WO2011043777A1 - Appareil et procédé de croissance des cristaux - Google Patents

Appareil et procédé de croissance des cristaux Download PDF

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Publication number
WO2011043777A1
WO2011043777A1 PCT/US2009/060072 US2009060072W WO2011043777A1 WO 2011043777 A1 WO2011043777 A1 WO 2011043777A1 US 2009060072 W US2009060072 W US 2009060072W WO 2011043777 A1 WO2011043777 A1 WO 2011043777A1
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WO
WIPO (PCT)
Prior art keywords
crystal
crucible
crystal growth
furnace
heating source
Prior art date
Application number
PCT/US2009/060072
Other languages
English (en)
Inventor
Weiguo Liu
A. Grant Elliot
Original Assignee
Axt, Inc.
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 Axt, Inc. filed Critical Axt, Inc.
Priority to PCT/US2009/060072 priority Critical patent/WO2011043777A1/fr
Priority to EP09850317.0A priority patent/EP2501844A4/fr
Priority to JP2012533126A priority patent/JP2013507313A/ja
Publication of WO2011043777A1 publication Critical patent/WO2011043777A1/fr

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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
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/007—Mechanisms for moving either the charge or the heater
    • 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
    • C30B11/003—Heating or cooling of the melt or the crystallised material
    • 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
    • C30B11/006—Controlling or regulating
    • 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
    • C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • 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
    • C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
    • C30B29/48—AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te

Definitions

  • Systems and methods herein relate generally to the growth of Group lll-V, ll-VI and related monocrvstalline compounds and in particular to a method and apparatus for growing such compounds with reduced body lineage.
  • the growth of a semiconductor crystal involves heating poiycrystalline raw material to its melting point ⁇ typically in excess of 1 ,200" C.) to create a poiycrystalline raw material melt, bringing the melt into contact with a high quality seed crystal, and allowing the crystallization of the melt when in contact with the seed crystal.
  • the crystallization of the melt forms an essentially cylindrical crystal ⁇ an ingot) along a vertical axis with the seed crystal below the poiycrystalline raw materials.
  • the equipment necessary to form the semiconductor crystal includes a crystal growth furnace, an ampoule, a crucible, and a crucible support.
  • the crucible has a lower, narrow portion, called a seed well.
  • Systems and methods consistent with the invention are directed to growth of moncrystalline compounds.
  • a method of bringing an ampoule with raw material within a furnace having a heating source growing a crystal using a vertical gradient freeze process wherein the crystallizing temperature gradient is moved relative to the crystal or furnace to melt the raw material and reform it as a monocrystalline compound, and growing the crystal using a vertical Bridgman process on the wherein the ampoule/heating source are moved relative each other to continue to melt the raw material and reform it as a monocrystalline compound.
  • Figure 1 is a cross sectional view of an examplary crystal growth apparatus 20 consistent with certain aspects related to the innovations herein;
  • FIG. 2 illustrates an exemplary crystal ingot with body lineage consistent with certain aspects related to the innovations herein
  • Figure 3 illustrates an exemplary method for crystal growth using Vertical Gradient Freeze (VGF) and Vertical Bridgman (VB) process steps consistent with certain aspects related to the innovations herein; and
  • VVF Vertical Gradient Freeze
  • VB Vertical Bridgman
  • Figure 4 illustrates an exemplary method for loading the crystal growth furnace shown in Figure 1 consistent with certain aspects related to the innovations herein.
  • the apparatus and method are particularly applicable to an apparatus and method for gallium arsenide (GaAs) crystal growth and it is in this context that the apparatus and method are described. It will be appreciated, however, that the apparatus and method has greater utility since the apparatus and method can be used to produce other Group lll-V, Group ll-VI and related monocrystalline compounds.
  • GaAs gallium arsenide
  • FIG. 1 is a cross sectional view of an example of a crystal growth apparatus 20.
  • the apparatus may include a crucible support 22 in a furnace 24, such as a furnace that establishes a crystallizing temperature gradient which may be used in a vertical gradient freeze (VGF) or vertical Bridgman (VB) crystal growing and/or, if the furnace is moveable, a vertical Bridgman-Stockbarger process.
  • the crucible support 22 provides physical support for and allows for thermal gradient control to an ampoule 26 (that in one implementation is made of quartz) that contains a crucible 27.
  • the crucible support 22, when the furnace is in operation, can be moved during the crystal growth process.
  • the crucible support is fixed and the furnace, when in operation, can be moved during the crystal growth process.
  • the crucible 27 may contain a seed crystal 28, a grown monocrystalline crystal/compound 30 formed on top of the seed crystal and raw melt material 32.
  • the crucible 27 may be a pyrolitic boron nitride (pBN) material with a cylindrical crystal growth portion 34, a smaller diameter seed well cylinder 36 and a tapered transition portion 44.
  • the crystal growth portion 34 has a diameter equal to the desired diameter of the crystal product.
  • the current industry standard crystal diameters are 2 inch, 3 inch, 4 inch, 5 inch, 6inch and 8 inch ingots that can be cut into wafers.
  • the seed well cylinder 36 may have a closed bottom and a diameter slightly larger than that of a high quality seed crystal 28, e.g., about 6-25 mm, and a length on the order of 30-100 mm.
  • the cylindrical crystal growth portion 34 and the seed well cylinder 36 may have straight walls or may taper outwardly on the order of one to a few degrees to facilitate the removal of the crystal from the crucible 27.
  • the tapered transition portion 38 between the growth portion 34 and the seed well cylinder 36 has an angled side wall pitched at, for example approximately 45-60 degrees, with a larger diameter equal to and connected to the growth zone wall and a narrower diameter equal to and connected to the seed well wall.
  • the angled side wall may also be at other angles that are more steep or less steep than 45-60 degrees.
  • the crucible 27 Before insertion in the crystal growth furnace 24, the crucible 27 is loaded with raw materials and inserted into the ampoule 26.
  • the ampoule 26 may be made of quartz.
  • the ampoule 26 has a shape similar to that of the crucible 27.
  • the crucible is cylindrical in a crystal growth region 40, cylindrical with a narrower diameter in its seed well region 42 and has a tapered transition region 44 between the two regions.
  • the crucible 27 fits inside the ampoule 26 with a narrow margin between them.
  • the ampoule 26 is closed at the bottom of its seed well region 42 and, like the crucible, sealed on top after the crucible and raw materials are loaded.
  • the bottom of the ampoule 26 has the same funnel shape as the crucible 27.
  • the crucible support 22 is required to accommodate this funnel shape and hold the ampoule 26 stable and upright inside the furnace 24.
  • the ampoule-crucible combination may retain different shapes, and the basic structure of the crucible support 22 would be changed accordingly to fit the specific different shape.
  • the stability and strength to the ampoule and its contents are provided through a solid, thin-wailed cylinder 50 of the crucible support 22.
  • the solid, thin-walled cylinder 50 accommodates the funnel end of the ampoule structure 26.
  • the crucible support cylinder 50 is made of a heat conducting material, preferably quartz.
  • silicon carbide and ceramic may also be utilized to form the crucible support cylinder 50.
  • the cylinder 50 makes a circle of contact with ampoule 26, where the upper rim of the cylinder 50 meets the shoulder of the ampoule's tapered region 38.
  • Such configuration leads to minimal solid-to-solid contact which ensures that little or no undesirable, relatively uncontrollable heat conduction occurs. As a result, heating is able to be generated by other, more controllable processes.
  • a low density insulating material such as ceramic fiber, fills the majority of the inside of the support cylinder 50 with only a hollow axial core 52 in approximately the center of the insulating material left empty to receive the seed well 42 of the ampoule 26.
  • the low-density insulating material may aiso comprise alumina fiber (1 ,800.degree. C), alumina-silica fiber (1 ,426. degree. C), and/or zirconia fiber (2,200.degree. C).
  • the insulating material is carefully placed in the crucible support 22. The weight of the ampoule 26, as it sits on top of the cylinder 50, pushes the insulating material down and forms the slanted insulating material edge 54.
  • the hollow core 52 extends downward to a small distance below the bottom of the ampoule seed well 42.
  • the hollow core 52 extends through the crucible support from the bottom of the seed well to the bottom of the furnace apparatus 24.
  • the hollow core 52 provides a cooling path from the center of the crystal. It contributes to cooling in the seed well and in the center of the growing crystal.
  • the low-density insulating material within the cylinder 50 obstructs the flow of heat radiation from a set of furnace heat elements 60 to the ampoule 26 in the seed well region 42, so this method requires the creation of a plurality of horizontal radiation channels/openings/tunnels 56 through the insulation material.
  • the radiation channels 56 penetrate the insulating material to provide heat radiation outlets to controllably transfer heat from the furnace heating elements 60 to the ampoule seed well 42.
  • the number, shape and diameter of the radiation channels 56 varies depending on specific conditions.
  • the radiation channels may also be slanted, bent or wave-like.
  • the radiation channels also do not necessary have to be continuous, as they may extend only partially through the insulating material. This helps minimize convection currents.
  • the diameter of these channels is small, on the order of a pencil width, so that convection airflow is insignificant. Larger holes with cross-sectional area on the order of a square inch or more can also be used according to other embodiments of the invention.
  • the radiation channels 56 through the insulating material also work in conjunction with the hollow core 52 in the center of the insulating material to radiate heat energy drawn from the center of the crystal, and cool the crystal with planar isothermal temperature gradient layers.
  • the radiation channels 56 enable temperature control and directly relate to crystal growth yield.
  • the furnace 24 as shown in Figure 1 is an example of a furnace that may be used for both Vertical Gradient Freeze (VGF) and Vertical Bridgman (VB) or Vertical Bridgman-Stockbarger (VBS) crystal growth processes. Other furnaces may also be used.
  • VGF Vertical Gradient Freeze
  • VB Vertical Bridgman
  • VBS Vertical Bridgman-Stockbarger
  • Other furnaces may also be used.
  • VGF crystal growth process the crystallizing temperature gradient within a heat source, which may itself be stationary, is being moved while the crystal is held stationary.
  • the heat source and its fixed crystallizing temperature gradient are kept stationary while the crystal is moved.
  • the heat source and its fixed crystallizing temperature gradient are moved while the crystal is kept stationary.
  • Figure 2 illustrates a crystal ingot 70 with body lineage 72.
  • the body lineage is typically formed when crystal growth occurs in more than one different growth plane.
  • the crystal at, and above, the body lineage is unusable and must be recycled.
  • the body lineage reduces the yield of the crystal growth process and it is desirable to reduce body lineage.
  • Some furnaces and processes change the angle of the tapered portion of the furnace, but this does not solve the body lineage problems.
  • a furnace and crystal growth process that overcomes this body lineage problem results in, for a given furnace, a longer length crystal which thus results in a larger yield.
  • FIG. 3 illustrates a method 80 for crystal growth using Vertical Gradient Freeze (VGF) and Vertical Bridgman (VB) process steps that reduce the body lineage resulting in longer crystals and higher yield.
  • VGF Vertical Gradient Freeze
  • VB Vertical Bridgman
  • the VB process may be used at approximately 12-15 mm (1/2 inch) above the tapered region 38 as shown in Figure 1.
  • the combination of the VGF and VB processes results in longer crystals with fewer body lineage.
  • the above method may be used with the furnace shown in Figure 1 , but may also be used with any other crystal growth furnace. The method may be used to grow crystals from 2 inch - 6 inch, or larger, in diameter.
  • a loading crucible 90 may be located above the crucible 27 and allows the crucible 27 to be loaded with more raw material.
  • the raw gallium arsenide material 92 is solid and therefore cannot be tightly packed into the crucible 27 to be melted.
  • the loading crucible is used to hold extra raw material that can be melted and then drain down into the crucible which results in a larger Gallium Arsenide charge in the crucible 27 which in turn results in a larger length Gallium Arsenide crystal.
  • about 65% of the raw material may be initially loaded into the loading crucible 90 and 35 % of the raw material is loaded directly into the crucible 27.
  • the above method for loading the crystal growth furnace a 15 kg charge may be loaded into the furnace that produces a 115 mm ingot with no lineage that results in 115 wafers.
  • a 6" (150 mm) diameter Gallium Arsenide grown using the above crystal growth furnace and method (VGF and VB combined) is described in more detail.
  • the dimensions of the crucible were 150 mm diameter and 170 mm length crystal growth region 40.
  • the diameter of the crucible in the seed well region 42 was 7 mm.
  • 14 kg of GaAs polycrystalline material was loaded for un-doped GaAs ingot growth use.
  • the GaAs seed crystal is inserted in the bottom portion of the pBN crucible 27.
  • 14kg of GaAs polycrystalline material, 100g of boron trioxide as the liquid sealant are added therein.
  • the charge loaded pBN crucible was inserted in a quartz ampoule.
  • the quartz ampoule was sealed under reduced pressure with a quartz cap.
  • the quartz ampoule is then loaded in the furnace and placed on the crucible support.
  • the quartz ampoule may be heated at the rate of approximately 270 ° C /hour.
  • the temperature point may be held until all of the polycrystalline Gallium Arsenide material melts (approximately 10 hours).
  • a VGF method was first used for crystal growth. The temperature may then be reduced in the lower heating zone slowly to let crystal growth starting at the seed part begin and continue through the transition region until the crystal growth region cools at the cooling rate 0.3-0.47 ° C /hour while maintaining the temperature gradient from 1.2 to 1.8 ° C/cm.
  • the VB process when the crystal has grown approximately one inch high in the crystal growth region, the VB process may be started.
  • the crucible down speed is precisely controlled so as to get a cooling rate of 0.29 ° C /hour and a temperature gradient of from 1.8 to 5.2 ° C /cm.
  • a resulting crystal of 81 mm length and high quality may be achieved via such a process, from a 105 mm long ingot, which is a crystal yield of 77%.
  • the single crystal substrate from starting growth portion to end of growth portion may have a carrier concentration of 9.02E6/cm 3 to 5.30E6/cm 3 and a resistivity of 1.33E8 ⁇ . ⁇ to .64E8 ⁇ . ⁇ .
  • the dislocation density may be 3000/cm 2 at the starting portion and 5000/cm 2 at the end of growth portion. It is well known in the art that one can, by making suitable changes to the various system parameters, operate the process in regimes beyond those demonstrated explicitly in the embodiments . While the foregoing has been with reference to a particular embodiment of the invention, it will be appreciated by those skilled in the art that changes in this

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

Abstract

L'invention concerne des systèmes et des procédés pour la croissance des cristaux à l'aide de processus de croissance VGF et VB pour réduire une lignée de corps. Un exemple de mode de réalisation présente un procédé consistant à insérer une ampoule contenant une matière première dans un four ayant une source de chauffage, à faire croître un cristal à l'aide d'un processus de congélation à gradient vertical dans lequel le gradient de température de cristallisation est déplacé par rapport au cristal et/ou au four pour faire fondre la matière première et la reformer en un composé monocristallin, et à faire croître le cristal à l'aide d'un processus de Bridgman vertical dans lequel l'ampoule/la source de chauffage sont déplacées l'une par rapport à l'autre pour poursuivre la fusion de la matière première et la reformer en un composé monocristallin.
PCT/US2009/060072 2009-10-08 2009-10-08 Appareil et procédé de croissance des cristaux WO2011043777A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
PCT/US2009/060072 WO2011043777A1 (fr) 2009-10-08 2009-10-08 Appareil et procédé de croissance des cristaux
EP09850317.0A EP2501844A4 (fr) 2009-10-08 2009-10-08 Appareil et procédé de croissance des cristaux
JP2012533126A JP2013507313A (ja) 2009-10-08 2009-10-08 結晶成長装置および結晶成長方法

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PCT/US2009/060072 WO2011043777A1 (fr) 2009-10-08 2009-10-08 Appareil et procédé de croissance des cristaux

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
TWI833617B (zh) * 2023-03-24 2024-02-21 國立勤益科技大學 晶體生長裝置

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020115871A1 (fr) * 2018-12-06 2020-06-11 住友電気工業株式会社 PROCÉDÉ DE FABRICATION DE SUBSTRAT DE GaAs ET DISPOSITIF DE CROISSANCE DE MONOCRISTAL DE GaAs
WO2023209867A1 (fr) * 2022-04-27 2023-11-02 住友電気工業株式会社 Substrat monocristallin semi-conducteur composé du groupe iii-v et son procédé de fabrication

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US6334897B1 (en) * 1998-03-31 2002-01-01 Japan Energy Corporation Method of manufacturing compound semiconductor single crystal
US6896729B2 (en) * 2001-07-05 2005-05-24 Axt, Inc. Method and apparatus for growing semiconductor crystals with a rigid support with carbon doping and resistivity control and thermal gradient control
US20080311417A1 (en) * 2007-06-06 2008-12-18 Freiberger Compound Materials Gmbh Arrangement and method for manufacturing a crystal from a melt of a raw material and single crystal

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JP2013507313A (ja) 2013-03-04
EP2501844A1 (fr) 2012-09-26
EP2501844A4 (fr) 2013-08-07

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