WO2011065239A1 - 単結晶の製造方法 - Google Patents
単結晶の製造方法 Download PDFInfo
- Publication number
- WO2011065239A1 WO2011065239A1 PCT/JP2010/070175 JP2010070175W WO2011065239A1 WO 2011065239 A1 WO2011065239 A1 WO 2011065239A1 JP 2010070175 W JP2010070175 W JP 2010070175W WO 2011065239 A1 WO2011065239 A1 WO 2011065239A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- single crystal
- producing
- seed crystal
- crystal according
- coating film
- Prior art date
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 37
- 239000013078 crystal Substances 0.000 claims abstract description 183
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 59
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 50
- 239000011248 coating agent Substances 0.000 claims abstract description 47
- 238000000576 coating method Methods 0.000 claims abstract description 47
- 239000000853 adhesive Substances 0.000 claims abstract description 45
- 230000001070 adhesive effect Effects 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 25
- 230000003746 surface roughness Effects 0.000 claims abstract description 16
- 238000010000 carbonizing Methods 0.000 claims abstract description 6
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 claims description 53
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 32
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 30
- 239000011347 resin Substances 0.000 claims description 23
- 229920005989 resin Polymers 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 12
- 238000009826 distribution Methods 0.000 claims description 11
- 239000006061 abrasive grain Substances 0.000 claims description 10
- 150000001720 carbohydrates Chemical class 0.000 claims description 10
- 239000010419 fine particle Substances 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 9
- 229910021470 non-graphitizable carbon Inorganic materials 0.000 claims description 7
- 238000005498 polishing Methods 0.000 claims description 7
- 238000004528 spin coating Methods 0.000 claims description 5
- 238000012937 correction Methods 0.000 claims description 2
- 239000000758 substrate Substances 0.000 description 13
- 239000000463 material Substances 0.000 description 11
- 229910002804 graphite Inorganic materials 0.000 description 10
- 239000010439 graphite Substances 0.000 description 10
- 238000000859 sublimation Methods 0.000 description 10
- 230000008022 sublimation Effects 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 229910003460 diamond Inorganic materials 0.000 description 8
- 239000010432 diamond Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 238000001953 recrystallisation Methods 0.000 description 8
- 239000004065 semiconductor Substances 0.000 description 8
- 238000001035 drying Methods 0.000 description 7
- 239000002002 slurry Substances 0.000 description 7
- 235000014633 carbohydrates Nutrition 0.000 description 6
- 229920002120 photoresistant polymer Polymers 0.000 description 5
- -1 for example Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000005011 phenolic resin Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000011800 void material Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- LZCLXQDLBQLTDK-UHFFFAOYSA-N ethyl 2-hydroxypropanoate Chemical compound CCOC(=O)C(C)O LZCLXQDLBQLTDK-UHFFFAOYSA-N 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000011344 liquid material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000003870 refractory metal Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- SVONRAPFKPVNKG-UHFFFAOYSA-N 2-ethoxyethyl acetate Chemical compound CCOCCOC(C)=O SVONRAPFKPVNKG-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
- 229910004613 CdTe Inorganic materials 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 229940116333 ethyl lactate Drugs 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 239000003779 heat-resistant material Substances 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229920003986 novolac Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 1
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
- C30B23/08—Epitaxial-layer growth by condensing ionised vapours
-
- 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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
- C30B23/025—Epitaxial-layer growth characterised by the substrate
-
- 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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/20—Deposition of semiconductor materials on a substrate, e.g. epitaxial growth solid phase epitaxy
Definitions
- the present invention relates to a method for producing a single crystal, and more particularly to a method for producing a single crystal using a seed crystal fixed on a pedestal.
- Silicon carbide has a larger band gap than silicon more commonly used in the semiconductor field. Therefore, a semiconductor device using silicon carbide has advantages such as high breakdown voltage, low on-resistance, and small deterioration in characteristics under a high temperature environment.
- the silicon carbide single crystal is manufactured using a sublimation recrystallization method. Specifically, a silicon carbide single crystal is grown on the surface of a seed crystal fixed on a pedestal. If the seed crystal is not uniformly fixed to the pedestal, the quality of the single crystal grown on the seed crystal can be reduced. Therefore, for example, the following two methods have been proposed for attaching the seed crystal to the pedestal.
- Patent Document 1 a composite structure of carbon having graphite fine particles and non-graphitizable carbon is formed at the interface between a seed crystal and a seed crystal pedestal during single crystal growth.
- carbon is uniformly formed throughout the pasting surface with the heat-resistant fine particles uniformly dispersed on the pasting surface as a core, thereby covering the seed crystal pasting surface. It is described that it is possible to prevent recrystallization from occurring on the crystal base attachment surface and to prevent etching that occurs at the initial stage of growth at the center of the seed crystal.
- Patent Document 2 a silicon carbide seed crystal having a protective film with a thickness of 0.5 to 5 ⁇ m formed on its back surface is mechanically attached to a graphite crucible lid. Is done. This publication describes that this protective film can prevent sublimation of Si atoms from the back surface of the seed crystal, thereby suppressing generation of voids in the crystal.
- Patent Document 1 the strength of fixing between the seed crystal and the pedestal may be insufficient depending on the material of the seed crystal.
- the temperature between the seed crystal and the pedestal is high, such as when a silicon carbide single crystal is grown, the strength of the fixation is likely to decrease. Therefore, part or all of the seed crystal may be detached from the pedestal, which may deteriorate the quality of the single crystal obtained.
- Patent Document 2 Japanese Patent Laid-Open No. 2003-226600
- the back surface of the seed crystal was not sufficiently protected.
- the effect of preventing sublimation on the back surface of the seed crystal is not sufficient, and the quality of the resulting single crystal may be deteriorated due to this effect.
- the present invention has been made in view of the above problems, and an object of the present invention is to provide a method for producing a single crystal, which can grow a high-quality single crystal using a seed crystal fixed on a pedestal. Is to provide.
- the method for producing a single crystal includes the following steps.
- a seed crystal having a front surface and a back surface is prepared.
- the surface roughness of the back surface of the seed crystal is increased.
- a coating film containing carbon is formed on the back surface of the seed crystal.
- the coating film and the base are brought into contact with each other with the adhesive interposed therebetween.
- the adhesive is cured to secure the seed crystal to the pedestal.
- a single crystal is grown on the seed crystal. Before the growth is performed, the coating film is carbonized to form a carbon film.
- the method for producing a single crystal according to another aspect of the present invention includes the following steps.
- a seed crystal having a front surface and a back surface is prepared.
- the back surface is an as-sliced surface formed by slicing with a wire saw.
- a coating film containing carbon is formed on the back surface of the seed crystal.
- the coating film and the base are brought into contact with each other with the adhesive interposed therebetween.
- the adhesive is cured to secure the seed crystal to the pedestal.
- a single crystal is grown on the seed crystal fixed to the pedestal. Before the growth is performed, the coating film is carbonized to form a carbon film.
- the step of increasing the surface roughness of the back surface is performed by processing the back surface with abrasive grains. More preferably, the particle size distribution of the abrasive grains has a component of 16 ⁇ m or more.
- the coating film is an organic film, and the carbon film is formed by carbonizing the organic film. More preferably, the organic film is formed from an organic resin. More preferably, the organic resin is a photosensitive resin.
- the step of forming the coating film is performed using a spin coating method.
- the pedestal is polished before the covering film and the pedestal are brought into contact with each other with the adhesive interposed therebetween.
- the adhesive contains a resin that becomes non-graphitizable carbon when heated, heat-resistant fine particles, and a solvent. More preferably, the adhesive includes a carbohydrate.
- the single crystal is a silicon carbide single crystal.
- the surface of the pedestal facing the seed crystal includes a surface made of carbon.
- a carbon film is provided on the back surface of the seed crystal when the single crystal is grown. Since the carbon film is made of carbon, the cured adhesive is used. To be joined uniformly and firmly. Further, this carbon film is formed with high adhesion on the back surface of the seed crystal, which is a surface having a large surface roughness. That is, the carbon film is firmly bonded to each of the adhesive and the seed crystal. Therefore, since the seed crystal and the pedestal are fixed uniformly and firmly via the adhesive, the quality of the single crystal grown on the seed crystal is improved.
- seed crystal 11 is prepared.
- the seed crystal 11 has a surface (a lower surface in the figure) that is a surface on which a single crystal is to be grown, and a back surface (an upper surface in the figure) that is a surface to be attached to the pedestal.
- seed crystal 11 is made of silicon carbide (SiC).
- the thickness of the seed crystal 11 (the vertical dimension in the figure) is, for example, not less than 0.5 mm and not more than 10 mm.
- the planar shape of the seed crystal 11 is, for example, a circle, and the diameter is preferably 25 mm or more, and more preferably 100 mm or more.
- the inclination of the plane orientation of the seed crystal from the (0001) plane, that is, the off angle is preferably 15 ° or less, and more preferably 5 ° or less.
- processing for increasing the surface roughness of the back surface of the seed crystal 11 is performed.
- This processing can be performed by polishing the back surface using abrasive grains having a sufficiently large particle diameter.
- the particle size distribution of the abrasive grains preferably has a component of 16 ⁇ m or more.
- the average grain size of the abrasive grains is preferably 5 ⁇ m or more and 50 ⁇ m or less, more preferably 10 ⁇ m or more and 30 ⁇ m or less, and further preferably 12 to 25 ⁇ m.
- the abrasive grains are diamond particles.
- the abrasive grains are used by being dispersed in a slurry. Therefore, the above polishing is preferably performed using a diamond slurry.
- a diamond slurry containing diamond particles having an average particle size of 5 ⁇ m or more and 50 ⁇ m or less and having a component of 16 ⁇ m or more in the particle size distribution is generally easily available.
- a back surface having a sufficiently large surface roughness from the beginning may be formed and used without polishing the back surface.
- the back surface of the seed crystal 11 formed by slicing with a wire saw may be used without polishing. That is, an as-sliced surface that is a surface formed by slicing and not polished thereafter may be used as the back surface.
- the above-mentioned abrasive grains are used in slicing with a wire saw.
- a coating film 21 containing carbon is formed on the back surface of the seed crystal 11.
- the surface roughness of the coating film 21 is made smaller than the surface roughness of the back surface of the seed crystal 11 on which the coating film 21 is formed.
- this formation is performed by application of a liquid material, more preferably the liquid material does not contain solid matter such as particulates.
- the thin coating film 21 can be formed easily and uniformly.
- the coating film 21 is an organic film in the present embodiment.
- This organic film is preferably formed from an organic resin.
- the organic resin for example, various resins such as an acrylic resin, a phenol resin, a urea resin, and an epoxy resin can be used, and a resin that is formed as a photosensitive resin that is crosslinked or decomposed by the action of light can also be used. it can.
- this photosensitive resin a positive type or negative type photoresist used for manufacturing a semiconductor device can be used, and since a coating technique by spin coating is established for these, the coating film 21 is used. Can be easily controlled.
- the spin coating method is performed as follows, for example.
- the seed crystal 11 is adsorbed on the holder.
- the seed crystal 11 is rotated by rotating the holder at a predetermined rotation speed.
- the photoresist is dropped on the rotating seed crystal 11, the photoresist is applied thinly and uniformly by continuing the rotation for a predetermined time.
- the rotation speed is 1000 to 10,000 rotations / minute
- the time is 10 to 100 seconds
- the coating thickness is 0.1 ⁇ m or more.
- the applied photoresist is solidified by drying.
- the drying temperature and time can be appropriately selected depending on the photoresist material and the coating thickness.
- the drying temperature is from 100 ° C. to 400 ° C.
- the drying time is from 5 minutes to 60 minutes.
- the time required for volatilization is, for example, 15 minutes at a thickness of 5 ⁇ m, 8 minutes at a thickness of 2 ⁇ m, and 3 minutes at a thickness of 1 ⁇ m.
- the coating film 21 can be formed by performing the steps of coating and drying once, but the thicker coating film 21 may be formed by repeating this process. If the number of repetitions is too large, it is not preferable because it takes more time than necessary for this step, and it is usually preferable to limit the number of repetitions to about 2 to 3 times.
- a pedestal 41 having a mounting surface on which the seed crystal 11 is to be mounted is prepared.
- This mounting surface preferably includes a surface made of carbon.
- the base 41 is made of graphite.
- the mounting surface is polished to improve the flatness of the mounting surface.
- the coating film 21 and the pedestal 41 are brought into contact with each other with the adhesive 31 interposed therebetween.
- this contact is performed such that the two are pressed against each other at a temperature of 50 ° C. to 120 ° C. and a pressure of 0.01 Pa to 1 MPa.
- the adhesive 31 is prevented from protruding from the region sandwiched between the seed crystal 11 and the pedestal 41, the adverse effect of the adhesive 31 is suppressed in the single crystal growth process using the seed crystal 11 described later. can do.
- the adhesive 31 preferably includes a resin that becomes non-graphitizable carbon by being carbonized by heating, heat-resistant fine particles, and a solvent, and more preferably includes a carbohydrate.
- the resin that becomes non-graphitizable carbon is, for example, a novolac resin, a phenol resin, or a furfuryl alcohol resin.
- the heat-resistant fine particles have a function of increasing the filling rate of the fixed layer by uniformly distributing the non-graphitizable carbon in the fixed layer formed by heating the adhesive 31 at a high temperature.
- a heat-resistant material such as carbon (C) such as graphite, silicon carbide (SiC), boron nitride (BN), or aluminum nitride (AlN) can be used.
- C carbon
- SiC silicon carbide
- BN boron nitride
- AlN aluminum nitride
- a refractory metal or a compound such as a carbide or nitride thereof can be used.
- tungsten (W), tantalum (Ta), molybdenum (Mo), titanium (Ti), zirconium (Zr), or hafnium (Hf) can be used.
- the particle diameter of the heat-resistant fine particles is, for example, 0.1 to 10 ⁇ m.
- Saccharides or their derivatives can be used as carbohydrates.
- the saccharide may be a monosaccharide such as glucose or a polysaccharide such as cellulose.
- the solvent a solvent capable of dissolving and dispersing the above resin and carbohydrate is appropriately selected.
- the solvent is not limited to a single type of liquid, and may be a mixed liquid of a plurality of types of liquid.
- a solvent containing alcohol that dissolves carbohydrates and cellosolve acetate that dissolves resin may be used.
- the ratio among the resin, carbohydrate, heat-resistant fine particles, and solvent in the adhesive 31 is appropriately selected so that appropriate adhesion and fixing strength of the seed crystal 11 can be obtained.
- the component of the adhesive 31 may include components other than the components described above, and may include additives such as a surfactant and a stabilizer.
- the application amount of the adhesive 31 is preferably 10 mg / cm 2 or more and 100 mg / cm 2 or less.
- the thickness of the adhesive 31 is preferably 100 ⁇ m or less, more preferably 50 ⁇ m or less.
- the pre-baking temperature is preferably 150 ° C. or higher.
- coating film 21 and adhesive 31 are heated.
- the coating film 21 is carbonized to become a carbon film 22. That is, the carbon film 22 is provided on the seed crystal 11.
- the adhesive 31 is cured between the carbon film 22 and the pedestal 41 by this heating, so that the fixed layer 32 is obtained. As a result, the seed crystal 11 is fixed to the pedestal 41.
- the above heating is performed at a temperature of 800 ° C. to 1800 ° C. for 1 hour to 10 hours, at a pressure of 0.13 kPa to atmospheric pressure, and in an inert gas atmosphere.
- the inert gas for example, helium, argon, or nitrogen gas is used.
- raw material 51 is stored in crucible 42.
- the single crystal to be grown is formed of SiC, for example, SiC powder is stored in a graphite crucible.
- the base 41 is attached so that the seed crystal 11 faces the inside of the crucible 42.
- the pedestal 41 may function as a lid for the crucible 42.
- a single crystal 52 is grown on the seed crystal 11.
- a sublimation recrystallization method can be used as this formation method. That is, the single crystal 52 can be grown by depositing the sublimate on the seed crystal 11 by sublimating the raw material 51 as indicated by the arrows in the figure.
- the temperature in this sublimation recrystallization method is, for example, 2100 ° C. or higher and 2500 ° C. or lower.
- the pressure in the sublimation recrystallization method is preferably 1.3 kPa or more and atmospheric pressure or less, and more preferably 13 kPa or less in order to increase the growth rate.
- the coating film 21 (FIG. 2) is already the carbon film 22 (FIG. 3).
- seed crystal 11 is bonded to pedestal 41 by fixing layer 32 without using carbon film 22 (FIG. 3).
- the fixing strength between the seed crystal 11 and the pedestal 41 may be insufficient.
- the fixing strength is likely to be reduced.
- the adhesive strength due to the fixed layer formed by curing the carbon-based adhesive is likely to decrease at a temperature of about 2000 ° C. that is commonly used for SiC growth.
- the seed crystal 11 may come off the pedestal, which may reduce the quality of the single crystal obtained.
- the seed crystal 11 is often made of SiC and the pedestal 41 is often made of graphite.
- a fixed layer formed by curing a carbon-based adhesive can bond carbon materials (graphite) with high strength, but does not bond carbon material and SiC with the same strength. Can not.
- the carbon film 22 is provided on the seed crystal 11, and the fixed layer 32 fixes between the carbon film 22 and the pedestal 41. That is, the fixed layer 32 is bonded to the carbon film 22 instead of the seed crystal 11. Therefore, since the bonding is performed directly without depending on the material of the seed crystal 11, the seed crystal 11 and the pedestal 41 can be more firmly fixed.
- the pedestal 41 is made of carbon such as graphite
- the pedestal 41 and the carbon film 22 are both made of carbon, so that both can be firmly bonded using a carbon-based adhesive.
- the surface roughness of the back surface of the seed crystal 11 is increased.
- the adhesion between the carbon film 22 formed by carbonization of the coating film 21 and the back surface of the seed crystal 11 can be improved.
- the surface roughness of the coating film 21 is smaller than the surface roughness of the back surface of the seed crystal 11 on which the coating film 21 is formed.
- seed crystal 11 provided with carbon film 22 having a thickness of 0.5 to 5 ⁇ m is fixed to pedestal 41 by mechanical fixing jig 33.
- the carbon film 22 and the pedestal 41 between the seed crystal 11 and the pedestal 41 There may be a gap at the interface. If a temperature distribution occurs in the growth surface of the seed crystal 11 corresponding to this gap distribution, a uniform single crystal cannot be obtained.
- the seed crystal 11 is fixed not by a mechanical jig but by a uniform and strong bond between the carbon film 22 and the fixed layer 32. Therefore, since the above gaps are unlikely to occur, the generation of the composition distribution and the temperature distribution in the seed crystal 11 is suppressed, so that the single crystal 52 can be manufactured more uniformly. This temperature distribution can be further suppressed by polishing the mounting surface of the pedestal 41.
- the seed crystal 11 is formed of SiC, but may be formed of other materials.
- this material for example, GaN, ZnSe, ZnS, CdS, CdTe, AlN, or BN can be used.
- the coating film 21 is carbonized when the adhesive 31 is cured, but the coating film 31 may be carbonized before the adhesive 31 is formed.
- a substrate such as an SiC substrate may be manufactured using the single crystal 52.
- Such a substrate is obtained, for example, by slicing the single crystal 52.
- Example 1 Referring to FIG. 1, an SiC substrate having a thickness of about 3 mm, a diameter of 60 mm, a polytype 4H, and a plane orientation (000-1) was prepared as seed crystal 11. The back side of the seed crystal 11 was mechanically polished using a diamond slurry having a particle size of about 15 ⁇ m.
- the seed crystal 11 was attached to the holder so that the back surface of the seed crystal 11 was exposed.
- the seed crystal 11 is rotated by rotating this holder at 1450 times / minute, about 20 mmg of a resist solution containing ethyl lactate and butyl acetate is dropped on the back surface with a dropper, and then for 20 seconds. The rotation was sustained.
- the resist solution was applied with a thickness of about 1 ⁇ m.
- the coating film 21 was formed by drying at 350 ° C. for 20 minutes.
- a graphite pedestal 41 having a mounting surface on which seed crystal 11 is to be mounted was prepared.
- the mounting surface was then polished using diamond slurry.
- an adhesive 31 containing a phenol resin, phenol, ethyl alcohol, formaldehyde, moisture, and a solid carbon component was prepared.
- the covering film 21 and the pedestal 41 were brought into contact with each other with the adhesive 31 interposed therebetween.
- the application amount of the adhesive 31 was about 25 mg / cm 2 and the thickness was about 40 ⁇ m. This contact was performed under conditions of 100 ° C. and 0.1 MPa.
- the adhesive 31 was pre-baked. Specifically, heat treatment was sequentially performed at 80 ° C. for 4 hours, 120 ° C. for 4 hours, and 200 ° C. for 1 hour.
- the coating film 21 and the adhesive 31 were heated. This heating was performed at 1150 ° C. for 1 hour in an 80 kPa helium gas atmosphere.
- the coating film 21 and the adhesive 31 were carbonized by this heating, so that the carbon film 22 and the fixed layer 32 (FIG. 3) both made of carbon were formed.
- SiC powder was stored as raw material 51 in graphite crucible 42.
- the pedestal 41 was attached so that the seed crystal 11 faces the inside of the crucible 42 and the pedestal 41 functions as a lid of the crucible 42.
- a SiC single crystal 52 was grown on the seed crystal 11 by a sublimation recrystallization method.
- the growth conditions were a temperature of 2400 ° C., a pressure of 1.7 kPa, and a time of 300 hours.
- an SiC substrate was obtained by slicing the obtained SiC single crystal 52.
- the void density was 0 / cm 2 and the micropipe density was 1 / cm 2 .
- Example 2 In the above example, the back side of the seed crystal was polished using a diamond slurry having a particle size of 15 ⁇ m. In this example, a diamond slurry having a particle size distribution of 16 ⁇ m or more was used. It was. According to this example, the adhesion between the back surface of the seed crystal 11 and the carbon film 22 was higher.
- the void density 120 / cm 2 and the micropipe density was 300 / cm 2 .
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
本発明の他の局面に従う単結晶の製造方法は、次の工程を有する。表面および裏面を有する種結晶が準備される。裏面はワイヤソーによるスライスによって形成されたアズスライス面である。種結晶の裏面上に、炭素を含む被覆膜が形成される。接着剤を挟んで被覆膜と台座とが互いに接触させられる。種結晶を台座に固定するために接着剤が硬化される。台座に固定された種結晶上に単結晶が成長させられる。上記成長が行われる前に、被覆膜が炭化されることによって炭素膜が形成される。
図1を参照して、種結晶11が準備される。種結晶11は、その上に単結晶が成長することになる面である表面(図中、下面)と、台座に取り付けられることになる面である裏面(図中、上面)とを有する。たとえば、種結晶11は炭化珪素(SiC)から形成されている。種結晶11の厚さ(図中、縦方向の寸法)は、たとえば0.5mm以上10mm以下である。また種結晶11の平面形状は、たとえば円形であり、その直径は、25mm以上が好ましく、100mm以上がより好ましい。また種結晶の面方位の(0001)面からの傾き、すなわちオフ角度は、15°以下が好ましく、5°以下がより好ましい。
また好ましくは、被覆膜21の表面粗さは、被覆膜21が形成される種結晶11の裏面の表面粗さに比して小さくされる。これにより台座41に接着される面の凹凸が小さくなるので、台座との接着が局所的に不十分となる部分が生じることを防止することができる。
図1を参照して、種結晶11として、厚さ約3mm、直径60mm、ポリタイプ4H、および面方位(000-1)を有するSiC基板が準備された。この種結晶11の裏面側が、粒径約15μmを有するダイヤモンドスラリーを用いて機械的に研磨された。
上記実施例においては種結晶の裏面側の研磨が粒径15μmを有するダイヤモンドスラリーを用いて行われたが、本実施例においては、粒度分布が粒径16μm以上の成分を有するダイヤモンドスラリーが用いられた。本実施例によれば、種結晶11の裏面と炭素膜22との密着性がより高かった。
第1の比較例(図5)の場合、昇華再結晶法を行うための昇温中、または単結晶の成長中に、3分の1の確率で種結晶11が台座41から落下した。この落下が生じなかった場合において得られたSiC基板の表面を評価したところ、ボイド密度は10/cm2、マイクロパイプ密度は50/cm2であった。
Claims (22)
- [規則91に基づく訂正 10.02.2011]
表面および裏面を有する種結晶(11)を準備する工程と、
前記種結晶(11)の前記裏面の表面粗さを大きくする工程と、
前記裏面の表面粗さを大きくする工程の後に、前記種結晶(11)の前記裏面上に、炭素を含む被覆膜を形成する工程と、
接着剤を挟んで前記被覆膜と台座(41)とを互いに接触させる工程と、
前記種結晶(11)を前記台座(41)に固定するために前記接着剤を硬化させる工程と、
前記台座(41)に固定された前記種結晶(11)上に単結晶を成長させる工程とを備え、
前記成長させる工程の前に、前記被覆膜が炭化されることによって炭素膜(22)が形成される、単結晶の製造方法。 - 前記裏面の表面粗さを大きくする工程は、前記裏面を砥粒を用いて処理することによって行われる、請求の範囲第1項に記載の単結晶の製造方法。
- 前記砥粒の粒度分布は16μm以上の成分を有する、請求の範囲第2項に記載の単結晶の製造方法。
- 前記被覆膜は有機膜であり、前記有機膜が炭化されることによって前記炭素膜(22)が形成される、請求の範囲第1項に記載の単結晶の製造方法。
- 前記有機膜は有機樹脂から形成される、請求の範囲第4項に記載の単結晶の製造方法。
- 前記有機樹脂は感光性樹脂である、請求の範囲第5項に記載の単結晶の製造方法。
- 前記被覆膜を形成する工程はスピンコート法を用いて行われる、請求の範囲第1項に記載の単結晶の製造方法。
- 前記接触させる工程の前に、前記台座(41)を研磨する工程をさらに備える、請求の範囲第1項に記載の単結晶の製造方法。
- 前記接着剤は、加熱されることによって難黒鉛化炭素となる樹脂と、耐熱性微粒子と、溶媒とを含む、請求の範囲第1項に記載の単結晶の製造方法。
- 前記接着剤は炭水化物を含む、請求の範囲第9項に記載の単結晶の製造方法。
- 前記種結晶(11)は炭化珪素から形成されている、請求の範囲第1項に記載の単結晶の製造方法。
- 前記台座(41)の前記種結晶(11)に面する面は炭素からなる面を含む、請求の範囲第1項に記載の単結晶の製造方法。
- 表面および裏面を有する種結晶(11)を準備する工程を備え、
前記裏面はワイヤソーによるスライスによって形成されたアズスライス面であり、さらに
前記種結晶(11)の前記裏面上に、炭素を含む被覆膜を形成する工程と、
接着剤を挟んで前記被覆膜と台座(41)とを互いに接触させる工程と、
前記種結晶(11)を前記台座(41)に固定するために前記接着剤を硬化させる工程と、
前記台座(41)に固定された前記種結晶(11)上に単結晶を成長させる工程とを備え、
前記成長させる工程の前に、前記被覆膜が炭化されることによって炭素膜(22)が形成される、単結晶の製造方法。 - 前記被覆膜は有機膜であり、前記有機膜が炭化されることによって前記炭素膜(22)が形成される、請求の範囲第13項に記載の単結晶の製造方法。
- 前記有機膜は有機樹脂から形成される、請求の範囲第14項に記載の単結晶の製造方法。
- 前記有機樹脂は感光性樹脂である、請求の範囲第15項に記載の単結晶の製造方法。
- 前記被覆膜を形成する工程はスピンコート法を用いて行われる、請求の範囲第13項に記載の単結晶の製造方法。
- 前記接触させる工程の前に、前記台座(41)を研磨する工程をさらに備える、請求の範囲第13項に記載の単結晶の製造方法。
- 前記接着剤は、加熱されることによって難黒鉛化炭素となる樹脂と、耐熱性微粒子と、溶媒とを含む、請求の範囲第13項に記載の単結晶の製造方法。
- 前記接着剤は炭水化物を含む、請求の範囲第19項に記載の単結晶の製造方法。
- 前記種結晶(11)は炭化珪素から形成されている、請求の範囲第13項に記載の単結晶の製造方法。
- 前記台座(41)の前記種結晶(11)に面する面は炭素からなる面を含む、請求の範囲第13項に記載の単結晶の製造方法。
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2011543208A JP5741444B2 (ja) | 2009-11-30 | 2010-11-12 | 単結晶の製造方法 |
CA2757206A CA2757206A1 (en) | 2009-11-30 | 2010-11-12 | Method of manufacturing single crystal |
US13/257,742 US9090992B2 (en) | 2009-11-30 | 2010-11-12 | Method of manufacturing single crystal |
EP10833086.1A EP2508653B1 (en) | 2009-11-30 | 2010-11-12 | Method for producing monocrystal |
CN201080019023.7A CN102414349B (zh) | 2009-11-30 | 2010-11-12 | 制造单晶的方法 |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2009272012 | 2009-11-30 | ||
JP2009-272012 | 2009-11-30 |
Publications (2)
Publication Number | Publication Date |
---|---|
WO2011065239A1 true WO2011065239A1 (ja) | 2011-06-03 |
WO2011065239A9 WO2011065239A9 (ja) | 2011-09-29 |
Family
ID=44066164
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2010/062432 WO2011065060A1 (ja) | 2009-11-30 | 2010-07-23 | 単結晶の製造方法 |
PCT/JP2010/070175 WO2011065239A1 (ja) | 2009-11-30 | 2010-11-12 | 単結晶の製造方法 |
Family Applications Before (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2010/062432 WO2011065060A1 (ja) | 2009-11-30 | 2010-07-23 | 単結晶の製造方法 |
Country Status (8)
Country | Link |
---|---|
US (1) | US9090992B2 (ja) |
EP (1) | EP2508653B1 (ja) |
JP (1) | JP5741444B2 (ja) |
KR (1) | KR20120022791A (ja) |
CN (1) | CN102414349B (ja) |
CA (1) | CA2757206A1 (ja) |
TW (1) | TW201126032A (ja) |
WO (2) | WO2011065060A1 (ja) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2015104925A1 (ja) * | 2014-01-10 | 2015-07-16 | 住友電気工業株式会社 | 種基板、インゴットおよびインゴットの製造方法 |
WO2016163157A1 (ja) * | 2015-04-09 | 2016-10-13 | 住友電気工業株式会社 | 炭化珪素単結晶の製造方法 |
JP2020066571A (ja) * | 2018-10-22 | 2020-04-30 | エスケイシー・カンパニー・リミテッドSkc Co., Ltd. | 保護膜を含む種結晶の製造方法、これを適用したインゴットの製造方法、保護膜を含む種結晶及び種結晶の付着方法 |
Families Citing this family (18)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP5696630B2 (ja) | 2011-09-21 | 2015-04-08 | 住友電気工業株式会社 | 炭化珪素基板およびその製造方法 |
US10793971B2 (en) | 2013-09-06 | 2020-10-06 | Gtat Corporation | Method and apparatus for producing bulk silicon carbide using a silicon carbide seed |
CN110670124B (zh) * | 2013-09-06 | 2021-07-30 | Gtat公司 | 生产大块硅碳化物的方法 |
DE112014004073T5 (de) * | 2013-09-06 | 2016-06-09 | Gtat Corporation | Apparatur zur Herstellung von Massen-Siliciumcarbid |
KR102245509B1 (ko) * | 2013-09-06 | 2021-04-28 | 지티에이티 코포레이션 | 저결함밀도를 갖는 벌크 탄화규소 |
CN103628141A (zh) * | 2013-12-11 | 2014-03-12 | 中国电子科技集团公司第二研究所 | 一种SiC单晶晶体质量均匀化方法 |
JP2016183108A (ja) * | 2016-07-27 | 2016-10-20 | 住友電気工業株式会社 | 炭化珪素基板 |
CN106757356A (zh) * | 2016-12-09 | 2017-05-31 | 河北同光晶体有限公司 | 一种SiC单晶生长过程中籽晶与石墨托的连接方法 |
KR102058870B1 (ko) * | 2017-11-29 | 2019-12-24 | 에스케이씨 주식회사 | 대구경 탄화규소 단결정 잉곳의 성장방법 |
CN110168147B (zh) | 2016-12-20 | 2022-01-28 | 赛尼克公司 | 大直径碳化硅单晶锭的培养方法 |
CN108048911A (zh) * | 2017-12-20 | 2018-05-18 | 中国科学院上海硅酸盐研究所 | 一种采用物理气相沉积技术生长大尺寸碳化硅晶体的方法 |
CN108118389A (zh) * | 2017-12-28 | 2018-06-05 | 河北同光晶体有限公司 | 一种高品质碳化硅单晶的籽晶的制备方法 |
CN110581056B (zh) * | 2018-06-08 | 2022-07-01 | 中国科学院化学研究所 | 单晶薄膜的制备方法、单晶薄膜及应用 |
KR102177759B1 (ko) * | 2018-12-13 | 2020-11-11 | 에스케이씨 주식회사 | 종자정 부착 방법 |
KR102242438B1 (ko) * | 2019-08-12 | 2021-04-20 | 에스케이씨 주식회사 | 종자정 부착 방법 |
KR102214314B1 (ko) * | 2019-08-22 | 2021-02-09 | 에스케이씨 주식회사 | 대구경 탄화규소 단결정 잉곳의 성장방법 |
CN111545428B (zh) * | 2020-05-15 | 2021-07-20 | 山东大学 | 一种用于氮化铝单晶生长籽晶背部镀膜的方法 |
CN115573041A (zh) * | 2022-09-09 | 2023-01-06 | 眉山博雅新材料股份有限公司 | 一种籽晶粘接方法和设备 |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS52134007A (en) * | 1976-04-30 | 1977-11-09 | Hamada Sangiyou Kk | Method of producing decorated board |
JP2001139394A (ja) | 1999-11-10 | 2001-05-22 | Toyota Central Res & Dev Lab Inc | 種結晶固定剤、種結晶固定方法およびそれらを用いた単結晶の製造方法 |
JP2003119098A (ja) * | 2001-10-16 | 2003-04-23 | Denso Corp | 種結晶の固定方法および固定状態の評価方法 |
JP2003226600A (ja) | 2002-02-05 | 2003-08-12 | Nippon Steel Corp | 炭化珪素単結晶育成用種結晶と炭化珪素単結晶インゴット及びこれらの製造方法 |
JP2009256193A (ja) * | 2008-03-21 | 2009-11-05 | Bridgestone Corp | 炭化ケイ素単結晶の製造方法 |
JP2010132464A (ja) * | 2008-12-02 | 2010-06-17 | Mitsubishi Electric Corp | 炭化珪素単結晶の製造方法 |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP4291886B2 (ja) | 1994-12-05 | 2009-07-08 | 住友電気工業株式会社 | 低欠陥ダイヤモンド単結晶及びその合成方法 |
JPH09268096A (ja) | 1996-03-29 | 1997-10-14 | Toyota Central Res & Dev Lab Inc | 単結晶の製造方法及び種結晶 |
EP0933450B1 (en) | 1998-01-19 | 2002-04-17 | Sumitomo Electric Industries, Ltd. | Method of making SiC single crystal and apparatus for making SiC single crystal |
JP4275308B2 (ja) * | 2000-12-28 | 2009-06-10 | 株式会社デンソー | 炭化珪素単結晶の製造方法およびその製造装置 |
US7141117B2 (en) | 2004-02-04 | 2006-11-28 | Matsushita Electric Industrial Co., Ltd. | Method of fixing seed crystal and method of manufacturing single crystal using the same |
US7497906B2 (en) * | 2006-03-08 | 2009-03-03 | Bridgestone Corporation | Seed crystal fixing apparatus and a method for fixing the seed crystal |
JP5250321B2 (ja) | 2008-07-04 | 2013-07-31 | 昭和電工株式会社 | 炭化珪素単結晶成長用種結晶の製造方法並びに炭化珪素単結晶の製造方法 |
-
2010
- 2010-07-23 WO PCT/JP2010/062432 patent/WO2011065060A1/ja active Application Filing
- 2010-11-12 CN CN201080019023.7A patent/CN102414349B/zh not_active Expired - Fee Related
- 2010-11-12 EP EP10833086.1A patent/EP2508653B1/en not_active Not-in-force
- 2010-11-12 US US13/257,742 patent/US9090992B2/en active Active
- 2010-11-12 WO PCT/JP2010/070175 patent/WO2011065239A1/ja active Application Filing
- 2010-11-12 CA CA2757206A patent/CA2757206A1/en not_active Abandoned
- 2010-11-12 KR KR1020117024629A patent/KR20120022791A/ko not_active Application Discontinuation
- 2010-11-12 JP JP2011543208A patent/JP5741444B2/ja not_active Expired - Fee Related
- 2010-11-22 TW TW099140239A patent/TW201126032A/zh unknown
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS52134007A (en) * | 1976-04-30 | 1977-11-09 | Hamada Sangiyou Kk | Method of producing decorated board |
JP2001139394A (ja) | 1999-11-10 | 2001-05-22 | Toyota Central Res & Dev Lab Inc | 種結晶固定剤、種結晶固定方法およびそれらを用いた単結晶の製造方法 |
JP2003119098A (ja) * | 2001-10-16 | 2003-04-23 | Denso Corp | 種結晶の固定方法および固定状態の評価方法 |
JP2003226600A (ja) | 2002-02-05 | 2003-08-12 | Nippon Steel Corp | 炭化珪素単結晶育成用種結晶と炭化珪素単結晶インゴット及びこれらの製造方法 |
JP2009256193A (ja) * | 2008-03-21 | 2009-11-05 | Bridgestone Corp | 炭化ケイ素単結晶の製造方法 |
JP2010132464A (ja) * | 2008-12-02 | 2010-06-17 | Mitsubishi Electric Corp | 炭化珪素単結晶の製造方法 |
Non-Patent Citations (1)
Title |
---|
See also references of EP2508653A4 |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2015104925A1 (ja) * | 2014-01-10 | 2015-07-16 | 住友電気工業株式会社 | 種基板、インゴットおよびインゴットの製造方法 |
JP2015131740A (ja) * | 2014-01-10 | 2015-07-23 | 住友電気工業株式会社 | 種基板、インゴットおよびインゴットの製造方法 |
WO2016163157A1 (ja) * | 2015-04-09 | 2016-10-13 | 住友電気工業株式会社 | 炭化珪素単結晶の製造方法 |
JP2020066571A (ja) * | 2018-10-22 | 2020-04-30 | エスケイシー・カンパニー・リミテッドSkc Co., Ltd. | 保護膜を含む種結晶の製造方法、これを適用したインゴットの製造方法、保護膜を含む種結晶及び種結晶の付着方法 |
US11268209B2 (en) | 2018-10-22 | 2022-03-08 | Senic Inc. | Seed crystal including protective film including a first layer with first filler and second layer with second filler |
JP7044265B2 (ja) | 2018-10-22 | 2022-03-30 | セニック・インコーポレイテッド | 保護膜を含む種結晶の製造方法、これを適用したインゴットの製造方法、保護膜を含む種結晶及び種結晶の付着方法 |
Also Published As
Publication number | Publication date |
---|---|
EP2508653B1 (en) | 2015-07-15 |
JPWO2011065239A1 (ja) | 2013-04-11 |
CN102414349A (zh) | 2012-04-11 |
JP5741444B2 (ja) | 2015-07-01 |
KR20120022791A (ko) | 2012-03-12 |
EP2508653A1 (en) | 2012-10-10 |
US20120006255A1 (en) | 2012-01-12 |
WO2011065239A9 (ja) | 2011-09-29 |
CA2757206A1 (en) | 2011-06-03 |
CN102414349B (zh) | 2015-02-18 |
US9090992B2 (en) | 2015-07-28 |
WO2011065060A1 (ja) | 2011-06-03 |
TW201126032A (en) | 2011-08-01 |
EP2508653A4 (en) | 2013-09-04 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP5741444B2 (ja) | 単結晶の製造方法 | |
JP5696630B2 (ja) | 炭化珪素基板およびその製造方法 | |
JP2011121815A (ja) | 単結晶の製造方法 | |
JP6241254B2 (ja) | 単結晶の製造方法 | |
US20110229719A1 (en) | Manufacturing method for crystal, manufacturing apparatus for crystal, and stacked film | |
JP2013237592A (ja) | 炭化珪素単結晶の製造方法 | |
JP5447206B2 (ja) | 炭化珪素単結晶の製造方法および炭化珪素基板 | |
JP2011006302A (ja) | 炭化珪素単結晶の製造方法 | |
JP2001139394A (ja) | 種結晶固定剤、種結晶固定方法およびそれらを用いた単結晶の製造方法 | |
JP2016183108A (ja) | 炭化珪素基板 | |
JP2012250865A (ja) | 単結晶の製造方法および種結晶固定剤 | |
JP4501657B2 (ja) | 炭化珪素単結晶成長用の種結晶固定方法 | |
JP5983824B2 (ja) | 炭化珪素基板 | |
JP5765499B2 (ja) | 炭化珪素基板 | |
JP2015129087A (ja) | 炭化珪素基板 | |
JP4457708B2 (ja) | 種結晶固定方法並びに単結晶の製造方法 | |
JP2015051892A (ja) | 炭化珪素インゴットの製造方法 | |
JP2015120605A (ja) | 炭化珪素単結晶の製造方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
WWE | Wipo information: entry into national phase |
Ref document number: 201080019023.7 Country of ref document: CN |
|
121 | Ep: the epo has been informed by wipo that ep was designated in this application |
Ref document number: 10833086 Country of ref document: EP Kind code of ref document: A1 |
|
WWE | Wipo information: entry into national phase |
Ref document number: 13257742 Country of ref document: US |
|
ENP | Entry into the national phase |
Ref document number: 2011543208 Country of ref document: JP Kind code of ref document: A |
|
WWE | Wipo information: entry into national phase |
Ref document number: 2757206 Country of ref document: CA |
|
ENP | Entry into the national phase |
Ref document number: 20117024629 Country of ref document: KR Kind code of ref document: A |
|
WWE | Wipo information: entry into national phase |
Ref document number: 2010833086 Country of ref document: EP |
|
NENP | Non-entry into the national phase |
Ref country code: DE |