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WO2013002540A2 - Appareil et procédé de croissance de monocristal de carbure de silicium - Google Patents

Appareil et procédé de croissance de monocristal de carbure de silicium Download PDF

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Publication number
WO2013002540A2
WO2013002540A2 PCT/KR2012/005048 KR2012005048W WO2013002540A2 WO 2013002540 A2 WO2013002540 A2 WO 2013002540A2 KR 2012005048 W KR2012005048 W KR 2012005048W WO 2013002540 A2 WO2013002540 A2 WO 2013002540A2
Authority
WO
WIPO (PCT)
Prior art keywords
silicon carbide
crucible
assisting tool
single crystal
heating element
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/KR2012/005048
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English (en)
Other versions
WO2013002540A3 (fr
Inventor
Young Shol Kim
Sun Hyuk Bae
Sung Wan Hong
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.)
SK Innovation Co Ltd
Original Assignee
SK Innovation Co Ltd
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 SK Innovation Co Ltd filed Critical SK Innovation Co Ltd
Priority to JP2014518794A priority Critical patent/JP5979740B2/ja
Publication of WO2013002540A2 publication Critical patent/WO2013002540A2/fr
Publication of WO2013002540A3 publication Critical patent/WO2013002540A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/80—Constructional details
    • 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
    • C30B17/00—Single-crystal growth onto a seed which remains in the melt during growth, e.g. Nacken-Kyropoulos 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
    • 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
    • C30B29/36—Carbides

Definitions

  • the present invention relates to an apparatus and a method for growing a silicon carbide single crystal by solution growth, and more particularly, to an apparatus and a method for growing a silicon carbide single crystal by solution growth at a high speed by allowing carbon contained in a graphite crucible to be smoothly dissolved in a silicon solution which is a main material.
  • the silicon carbide has excellent mechanical strength, excellent thermal and chemical stability, significantly high thermal conductivity of 4W/cm 2 or more, and an operation limit temperature of 650 °C or less, which is significantly higher than 200 °C corresponding to an operation limit temperature of the silicon.
  • the silicon carbides having crystal structures of a 3C silicon carbide, a 4H silicon carbide, and a 6H silicon carbide have a bandgap of 2.5 eV or more which is two times or more higher than that of the silicon, they are significantly excellent as a semiconductor material for a high power and low loss converting apparatus, such that they have been recently spotlighted as a semiconductor material for an optical semiconductor and power conversion, such as a light emitting diode (LED).
  • LED light emitting diode
  • a method for growing a silicon carbide single crystal there are the Acheson method of allowing carbon and silica to react with each other in a high temperature electric furnace of 2000 °C or more and a sublimation method of sublimating a silicon carbide (SiC) raw material at a high temperature of 2000 °C or more to grow a single crystal.
  • a method of chemically depositing a gas source has been used.
  • the sublimation method also has a limitation in view of a production cost since the sublimation method is generally performed at a high temperature of 2200 °C or more and it is more likely that several faults such as a micropipe and a stacking fault will be generated.
  • the Czochralski method is a method of growing a single crystal from a melt. A shape or a property of the crystal is determined according to a pulling rate (a growth speed), a rotation speed, a temperature gradient, or a crystal orientation.
  • a pulling rate a growth speed
  • a rotation speed a rotation speed
  • a temperature gradient a temperature gradient
  • crystal orientation a crystal orientation of the crystal.
  • silicon or silicon carbide powders are charged in a graphite crucible and a temperature is then raised from 1600 °C to a high temperature of 1900 °C to allow crystals to be grown from a surface of a silicon carbide seed positioned at an upper portion of the furnace.
  • a crystal growth speed is 50 ⁇ m/hr which is significantly low, such that economic efficiency is low.
  • titanium (Ti) or manganese (Mg) was mixed with silicon (Si) in a predetermined ratio to increase a crystal growth speed.
  • a graphite crucible is generally used as a supply source of carbon for growing a crystal. That is, carbon atoms composing the graphite crucible are separated in a liquid state and then spread in a solution. Some of the spread carbon atoms move to a silicon carbide single crystal growth portion, such that a single crystal is grown. However, a difference is generated between a carbon concentration in the vicinity of a crucible to which the carbon atoms are supplied and a carbon concentration in the vicinity of a single crystal growth portion at which a carbon atom is synthesized as a silicon carbide to thereby disappear.
  • a carbon concentration in a solution in the crucible within a closed growth furnace operated at a high temperature is required to be uniform to actually increase a carbon concentration in the vicinity of the single crystal growth portion.
  • a seed fixing bar to which a seed is fixed is rotated and/or a crucible is rotated to increase uniformity of a carbon concentration in a solution.
  • An object of the present invention is to provide an apparatus and a method for growing a silicon carbide single crystal capable of growing the silicon carbide single crystal at a more rapid speed.
  • an apparatus for growing a silicon carbide single crystal includes: a reaction chamber that is in a predetermined pressure state; a crucible that is provided in the reaction chamber, includes silicon (Si) or silicon carbide (SiC) powders or a mixture thereof charged therein, includes a silicon carbide seed provided at an upper portion of an inner side thereof and growing a silicon carbide and a seed connection bar extended from the silicon carbide seed, and is made of a graphite material; and a heating element that heats the crucible, wherein an inner portion of the crucible is provided with a cylindrical assisting tool having a plurality of pores formed at least at a side thereof and made of the graphite material.
  • the cylindrical assisting tool may have a thickness of 1 mm or more and include the pore having a size of 2 mm or more.
  • the thickness is smaller than the above-mentioned value, it is difficult to manufacture the cylindrical assisting tool, and the cylindrical assisting tool is broken during growth, such that it is difficult to maintain its shape.
  • the size of the pore is smaller than the above-mentioned value, workability is bad, and a flow of introduced carbon in the crucible is impeded, such that growth of the silicon carbide single crystal may be impeded.
  • the silicon carbide seed may be provided so as to be rotatable with respect to the crucible with the aid of the seed connection bar.
  • the silicon carbide seed may be provided so as to be vertically movable with respect to the crucible with the aid of the seed connection bar.
  • the apparatus may further include a rotation support that is disposed beneath the crucible to rotate the crucible.
  • the crucible itself disposed in the reaction chamber may rotate by the rotation support, such that silicon (Si) and carbon filled in the crucible may more rapidly contact each other, thereby increasing a growth speed of the silicon carbide single crystal.
  • the heating element may be disposed at any place in the vicinity of the crucible. However, it is preferable that the heating element is disposed on an outer peripheral surface of the crucible in order to increase operability of the cylindrical assisting tool.
  • the heating element any heating element having heating characteristics or performing a heating operation, typically, a resistive heating element or an induction heating type heating element may be used.
  • a temperature gradient in the crucible by the heating element may be 5°C/cm 2 or more in a vertical direction.
  • An inner portion of the reaction chamber may be filled with inert gas such as Argon or Helium gas and may be maintained at a pressure of 0.3 to 50 kgf/cm 2 .
  • the growth is performed at a pressure of 1 to 2 kgf/cm 2 .
  • a vacuum pump and a gas cylinder for controlling the atmosphere are connected to the reaction chamber through a valve.
  • a bottom surface of the cylindrical assisting tool may be further provided with a wing shaped assisting tool inducing a fluid flow in a predetermined direction and made of the graphite material.
  • the wing shaped assisting tool serves to allow a fluid flow by rotation of the silicon carbide seed and/or a fluid flow according to rotation of the crucible by the rotation support provided beneath the crucible to be selectively directed toward one direction to give a material such as carbon, or the like, faster and more contact opportunities with the silicon carbide seed, thereby increasing a formation speed of the silicon carbide single crystal.
  • a carbon concentration in the vicinity of a silicon carbide seed increases, such that a growth speed of a silicon carbide single crystal increases.
  • FIG. 1 is a cross-sectional view schematically showing main parts of an apparatus for growing a silicon carbide single crystal according to a preferable embodiment of the present invention.
  • FIG. 2 is a schematic perspective view of a porous cylindrical assisting tool shown in FIG. 1 and made of a graphite material.
  • FIG. 3 is a view showing a fluid flow in a crucible provided in the apparatus for growing a silicon carbide single crystal according to the preferable embodiment of the present invention.
  • FIG. 4 is a cross-sectional view schematically showing main parts of an apparatus for growing a silicon carbide single crystal according to a more preferable embodiment of the present invention.
  • FIG. 5 is a perspective view of a wing shaped assisting tool shown in FIG. 4 and made of a graphite material.
  • FIG. 6 is a view showing a fluid flow induced through the wing shaped assisting tool made of a graphite material and provided in the apparatus for growing a silicon carbide single crystal according to the more preferable embodiment of the present invention.
  • Reaction Chamber 30 Crucible (made of Graphite Material)
  • Heating Element 70 Cylindrical Assisting Tool (made of Graphite Material)
  • FIG. 1 schematically shows main parts of an apparatus for growing a silicon carbide single crystal according to a preferable embodiment of the present invention
  • FIG. 2 schematically shows a porous cylindrical assisting tool shown in FIG. 1 and made of a graphite material
  • FIG. 3 shows a fluid flow in a crucible provided in the apparatus for growing a silicon carbide single crystal shown in FIG. 1.
  • the apparatus 1 for growing a silicon carbide single crystal is configured to include a reaction chamber 10, a crucible 30 provided in the reaction chamber 10, a heating element 50 heating the crucible 30, and a cylindrical assisting tool 70 provided in the crucible 30.
  • the reaction chamber 10 is filled with inert gas such as Argon or Helium, and has a pressure of a level of 0.3 to 50 kgf/cm 2 .
  • inert gas such as Argon or Helium
  • a vacuum pump and a gas cylinder for controlling the atmosphere are connected to the reaction chamber 10 through a valve.
  • the crucible 30 is provided in the reaction chamber 10, as described above, and includes silicon (Si) or silicon carbide (SiC) powders or a mixture thereof charged therein.
  • the crucible 30 may be made of a graphite material and be utilized as a supply source of carbon in itself.
  • An upper portion of an inner side of the crucible 30 is provided with a silicon carbide seed 32 growing a silicon carbide with the aid of a seed connection bar 34, as shown in FIG. 1.
  • the seed connection bar 34 is provided so as to be rotatable with respect to an upper end portion of the crucible 30, if needed.
  • the seed connection bar 34 is provided so as to be vertically movable with respect to an upper end portion of the crucible 30 if needed, as a single crystal grows. Therefore, the silicon carbide seed 32 is also provided so as to be rotatable and provided so as to be vertically movable.
  • This heating element 50 may be any heating element having heating characteristics. According to the present invention, a resistive heating element or an induction heating type heating element may be used.
  • An inner portion of the crucible 30 is provided with the cylindrical assisting tool 70 made of a graphite material, as shown in FIG. 1.
  • a side of this cylindrical assisting tool 70 is formed with a plurality of pores, as shown in FIG. 2.
  • This cylindrical assisting tool 70 made of the graphite material allows more carbons to be dissolved in a silicon containing solution to increase a carbon concentration in the vicinity of a portion at which the single crystal is grown, thereby increasing a growth speed of the silicon carbide single crystal.
  • This cylindrical assisting tool 70 becomes a carbon supply source in itself.
  • a flow of the silicon and additives through the pores 72 of the cylindrical assisting tool 70 is generated by heating of the crucible 30 by the heating element 50 as shown in FIG. 3, rotation of the silicon carbide seed 32, if needed, and/or rotation of a rotation support 40 to be described below to further increase a supply amount and speed of a carbon supply source.
  • a carbon dissolution amount from the cylindrical assisting tool 70 increases, and a carbon concentration in the vicinity of a crystal growth portion of the silicon carbide seed further increases by the above-mentioned flow, thereby increasing a growth speed of the silicon carbide single crystal.
  • a lower portion of the crucible 30 is provided with the rotation support 40.
  • This rotation support 40 may rotate, if needed, to allow the crucible to rotate at a predetermined speed.
  • the carbon from the crucible 30 and the carbon from the cylindrical assisting tool 70 are rapidly dissolved in the silicon containing solution by this rotation and the carbon concentration in the vicinity of the silicon carbide seed 32 increases by this rotation, such that the growth speed of the silicon carbide single crystal further increases.
  • FIG. 4 schematically shows main parts of an apparatus for growing a silicon carbide single crystal according to a more preferable embodiment of the present invention
  • FIG. 5 schematically shows a wing shaped assisting tool shown in FIG. 4 and made of a graphite material
  • FIG. 6 shows a fluid flow induced through the wing shaped assisting tool made of a graphite material and provided in the apparatus for growing a silicon carbide single crystal according to the more preferable embodiment of the present invention.
  • the apparatus for growing a silicon carbide single crystal according to the more preferable embodiment of the present invention further includes the wing shaped assisting tool 90 formed at the bottom of the crucible 30 and made of the graphite material, in addition to the components of the apparatus 1 for growing a silicon carbide single crystal according to the preferable embodiment of the present invention described above.
  • the wing shaped assisting tool 90 made of the graphite material and pertaining to a partial configuration of the present invention is provided together with the above-mentioned cylindrical assisting tool 70 in the present invention, it may be recognized by those skilled in the art sufficiently aware of the present specification that the wing shaped assisting tool 90 may be singly provided without the above-mentioned cylindrical assisting tool 70.
  • the wing shaped assisting tool 90 made of the graphite material and pertaining to a partial configuration of the present invention is provided at the bottom of the crucible 30 in order to induce a fluid flow in a predetermined direction.
  • the wing shaped assisting tool 90 may be singly provided or provided together with the above-mentioned cylindrical assisting tool 70.
  • the wing shaped assisting tool 90 may be provided at a lower end in the cylindrical assisting tool 70 or be separately provided in a state in which it is spaced apart from the cylindrical assisting tool 70 by a predetermined distance.
  • the cylindrical assisting tool 70 needs to be spatially fixed by a separate unit from a bottom surface, an inner peripheral surface, or an inner side of an upper portion of the crucible 30 and needs to be fixed so as to be spatially spaced from the wing shaped assisting tool 90 by a separate unit from the wing shaped assisting tool 90.
  • the wing shaped assisting tool 90 is configured so that a fluid may flow in one direction, particularly as shown in FIG. 5. Further, since the wing shaped assisting tool 90 is made of the graphite material, it is used as a carbon supply source in itself. In the case in which a rotation flow is generated by rotation of the silicon carbide seed 32 and/or the rotation support 40, the wing shaped assisting tool 90 as described above capable of inducing a unidirectional flow further doubles the rotation flow to increase the carbon concentration in the vicinity of the silicon carbide seed 32.
  • the wing shaped assisting tool 90 induces the fluid flow generated by the heating of the crucible 30 by the heating element 40 in one direction to increase the carbon concentration in the vicinity of the silicon carbide seed 32, thereby making it possible to increase the carbon concentration in the vicinity of a portion at which the silicon carbide single crystal is grown.
  • the number and the shape of wings are not limited to those of wings shown in FIGS. 3 to 5.

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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 un appareil et un procédé de croissance de monocristal de carbure de silicium par croissance en solution Cet appareil de croissance de monocristal de carbure de silicium comprend : une chambre de réaction se trouvant dans un état de pression prédéterminé; un creuset logé dans la chambre de réaction, contenant des poudres de silicium (Si) ou de carbure de silicium (SiC) ou un mélange de celles-ci, un germe de carbure de silicium sur une partie supérieure de sa face intérieure et permettant la croissance d'un carbure de silicium, et une barre de raccordement de germe s'étendant à partir du germe de carbure de silicium, constituée de matériau de graphite; et un élément chauffant qui chauffe le creuset. Une partie intérieure du creuset présente un outil d'assistance cylindrique comportant une pluralité de pores formés au moins sur un côté de ce dernier et constitué de matériau de graphite.
PCT/KR2012/005048 2011-06-29 2012-06-26 Appareil et procédé de croissance de monocristal de carbure de silicium Ceased WO2013002540A2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2014518794A JP5979740B2 (ja) 2011-06-29 2012-06-26 炭化ケイ素単結晶成長装置及びその方法

Applications Claiming Priority (2)

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KR1020110063656A KR20130007109A (ko) 2011-06-29 2011-06-29 탄화규소 단결정 성장 장치 및 그 방법
KR10-2011-0063656 2011-06-29

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WO2013002540A2 true WO2013002540A2 (fr) 2013-01-03
WO2013002540A3 WO2013002540A3 (fr) 2013-04-11

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111676519A (zh) * 2020-08-05 2020-09-18 郑红军 碳化硅晶体熔体生长装置
WO2023201934A1 (fr) * 2022-04-22 2023-10-26 中电化合物半导体有限公司 Appareil et procédé destinés à faire croître un monocristal de carbure de silicium par le procédé pvt

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KR101636435B1 (ko) * 2014-10-22 2016-07-06 한국세라믹기술원 다공성 흑연도가니 및 이를 이용한 탄화규소 단결정의 용액성장 제조방법
KR101633183B1 (ko) * 2014-10-27 2016-06-24 오씨아이 주식회사 잉곳 제조 장치
JP2017119594A (ja) * 2015-12-28 2017-07-06 東洋炭素株式会社 単結晶ＳｉＣの製造方法及び収容容器
WO2017183747A1 (fr) * 2016-04-21 2017-10-26 한국세라믹기술원 Creuset destiné à une solution de croissance et procédé de croissance d'une solution à l'intérieur d'un creuset
CN105970295B (zh) * 2016-06-24 2018-04-10 山东天岳先进材料科技有限公司 一种液相法生长碳化硅晶体的装置及方法
KR102103884B1 (ko) * 2016-09-30 2020-04-23 주식회사 엘지화학 실리콘카바이드 단결정의 제조 장치 및 제조 방법
KR102088924B1 (ko) * 2018-09-06 2020-03-13 에스케이씨 주식회사 탄화규소 단결정 잉곳 성장 장치
KR102479334B1 (ko) * 2018-10-11 2022-12-19 주식회사 엘지화학 실리콘카바이드 단결정의 제조 장치 및 제조 방법
KR102166640B1 (ko) * 2018-11-09 2020-10-16 일진디스플레이(주) 탄화규소 단결정 성장장치용 지그

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Publication number Priority date Publication date Assignee Title
CN111676519A (zh) * 2020-08-05 2020-09-18 郑红军 碳化硅晶体熔体生长装置
WO2023201934A1 (fr) * 2022-04-22 2023-10-26 中电化合物半导体有限公司 Appareil et procédé destinés à faire croître un monocristal de carbure de silicium par le procédé pvt

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WO2013002540A3 (fr) 2013-04-11
JP5979740B2 (ja) 2016-08-31
KR20130007109A (ko) 2013-01-18
JP2014518195A (ja) 2014-07-28

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