WO2014148156A1 - Creuset pour développer un monocristal de saphir et procédé pour développer un monocristal de saphir - Google Patents

Creuset pour développer un monocristal de saphir et procédé pour développer un monocristal de saphir Download PDF

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Publication number
WO2014148156A1
WO2014148156A1 PCT/JP2014/053296 JP2014053296W WO2014148156A1 WO 2014148156 A1 WO2014148156 A1 WO 2014148156A1 JP 2014053296 W JP2014053296 W JP 2014053296W WO 2014148156 A1 WO2014148156 A1 WO 2014148156A1
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crucible
single crystal
sapphire
sapphire single
growing
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PCT/JP2014/053296
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English (en)
Japanese (ja)
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大 田賀
聖一 星
博 横山
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株式会社アライドマテリアル
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Priority to JP2014528748A priority Critical patent/JP5650869B1/ja
Publication of WO2014148156A1 publication Critical patent/WO2014148156A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/04—Alloys based on tungsten or molybdenum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/045—Alloys based on refractory metals
    • 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
    • C30B29/16—Oxides
    • C30B29/20—Aluminium oxides
    • 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
    • C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
    • C30B35/002—Crucibles or containers

Definitions

  • the present invention relates to a crucible for growing a sapphire single crystal and a method for growing a sapphire single crystal.
  • Sapphire single crystal is a material excellent in transmittance and mechanical properties, and is widely used, for example, as an optical material, and has been increasingly used as an epitaxial substrate for GaN growth.
  • This sapphire single crystal has been conventionally used by using a pulling method (also called Czochralski method, CZ method, etc.) EFG method (Edge-defined.fFilm-fed Growth) method or Kyropoulos method using a crucible made of iridium, tungsten, molybdenum or the like. It was obtained by growing from a seed crystal.
  • a pulling method also called Czochralski method, CZ method, etc.
  • EFG method Edge-defined.fFilm-fed Growth
  • Kyropoulos method using a crucible made of iridium, tungsten, molybdenum or the like. It was obtained by growing from a seed crystal.
  • the HEM (Heat-Exchange Method) method has come to be used as a growth method that can cope with an increase in the size of the sapphire single crystal (Non-patent Document 1).
  • molybdenum is widely used as a crucible material because it is less expensive than iridium and tungsten (Patent Document 1).
  • prescribed internal angle dimension may be formed in the part which connects the bottom part and side part of a crucible (patent documents 5, 6).
  • molten alumina erodes the molybdenum crystal grain boundary, and as a result, molybdenum particles of the order of several tens of ⁇ m to mm fall off and enter the sapphire crystal, thereby coloring the sapphire crystal. In some cases, the crystallinity is deteriorated.
  • the present invention has been made in view of the above problems, and an object thereof is to provide a crucible for growing a sapphire single crystal having a structure capable of suppressing mixing of crucible components into dissolved sapphire.
  • the present inventor examined again the conditions necessary for the crucible capable of suppressing the mixing of the crucible components into the melted sapphire, particularly the shape of the inner peripheral surface of the crucible in contact with sapphire.
  • the inventor of the present invention paid attention to the shape of the R portion that connects the cylindrical portion and the flat bottom portion in an equal-thickness cylindrical crucible.
  • the shape of the R part is desirably larger to some extent from the viewpoint of workability when manufacturing a crucible.
  • the portion corresponding to the R portion is different from the portion corresponding to the cylindrical portion in size and shape, and is therefore discarded when a wafer or the like is cut out from the sapphire single crystal. Part.
  • a sapphire single crystal can be manufactured with a high yield when the R portion is as small as possible.
  • the present inventor can suppress the mixing of the crucible component into the melted sapphire by increasing the R portion to a certain size, and can improve the yield.
  • the inventors have found that this is possible and have come to make the present invention.
  • the first aspect of the present invention is composed of molybdenum or tungsten, or an alloy of molybdenum and tungsten, and inevitable impurities, and is integrated with the cylindrical portion and one end portion of the cylindrical portion via the R portion.
  • a second aspect of the present invention is a sapphire single crystal growth method using the sapphire single crystal growth crucible described in the first aspect.
  • a crucible for growing a sapphire single crystal having a structure capable of suppressing mixing of crucible components into dissolved sapphire.
  • the crucible 1 for growing a sapphire single crystal a crucible for growing a single crystal using a CZ method, an EFG method or the like is illustrated.
  • the crucible 1 for growing a sapphire single crystal has a cylindrical portion 3 and a flat bottom 7 that is integrally provided at one end of the cylindrical portion 3 with an R portion 5 without a joint. It is a uniform cylindrical shape.
  • molybdenum, tungsten, or an alloy of molybdenum and tungsten is preferably used as a metal material that can withstand the melting temperature of sapphire (alumina) and has high strength.
  • tungsten and molybdenum can form a solid solution type alloy.
  • alloys include 90 mass% molybdenum-10 mass% tungsten alloy (abbreviation 9 MW), 70 mass% molybdenum-30 mass% tungsten alloy (7 MW), 50 mass% molybdenum-50 mass% tungsten alloy (5 MW), and the like. is there.
  • the minimum tungsten content necessary for exhibiting the effect of alloying is 5% by mass. Therefore, the tungsten content is preferably at least 5% by mass.
  • the upper limit of the alloy amount is 50% by mass.
  • the purity of the above material is preferably 99.9% by mass or more, and the remainder is inevitable impurities. This is because erosion of the molten sapphire on the inner surface of the crucible is unavoidable, but a high-purity material of this level requires very little impurity contamination, and problems such as coloring can be avoided.
  • TMIAS tungsten-molybdenum industry association standard
  • the cylindrical portion 3 has an inner diameter (opening portion diameter D) corresponding to the diameter of the sapphire single crystal wafer to be grown.
  • the diameter of the wafer includes a 4-inch wafer and a 6-inch wafer.
  • it is desirable that at least the opening diameter D of the crucible is 200 mm. Further, in the future, it is predicted that a crucible having an opening diameter of 400 mm and a crucible having an opening diameter of 660 mm will be generated. Therefore, the opening diameter D is in a range where a range of 200 mm or more and 660 mm or less is assumed. is there.
  • the flat bottom 7 is a bottom portion having a flat shape.
  • the cylindrical portion 3 and the flat bottom 7 have a thickness of 5 mm or more and 15 mm or less.
  • the weight of a sapphire ingot is about 25 kg for a diameter of 200 mm and a height of 200 mm, and about 85 kg for a diameter of 300 mm and a height of 300 mm.
  • increasing the thickness of the crucible is one measure. This is because the thickness needs to be increased as the diameter of the crucible opening increases, so that it needs to be at least 5 mm.
  • the weight of the crucible increases.
  • the weight of a molybdenum crucible having an opening diameter of 300 mm, a height of 300 mm, and a thickness of 15 mm is about 55 kg. If the weight exceeds this value, the load-carrying countermeasures of the crystal growth apparatus become large, so the thickness is preferably 15 mm or less.
  • the R portion 5 is a portion that connects the cylindrical portion 3 and the flat bottom 7, and the cross-sectional shape parallel to the axial direction of the crucible has an arc shape.
  • the present inventors have found that mixing the crucible component into the melted sapphire can be suppressed by setting the inner angle dimension 5a (arc radius) of the R portion 5 within a predetermined range.
  • the inner angle dimension 5a of the R portion 5 is set to 20 mm or more and 40 mm or less, it is possible to suppress the metal particles constituting the R portion 5 from dropping out and mixing into the sapphire crystal during sapphire growth. Become.
  • sapphire melted in the crucible is a high-temperature fluid, but when the inner angle dimension 5a of the R portion 5 is less than 20 mm, the convection of sapphire during melting is not smooth, so the temperature in the R portion 5 is other than that. It is considered that a so-called “heat pool”, which is higher than the portion, occurs, and the metal particles constituting the crucible component of the R portion 5 drop off and enter the sapphire crystal.
  • the inner angle dimension 5a of the R part 5 is less than 20 mm, the convection is turbulent in the R part 5 and the sapphire solution vortex becomes more intense than the others, which is considered to promote erosion.
  • the inner angle dimension 5a of the R portion 5 is 20 mm or more.
  • the crucible shape becomes a shape close to a round bottom instead of a flat bottom, and the portion discarded when cutting a wafer or the like from a sapphire single crystal increases, resulting in a deterioration in yield.
  • the convection of the molten sapphire is different from that of a flat bottom, and mixing of crucible components may not be suppressed, which is not preferable.
  • the surface shape of the sapphire single crystal growth crucible 1 is desirably a shape capable of suppressing the mixing of the crucible components into the melted sapphire.
  • the inner circumference in contact with sapphire is Ry 7 ⁇ m or less and Ra 1 ⁇ m or less. Is desirable.
  • H / D which is a ratio of the crucible height (H) and the opening diameter (D)
  • H / D which is a ratio of the crucible height (H) and the opening diameter (D)
  • H / D is 1.4 or less.
  • a tall crucible is advantageous for the production of a larger ingot, but from the viewpoint of the design and production of growth equipment, a tall crucible has an external heating structure and arrangement, This is because there are many problems such as the vertical holding structure of the crucible, and on the other hand, from the standpoint of crucible production, there are restrictions on the molding technology into the crucible shape. Therefore, the limit of H / D is 1.4.
  • the method for producing the sapphire single crystal growth crucible 1 is not particularly limited as long as the sapphire single crystal growth crucible having the above-mentioned shape and composition can be produced. Examples thereof are as follows. be able to. Hereinafter, an example of the manufacturing method will be described with reference to FIG.
  • raw materials for the crucible are prepared. Specifically, when pure molybdenum is used as the material for the sapphire single crystal growth crucible 1, the raw material is a molybdenum powder having an Fsss (Fisher Sub-Sieve Sizer) particle size of 4 to 5 ⁇ m and a purity of 99.9% by mass or more. It is desirable to use
  • Fsss Fisher Sub-Sieve Sizer
  • tungsten-molybdenum alloy when used, a tungsten powder having a Fsss particle size of 2 to 3 ⁇ m and a purity of 99.9% by mass or more as a raw material for the crucible, and a molybdenum having a Fsss particle size of 4 to 5 ⁇ m and a purity of 99.9% by mass or more.
  • the powder is weighed at the desired alloy weight ratio.
  • Typical alloy types are 90 mass% Mo-10 mass% W (abbreviated as 9 MW), 70 mass% Mo-30 mass% W (7 MW), 50 mass% Mo-50 mass% W (5 MW). .
  • tungsten powder having a Fsss particle size of 2 to 3 ⁇ m and a purity of 99.9% by mass or more.
  • the raw material powder is filled into a rubber having the shape of a desired molded body, the open port is sealed with a stopper, and then the rubber is evacuated. After the evacuation is completed, the rubber is loaded into a CIP (Cold Isostatic Pressing) apparatus and molded by applying water pressure according to a predetermined procedure. After depressurization, the rubber is taken out from the CIP device to wipe off moisture on the surface, the stopper is opened, and the powder compact is taken out.
  • CIP Cold Isostatic Pressing
  • the powder compact is sintered at 2000 ° C. or higher for 20 hours in a batch type or continuous hydrogen sintering furnace.
  • a higher temperature and longer sintering treatment is preferable for improving the sintered density.
  • the sintered material is a plate-like sintered body having a thickness of 30 mm, a width of 300 mm, a length of 300 mm, and a weight of about 28 kg.
  • the crucible shape is formed by sintering, Is a crucible-shaped sintered body.
  • the theoretical density ratio of the obtained sintered body is 95% or more. This is because if the theoretical density ratio is 95% or more, the densification of the powder particles proceeds, or the high-density strength is improved by high densification due to plastic deformation, and the erosion resistance is further improved.
  • the theoretical density ratio here means a value obtained by measurement by the Archimedes method. In the case of an as-sintered crucible (a crucible without surface polishing), the crucible is completed here.
  • the above-described hot-rolled material has an oxidized surface and is covered with a light yellow or dark oxide. Therefore, after reducing the surface oxide at a temperature of 900 ° C. using a hydrogen reduction furnace, this is dissolved and removed with a strong acid to form the surface of the metal background.
  • the rolled sheet is cut by an appropriate cutting method such as discharge wire cutting or plasma cutting to obtain a disk-shaped blank for drawing.
  • the crucible 1 for growing a sapphire single crystal is composed of molybdenum, tungsten, or an alloy of molybdenum and tungsten and an inevitable impurity, and includes a cylindrical portion 3 and one end portion of the cylindrical portion 3.
  • the inner portion 5a of the R portion 5 has a flat bottom 7 which is integrally provided through the R portion 5 without a joint, and the inner angle dimension 5a of the R portion 5 is 20 mm or more and 40 mm or less.
  • the crucible 1 for growing a sapphire single crystal has a structure capable of suppressing mixing of crucible components into the dissolved sapphire.
  • Example 1 An attempt was made to produce a crucible 1 for growing a sapphire single crystal of a 9 MW alloy (theoretical density: 10.70 g / cm 3 ) by sintering.
  • the specific procedure is as follows.
  • the inside of the rubber was evacuated for about 30 minutes to confirm that there was no air leak.
  • the rubber surface was washed with water to remove the adhering powders, and then inserted into a CIP apparatus and subjected to hydrostatic pressure. After holding at a pressure of 2 ton / cm 2 for about 10 minutes, the pressure was released and the CIP molding operation was completed. After removing the rubber from the CIP apparatus and wiping and removing the moisture on the surface, the stopper was removed and opened. Thereafter, a crucible-shaped tungsten-molybdenum mixed powder molded body was taken out from the rubber, and burrs and protrusions were removed by sanding or the like.
  • the molded body is inserted into a hydrogen sintering furnace, sintered at 2000 ° C. for 20 hours, and a tungsten-molybdenum alloy sintered crucible material having a specific gravity of about 10.2 (theoretical density ratio of about 95%).
  • the sintered crucible material was made into the required shape and dimensions by cutting such as a lathe.
  • the obtained crucible was placed in a wet blasting apparatus, and surface treatment was performed by spraying alumina abrasive grains (particle size 100 mesh) on the inner and outer surfaces. Thereafter, the abrasive grains remaining on the crucible surface were removed with jet water and dried. Furthermore, after the dried crucible is placed in the electrolyte bath and filled with the electrolyte solution, a negative electrode material is placed in the electrolyte solution inside the crucible, and electrical connection is made so that the crucible becomes a positive electrode. Applied to start electropolishing. After processing for about 1 hour, the connection was removed, the electrode was removed, the chemical solution was discharged, and the crucible was taken out from the liquid bath. Further, the crucible was placed in a neutralization chemical solution tank and neutralized with the adhering chemical solution, and then washed with water, washed with hot water and dried to finish a product crucible.
  • alumina abrasive grains particle size 100 mesh
  • a 7 MW alloy (theoretical density of 11.88 g / cm 3 ) crucible and a 5 MW (theoretical density of 13.35 g / cm 3 ) crucible can be manufactured in the same procedure. Further, by using pure tungsten and pure molybdenum as raw materials, a tungsten crucible and molybdenum can be obtained in the same manner.
  • Example 2 A 9 MW alloy crucible having an opening diameter of 300 mm, a height of 300 mm, and a thickness of 10 mm was manufactured by a spatula drawing. The specific procedure is as follows.
  • a mixed powder was prepared in the same manner as in Example 1.
  • CIP molding was performed on the mixed powder.
  • a blank material is produced by performing plastic working such as rolling on the molded body after sintering.
  • the other conditions were the same as in Example 1.
  • sintering was performed in the same manner as in Example 1 to obtain a sintered alloy sintered material for rolling (theoretical density ratio: about 95%) having a thickness of 30 mm, a length and width of 370 mm, and a specific gravity of about 10.2.
  • the sintered material was rolled using a four-high rolling mill for hot rolling.
  • the size of the blank material necessary for molding into a crucible having an opening diameter of 300 mm, a height of 300 mm, and a thickness of 10 mm was set to a thickness of 12 mm and a diameter of 550 mm, and was executed based on a rolling schedule.
  • a sintered body heated to 1400 ° C. in a hydrogen furnace is rolled out to about 570 mm and hot-rolled, then the rolling direction is changed, and finally the heating temperature is lowered appropriately to 800 ° C.
  • Unidirectional rolling was repeated to obtain a hot-rolled cross-rolled alloy sheet having a thickness of approximately 12 mm, a width of 570 mm, and a length of 570 mm.
  • the alloy plate whose surface is covered with a light yellow oxide is inserted into a hydrogen annealing furnace for annealing heat treatment maintained at 930 ° C., heated and maintained for about 30 minutes, and then placed in a hydrogen atmosphere cooling zone. It was moved, cooled to room temperature, and taken out of the furnace. After this treatment, the reduced surface deposits were dissolved and removed in strong acid, washed with water and dried to obtain an alloy plate with a flat alloy background.
  • a 5 MW alloy sheet obtained a rolled sheet having a theoretical density ratio of 98.9% (specific gravity: 13.20) and a purity of 99.9% by mass.
  • a blank material to be subjected to spatula drawing was cut out from the obtained rolled plate to a thickness of 12 mm and a diameter of 550 mm with a discharge wire cutting machine.
  • This blank material is applied to the portion corresponding to the bottom of the drawing type crucible attached to the spatula drawing machine, and the blank material is fixed with a push rod while taking out the center of rotation.
  • the drawing die / blank material / push bar integrated in series are simultaneously rotated, the blank material is heated to a red hot state of 600 ° C. to 700 ° C. with a burner. In this state, the roller (spar) was drawn out and formed into a crucible shape following the drawing die.
  • the phenomenon caused by the characteristics and quality of the blank material is caused by intragranular cracks that appear during the work to follow the dimensions and shape of the outer angle close to the bottom, and the opening at the time that is close to the end of processing.
  • intragranular cracks that appear during the work to follow the dimensions and shape of the outer angle close to the bottom, and the opening at the time that is close to the end of processing.
  • layered delamination and intergranular cracking are mainly caused by low blank material strength and crystal grain size.
  • the particle size is about 10 ⁇ m to 50 ⁇ m, the material strength is high and it can withstand deformation, but if it is a coarse particle of about 300 ⁇ m to 500 ⁇ m, it is too low to endure deformation and breaks.
  • the obtained crucible having an opening diameter of 300 mm and a height of 300 mm was inserted into a hydrogen annealing furnace for annealing and heat treatment, and the surface oxide film was reduced, followed by dissolution / removal of surface deposits in a strong acid solution. A rough crucible with an alloy background was obtained.
  • the above-mentioned sintered crucible material or rough crucible was set on a lathe and processed into a desired shape and size with a cutting blade to obtain a cutting finished crucible.
  • the crucible 1 for growing a sapphire single crystal using a spatula drawing process could be manufactured by the above procedure.
  • Example 3 In order to confirm the effect of reducing the erosion due to the alumina inside the wall, which is influenced by the inner angle dimension of the R portion 5, 9 MW alloy and pure molybdenum are used as materials, the opening diameter is 300 mm, and the height is the same as in Example 1.
  • a crucible with 300 mm, a thickness of 10 mm, and an internal angle dimension of the R portion 5 of 10 mm, 20 mm, 30 mm, 40 mm, and 50 mm, respectively, is prepared for sapphire growth, and the degree of erosion is evaluated by measuring the coloration and thickness change did.
  • Sapphire growth was performed at 2150 ° C. using a sapphire growth apparatus, and sapphire growth was repeated 10 times.
  • the observation site of the thickness change was performed in a portion where the wall portion where the most erosion occurred was transferred to the R portion 5.
  • the size of the crucible before use was measured with a three-dimensional shape measuring instrument (Faro-Edge), and the crucible after 10 uses was broken at the time of disposal and measured with an optical microscope.
  • the inner surface of the crucible was subjected to the same electrolytic polishing treatment as in Example 1 and subjected to an erosion experiment.
  • the results are shown in Tables 1 and 2.
  • Table 1 shows the results when a 9 MW alloy was used as the crucible material
  • Table 2 shows the results when pure molybdenum was used.
  • the change in thickness and the presence or absence of coloring were the same as in the case of 20 mm.
  • the effective diameter of the obtained sapphire single crystal becomes small, and deterioration of the yield of sapphire becomes a problem.
  • Example 4 A 9 MW, 7 MW, and 5 MW alloy crucible with an inner angle dimension of the R portion 5 of 30 mm was manufactured in the same procedure as in Example 3.
  • an electrolytic polishing treatment was performed in the same procedure as described above.
  • the crucible was installed in a wet blasting apparatus, and alumina abrasive grains (particle size 100 mesh) were sprayed on the inner and outer surfaces to perform surface treatment. After blasting, the abrasive grains remaining on the crucible surface were removed with jet water and dried.
  • the electrolytic polishing conditions were the following two types A and B, respectively.
  • Condition A Voltage 35 V, current density 300 mA / cm 2 , polishing time 60 minutes
  • Condition B Voltage 35 V, current density 1300 mA / cm 2 , polishing time 30 minutes
  • a 9 MW alloy crucible in which the inner angle dimension of the R portion 5 was 30 mm was manufactured under the same conditions as the electrolytic polishing conditions: voltage 35V, current density 1500 mA / cm 2 , polishing time 30 minutes, and other conditions. .
  • the prepared crucible was used to dissolve sapphire using the same sapphire growing apparatus as in Example 3 and held at 2150 ° C. for 50 hours, and then the sapphire was taken out and the presence or absence of coloring was observed in the same manner as in Example 3. .
  • the obtained sapphire ingot was not colored and was a normal sapphire ingot.

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

Le problème à résoudre dans le cadre de la présente invention est de proposer un creuset, ledit creuset étant utilisé pour développer un monocristal de saphir et possédant une structure qui puisse supprimer la contamination de saphir fondu par des composants de creuset. Le creuset (1) pour développer un monocristal de saphir est conçu à partir d'impuretés inévitables et de molybdène, de tungstène, ou d'un alliage de molybdène et de tungstène, et présente une forme tubulaire cylindrique qui comporte une section tubulaire cylindrique (3) et un fond plat (7) prévu d'une seule pièce sur une extrémité de la section tubulaire cylindrique (3), une section R (5) se trouvant entre ledit fond plat et ladite section tubulaire cylindrique.
PCT/JP2014/053296 2013-03-21 2014-02-13 Creuset pour développer un monocristal de saphir et procédé pour développer un monocristal de saphir WO2014148156A1 (fr)

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WO2022140806A1 (fr) * 2020-12-29 2022-07-07 Fametec Gmbh Dispositif pour faire croître un monocristal produit de manière artificielle, en particulier un monocristal de saphir

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KR102187449B1 (ko) * 2019-05-28 2020-12-11 에스케이씨 주식회사 탄화규소 잉곳의 제조방법, 탄화규소 잉곳 및 이의 성장 시스템
KR102276450B1 (ko) 2019-10-29 2021-07-12 에스케이씨 주식회사 탄화규소 잉곳의 제조방법, 탄화규소 웨이퍼의 제조방법 및 이의 성장 시스템
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