WO2008018322A1 - Monocristal de carbure de silicium et son procédé de production - Google Patents

Monocristal de carbure de silicium et son procédé de production Download PDF

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Publication number
WO2008018322A1
WO2008018322A1 PCT/JP2007/064970 JP2007064970W WO2008018322A1 WO 2008018322 A1 WO2008018322 A1 WO 2008018322A1 JP 2007064970 W JP2007064970 W JP 2007064970W WO 2008018322 A1 WO2008018322 A1 WO 2008018322A1
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WIPO (PCT)
Prior art keywords
silicon carbide
raw material
single crystal
producing
crystal
Prior art date
Application number
PCT/JP2007/064970
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English (en)
Japanese (ja)
Inventor
Masanori Ikari
Toru Kaneniwa
Takao Abe
Original Assignee
Shin-Etsu Chemical Co., Ltd.
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Filing date
Publication date
Application filed by Shin-Etsu Chemical Co., Ltd. filed Critical Shin-Etsu Chemical Co., Ltd.
Publication of WO2008018322A1 publication Critical patent/WO2008018322A1/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
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/10—Heating of the reaction chamber or the substrate
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies

Definitions

  • the present invention relates to a single crystal silicon carbide used as a semiconductor device material or LED material and a method for producing the same.
  • Single-crystal silicon carbide is useful as a material for harsh environment-resistant devices and power devices because of its large crystal bond energy, large dielectric breakdown electric field, and high thermal conductivity.
  • its lattice constant is close to that of GaN, so it is useful as a substrate material for GaN LED.
  • this single crystal silicon carbide is produced by using a Rayleigh method in which silicon carbide powder is sublimated in a graphite crucible and single crystal silicon carbide is recrystallized on the inner wall of the graphite crucible, or a raw material based on this Rayleigh method.
  • An optimized Rayleigh method in which silicon carbide seed single crystals are placed in the part to be recrystallized by optimizing the arrangement and temperature distribution and epitaxially recrystallized, and a gas source that is a silicon carbide production source is heated by a carrier gas.
  • the silicon carbide powder is transferred to the silicon carbide seed single crystal and is epitaxially grown while chemically reacting on the crystal surface.
  • the CVD method is used.
  • There is a sublimation proximity method in which recrystallization growth is epitaxially grown on a seed single crystal.
  • each of these single crystal silicon carbide manufacturing methods is considered to have a problem.
  • the Rayleigh method can produce single crystal silicon carbide with good crystallinity, but crystal growth is based on spontaneous nucleation, so shape control and crystal surface control are difficult, and large-diameter wafers can be obtained. There is a problem that can not be.
  • the improved Rayleigh method can obtain a large-diameter single-crystal silicon carbide ingot at a high speed of several hundreds of 11 m / h, it grows in a spiral manner, resulting in the generation of many micropipes in the crystal. There's a problem.
  • the CVD method can produce high-quality single crystal silicon carbide with high purity and low defect density, but due to the epitaxial growth in a dilute gas source, the growth rate is slow, about 10 11 m / h.
  • the problem of not being able to obtain a single crystal silicon carbide ingot is there.
  • In the sublimation proximity method there is a problem that it is impossible to obtain a long single-crystal silicon carbide ingot due to restrictions on the force structure that can realize high-purity silicon carbide epitaxial growth with a relatively simple structure.
  • the method for producing single-crystal silicon carbide disclosed in Patent Document 1 includes a silicon carbide seed single crystal that is maintained in an inert gas atmosphere in a heated state. It is configured to supply silicon dioxide ultrafine particles and carbon ultrafine particles, which are raw materials for producing single crystal silicon carbide, to the surface from the outside.
  • silicon carbide powder which is a raw material for producing single crystal silicon carbide
  • the vapor pressure of silicon carbide in the atmosphere near the surface of the silicon carbide seed single crystal is low. For this reason, when the silicon carbide seed single crystal is held in a heated state, there is a concern that self-decomposition and / or etching with an atmospheric gas is caused.
  • the surface of the silicon carbide seed single crystal becomes rough due to decomposition and / or etching, the degree of supersaturation on the surface of the silicon carbide seed single crystal due to the difference in the fine shape of the surface of the silicon carbide seed single crystal.
  • the variation in the thickness is increased and epitaxial growth is performed on the surface, dislocation increases, polycrystallization occurs, and the crystal quality of the epitaxially grown silicon carbide is remarkably lowered. Therefore, in order to obtain high-quality single-crystal silicon carbide by the method for producing single-crystal silicon carbide disclosed in Patent Document 1, the surface of the silicon carbide seed single crystal must be decomposed while being heated. And / or the occurrence of etching needs to be prevented or avoided by some means.
  • Patent Document 1 Japanese Patent No. 3505597
  • the present invention has been made in order to solve the above-described problems, and an object of the present invention is to prevent dislocation and / or etching by preventing decomposition and / or etching of the seed crystal surface. Another object of the present invention is to provide high-quality single crystal silicon carbide in which defects such as micropipes are suppressed and a method for producing the same.
  • the single crystal silicon carbide is produced on the silicon carbide seed crystal before the decomposition prevention step before the surface temperature of the crucible reaches a temperature at which the surface of the silicon carbide seed crystal is decomposed and / or etched.
  • a method for producing single-crystal silicon carbide according to (1) which is a raw material preliminary supply step for starting continuous supply of raw materials for use;
  • the raw material pre-feeding process is started from the time when the surface temperature of the crucible is 1,970 ° C. force, 2,100 ° C. Method for producing crystalline silicon carbide,
  • the silicon carbide manufacturing raw material supplied in the decomposition prevention step is the same type as the silicon carbide manufacturing raw material supplied in the growth step (2) to (5) V, single crystal silicon carbide according to any one of Manufacturing method, (7)
  • the raw materials for silicon carbide production supplied in the decomposition prevention process and the growth process are silica particles and carbon particles, and the weight ratio of silica / carbon is 1.5-5 (2)-(6) Or a method for producing single-crystal silicon carbide according to any one of the above,
  • FIG. 1 is a conceptual diagram showing an example of a production apparatus used for producing single crystal silicon carbide.
  • a method for producing a silicon carbide single crystal of the present invention is an arrangement in which a susceptor to which a silicon carbide seed crystal is fixed and a raw material supply pipe for supplying a raw material for producing single crystal silicon carbide from the outside are arranged in a crucible.
  • a step of preventing the decomposition and / or etching of the silicon carbide seed crystal surface when the crucible is heated by external heating, and the temperature inside the crucible is further raised to a single crystal growth temperature. Maintaining this single crystal growth temperature, the silicon carbide seed crystal And a growth step of growing single crystal silicon carbide by continuously supplying a raw material for producing silicon carbide on the surface.
  • a susceptor having a silicon carbide seed crystal fixed and a raw material supply pipe are arranged in a crucible.
  • the shape of the crucible used in the present invention is not particularly limited, and can be appropriately selected according to the size and shape of the target single crystal silicon carbide.
  • the material of the crucible is made of graphite suitable as a high-temperature heat source.
  • a silicon carbide single crystal is preferred, and a silicon carbide single crystal is more preferably used in the form of a wafer.
  • the shape of the susceptor that holds the silicon carbide seed crystal, the silicon carbide seed single crystal, or the silicon carbide seed single crystal wafer is not particularly limited, and can be exemplified by a cylindrical shape, which matches the size and shape of the target silicon carbide seed crystal. A shape other than the wafer can be selected as appropriate.
  • the material of the susceptor is preferably made of Graphite, taking into consideration the operating temperature range.
  • the normal direction of the surface holding the silicon carbide seed single crystal at the upper end or the lower end of the susceptor can be freely set from approximately parallel to the vertical direction of the susceptor to a maximum 45 ° inclination.
  • the silicon carbide seed crystal used in the present invention preferably has the ability to use a silicon carbide single crystal in the form of a wafer.
  • S The type, size, and shape of the seed single crystal wafer are not particularly limited, and are intended. It can be appropriately selected depending on the type, size, and shape of the single crystal silicon carbide.
  • a silicon carbide single crystal wafer obtained by pretreating a silicon carbide single crystal obtained by the modified Rayleigh method as necessary can be suitably used.
  • the seed crystal may be a just substrate or an off-angle substrate. Examples of the silicon carbide seed crystal include a just-face Si face substrate and a (0001) Si face substrate having an off angle of several degrees.
  • the shape of the raw material supply pipe for continuously supplying the raw material for producing single crystal silicon carbide is not particularly limited, and a hollow cylinder can be exemplified, and its specific shape is appropriately selected according to the size and shape of the target single crystal silicon carbide. Can be selected.
  • the material of the supply pipe should take into account the operating temperature range. Preferably it is made of Graphite.
  • the raw material supply pipe may be arranged at a right angle or obliquely opposite to the susceptor to which the silicon carbide seed single crystal is fixed in the crucible.
  • a decomposition preventing step for preventing the decomposition and / or etching of the silicon carbide seed crystal surface, and further raising the temperature in the crucible to the single crystal growth temperature.
  • a growth step is performed in which the growth temperature is maintained and the supply of the raw material for silicon carbide production is continued on the surface of the silicon carbide seed crystal to grow single crystal silicon carbide.
  • the raw material for producing silicon carbide is supplied to the surface of the silicon carbide seed crystal from the temperature at which the seed crystal decomposition and / or etching starts. This is also called “preliminary supply”.
  • silica particles and carbon particles or secondary particles composed of silica particles and carbon particles can be suitably used as a raw material for producing single crystal silicon carbide used in the present invention.
  • the type, particle size, and particle shape of these silica particles and carbon particles are not particularly limited.
  • high-purity silica (fomed silica) obtained by flame hydrolysis or high-purity carbon black is preferable.
  • Both silica particles and carbon particles are preferably fine particles with a primary particle size of lOOnm or less. Fine particles of 40 nm or less are more preferred. Ultrafine particles of 20 nm or less are more preferred. Ultrafine particles of 5 to 20 nm are particularly preferred. .
  • the ratio of the supply amount of the silica particles and the carbon particles is not particularly limited, and is a force S that allows a desired composition ratio to be appropriately selected. It is. Two or more kinds of silica particles and carbon particles may be mixed and used. The silica particles and carbon particles may be pretreated or a small amount of other components may be added as necessary.
  • the silica particles and the carbon particles may be supplied onto the silicon carbide seed single crystal wafer as long as both the preliminary supply stage and the single crystal growth stage can be continuously supplied without interruption. It is not specifically limited, For example, use of the apparatus which can carry out powder conveyance continuously like a commercially available powder feeder is mentioned. However, the supply line of the raw material for manufacturing single crystal silicon carbide and the inside of the single crystal silicon carbide manufacturing apparatus are free of argon to prevent oxygen contamination. It is preferable to have a methic structure substituted with an inert gas such as helium
  • the supply conditions for the silicon carbide production raw material substantially consisting of the silica particles and the carbon particles to the surface of the silicon carbide single crystal wafer are as follows: Even if the raw materials for producing the single crystal silicon carbide are mixed in advance on the silicon carbide seed single crystal wafer, they are supplied separately and mixed on the surface of the silicon carbide seed single crystal wafer. You may do it. In the growth process, the raw material for producing silicon carbide is supplied to the surface of the growing silicon carbide single crystal, and the single crystal silicon carbide gradually grows and becomes longer. Also, when doping into single crystal silicon carbide, the single crystal silicon carbide described above is used.
  • the raw material for production may be mixed as a solid source, or the doping component may be mixed as a gas source in the atmosphere in the single crystal silicon carbide production apparatus.
  • valence electrons can be controlled by doping with N A1 (CH 3) B H or the like.
  • the configuration of the single-crystal silicon carbide manufacturing apparatus used for obtaining the single-crystal silicon carbide of the present invention is not particularly limited.
  • the size, heating method, material, raw material supply method, atmosphere adjustment method, temperature control method, etc. depend on the size, shape and type of the target single crystal silicon carbide, and the type and amount of the raw material for manufacturing single crystal silicon carbide. It can be selected as appropriate.
  • PID temperature control technology can be used for temperature measurement and temperature control.
  • the production temperature of single-crystal silicon carbide is not particularly limited, and can be set as appropriate according to the size, type, etc. of the desired single-crystal silicon carbide, and the preferred production temperature is 1,6002,400 ° C. This temperature can be measured, for example, as the temperature outside the crucible.
  • a silicon carbide seed single crystal wafer table as a raw material for producing single crystal silicon carbide is provided. It is preferable to start the supply to the surface within the range of 1,970 ° C to 2,100 ° C. Decomposition or etching of the silicon carbide seed crystal surface can be efficiently prevented by preliminary supply of the raw material within this temperature range.
  • the raw material preliminary supply it is preferable to manufacture the target single crystal silicon carbide by heating the crucible to a more preferable manufacturing (growth) temperature while continuing to supply the raw material for manufacturing single crystal silicon carbide.
  • the production temperature in this case is, for example, a crucible. Refers to the outside temperature.
  • FIG. 1 is a conceptual diagram showing an example of an apparatus for producing single crystal silicon carbide of the present invention.
  • a high frequency induction heating furnace is used as one embodiment.
  • Water cooled chamber is used as one embodiment.
  • a carbon cylindrical crucible 2 (diameter: 100 mm, height: 150 mm) is disposed in 1, and a high-frequency induction heating coil 3 is disposed outside the water-cooled chamber 1.
  • a susceptor 5 for holding a silicon carbide single crystal wafer is inserted through the lower portion of the cylindrical crucible 2.
  • the susceptor 5 extends to the outside of the cylindrical crucible 2 and can be rotated about the central axis of the susceptor 5 by a rotating mechanism (not shown).
  • the raw material supply pipe 6 for supplying the raw material particles for producing single crystal silicon carbide passes through the upper part of the cylindrical crucible on the opposite side of the susceptor and extends outward, and is directly outside the chamber. It stretches.
  • the raw material supply pipe 6 is disposed outside the high-frequency induction heating furnace in the previous period, and is provided with a plurality of raw material storage tanks 7, 7 ', each having flow control valves 8, 8' that can independently adjust the supply amount. And connected to a supply source (not shown) of an inert carrier gas A whose flow rate can be adjusted.
  • Silica particles and carbon particles from raw material storage tanks 7 and 7 ' respectively. Both particles can be supplied together with argon gas to the silicon carbide seed crystal surface.
  • the silica and carbon powder are filled into the raw material storage tanks 7 and 7 'independently, and the supply from each storage layer is adjusted, and then inert By flowing the carrier gas A while adjusting the flow rate, the raw material for producing single crystal silicon carbide can be continuously supplied into the cylindrical crucible by a set amount.
  • the high-frequency induction heating furnace can be controlled by a vacuum exhaust system and a pressure control system (not shown), and includes an inert gas replacement mechanism (not shown).
  • the supplied inert carrier gas A is discharged from a duct (not shown) provided in the chamber 1.
  • single-crystal silicon carbide was produced under the following conditions.
  • a silicon carbide single crystal wafer was fixed to the end face of the susceptor that was inserted through the cylindrical crucible.
  • the silicon carbide single crystal wafer used here either single crystal silicon carbide manufactured by the Rayleigh method or single crystal silicon carbide manufactured by the modified Rayleigh method was used.
  • Carbon Carbon Black M A600 manufactured by Mitsubishi Chemical Corporation
  • silica Alignment 380 manufactured by Nippon Aerosil Co., Ltd.
  • the inside of the high frequency induction heating furnace was replaced with an inert gas.
  • the inert gas high-purity helium preferred by high-purity argon may be used.
  • N is doped, high-purity nitrogen can also be used.
  • the temperature outside the carbon cylindrical crucible is 1, 900-1, 970 ° C. (Example A), 1, 970-2, 100 ° C. (Example B) or 2,100-2,140 ° C (Comparative Example C) was heated to a temperature.
  • the temperature outside the cylindrical crucible is preferably less than 1, 970 ° C.
  • the 6H type was manufactured. This was omitted for the production of single crystal silicon carbide at temperatures below 1,970 ° C.
  • the susceptor on which the silicon carbide seed single crystal wafer of each example was fixed was rotated at a rotation speed of 0 to 20 rpm.
  • the inert carrier gas (high-purity argon or high-purity helium) is flowed at a flow rate of 0.5 to 101 / min, and the carrier gas is used together with the raw material for producing single-crystal silicon carbide. Then, the supply to the surface of each of the silicon carbide seed single crystal wafers arranged in the facing portion in the cylindrical crucible through the supply pipe was started. In this state, the temperature was further increased until the temperature outside the cylindrical crucible of Example A, B or Comparative Example C was in the range of 2,140-2,400 ° C.
  • the single crystal silicon carbide of Example A, B or Comparative Example C has the desired size and thickness while keeping the temperature outside the cylindrical crucible of each of the above examples constant.
  • the single crystal silicon carbide of each of the above examples was manufactured by continuously supplying the raw material for manufacturing the single crystal silicon carbide.
  • the desired temperature was appropriately adjusted because it varies depending on the atmospheric pressure, the raw material mixture ratio for producing single crystal silicon carbide, the type of silicon carbide single crystal wafer, and the like.
  • Comparative Example D the temperature outside the cylindrical crucible was heated up to a temperature in the range of 2, 140-2, 400 ° C, and this temperature was kept constant.
  • the inert carrier gas high purity argon or high purity helium
  • the inert carrier gas is adjusted to a flow rate of 0.5 to 101 / min while the susceptor to which the crystal wafer is fixed is rotated at a rotation speed of 0 to 20 rpm.
  • the single crystal silicon carbide manufacturing raw material is continuously supplied through the raw material supply pipe onto the surface of the silicon carbide seed single crystal wafer disposed at the opposing portion in the cylindrical crucible. was also manufactured.
  • Table 1 summarizes the results of single-crystal silicon carbide production under the above four conditions. Both the examples and comparative examples were manufactured for a total of 3 hours to produce single crystal silicon carbide with a thickness of 1.2 mm. The power to build was s. However, in the comparative example, the surface roughness of the silicon carbide seed single crystal occurred, and as a result, a number of dislocations and MP (micropipes) were generated in the manufactured single crystal silicon carbide. On the other hand, in Example B, no surface deterioration was observed, and high-quality single crystal silicon carbide with few defects such as dislocations, polycrystals, and micropipes could be produced.
  • Example A In the case of Example A, no surface deterioration was observed, but since the raw material supply start temperature was too low, 3C crystals were deposited on the surface of the silicon carbide seed single crystal, resulting in a high quality single 6H single crystal. Instead, it became polymorphic mixed polycrystalline.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

Monocristal de carbure de silicium de haute qualité qui, en empêchant la décomposition et/ou la gravure à la surface du cristal germe, parvient à l'inhibition des défauts, tels que les microtuyaux, tout en empêchant la formation de dislocation et de polycristal; et procédé de production de celui-ci. Le procédé de production d'un monocristal de carbure de silicium est caractérisé en ce qu'il comprend l'étape consistant à placer dans un creuset un suscepteur ayant un cristal germe de carbure de silicium qui y est fixé et un tuyau d'alimentation en matière première destiné à fournir une matière première pour la production d'un monocristal de carbure de silicium depuis l'extérieur; l'étape empêchant la décomposition lors de la phase d'augmentation de la température du creuset par chauffage externe, en empêchant la décomposition et/ou la gravure de la surface du cristal germe de carbure de silicium; et l'étape de croissance consistant à continuer de chauffer l'intérieur du creuset jusqu'à une température de croissance du monocristal, en maintenant la température de croissance du monocristal, et en poursuivant l'alimentation en matière première pour la production de carbure de silicium à la surface du cristal germe de carbure de silicium pour ainsi parvenir à la croissance de monocristal de carbure de silicium.
PCT/JP2007/064970 2006-08-10 2007-07-31 Monocristal de carbure de silicium et son procédé de production WO2008018322A1 (fr)

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JP2006218101A JP2008037729A (ja) 2006-08-10 2006-08-10 単結晶炭化珪素及びその製造方法
JP2006-218101 2006-08-10

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KR20130007109A (ko) * 2011-06-29 2013-01-18 에스케이이노베이션 주식회사 탄화규소 단결정 성장 장치 및 그 방법
KR20130002616A (ko) * 2011-06-29 2013-01-08 에스케이이노베이션 주식회사 탄화규소 단결정 성장 장치 및 그 방법

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001233697A (ja) * 2000-02-23 2001-08-28 Nippon Pillar Packing Co Ltd 炭化珪素単結晶
JP2004099414A (ja) * 2002-09-13 2004-04-02 National Institute Of Advanced Industrial & Technology 炭化珪素単結晶の製造方法

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001233697A (ja) * 2000-02-23 2001-08-28 Nippon Pillar Packing Co Ltd 炭化珪素単結晶
JP2004099414A (ja) * 2002-09-13 2004-04-02 National Institute Of Advanced Industrial & Technology 炭化珪素単結晶の製造方法

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