WO2009128224A1 - Procede de production de substrat en carbure de silicium cristallin - Google Patents

Procede de production de substrat en carbure de silicium cristallin Download PDF

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Publication number
WO2009128224A1
WO2009128224A1 PCT/JP2009/001646 JP2009001646W WO2009128224A1 WO 2009128224 A1 WO2009128224 A1 WO 2009128224A1 JP 2009001646 W JP2009001646 W JP 2009001646W WO 2009128224 A1 WO2009128224 A1 WO 2009128224A1
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WO
WIPO (PCT)
Prior art keywords
hot isostatic
sic
silicon carbide
isostatic pressing
crystalline
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PCT/JP2009/001646
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English (en)
Japanese (ja)
Inventor
村松一生
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株式会社インキュベーション・アライアンス
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Publication of WO2009128224A1 publication Critical patent/WO2009128224A1/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
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/36—Carbides
    • 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
    • C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • C30B33/02—Heat treatment
    • 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
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02367—Substrates
    • H01L21/0237—Materials
    • H01L21/02373—Group 14 semiconducting materials
    • H01L21/02378—Silicon carbide
    • 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
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02656—Special treatments
    • H01L21/02664—Aftertreatments
    • H01L21/02667—Crystallisation or recrystallisation of non-monocrystalline semiconductor materials, e.g. regrowth

Definitions

  • the present invention relates to a method for manufacturing a crystalline silicon carbide substrate suitable as a substrate material for power devices, high-frequency devices, LEDs, and the like.
  • Silicon carbide has a short bond distance between Si and C, which are constituent atoms, The semiconductor is characterized by a large band gap, and has a very high chemical stability due to a short interatomic bond distance. Also because of its structure, high thermal conductivity, It has the characteristics of saturated electron drift velocity and high breakdown field strength. It is attractive as a semiconductor device material that handles high power. If an electronic device using SiC is realized, high-power, low-loss, high-speed semiconductor devices can be applied to power systems, industrial equipment, automobiles, and home appliances. A significant energy saving effect can be expected.
  • SiC is similar in crystal structure, Short wavelength optical device based on gallium nitride (GaN) due to its conductivity and high thermal conductivity, It is optimal for high-power, high-frequency devices and occupies an important position as a substrate material for GaN-based semiconductor thin films.
  • GaN gallium nitride
  • SiC exhibits polytypes having a crystallographically identical composition but different laminated structures. There are many types of polytypes, but 3C, 6H, The 4H one has been developed and put into practical use. (The numbers represent the repetition period in the C-axis direction, C is cubic and H is hexagonal). Generally, 3C SiC is known as a low temperature stable polytype, and 6H and 4H are known as high temperature stable polytypes. What has been developed as a substrate material for semiconductor devices is hexagonal SiC such as 6H and 4H.
  • the method currently used for crystal growth of large SiC is a seeded sublimation recrystallization method called an improved Rayleigh method.
  • This method is characterized by controlling the raw material transport process by filling a growth system with a temperature gradient with an inert gas, and controlling the nucleation process of crystal growth by using a seed crystal. Vapor consisting of Si and C sublimated from the raw material is transported by diffusion in the inert gas, and condensed in a supersaturated state on the seed crystal at a temperature lower than that of the raw material. Yu. M. Tailov and V.M. F. Tsvektov, Journal of Cristal Growth, vol. 52 (1981) pp 146-150
  • Dislocation defects existing in crystalline SiC have a bad influence on the device, and thus reduction thereof is required.
  • Dislocations in a crystal are roughly classified according to the extension direction, and are classified into two types: threading dislocations extending in the C-axis direction, which is the crystal growth direction, and basal plane dislocations existing in the basal plane perpendicular to the growth direction.
  • the threading dislocation is considered to cause breakdown voltage degradation of the SiC element, and the basal plane dislocation is considered to cause forward characteristic degradation of the bipolar device.
  • the biggest problem of SiC produced by the improved Rayleigh method is the existence of hollow through defects called micropipes.
  • the micropipe defect which is a hollow defect having a diameter of several ⁇ m that penetrates in the growth direction, is inherited during the growth of the epitaxial thin film and becomes a fatal defect for the device.
  • an object of the present invention is to provide a method for producing a crystalline SiC substrate that can be suitably used for industrially producing power devices, high-frequency devices, and LED elements at low cost.
  • crystal defects such as dislocations inherent in the crystalline SiC material, material distortion, It is reduced by performing a hot isostatic pressing process under a predetermined condition.
  • a cylinder with two congruent plane figures as the bottom It includes a step of subjecting the SiC material formed in a vertical column shape to hot isostatic pressing.
  • a carbonaceous or silicon carbide film is formed on the outer surface of the SiC material in advance of the hot isostatic pressing process in order to reduce the open pores of the crystalline SiC material. More specifically, the carbonaceous film is composed of amorphous carbon including diamond-like carbon.
  • defects and strains in the crystalline SiC material are reduced by isotropic high-temperature and high-pressure treatment with an atmospheric gas such as argon gas, It is possible to provide a large-sized substrate material suitable for manufacturing high-frequency devices and LED elements at low cost.
  • the outer surface of the crystalline SiC ingot material manufactured by various manufacturing methods such as the Rayleigh method, the improved Rayleigh method, the high temperature CVD method, and the solution method is processed into a predetermined symmetrical shape such as a cylinder or a vertical column by grinding.
  • a predetermined symmetrical shape such as a cylinder or a vertical column by grinding.
  • For grinding use a fixed whetstone such as electrodeposited diamond to avoid introducing processing damage to the material surface as much as possible to avoid problems such as material cracking in subsequent manufacturing processes.
  • isotropic pressure as uniformly as possible inside the material, so that the above shape processing is important.
  • the outer surface of the SiC material is carbonaceous, prior to the hot isostatic pressing treatment, Cover with SiC or the like.
  • the material to be coated is determined by the thermal expansion coefficient in the surface orientation of each surface of the crystalline SiC material. Since the thermal expansion coefficients of the surface of each material differ depending on the crystal form of the material to be processed, that is, polytypes such as 3C, 4H, 6H, etc. select. In particular, in the case of hexagonal crystals such as 4H and 6H, the difference in thermal expansion coefficient between the in-plane and c-axis directions is large.
  • a coating material having an appropriate thermal expansion coefficient is selected according to the orientation of the ingot processed into a predetermined shape.
  • the difference in thermal expansion coefficient between the material to be treated and the coating material is large, the coating material is peeled off during the hot isostatic pressing process, and a sufficient effect cannot be obtained.
  • Amorphous carbon films such as diamond-like carbon formed by ionization vapor deposition, plasma CVD, cathodic arc, unbalanced magnetron sputtering, plasma ion implantation, etc. are suitable for use as sealing materials. it can.
  • Amorphous carbon film has isotropic physical properties, and the thermal expansion coefficient can be controlled by the amount of residual hydrogen, etc., so that defects in processed materials can be effectively reduced during subsequent hot isostatic pressing. Can do.
  • FIG. 1 shows an outline of the manufacturing process of the present invention.
  • Example 1 Crystal SiC material manufactured by the modified Rayleigh method with outer diameter of 55mm x 100mm Were inserted into a crucible with an isotropic graphite lid having an inner diameter of 55.5 mm, and lightly tightened and held with upper and lower screw-type lids. Crystalline SiC
  • the graphite crucible in which the material was inserted was loaded into a pressure vessel of a hot isostatic press and a hot isostatic press using argon gas was performed.
  • the processing pattern of the hot isostatic pressurization process is to increase the pressure at a rate of 200 MPa per hour and 20 MPa per hour after depressurization at 300 ° C. to remove moisture and the like, After holding at 2500 ° C.
  • the temperature is lowered at a predetermined rate.
  • the crystal SiC material after hot isostatic pressing is sliced to a thickness of 0.25 mm with a diamond-fixed saw wire, and then the surface is polished by lapping and polishing using diamond abrasive grains. Wafers were manufactured.
  • Crystal SiC material manufactured by the modified Rayleigh method is 55 mm in outer diameter and 0.25 mm in thickness. It was processed into a cylindrical wafer shape of mm, and then inserted into a crucible with an isotropic graphite lid having an inner diameter of 55.5 mm through a graphite spacer, and lightly tightened and held with upper and lower screw-type lids. .
  • a graphite crucible in which a crystalline SiC material was inserted was loaded into a pressure vessel of a hot isostatic press, and hot isostatic press using argon gas was performed. The processing pattern of hot isostatic pressing is 300 ° C.
  • the temperature was increased and the pressure increased at a rate of 200 MPa per hour and 20 MPa per hour at 2500 ° C. and 200 MPa. After holding for 1 hour, the temperature was lowered and the pressure was lowered at a predetermined rate.
  • the surface of the crystalline SiC material after hot isostatic pressing was polished by lapping and polishing using diamond abrasive grains to produce a crystalline SiC wafer having both mirror surfaces.
  • the lifetime map of the manufactured crystalline SiC wafer was measured by the ⁇ -PCD method, the time difference in lifetime from the center to the outer periphery was 30% compared to the comparative material manufactured without hot isostatic pressing. Improved and crystalline SiC Wafer distortion was improved.
  • Crystal SiC material manufactured by the modified Rayleigh method is 55 mm in outer diameter and 0.25 mm in thickness. Then, it was processed into a cylindrical wafer shape of mm, and diamond-like carbon having a thickness of 2 ⁇ m was formed on the entire surface of the wafer using an unbalanced magnetron sputtering apparatus. Next, it was inserted into a crucible with an isotropic graphite lid having an inner diameter of 55.5 mm through a graphite spacer, and lightly tightened and held with upper and lower screw-type lids.
  • a graphite crucible in which a crystalline SiC material was inserted was loaded into a pressure vessel of a hot isostatic press, and hot isostatic press using argon gas was performed.
  • the processing pattern of hot isostatic pressing is After depressurizing at 300 ° C. and removing moisture, etc., the temperature was raised and increased at a rate of 100 MPa per hour and 10 MPa per hour at 2500 ° C. and 200 MPa. After holding for 1 hour, the temperature was lowered and the pressure was lowered at a predetermined rate. Lapping the crystalline SiC material after hot isostatic pressing using diamond abrasives, The surface was polished by polishing to produce a crystalline SiC wafer having both mirror surfaces.
  • the lifetime map of the manufactured crystalline SiC wafer by ⁇ -PCD method was measured, and the time difference in lifetime from the center to the outer periphery was 50% compared to the comparative material manufactured without hot isostatic pressing. Improved and crystalline SiC Wafer distortion has been greatly improved.

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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)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

L’invention concerne un procédé de production d’un substrat SiC cristallin de grande dimension ne présentant sensiblement pas de défauts cristallins ni de déformations et pouvant être produit à faible coût. Ce substrat SiC cristallin, sensiblement exempt de défauts cristallins et de déformations, présente une grande dimension et peut être produit en série, à faible coût, la production consistant à soumettre un matériau SiC à forme cylindrique ou colonnaire à un traitement par pressage isostatique à chaud ou à former un film carboné ou de carbure de silicium sur la surface externe d’un matériau SiC avant le traitement par pressage isostatique à chaud, de sorte à réduire les pores ouverts du matériau SiC cristallin, puis à soumettre l’ensemble au traitement par pressage isostatique à chaud.
PCT/JP2009/001646 2008-04-14 2009-04-08 Procede de production de substrat en carbure de silicium cristallin WO2009128224A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2008127677A JP2009256159A (ja) 2008-04-14 2008-04-14 結晶炭化珪素基板の製造方法
JP2008-127677 2008-04-14

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Publication Number Publication Date
WO2009128224A1 true WO2009128224A1 (fr) 2009-10-22

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WO (1) WO2009128224A1 (fr)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20130006442A (ko) * 2010-03-23 2013-01-16 스미토모덴키고교가부시키가이샤 반도체 장치 및 그 제조 방법
JP2011199132A (ja) * 2010-03-23 2011-10-06 Sumitomo Electric Ind Ltd 半導体装置およびその製造方法
JP6473455B2 (ja) * 2013-09-06 2019-02-20 ジーティーエイティー コーポレーションＧｔａｔ Ｃｏｒｐｏｒａｔｉｏｎ 炭化ケイ素シードを用いたバルクの炭化ケイ素の製造方法及び装置
WO2017073333A1 (fr) * 2015-10-27 2017-05-04 住友電気工業株式会社 Plaque de base en carbure de silicium

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002179498A (ja) * 2000-12-12 2002-06-26 Denso Corp 炭化珪素単結晶の製造方法
JP2007015918A (ja) * 2002-06-27 2007-01-25 General Electric Co <Ge> 結晶中の欠陥濃度低減方法

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002179498A (ja) * 2000-12-12 2002-06-26 Denso Corp 炭化珪素単結晶の製造方法
JP2007015918A (ja) * 2002-06-27 2007-01-25 General Electric Co <Ge> 結晶中の欠陥濃度低減方法

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