WO2014137072A1 - Appareil et procédé destinés à faire croître des monocristaux de carbure de silicium - Google Patents

Appareil et procédé destinés à faire croître des monocristaux de carbure de silicium Download PDF

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Publication number
WO2014137072A1
WO2014137072A1 PCT/KR2014/000587 KR2014000587W WO2014137072A1 WO 2014137072 A1 WO2014137072 A1 WO 2014137072A1 KR 2014000587 W KR2014000587 W KR 2014000587W WO 2014137072 A1 WO2014137072 A1 WO 2014137072A1
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WO
WIPO (PCT)
Prior art keywords
crucible
single crystals
silicon carbide
carbide single
seed
Prior art date
Application number
PCT/KR2014/000587
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English (en)
Inventor
Jung Gyu Kim
Jong Hwi Park
Kap Ryeol Ku
Myung Ok Kyun
Jung Woo Choi
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Skc Co., Ltd.
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Publication date
Application filed by Skc Co., Ltd. filed Critical Skc Co., Ltd.
Publication of WO2014137072A1 publication Critical patent/WO2014137072A1/fr

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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
    • 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
    • C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
    • C30B23/02—Epitaxial-layer growth
    • C30B23/06—Heating of the deposition chamber, the substrate or the materials to be evaporated
    • C30B23/066—Heating of the material to be evaporated
    • 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
    • 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 silicon carbide single crystals, more particularly to an apparatus and a method for growing high-quality silicon carbide (SiC) single crystals by coating the inner wall of a crucible or a seed holder with tungsten (W).
  • SiC silicon carbide
  • SiC silicon
  • GaN, AlN, ZnO gallium-oxide-semiconductor
  • SiC gallium-oxide-semiconductor
  • SiC gallium-oxide-semiconductor
  • GaN, AlN, ZnO substrates since SiC has superior thermal conductivity of about 4.6 W/cmoC and can be produced into a large-sized substrate with a diameter of 2 inches or greater, it is favored over GaN, AlN or ZnO substrates.
  • SiC crystals are classified based on their growth temperature. 6H-SiC single crystal is used in LED devices and 4H-SiC single crystal is used in power devices. At present, 4H-SiC single-crystal substrates are favored in the aspects of environment friendliness and power loss reduction.
  • a seed (4H-SiC or 6H-SiC) is attached on a seed holder and a 4H-SiC or 6H-SiC single crystal is grown on the seed (4H-SiC or 6H-SiC).
  • the seed (4H-SiC or 6H-SiC) is attached so as to be in contact with the seed holder.
  • the 4H-SiC or 6H-SiC single crystal is grown on the seed (4H-SiC or 6H-SiC) as time goes on.
  • PCT/US2000/41076 discloses use of a graphite crucible coated with a thin coating of a metal carbide, particularly a carbide selected from a group consisting of tantalum carbide, hafnium carbide, niobium carbide, titanium carbide, zirconium carbide, tungsten carbide, and vanadium carbide.
  • PCT/US2005/006058 discloses a Czochralski (CZ) system for growth of a single-crystal silicon ingot from a molten silicon feedstock, including: a low low-aspect-ratio, wide-diameter crucible including a base and side walls for holding a quantity of molten silicon at a melt/crystal interface with respect to a seed crystal for growing an ingot from the molten material; a pre-melter for providing a continuous source of molten silicon feedstock to the crucible, such that the melt/crystal interface is maintained at a desired level without vertical travel of the crucible; a plurality of pull chambers rotatably disposed with respect to the crucible for pulling the seed crystal so as to form an ingot such that the crucible for each pull chamber is replenished at a desired level by the pre-melter; and an annular heating means disposed beneath the base of the crucible with a fixed distance for providing a uniform thermal distribution across the cruci
  • Tungsten is advantageous in that manufacturing cost is lower as compared to the previously used material and can prevent inclusion of carbon, which negatively affects crystal quality, since it can act as carbon getter by reacting with free carbon in the crucible.
  • a graphite crucible is used to grow silicon carbide single crystals.
  • the graphite crucible is heated by induction heating.
  • the reaction occurring on the surface of the crucible varies depending on the material of the crucible.
  • carbon is supplied as a source for the growth of silicon carbide single crystals, resulting in defects as the increased carbon acts as impurity.
  • loss of the graphite crucible occurs as the sublimed silicon etches the graphite crucible.
  • seed back etching or other problem occurs at the portion where the seed is attached to the graphite.
  • the present invention is directed to providing an apparatus and a method for growing high-quality silicon carbide single crystals capable of preventing formation of defects caused by inclusion of carbon from a graphite crucible and capable of preventing crucible etching and seed back etching by coating the graphite crucible with tungsten.
  • the present invention provides an apparatus for growing silicon carbide single crystals using a seed holder coated with tungsten (W) and a method for growing silicon carbide single crystals using same.
  • the present invention provides an apparatus for growing silicon carbide single crystals using a graphite crucible coated with tungsten (W) and a method for growing silicon carbide single crystals using same.
  • the present invention provides an apparatus for growing silicon carbide single crystals, including: a crucible comprising a hollow portion inside thereof and a tungsten film layer covering all or part of an inner wall thereof; an insulating material covering all or part of an outer wall of the crucible; and a heating means disposed outside the insulating material, and a method for growing silicon carbide single crystals using same.
  • silicon carbide single crystals of higher quality than the single crystals grown using the existing graphite crucible can be produced.
  • Figs. 1a and 1b are respectively a cross-sectional view and a plan view of a seed attached to a seed holder.
  • Figs. 2a and 2b are respectively a cross-sectional view and a plan view of silicon carbide single crystals grown from a seed attached to a seed holder.
  • Fig. 3 is a cross-sectional view of an apparatus for growing silicon carbide single crystals according to an exemplary embodiment of the present invention.
  • Fig. 4 is a plan view of silicon carbide single crystals (ingot) grown in Comparative Example.
  • Fig. 5 is a plan view of silicon carbide single crystals grown in Example.
  • Fig. 6 is a longitudinal cross-sectional view of silicon carbide single crystals (ingot) grown in Comparative Example.
  • Fig. 7 is a longitudinal cross-sectional view of silicon carbide single crystals grown in Example.
  • Fig. 8 shows Si-face rocking curves of silicon carbide single crystals grown in Comparative Example.
  • Fig. 9 shows Si-face rocking curves of silicon carbide single crystals grown in Example.
  • the present invention provides an apparatus for growing silicon carbide single crystals, including: a crucible including a hollow portion inside thereof and a tungsten film layer covering all or part of an inner wall thereof; an insulating material covering all or part of an outer wall of the crucible; and a heating means disposed outside the insulating material.
  • the apparatus for growing silicon carbide single crystals includes a seed holder located above the hollow portion, the seed holder having a tungsten film layer formed on one surface thereof to which the seed is attached.
  • the present invention also provides a method for growing silicon carbide single crystals using a seed holder coated with tungsten or a graphite crucible coated with tungsten.
  • the method for growing single crystals according to the present invention is a method for growing 4H-SiC or 6H-SiC single crystals on a 4H-SiC or 6H-SiC seed using a graphite crucible coated with tungsten and includes coating an existing graphite crucible with tungsten and growing silicon carbide single crystals on a seed attached to one surface of a seed holder.
  • the seed holder made from high-density graphite may be coated with tungsten and a seed may be attached thereto.
  • the seed holder with the seed attached may be disposed at an upper portion in the graphite crucible and silicon carbide single crystals may be grown on the seed.
  • tungsten which has the highest melting point of all metals, is used to capture carbon during growth of single crystals.
  • the melting points of metals that serve similar roles are described in Table 1.
  • tungsten as in the present invention is advantageous in that a) inclusion of the metal during the growth of silicon carbide single crystals is reduced because of high melting point, b) the material is easily available than the existing carbon-capturing materials and thus is less costly, c) the temperature of the seed can be lowered by about 100 oC because of low infrared emissivity of 0.5 (graphite: 0.85-0.95), d) crucible etching caused by sublimed silicon source can be prevented, and e) seed back etching and inclusion of carbon into ingot can be prevented.
  • Figs. 1a and 1b are respectively a cross-sectional view and a plan view of a seed attached to a seed holder.
  • Figs. 2a and 2b are respectively a cross-sectional view and a plan view of silicon carbide single crystals grown from a seed attached to a seed holder.
  • Fig. 3 is a cross-sectional view of an apparatus for growing silicon carbide single crystals according to an exemplary embodiment of the present invention.
  • An apparatus for growing silicon carbide single crystals includes a tungsten film layer 600 formed on one surface of a seed holder 100. A seed 200 is attached on the tungsten film layer 600.
  • the seed holder 100 may be formed of graphite, but is not particularly limited in its material.
  • the tungsten film layer 600 may be formed by thermal spray coating, chemical vapor deposition (CVD), etc., but is not particularly limited in the formation method.
  • the tungsten film layer 600 may be formed to cover all or part of one surface of the seed holder, and may also be formed to cover the side surface of the seed holder.
  • the tungsten film layer 600 may have a thickness of 50-500 ⁇ m, but is not particularly limited in its thickness.
  • the seed 200 may have different crystal structures depending on the crystal desired to grow, e.g., 4H-SiC, 6H-SiC, 3C-SiC or 15R-SiC.
  • a tungsten film layer 600 may be formed inside the crucible.
  • an apparatus for growing silicon carbide single crystals may include a crucible 510 in which a feedstock is loaded, a seed holder 100 to which a seed 200 is attached, an insulating material 520 surrounding the crucible 510, a quartz tube 530 and a heating means 540 disposed outside the quartz tube 530 for heating the crucible 510.
  • the apparatus may further include a controller (not shown) for independently operating the heating means 540.
  • the crucible 510 is prepared from a material having a melting point higher than the sublimation temperature of silicon carbide.
  • it may be made from graphite and the tungsten film layer 600 may be present on an inner wall of the crucible 510.
  • the feedstock A loaded in the crucible 510 may include, e.g., silicon carbide powder.
  • the seed holder 100 is prepared using high-density graphite. As described above, the seed 200 is attached to the seed holder 100 having the tungsten film layer 600 formed thereon. The seed holder 100 with the seed 200 attached is disposed at an upper portion in the crucible 510 so as to grow single crystals 300 on the seed 200.
  • the insulating material 520 and the quartz tube 530 are disposed outside the crucible 510 and maintain the temperature of the crucible 510 at a crystal growth temperature. Since the crystal growth temperature of silicon carbide is very high, a graphite felt prepared by compressing graphite fiber into a tubular cylinder with a predetermined thickness may be used as the insulating material 520. Also, the insulating material 520 may be formed as a plurality of layers to surround the crucible 510.
  • the heating means 540 is disposed outside the quartz tube 530.
  • a high-frequency induction coil may be used as the heating means 540.
  • the crucible 510 may be heated by allowing a high-frequency current to flow in the high-frequency induction coil and, consequently, the feedstock A may be heated to a desired temperature.
  • a method for growing single crystals according to an exemplary embodiment of the present invention is a method for growing single crystals 300 on a seed 200.
  • a seed 200 is prepared first.
  • 4H-SiC or 6H-SiC was used as the seed 200 in Example, other various kinds of seeds (3C-SiC, 15R-SiC, etc.) may be used without being limited thereto.
  • the seed 200 may have a circular shape with a diameter of 2 inches or greater.
  • the seed 200 is attached onto a seed holder 100.
  • the seed 200 is attached onto a seed holder 100 having a tungsten film layer 600 formed thereon.
  • the seed 200 may be attached on the seed holder 100 using a carbon paste or a photoresist.
  • various adhesives capable of attaching the seed 200 on the seed holder 100 may be used without being limited thereto.
  • the seed holder 100 having the seed 200 attached is inserted in an apparatus for growing single crystals and then single crystals 300 are grown on the seed 200.
  • the seed holder 100 having the seed 200 attached may be inserted into the apparatus using a guide ring.
  • a lower surface of the seed holder 100 is attached to an upper portion inside a crucible 510, such that an upper surface of the seed holder 100 having the seed 200 attached faces an upper side of the crucible 510.
  • a feedstock A e.g., SiC powder
  • impurities contained in the crucible 510 are removed by heating for 2-3 hours at 1300-1500 oC in vacuo. Subsequently, air remaining inside the crucible 510 and between the crucible 510 and an insulating material 520 is removed by injecting an inert gas, e.g. argon (Ar) gas. Then, after raising pressure to atmospheric pressure, the crucible 510 is heated to 2000-2300 oC using a heating means 540.
  • the reason why atmospheric pressure is maintained is to prevent polymorphism, i.e., formation of unwanted crystals in the early stage of crystal growth. That is to say, the feedstock A is first heated to the crystal growth temperature while maintaining atmospheric pressure. Then, single crystals 300 are grown by subliming the feedstock A by lowering the pressure inside the crucible to 5-30 Torr and maintain the pressure.
  • the silicon carbide single crystals grown using the crucible and the seed holder having the tungsten film layers 600 exhibit fewer defects than the single crystals grown using the existing graphite crucible and seed holder. Accordingly, by growing single crystals using a graphite crucible having a tungsten film layer 600 formed thereon, silicon carbide single crystals having fewer defects can be grown.
  • Silicon carbide single crystals were grown using a graphite crucible having a tungsten film layer and a seed holder having a tungsten film layer.
  • the tungsten film layers were formed by thermal spray coating to a thickness of 100 ⁇ m.
  • impurities contained in the graphite crucible were removed by heating for 2-3 hours at about 1400 oC in vacuo. Subsequently, air remaining in the graphite crucible and between the graphite crucible and the insulating material was removed by injecting argon (Ar) gas. Then, after raising pressure to atmospheric pressure, the graphite crucible was heated to about 2200 oC using a heating means. Subsequently, silicon carbide single crystals were grown for 70 hours by lowering the pressure inside the graphite crucible to about 10 Torr.
  • Ar argon
  • Silicon carbide single crystals were grown in the same manner as in Example, except that a graphite crucible without a tungsten film layer and a seed holder without a tungsten film layer were used.
  • Fig. 4 is a plan view of the silicon carbide single crystals (ingot) grown in Comparative Example
  • Fig. 5 is a plan view of the silicon carbide single crystals grown in Example. As shown in Fig. 4 and Fig. 5, when the crucible and the seed holder having the tungsten film layers were used (Example), the quality of the single crystals was very superior.
  • Fig. 6 is a longitudinal cross-sectional view of the silicon carbide single crystals (ingot) grown in Comparative Example
  • Fig. 7 is a longitudinal cross-sectional view of the silicon carbide single crystals grown in Example.
  • Fig. 8 shows Si-face rocking curves of the silicon carbide single crystals grown in Comparative Example
  • Fig. 9 shows Si-face rocking curves of the silicon carbide single crystals grown in Example.
  • the Si-face rocking curve is used to evaluate the quantity or quality of grown single crystals.
  • a smaller full width at half maximum (FWHM) indicates better quantity or quality of single crystals.
  • the FWHM of the silicon carbide single crystals prepared in Comparative Example was 38-55 arcsec, suggesting low crystallinity.
  • the FWHM of the silicon carbide single crystals prepared in Example was 38-40 arcsec, suggesting much superior crystallinity.
  • an apparatus and a method for growing silicon carbide single crystals according to the present invention can grow high-quality silicon carbide single crystals by preventing etching of a graphite crucible by a tungsten film layer formed on an inner wall of the crucible and by preventing seed back etching at a portion where a seed is attached to a seed holder by a tungsten film layer formed on at least one surface of the seed holder.

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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

La présente invention concerne un appareil et un procédé destinés à faire croître des monocristaux de carbure de silicium de haute qualité par application d'un revêtement de tungstène (W) sur une paroi interne d'un creuset en graphite existant. Selon la présente invention, on peut faire croître des monocristaux de carbure de silicium de haute qualité par application d'un revêtement de tungstène (W) sur la paroi interne du creuset en graphite existant.
PCT/KR2014/000587 2013-03-07 2014-01-21 Appareil et procédé destinés à faire croître des monocristaux de carbure de silicium WO2014137072A1 (fr)

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KR10-2013-0024295 2013-03-07
KR1020130024295A KR101458183B1 (ko) 2013-03-07 2013-03-07 탄화규소 단결정 성장 장치 및 방법

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108707966A (zh) * 2018-08-27 2018-10-26 山东大学 一种低氮含量SiC单晶生长装置及其应用
EP3816331A1 (fr) * 2019-10-29 2021-05-05 SKC Co., Ltd. Tranche de sic et procédé de préparation d'une tranche de sic

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KR102675266B1 (ko) * 2017-12-04 2024-06-14 신에쓰 가가꾸 고교 가부시끼가이샤 탄화탄탈 피복 탄소 재료 및 그 제조 방법, 반도체 단결정 제조 장치용 부재
KR102090084B1 (ko) 2018-08-30 2020-03-17 에스케이씨 주식회사 반절연 탄화규소 단결정 잉곳을 성장시키는 방법
KR102090085B1 (ko) 2018-08-30 2020-03-17 에스케이씨 주식회사 반절연 탄화규소 단결정 잉곳을 성장시키는 방법
CN111074338B (zh) 2018-10-22 2022-09-20 赛尼克公司 具有保护膜的籽晶及其制备方法和附着方法、采用该籽晶的晶锭的制备方法
KR102102543B1 (ko) * 2018-10-22 2020-04-20 에스케이씨 주식회사 보호막을 포함하는 종자정의 제조방법, 이를 적용한 잉곳의 제조방법 및 보호막을 포함하는 종자정

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US20020096108A1 (en) * 1999-07-07 2002-07-25 Harald Kuhn Device having a foil-lined crucible for the sublimation growth of an SiC single crystal
KR20060115891A (ko) * 2003-12-03 2006-11-10 제너럴 일렉트릭 캄파니 기포 함량이 감소된 석영 도가니 및 이의 제조방법
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108707966A (zh) * 2018-08-27 2018-10-26 山东大学 一种低氮含量SiC单晶生长装置及其应用
EP3816331A1 (fr) * 2019-10-29 2021-05-05 SKC Co., Ltd. Tranche de sic et procédé de préparation d'une tranche de sic
US11708644B2 (en) 2019-10-29 2023-07-25 Senic Inc. Method for preparing SiC ingot, method for preparing SiC wafer and the SiC wafer prepared therefrom

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KR101458183B1 (ko) 2014-11-05

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