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WO2003038161A1 - Appareil pour matiere faiblement fondue permettant d'effectuer une fabrication de cristal semi-continue czochralski - Google Patents

Appareil pour matiere faiblement fondue permettant d'effectuer une fabrication de cristal semi-continue czochralski Download PDF

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Publication number
WO2003038161A1
WO2003038161A1 PCT/US2001/046211 US0146211W WO03038161A1 WO 2003038161 A1 WO2003038161 A1 WO 2003038161A1 US 0146211 W US0146211 W US 0146211W WO 03038161 A1 WO03038161 A1 WO 03038161A1
Authority
WO
WIPO (PCT)
Prior art keywords
crucible
melt
compartment
growth
shallow
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/US2001/046211
Other languages
English (en)
Inventor
Tihu Wang
Theodore F. Ciszek
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.)
Midwest Research Institute
Original Assignee
Midwest Research Institute
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 Midwest Research Institute filed Critical Midwest Research Institute
Priority to PCT/US2001/046211 priority Critical patent/WO2003038161A1/fr
Priority to US10/494,482 priority patent/US6984263B2/en
Publication of WO2003038161A1 publication Critical patent/WO2003038161A1/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
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/06—Silicon
    • 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
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
    • 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
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/10—Crucibles or containers for supporting the melt
    • C30B15/12—Double crucible methods
    • 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
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/14—Heating of the melt or the crystallised materials

Definitions

  • the present invention relates to growing crystals without encountering the problems normally associated with conventional Czochralski crystal growth of: strong melt convection that causes deteriorated crystal quality; constantly changing thermal conditions; segregation causing non-uniformity in dopant concentrations; a slow growth rate and an uncontrollable interface shape; slow turn around between crystal ingots; and significant loss of feedstock materials if a growth run fails.
  • the invention eliminates the foregoing problems through the use of a shallow melt with a heat shield and an interface heater-heat sink to overcome microdefects, stress management and defect minimization, swift turnaround between crystal ingots, and the saving of feedstock materials through the use of a double barrier that offsets connecting holes for replenishing the melt.
  • Affecting crystal growth using the conventional Czochralski (CZ) process has been accomplished utilizing a pulling apparatus employing the CZ technique comprising: A gas type chamber; a crucible for storing a semiconductor melt that is positioned inside the chamber; a heater for heating the semiconductor melt; and a pulling mechanism for pulling a single crystal of the semiconductor.
  • a seed crystal of the single crystal of the semiconductor is immersed in the semiconductor melt inside the crucible, whereupon the seed crystal is gradually pulled upwards, thereby growing a large diameter single crystal of the semiconductor having the same orientation as the seed crystal.
  • a method of the version adopted a double-wall crucible formed by disposing a cylindrical partition wall in an outer crucible to operate the crucible by supplying solid or fused silicon as a raw material, either batch wise or continuously, into the crucible through a gap between the inner surface of the outer crucible and the outer surface of the cylindrical partition wall and pulling a silicon single crystal from the molten mass of silicon in the cylindrical partition wall.
  • U.S. Patent 5,871,581 discloses a single crystal pulling apparatus comprising: a gas tight container; a double crucible for storing a semiconductor melt inside the gas tight container, the double crucible including an outer crucible and an inner crucible connected at a lower edge; source material supply means, disposed between the outer crucible and the inner crucible, for continuously adding source material to the semiconductor melt; and a flow restriction member, disposed inside the semiconductor melt region between the outer crucible and the inner crucible, for restricting the flow of the semiconductor melt.
  • a crucible for pulling silicon single crystal is disclosed in U.S. Patent 5,720,809.
  • the crucible is constructed by coaxially disposing a cylindrical partition wall inside an outer crucible for holding a molten mass of silicon as a raw material and operated by heating the outer crucible and meanwhile supplying the raw material silicon to the gap between the outer crucible and the cylindrical partition wall and introducing the consequently produced molten mass of silicon into the interior of the cylindrical partition wall via a passage below the surface of the molten mass interconnecting the outer crucible and the inside of the cylindrical partition wall and meanwhile pulling the single crystal bar from the molten mass of silicon inside the cylindrical partition wall, which double-wall crucible is characterized in that at least the cylindrical partition wall is formed of quartz glass having a hydroxyl group (OH group) content of not more than 30 ppm.
  • OH group hydroxyl group
  • One object of the present invention is to provide a semicontinuous Czochralski crystal growth from a shallow melt apparatus that overcomes the increase of microdefects during crystal growth.
  • Another object of the present invention is to provide a semicontinuous Czochralski method of crystal growth from a shallow melt apparatus that lessens stress management and minimizes defects in the crystal growth.
  • a further object of the present invention is to provide a semicontinuous Czochralski method of crystal growth from a shallow melt apparatus that hastens turn around between crystal ingots.
  • a yet further object of the present invention is to provide a semicontinuous Czochralski method of crystal growth from a shallow melt apparatus that saves feed stock materials.
  • Another object yet still of the present invention is to provide a semicontinuous Czochralski method of crystal growth from a shallow melt apparatus that offsets connecting holes for replenishing the melt.
  • the CZ crystal growth methods of the invention are accomplished by the use of: a crucible with a deepened periphery to prevent snapping (i.e., a sudden uncontrollable motion) of a shallow melt to reduce turbulent melt convection; a double barrier to isolate heat in the feeding compartment from the growth compartment to melt solid feeding materials and minimize thermal impact to the growing crystal; an interface thermal gradient control, wherein a shallow melt in the growth compartment allows for a much better thermal gradient control near the interface; and an interface heater or a heat sink under the growth compartment, to obtain a concave or a convex interface shape.
  • FIG.l shows the apparatus (including crucible) for a conventional CZ crystal growth process. .. _ _ ._ . . . _
  • FIG. 2 depicts apparatus of the invention for providing semicontinuous CZ crystal growth from a shallow melt.
  • FIG. 3 shows the melt motion where the interface energy is larger than the surface energy (i.e., non-wetting crucible, ⁇ > 90 degrees), where the melt will tend to ball-up.
  • FIG. 4 depicts the asymmetric melt that ensues when both melt surface energy and the interface energy are very high compared to gravity potential energy.
  • FIG. 5 depicts a melt stabilized from a round or rectangular crucible when a deepened periphery traps the melt around the edge and prevents snapping.
  • FIG. 6 depicts a top view of the growth department in a round double barrier crucible for semiconductor ingot growth where melt connecting holes are utilized outside of the growth compartment but inside of the feed compartment.
  • FIG. 7 depicts a side view of a rectangular double-barrier crucible for a sheet or ribbon- shaped crystal growth and shows the melt connecting holes outside of the growth compartment but inside of the feed compartment.
  • the essential elements of the crucible comprises a crucible with a deepened periphery to prevent snapping of a shallow melt, and has a double barrier to isolate heat in the feeding compartment from that in the growth compartment, and further contains an interface thermal gradient control.
  • FIG. 1 shows a conventional CZ crystal growth apparatus and a melt crucible 10, as used therein.
  • a large quantity of feed stock materials must be preloaded in the deep crucible or melt crucible to grow a large ingot.
  • the invention apparatus features a shallow melt crucible 20 (particularly in the region immediately under the crystal/liquid interface) with an insulation or heat shield 21 and an interface heater/heat sink 22, and these features overcome the problems of: strong melt convection leading to deteriorated crystal quality; a slow growth rate and a generally incontrollable interface shape; slow turnaround between crystal ingots and a significant loss of feed stock materials if a growth run fails.
  • the double barrier 23 with off setting connecting holes 24 for replenishing the melt eliminates the problem of constantly changing thermal conditions even with synchronized crucible lift and segregation cost non-uniformity in dopant concentrations. Further, a deepened periphery 25 in the crucible prevents the shallow melt from snapping and additionally acts as a feed compartment.
  • One aspect of the invention discovery is that a crucible with a deepened periphery prevents snapping of a shallow melt.
  • Turbulence is related to the Grashof number:
  • g is the gravity
  • ⁇ is the thermal expansion coefficient of silicon melt
  • L is the melt height
  • ⁇ T is the vertical temperature difference in the melt
  • v is the dynamic viscosity of silicon melt.
  • the melt/gas and melt/crucible interface have energy contents proportional to their areas. Therefore, the melt shrinks to minimize energy.
  • the energy per unit area can also be regarded as a surface/interface tension, or force per unit length.
  • the total free energy of the melt maybe defined as follows:
  • ⁇ is the surface energies (melt/crucible interface and free surface) per unit area
  • A is the area of the surfaces
  • p is the melt density
  • P is the internal pressure in the melt
  • z is the vertical coordinate
  • z 0 vertical reference position
  • P 0 is a reference pressure
  • ⁇ is the surface tension of the melt
  • r, and r 2 are the two nominal radii of the melt surface curvature
  • ⁇ is the angle between the tangent of the melt edge and the crucible wall on the melt side.
  • melt motion MM is depicted in the direction of the arrows in FIG. 3.
  • melt surface energy and interface energy are very high compared to the gravity potential energy, the melt may retreat from one side and travel to the other side of the crucible, causing undesired asymmetry in the melt shape and temperature distribution. Both situatuations are called melt snapping.
  • the asymmetric melt is depicted in FIG. 4.
  • a double barrier is used to isolate heat in the feeding compartment from that in the growth compartment, and as a result of this configuration, the over heated feed compartment functions to melt solid feeding materials and minimizes thermal impact to the growing crystal.
  • the heat transfer is comprised of:
  • k is the thermal conductivity
  • T temperature
  • ⁇ is the Stefan-Boltzmann constant
  • e is the emisivity
  • C p is the heat capacity of silicon melt
  • p is the silicon melt density
  • N is the amount of silicon melt being transferred
  • E is the length of melt travel.
  • the double barrier (with offsetting connecting holes) crucible serves to: ReduceNT; .. .
  • a round double barrier crucible is utilized for semiconductor ingot growth.
  • a top view of a round double barrier crucible is depicted in FIG 6, and shows the growth compartment GC, melt connecting holes MCH, and the feed compartment FC.
  • a round double barrier crucible is utilized for semiconductor ingot growth.
  • a top view of a round double barrier crucible is depicted in FIG. 6, and shows the growth compartment GC, melt connecting holes MCH, and the feed compartment FC.
  • a rectangular double-barrier crucible is utilized for sheet or ribbon-shaped crystal growth.
  • the rectangular double-barrier crucible is shown in FIG. 7.
  • the double barrier crucible of the invention utilizes an interface thermal gradient control in that the shallow melt in the growth compartment operates as a thermal gradient control and allows for a much better thermal gradient control near the interface.
  • an interface heater or a heat sink under the growth compartment as shown in FIG. 2, a concave or convex interface shape may be obtained.
  • the crystal growth rate v is determined by the vertical thermal gradients in the crystal and in the melt near the interface:
  • an increase in the crystal growth rate maybe obtained with the combination of a heat shield employed on top of the feeding compartment and an interface heat sink or heater under the growth compartment.
  • the shallow melt allows close proximity between this interface heat sink/heat source and the solid/liquid interface, thus affording easier control of heat transport.

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  • 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

Dans un appareil de tirage de cristal unique permettant d'effectuer un procédé de croissance de cristal Czochralski, l'amélioration d'un creuset (20) pour matière faiblement fondue permet d'éliminer la nécessité de précharger une grande quantité de matériaux de charge dans un creuset profond pour permettre de fabriquer un grand lingot. Cet appareil comprend un contenant étanche au gaz; un creuset à périphérie approfondie (25) permettant d'empêcher le croquage d'une matière faiblement fondue et de réduire les convections de fusion turbulentes; un moyen d'alimentation source permettant d'ajouter un matériau source à la matière fondue semi-conductrice; une double barrière (23) permettant de minimiser le transfert de chaleur entre la périphérie approfondie (25) et la matière faiblement fondue située dans le compartiment de fabrication; des orifices de décalage (24) situés dans la double barrière (23) permettant d'augmenter la longueur de la course de fusion entre la périphérie approfondie (25) et le compartiment de fabrication peu profond. L'interface dispositif permettant de fournir de la chaleur/dissipée et de la chaleur (22) permet de contrôler la forme d'interface et la vitesse de fabrication du cristal.
PCT/US2001/046211 2001-11-01 2001-11-01 Appareil pour matiere faiblement fondue permettant d'effectuer une fabrication de cristal semi-continue czochralski Ceased WO2003038161A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
PCT/US2001/046211 WO2003038161A1 (fr) 2001-11-01 2001-11-01 Appareil pour matiere faiblement fondue permettant d'effectuer une fabrication de cristal semi-continue czochralski
US10/494,482 US6984263B2 (en) 2001-11-01 2001-11-01 Shallow melt apparatus for semicontinuous czochralski crystal growth

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/US2001/046211 WO2003038161A1 (fr) 2001-11-01 2001-11-01 Appareil pour matiere faiblement fondue permettant d'effectuer une fabrication de cristal semi-continue czochralski

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WO2003038161A1 true WO2003038161A1 (fr) 2003-05-08

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005084225A3 (fr) * 2004-02-27 2007-05-18 Solaicx Inc Systeme de croissance continue de silicium monocristallin
CN106133208A (zh) * 2014-03-27 2016-11-16 瓦里安半导体设备公司 硅熔体中控制热流的装置
WO2017019453A1 (fr) * 2015-07-27 2017-02-02 Sunedison, Inc. Systèmes et procédés de croissance cristalline à faible teneur en oxygène utilisant un procédé czochralski continu double couche

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5871581A (en) * 1996-01-12 1999-02-16 Mitsubishi Materials Silicon Corporation Single crystal pulling apparatus
US5891245A (en) * 1996-01-11 1999-04-06 Mitsubishi Materials Sillcon Corporation Single crystal pulling method and apparatus for its implementation

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5891245A (en) * 1996-01-11 1999-04-06 Mitsubishi Materials Sillcon Corporation Single crystal pulling method and apparatus for its implementation
US5871581A (en) * 1996-01-12 1999-02-16 Mitsubishi Materials Silicon Corporation Single crystal pulling apparatus

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7635414B2 (en) 2003-11-03 2009-12-22 Solaicx, Inc. System for continuous growing of monocrystalline silicon
US8317919B2 (en) 2003-11-03 2012-11-27 Solaicx, Inc. System for continuous growing of monocrystalline silicon
WO2005084225A3 (fr) * 2004-02-27 2007-05-18 Solaicx Inc Systeme de croissance continue de silicium monocristallin
CN106133208A (zh) * 2014-03-27 2016-11-16 瓦里安半导体设备公司 硅熔体中控制热流的装置
EP3122921A4 (fr) * 2014-03-27 2017-11-08 Varian Semiconductor Equipment Associates, Inc. Appareil pour le réglage du flux de chaleur au sein d'une masse fondue de silicium
US10415151B1 (en) 2014-03-27 2019-09-17 Varian Semiconductor Equipment Associates, Inc Apparatus for controlling heat flow within a silicon melt
CN106133208B (zh) * 2014-03-27 2020-04-28 瓦里安半导体设备公司 用于控制熔体内的热流的装置及其处理方法
WO2017019453A1 (fr) * 2015-07-27 2017-02-02 Sunedison, Inc. Systèmes et procédés de croissance cristalline à faible teneur en oxygène utilisant un procédé czochralski continu double couche

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