to the invention. Here too, an improved form of the phase boundary could be achieved.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

L'invention se rapporte au domaine de la science des matériaux et concerne un procédé et un dispositif de tirage de monocristaux par tirage par zone, ces monocristaux étant utilisés par exemple pour des alliages intermétalliques ou des semi-conducteurs. L'objectif de l'invention est de perfectionner ce procédé et ce dispositif de sorte qu'ils permettent d'obtenir un monocristal présentant une qualité améliorée. A cet effet, le procédé selon l'invention consiste à agir sur l'écoulement au niveau de la masse en fusion par l'intermédiaire d'une force volumétrique, produite au moyen d'un décalage de phases entre les courants électriques circulant à travers deux bobines d'induction, en vue d'obtenir un écoulement radial méridien de la masse en fusion pouvant être régulé au niveau du sens et de l'intensité. Par ailleurs, le dispositif selon l'invention se caractérise en ce qu'une bobine secondaire est disposée au-dessus ou au-dessous de la bobine primaire, ces deux bobines présentant chacune un circuit oscillant permettant de définir un décalage de phases entre les deux bobines.
PCT/EP2004/051171 2003-06-20 2004-06-18 Procede et dispositif de tirage de monocristaux par tirage par zone Ceased WO2004113596A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP04741840A EP1641963A1 (fr) 2003-06-20 2004-06-18 Procede et dispositif de tirage de monocristaux par tirage par zone

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE2003128859 DE10328859B4 (de) 2003-06-20 2003-06-20 Verfahren und Vorrichtung zum Ziehen von Einkristallen durch Zonenziehen
DE10328859.7 2003-06-20

Publications (1)

Publication Number Publication Date
WO2004113596A1 true WO2004113596A1 (fr) 2004-12-29

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PCT/EP2004/051171 Ceased WO2004113596A1 (fr) 2003-06-20 2004-06-18 Procede et dispositif de tirage de monocristaux par tirage par zone

Country Status (3)

Country Link
EP (1) EP1641963A1 (fr)
DE (1) DE10328859B4 (fr)
WO (1) WO2004113596A1 (fr)

Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2686864A (en) * 1951-01-17 1954-08-17 Westinghouse Electric Corp Magnetic levitation and heating of conductive materials
US2905798A (en) * 1958-09-15 1959-09-22 Lindberg Eng Co Induction heating apparatus
US3121619A (en) * 1959-10-19 1964-02-18 Philips Corp Zone-melting method and apparatus
US3179502A (en) * 1961-03-17 1965-04-20 Siemens Ag Method and means for floating-zone melting of rod-shaped bodies of crystallizable semiconducting or conducting material
DE1221379B (de) * 1964-05-11 1966-07-21 Halbleiterwerk Frankfurt Oder Verfahren zum induktiven tiegelfreien Schmelzen von Materialien, insbesondere von Halbleitermaterialien
DE2212310A1 (de) * 1972-03-14 1973-09-20 Siemens Ag Verfahren zur beeinflussung des radialen widerstandsverlaufes in einem halbleitereinkristallstab beim tiegelfreien zonenschmelzen
JPS63291887A (ja) * 1987-05-25 1988-11-29 Shin Etsu Handotai Co Ltd 半導体単結晶製造装置
EP0292920A1 (fr) * 1987-05-25 1988-11-30 Shin-Etsu Handotai Company Limited Appareil de chauffage par induction HF
DD263310A1 (de) * 1987-08-17 1988-12-28 Akad Wissenschaften Ddr Verfahren zur halbleiterkristallzuechtung aus elektrisch leitfaehigen schmelzen
JPH0864354A (ja) * 1994-08-26 1996-03-08 Semiconductor Res Found 高周波誘導加熱コイル装置
DE19704075A1 (de) * 1997-02-04 1998-08-06 Rossendorf Forschzent Verfahren und Vorrichtung zur Herstellung von Einkristallen in Ampullen unter Magnetfeldeinfluß
DE10051885A1 (de) * 2000-10-19 2002-05-02 Wacker Siltronic Halbleitermat Verfahren zum Ziehen eines Einkristalls durch Zonenziehen

Family Cites Families (7)

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Publication number Priority date Publication date Assignee Title
DE1242578B (de) * 1960-09-29 1967-06-22 Siemens Ag Vorrichtung zum Herstellen von bandfoermigen, dendritisch gewachsenen, hochreinen Halbleiterkristallen
DE1280446B (de) * 1965-08-21 1968-10-17 Deutsche Edelstahlwerke Ag Vorrichtung zur Veraenderung der spezifischen Heizleistung eines Induktors
DE1519888B2 (de) * 1966-04-15 1970-04-16 Siemens AG, 1000 Berlin u. 8000 München Verfahren zum tiegelfreien Zonenschmelzen
DD86806A1 (de) * 1970-11-27 1972-01-05 Verfahren zum tiegellosen Herstellen von versetzungsfreien Halbleitereinkristallen
AT368824B (de) * 1978-04-11 1982-11-10 Vertina Anstalt Einrichtung zum induktiven erwaermen von stangenfoermigen werkstuecken
DE3616595A1 (de) * 1986-05-16 1987-11-19 Siemens Ag Schaltungsanordnung fuer das tiegelfreie zonenziehen von halbleiterstaeben
DE10102126A1 (de) * 2001-01-18 2002-08-22 Wacker Siltronic Halbleitermat Verfahren und Vorrichtung zum Herstellen eines Einkristalls aus Silicium

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2686864A (en) * 1951-01-17 1954-08-17 Westinghouse Electric Corp Magnetic levitation and heating of conductive materials
US2905798A (en) * 1958-09-15 1959-09-22 Lindberg Eng Co Induction heating apparatus
US3121619A (en) * 1959-10-19 1964-02-18 Philips Corp Zone-melting method and apparatus
US3179502A (en) * 1961-03-17 1965-04-20 Siemens Ag Method and means for floating-zone melting of rod-shaped bodies of crystallizable semiconducting or conducting material
DE1221379B (de) * 1964-05-11 1966-07-21 Halbleiterwerk Frankfurt Oder Verfahren zum induktiven tiegelfreien Schmelzen von Materialien, insbesondere von Halbleitermaterialien
DE2212310A1 (de) * 1972-03-14 1973-09-20 Siemens Ag Verfahren zur beeinflussung des radialen widerstandsverlaufes in einem halbleitereinkristallstab beim tiegelfreien zonenschmelzen
JPS63291887A (ja) * 1987-05-25 1988-11-29 Shin Etsu Handotai Co Ltd 半導体単結晶製造装置
EP0292920A1 (fr) * 1987-05-25 1988-11-30 Shin-Etsu Handotai Company Limited Appareil de chauffage par induction HF
DD263310A1 (de) * 1987-08-17 1988-12-28 Akad Wissenschaften Ddr Verfahren zur halbleiterkristallzuechtung aus elektrisch leitfaehigen schmelzen
JPH0864354A (ja) * 1994-08-26 1996-03-08 Semiconductor Res Found 高周波誘導加熱コイル装置
DE19704075A1 (de) * 1997-02-04 1998-08-06 Rossendorf Forschzent Verfahren und Vorrichtung zur Herstellung von Einkristallen in Ampullen unter Magnetfeldeinfluß
DE10051885A1 (de) * 2000-10-19 2002-05-02 Wacker Siltronic Halbleitermat Verfahren zum Ziehen eines Einkristalls durch Zonenziehen

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Title
MUHLBAUER A ET AL: "Interface shape, heat transfer and fluid flow in the floating zone growth of large silicon crystals with the needle-eye technique", JOURNAL OF CRYSTAL GROWTH, NORTH-HOLLAND PUBLISHING CO. AMSTERDAM, NL, vol. 151, no. 1/2, 1 May 1995 (1995-05-01), pages 66 - 79, XP004003558, ISSN: 0022-0248 *
PATENT ABSTRACTS OF JAPAN vol. 0131, no. 19 (C - 579) 23 March 1989 (1989-03-23) *
PATENT ABSTRACTS OF JAPAN vol. 1996, no. 07 31 July 1996 (1996-07-31) *
ZHANG S Y ET AL: "Computer simulations of fluid flow and heat transfer in metal strip heating zone crystal growth", JOURNAL OF CRYSTAL GROWTH, NORTH-HOLLAND PUBLISHING CO. AMSTERDAM, NL, vol. 243, no. 3-4, September 2002 (2002-09-01), pages 410 - 418, XP004378934, ISSN: 0022-0248 *

Also Published As

Publication number Publication date
DE10328859A1 (de) 2005-01-27
DE10328859B4 (de) 2007-09-27
EP1641963A1 (fr) 2006-04-05

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