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WO2025089583A1 - Procédé de fabrication d'un lingot de carbure de silicium - Google Patents

Procédé de fabrication d'un lingot de carbure de silicium Download PDF

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Publication number
WO2025089583A1
WO2025089583A1 PCT/KR2024/012391 KR2024012391W WO2025089583A1 WO 2025089583 A1 WO2025089583 A1 WO 2025089583A1 KR 2024012391 W KR2024012391 W KR 2024012391W WO 2025089583 A1 WO2025089583 A1 WO 2025089583A1
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Prior art keywords
silicon carbide
internal space
temperature
carbide ingot
manufacturing
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English (en)
Korean (ko)
Inventor
이채영
김수호
이승준
최정우
박종휘
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Senic Inc
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Senic Inc
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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
    • C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
    • C30B23/02—Epitaxial-layer growth
    • C30B23/06—Heating of the deposition chamber, the substrate or the materials to be evaporated
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/36—Carbides

Definitions

  • Silicon carbide has excellent heat resistance and mechanical strength, is resistant to radiation, and can be produced as a large-diameter substrate.
  • silicon carbide has excellent physical strength and chemical resistance, a large energy band gap, and high electron saturation drift velocity and withstand pressure. Therefore, it is widely used in semiconductor devices that require high power, high efficiency, high withstand pressure, and large capacity, as well as in abrasives, bearings, and refractory plates.
  • Silicon carbide is manufactured through various methods, such as heat treatment or electric current treatment of carbon raw materials such as silicon carbide waste.
  • Conventional methods include the Acheson method, reaction sintering, atmospheric pressure sintering, or CVD (chemical vapor deposition) method.
  • CVD chemical vapor deposition
  • Japanese Patent Publication No. 2002-326876 discloses a method for manufacturing a silicon carbide precursor by reacting it at high temperature under an inert gas condition such as argon (Ar) after a heat treatment process in order to polymerize or cross-link a silicon source and a carbon source.
  • an inert gas condition such as argon (Ar)
  • this process has the problem that the manufacturing cost is high and the powder size is not uniform because it is heat treated at a high temperature of 1,800°C to 2,100°C under a vacuum or inert gas condition.
  • wafers used in the solar cell and semiconductor industries are manufactured by growing silicon ingots in crucibles made of graphite, etc., and during the manufacturing process, not only waste slurry containing silicon carbide is generated, but also a significant amount of silicon carbide waste adsorbed on the inner walls of the crucible is generated. However, until now, such waste has been landfilled, causing environmental problems and incurring high disposal costs.
  • the present invention provides a method for manufacturing a silicon carbide ingot having a low occurrence of defects, an excellent growth rate, and improved crystal quality.
  • a method for manufacturing a silicon carbide ingot according to the present invention comprises the steps of arranging silicon carbide raw materials and seed crystals in a reaction vessel having an internal space, the step of firstly heating the temperature of the internal space by a heating means surrounding the reaction vessel, the step of secondly heating the temperature of the internal space by the heating means while depressurizing the internal space, the step of inducing growth of the silicon carbide ingot under the depressurized pressure when the depressurization of the internal space is completed, and the step of cooling the temperature of the internal space to room temperature, wherein the internal space includes an upper portion where the seed crystals are arranged and a lower portion where the silicon carbide raw material is arranged, and in the second temperature raising step, a difference between the temperature of the upper portion of the internal space and the temperature of the lower portion of the internal space is maintained at 50°C to 100°C.
  • the first heating step can be performed until depressurization of the internal space begins.
  • the second heating step can be performed until the depressurization of the internal space is completed.
  • the upper temperature of the internal space may be 2,200°C to 2,250°C.
  • the lower temperature of the internal space in the second heating step may be 2,250°C to 2,350°C.
  • the difference between the upper temperature of the internal space and the lower temperature of the internal space can be maintained at 50° C. to 200° C.
  • the difference between the upper temperature of the internal space and the lower temperature of the internal space can be maintained at 40° C. to 60° C.
  • the heating means may include a plurality of coils that move in the height direction of the reaction vessel and generate an induced current in the reaction vessel.
  • the distance between the coil and the reaction vessel may be 60 mm to 600 mm.
  • the diameter of each of the plurality of coils may be from 5 mm to 40 mm, and the spacing between the plurality of coils may be from 5 mm to 30 mm.
  • the center position of the coil according to the above formula 1 can satisfy 53% to 57%.
  • the center position of the coil according to the formula 1 in the step of inducing growth of the silicon carbide ingot, can satisfy 20% to 50%.
  • the method for manufacturing a silicon carbide ingot according to the present invention comprises a step of increasing the temperature of an internal space by a heating means while depressurizing the internal space, wherein the difference between the upper temperature of the internal space and the lower temperature of the internal space is maintained at 50°C to 100°C.
  • the difference between the upper temperature of the internal space and the lower temperature of the internal space can be maintained at 50°C to 200°C.
  • the process temperature After the ratio of carbon and silicon is stabilized in this way, by adjusting the process temperature to a different process temperature range from the previous process temperature, the deposition rate of silicon carbide gas on the seed crystal increases, so that the growth rate of the silicon carbide ingot can be improved.
  • a silicon carbide ingot substantially free of defects and having improved crystal quality, a wafer manufactured therefrom, and the like can be provided.
  • Figure 1 is a flow chart schematically illustrating a manufacturing method according to the present invention.
  • FIG. 2 is a flowchart specifically illustrating step S10.
  • FIG. 3 is a flowchart specifically illustrating step S20.
  • FIG. 4 is a flowchart specifically illustrating step S50.
  • FIGS. 5 and 6 schematically illustrate a cross-section of a silicon carbide ingot manufacturing device for manufacturing a silicon carbide ingot according to one embodiment of the invention.
  • Figure 7 schematically illustrates the position of the coil at step S30.
  • Figure 9 is a photograph of the surface of a silicon carbide ingot according to Example 1 taken using an optical microscope.
  • Figure 10 is a photograph of the surface of a silicon carbide ingot according to Comparative Example 1 taken using an optical microscope.
  • Figure 11 is a photograph of the surface of a silicon carbide ingot according to Comparative Example 2 taken using an optical microscope.
  • Figure 12 is a photograph of the surface of a silicon carbide wafer sample according to Example 1 taken using an optical microscope.
  • Figure 13 is a photograph of the surface of a silicon carbide wafer sample according to Comparative Example 1 taken using an optical microscope.
  • Figure 14 is a photograph of the surface of a silicon carbide wafer sample according to Comparative Example 2 taken using an optical microscope.
  • a and/or B in this specification or application means “A, B, or A and B.”
  • a certain configuration is “connected” to another configuration, this includes not only the case where it is “directly connected,” but also the case where it is “connected with another configuration in between.”
  • B being located on A means that B is located in direct contact with A or that B is located on A with another layer located in between, and is not limited to being interpreted as being located in contact with the surface of A.
  • the singular expression is interpreted to include the singular or plural as interpreted in the context unless specifically stated otherwise.
  • the respective embodiments may be combined with each other, unless they are technically incompatible with each other.
  • a method for manufacturing a silicon carbide ingot according to the present invention comprises the steps of arranging silicon carbide raw materials and seed crystals in a reaction vessel having an internal space, the step of firstly heating the temperature of the internal space by a heating means surrounding the reaction vessel, the step of secondly heating the temperature of the internal space by the heating means while depressurizing the internal space, the step of inducing growth of the silicon carbide ingot under the depressurized pressure when the depressurization of the internal space is completed, and the step of cooling the temperature of the internal space to room temperature, wherein the internal space includes an upper portion where the seed crystals are arranged and a lower portion where the silicon carbide raw material is arranged, and in the second temperature raising step, a difference between the temperature of the upper portion of the internal space and the temperature of the lower portion of the internal space is maintained at 50°C to 100°C.
  • FIG. 1 is a flow chart schematically illustrating a manufacturing method according to the present invention
  • FIG. 2 is a flow chart specifically illustrating step S10
  • FIGS. 5 and 6 schematically illustrate cross-sections of a silicon carbide ingot manufacturing device for manufacturing a silicon carbide ingot according to one embodiment of the invention.
  • the manufacturing method includes a step of placing silicon carbide raw material (20) and seed crystals (30) (S10).
  • the above step S10 may include a step (S11) of arranging the silicon carbide raw material (20) and the seed crystal (30) so as to face each other, a step (S12) of sealing the internal space of the reaction vessel (10), a step (S13) of arranging an insulating material (40) surrounding the reaction vessel (10), and a step of arranging a heating means (60) outside the reaction vessel (10) and the insulating material (40).
  • the silicon carbide raw material (20) of the above step S11 may include silicon carbide.
  • the above silicon carbide raw material (20) may include ⁇ -phase silicon carbide and/or ⁇ -phase silicon carbide.
  • the above silicon carbide raw material (20) may include a silicon carbide single crystal and/or a silicon carbide polycrystal.
  • the above silicon carbide raw material (20) may further contain unwanted impurities in addition to silicon carbide.
  • the above silicon carbide raw material (20) may further contain a carbon-based material such as graphite as an impurity.
  • the carbon-based material may be derived from a graphite crucible, etc.
  • the carbon-based material may be included in the silicon carbide raw material (20) in an amount of about 1 wt% to about 60 wt%.
  • the carbon-based material may be included in the silicon carbide raw material (20) in an amount of about 2 wt% to about 60 wt%.
  • the carbon-based material may be included in the silicon carbide raw material (20) in an amount of about 5 wt% to about 60 wt%.
  • the carbon-based material may be included in the silicon carbide raw material (20) in an amount of about 5 wt% to about 50 wt%.
  • the carbon-based material may be included in the silicon carbide raw material (20) in an amount of about 50 wt% or less.
  • the carbon-based material may be included in the silicon carbide raw material (20) in an amount of about 45 wt% or less.
  • the carbon-based material may be included in the silicon carbide raw material (20) in an amount of about 40 wt% or less.
  • the carbon-based material may be included in the silicon carbide raw material (20) in an amount of about 1 wt% to about 50 wt%.
  • the carbon-based material may be included in the silicon carbide raw material (20) in an amount of about 5 wt% to about 45 wt%.
  • the carbon-based material may be included in the silicon carbide raw material (20) in an amount of about 10 wt% to about 40 wt%.
  • the carbon-based material may be included in the silicon carbide raw material (20) in an amount of about 10 wt% to about 35 wt%.
  • the carbon-based material may be included in the silicon carbide raw material (20) in an amount of about 10 wt% to about 30 wt%.
  • the carbon-based material may be included in the silicon carbide raw material (20) in an amount of about 10 wt% to about 20 wt%.
  • the above silicon carbide raw material (20) may further include free silicon as the impurity.
  • the free silicon may be derived from a silicon substrate and/or a silicon component, etc.
  • the silicon component may be a component used in semiconductor equipment, such as a focus ring.
  • the free silicon may be included in the silicon carbide raw material in an amount of about 0.01 wt% to about 10 wt%.
  • the above silicon carbide raw material (20) may further include metal impurities.
  • the metal impurities may be at least one selected from the group consisting of lithium, boron, sodium, aluminum, phosphorus, potassium, calcium, titanium, vanadium, chromium, manganese, iron, nickel, copper, zinc, strontium, zirconium, molybdenum, tin, barium, tungsten, or lead.
  • the content of the metal impurity may be about 0.1 ppm to 13 ppm based on the total weight of the silicon carbide raw material (20).
  • the content of the metal impurity may be about 0.3 ppm to 12 ppm.
  • the content of the metal impurity may be about 0.5 ppm to 8 ppm.
  • the content of the metal impurity may be about 0.8 ppm to 10 ppm.
  • the content of the metal impurity may be about 1 ppm to 6 ppm.
  • the content of the metal impurity may be about 0.1 ppm to 5 ppm.
  • the content of the metal impurity may be about 0.5 ppm to 3 ppm.
  • the content of the metal impurity may be about 0.5 ppm to 2 ppm.
  • the above silicon carbide raw material (20) may further contain non-metallic impurities.
  • the non-metallic impurities may be selected from the group consisting of fluorine, nitrogen, chlorine, or phosphorus.
  • the content of the nonmetallic impurities may be about 0.01 ppm to 30 ppm based on the total weight of the silicon carbide raw material (20).
  • the content of the nonmetallic impurities may be about 0.3 ppm to 20 ppm.
  • the content of the nonmetallic impurities may be about 0.5 ppm to 15 ppm.
  • the content of the nonmetallic impurities may be about 1 ppm to 15 ppm.
  • the content of the nonmetallic impurities may be about 3 ppm to 13 ppm.
  • the content of the nonmetallic impurities may be about 1 ppm to 10 ppm.
  • the content of the nonmetallic impurities may be about 5 ppm to 15 ppm.
  • the content of the nonmetallic impurities may be about 5 ppm to 12 ppm.
  • the above silicon carbide raw material (20) may contain about 30 wt% or more of particles having a particle size of about 100 ⁇ m or more.
  • the above silicon carbide raw material (20) may contain about 50 wt% or more of particles having a particle size of about 100 ⁇ m or more.
  • the above silicon carbide raw material (20) may contain about 70 wt% or more of particles having a particle size of about 100 ⁇ m or more.
  • the above silicon carbide raw material (20) may contain about 30 wt% or more of particles having a particle diameter of about 1 mm or more.
  • the above silicon carbide raw material (20) may contain about 50 wt% or more of particles having a particle diameter of about 1 mm or more.
  • the above silicon carbide raw material (20) may contain about 70 wt% or more of particles having a particle diameter of about 1 mm or more.
  • the above silicon carbide raw material (20) may contain about 30 wt% or more of particles having a particle size of about 10 mm or more.
  • the above silicon carbide raw material (20) may contain about 50 wt% or more of particles having a particle size of about 10 mm or more.
  • the above silicon carbide raw material (20) may contain about 70 wt% or more of particles having a particle size of about 10 mm or more.
  • a sphere having the same volume as the volume of the particle is assumed, and the diameter of the sphere is defined as the particle diameter.
  • the above silicon carbide raw material (20) may be derived from a substrate including silicon carbide.
  • the above silicon carbide raw material (20) may be derived from a wafer including silicon carbide as a whole.
  • the above silicon carbide raw material (20) may be derived from a silicon carbide layer deposited on a substrate such as silicon.
  • the above silicon carbide raw material (20) may be derived from a silicon carbide single crystal ingot.
  • the silicon carbide single crystal ingot may be generated during the manufacturing process and discarded due to defects.
  • the above silicon carbide raw material (20) may be derived from a silicon carbide polycrystal.
  • the above silicon carbide raw material (20) may be derived from a silicon carbide sintered body.
  • the silicon carbide sintered body may be formed by sintering silicon carbide powder.
  • the silicon carbide sintered body may be a component included in semiconductor manufacturing equipment.
  • the above silicon carbide raw material (20) may be derived from a graphite component including a silicon carbide layer.
  • the graphite component may include a crucible or the like for forming a silicon carbide ingot.
  • the above silicon carbide raw material (20) may be derived from a component of a semiconductor device including a silicon carbide layer.
  • the silicon carbide layer may be formed by depositing silicon carbide on the surface of a silicon component or the like through a chemical vapor deposition (CVD) process.
  • the above silicon carbide raw material (20) may have a lump shape.
  • the above silicon carbide raw material (20) may have a plate shape.
  • the above silicon carbide raw material (20) may have a block shape. At least one silicon carbide block may be included in the crucible body (11).
  • the apparent volume of the silicon carbide block may be about 1 cm3 or more.
  • the apparent volume of the silicon carbide block may be about 5 cm3 or more.
  • the apparent volume of the silicon carbide block may be about 10 cm3 or more.
  • the apparent volume of the silicon carbide block may be about 20 cm3 or more.
  • the apparent volume of the silicon carbide block may be about 100 cm3 or more.
  • the apparent volume of the silicon carbide block may be about 1,000 cm3 or more.
  • the apparent volume of the silicon carbide block may be about 5,000 cm3 or more.
  • the apparent volume of the silicon carbide block may be about 1 m3 or less.
  • the apparent volume of the silicon carbide block may be smaller than the volume of the internal space of the crucible body (11).
  • the apparent volume may be a volume measured based on the outer shape of the silicon carbide block.
  • the apparent volume may be a volume measured on the assumption that there are no pores at all within the silicon carbide block.
  • the apparent volume may be a value obtained by adding the volume of silicon carbide within the silicon carbide block and the volume of pores within the silicon carbide block.
  • the above silicon carbide block may have a columnar shape, such as a cylindrical column or a polygonal column.
  • the above silicon carbide block may have a polyhedral shape.
  • the above silicon carbide block may have a plate shape.
  • the above silicon carbide block may have a horn shape, such as a cone or a polygonal horn.
  • the above silicon carbide block may have a donut shape.
  • the above silicon carbide block may have a shape in which a portion is cut.
  • the above silicon carbide block may be a single crystal or a polycrystalline one.
  • the above silicon carbide block may be a sintered body. That is, the above silicon carbide block may be formed in the form of a block by sintering silicon carbide particles or the like.
  • the above silicon carbide block may be formed by depositing silicon carbide by chemical vapor deposition.
  • the above silicon carbide block may be formed by depositing silicon carbide by physical vapor deposition.
  • the above silicon carbide block may include ⁇ -phase silicon carbide or ⁇ -phase silicon carbide.
  • the above silicon carbide block may have high thermal conductivity.
  • the thermal conductivity of the silicon carbide block may be about 10 W/mK or more.
  • the thermal conductivity of the silicon carbide block may be about 20 W/mK or more.
  • the thermal conductivity of the silicon carbide block may be about 30 W/mK or more.
  • the thermal conductivity of the silicon carbide block may be about 50 W/mK or more.
  • the thermal conductivity of the silicon carbide block may be about 70 W/mK or more.
  • the thermal conductivity of the silicon carbide block may be about 100 W/mK or more.
  • the thermal conductivity of the silicon carbide block may be about 110 W/mK or more.
  • the upper limit of the thermal conductivity of the silicon carbide block may be about 2,000 W/mK.
  • the above silicon carbide block can have anisotropic thermal conductivity.
  • the silicon carbide block can be arranged to have a thermal conductivity of about 10 W/mK or more in a horizontal direction.
  • the silicon carbide block can be arranged to have a thermal conductivity of about 20 W/mK or more in a horizontal direction.
  • the silicon carbide block can be arranged to have a thermal conductivity of about 30 W/mK or more in a horizontal direction.
  • the silicon carbide block can be arranged to have a thermal conductivity of about 40 W/mK or more in a horizontal direction.
  • the silicon carbide block can be arranged to have a thermal conductivity of about 50 W/mK or more in a horizontal direction.
  • the silicon carbide block can be arranged to have a thermal conductivity of about 70 W/mK or more in a horizontal direction.
  • the silicon carbide block can be arranged to have a thermal conductivity of about 100 W/mK or more in a horizontal direction.
  • the above silicon carbide block can be arranged to have a thermal conductivity of about 110 W/mK or more in the horizontal direction.
  • the upper limit of the thermal conductivity of the silicon carbide block in the horizontal direction can be about 2,000 W/mK. Since the silicon carbide block has a thermal conductivity in the above range, heat generated from the crucible body (31) can be efficiently transferred to the center of the internal space of the crucible body (11). Accordingly, the temperature gradient in the horizontal direction can be minimized inside the crucible body (11).
  • the diameter of the silicon carbide block may be substantially the same as the inner diameter of the crucible body (11).
  • the silicon carbide block may almost completely fill the lower portion of the crucible body (11). At least a portion of the outer surface of the silicon carbide block may be in direct contact with the inner surface of the crucible body (11). Of the outer surface of the silicon carbide block, a portion in contact with the inner surface of the crucible body (11) may be about 20% or more. When the crucible body (11) and the silicon carbide block are in partial contact, heat generated in the crucible body (11) can be easily transferred to the silicon carbide block.
  • the seed cell (31) in the above step S11 can be placed at the upper part of the internal space and can be placed facing each other with the silicon carbide raw material (20).
  • the above seed (30) may be any one of wafers to which an off-angle is applied, which is an angle selected in the range of 0 to 8 degrees with respect to the (0001) plane.
  • the above seed crystal (30) may be a substantially single-crystal 4H silicon carbide (SiC) ingot with minimal defects or polymorphic inclusions.
  • the above seed crystal (30) may be substantially made of 4H silicon carbide (SiC).
  • the seed well (30) may have a diameter of 4 inches or more, 5 inches or more, or 6 inches or more.
  • the seed well (30) may have a diameter of 4 to 12 inches, 4 to 10 inches, or 6 to 8 inches.
  • the seed crystal (30) may be bonded to a seed crystal holder (not shown).
  • the seed crystal holder may include graphite.
  • the seed crystal holder may be made of graphite.
  • the seed crystal holder may include anisotropic graphite and/or isotropic graphite.
  • the seed crystal holder (not shown) may be made of anisotropic graphite and/or isotropic graphite.
  • the seed holder may have high thermal conductivity.
  • the seed holder may have high thermal conductivity in a horizontal direction.
  • the seed holder may have thermal conductivity of at least about 100 W/mK in at least one direction.
  • the seed holder may have thermal conductivity of at least about 110 W/mK in at least one direction.
  • the seed holder may have thermal conductivity of at least about 120 W/mK in at least one direction.
  • the seed holder may have thermal conductivity of at least about 130 W/mK in at least one direction.
  • the seed holder may have thermal conductivity of at least about 140 W/mK in at least one direction.
  • the seed holder may have thermal conductivity of at least about 150 W/mK in at least one direction.
  • the crucible cover (12) and the seed holder may be formed integrally with each other.
  • the crucible cover (12) and the seed holder may be formed of graphite.
  • the crucible cover (12) and the seed holder may have a thermal conductivity of about 100 W/mK or more in at least one direction among the horizontal directions.
  • the crucible cover (12) and the seed holder may have a thermal conductivity of about 110 W/mK or more in at least one direction among the horizontal directions.
  • the crucible cover (12) and the seed holder may have substantially the same thermal conductivity according to the direction.
  • the seed electrode (30) and the seed electrode holder may be bonded to each other by an adhesive layer (not shown).
  • the adhesive layer may include a carbonized material such as a graphite filler and a phenol resin.
  • the adhesive layer may have a low porosity.
  • the seed electrode (30) may be arranged so that the C-side faces downward.
  • the above step S12 can seal the internal space of the reaction vessel (10).
  • the above reaction vessel (10) may include a crucible body (11) and a crucible cover (12).
  • the crucible body (11) may accommodate the silicon carbide raw material (20).
  • the above crucible body (11) may include graphite.
  • the above crucible body (11) may be made of graphite.
  • the above crucible body (11) may be a graphite crucible.
  • the above crucible body (11) may be a conductor.
  • the above crucible body (11) may be heated by the resistance heat induced by the above heating means (60).
  • the density of the crucible body (11) may be 1.70 g/cm3 to 1.90 g/cm3.
  • the density of the crucible body (11) may be 1.75 g/cm3 to 1.90 g/cm3.
  • the density of the crucible body (11) may be 1.75 g/cm3 to 1.85 g/cm3.
  • the above crucible cover (12) is placed on the upper part of the crucible body (11) and can cover the entrance of the crucible body (11).
  • the crucible cover (12) can have a circular plate shape.
  • the crucible cover (12) can completely cover the entrance of the crucible body (11).
  • the crucible cover (12) can have a shape corresponding to the entrance of the crucible body (11).
  • the thickness of the crucible cover (12) may be from about 10 mm to about 50 mm.
  • the thickness of the crucible cover (12) may be from about 15 mm to about 50 mm.
  • the thickness of the crucible cover (12) may be from about 15 mm to about 45 mm.
  • the density of the crucible cover (12) may be 1.70 g/cm3 to 1.90 g/cm3.
  • the density of the crucible cover (12) may be 1.75 g/cm3 to 1.90 g/cm3.
  • the density of the crucible cover (12) may be 1.75 g/cm3 to 1.85 g/cm3.
  • the above crucible cover (12) may include graphite.
  • the above crucible cover (12) may be substantially made of graphite.
  • the above crucible cover (12) may be applied to have a form that covers the entire opening of the above crucible body (11).
  • the above crucible cover (12) may be applied to cover a part of the opening of the crucible body (11) or may include a through hole (not shown).
  • the crucible body (11) and the crucible cover (12) may be assembled to form the reaction vessel (10).
  • the above step S13 can place an insulating material (40) surrounding the reaction vessel (10).
  • the above insulation (40) can affect the temperature gradient of the reaction vessel (10) or the internal space of the reaction vessel (10) in a colon growth atmosphere.
  • the above insulation (40) can include graphite insulation.
  • the above insulation (40) can include rayon-based graphite felt or pitch-based graphite felt.
  • the above insulation (40) may include a first insulation material wrapping the crucible body (11), and a second insulation material wrapping the crucible cover (12).
  • the first insulation material may form a gap of 0 mm to 10 mm with the crucible body (11).
  • the first insulation material may form a gap of 0 mm to 5 mm with the crucible body (11).
  • the first insulation material may form a gap of 0 mm to 3 mm with the crucible body (11).
  • the first insulation material may form a gap of 1 mm to 3 mm with the crucible body (11).
  • the gap may act as a buffer according to a change in the volume of the crucible body (11).
  • the second insulation material may be formed with a gap of 0 mm to 10 mm from the crucible cover (12).
  • the second insulation material may be formed with a gap of 0 mm to 5 mm from the crucible cover (12).
  • the second insulation material may be formed with a gap of 0 mm to 3 mm from the crucible cover (12).
  • the second insulation material may be formed with a gap of 1 mm to 3 mm from the crucible cover (12).
  • the gap may act as a buffer according to a change in the volume of the crucible cover (12).
  • At least some of the second insulating material may have a void space. By having the void space in the second insulating material, heat generated from the crucible can be smoothly dissipated.
  • the above insulation (40) may have a density of 0.12 g/cc to 0.30 g/cc.
  • the above insulation (40) may have a density of 0.13 g/cc to 0.25 g/cc.
  • the above insulation (40) may have a density of 0.14 g/cc to 0.20 g/cc.
  • the above insulation (40) may have a porosity of 73 vol% to 95 vol%.
  • the above insulation (40) may have a porosity of 76 vol% to 93 vol%.
  • the above insulation (40) may have a porosity of 81 vol% to 91 vol%.
  • the above insulation (40) may have a compressive strength of 0.21 MPa or more.
  • the above insulation (40) may have a compressive strength of 0.49 MPa or more.
  • the above insulation (40) may have a compressive strength of 0.78 MPa or more.
  • the above insulation (40) may have a compressive strength of 3 MPa or less.
  • the above insulation (40) may have a compressive strength of 2.5 MPa or less.
  • the thickness of the above insulation (40) may be 20 mm or more.
  • the thickness of the above insulation (40) may be 30 mm or more.
  • the thickness of the above insulation (40) may be 150 mm or less.
  • the thickness of the above insulation (40) may be 120 mm or less.
  • the thickness of the above insulation (40) may be 80 mm or less.
  • the above insulation material (40) may have a density of 0.12 g/cc to 0.30 g/cc and a porosity of 72 vol% to 90 vol%.
  • the shape of the silicon carbide ingot being manufactured can be suppressed from growing concavely or excessively convexly, and the phenomenon of polymorphic quality deteriorating or cracks occurring in the silicon carbide ingot can be reduced.
  • the above step S14 can place a heating means (60) outside the reaction vessel (10) and insulation material (40).
  • the reaction vessel (10) or the internal space of the reaction vessel (10) can be heated by the heating means (60).
  • the heating means (60) can move in the height direction (Y) of the reaction vessel and can include a plurality of coils (60) that generate an induced current in the reaction vessel (10).
  • the plurality of coils (60) can be formed along the outer surface of the insulation material (40).
  • the heating means (60) can move substantially parallel to the reaction vessel (10). Accordingly, the relative position between the heating means (60) and the reaction vessel (10) can be changed, so that a temperature gradient in the internal space of the reaction vessel (10) can be induced. In addition, a temperature difference can be generated between the upper temperature (T1) of the internal space and the lower temperature (T2) of the internal space by the heating means (60).
  • the distance (d2) between the coil (60) and the reaction vessel (10) may be 60 mm to 600 mm.
  • the distance (d2) between the coil (60) and the reaction vessel (10) may be 60 mm to 550 mm.
  • the distance (d2) between the coil (60) and the reaction vessel (10) may be 60 mm to 500 mm.
  • the distance (d2) between the coil (60) and the reaction vessel (10) may be 60 mm to 450 mm.
  • the distance (d2) means the distance from the outer surface of the reaction vessel (10) to the center point of the coil (60).
  • the diameter (r) of each of the plurality of coils (60) may be 5 mm to 40 mm, and the spacing (d1) between the plurality of coils (60) may be 5 mm to 30 mm.
  • the diameter (r) of each of the plurality of coils (60) may be 5 mm to 30 mm, and the spacing (d1) between the plurality of coils (60) may be 10 mm to 30 mm.
  • the diameter (r) of each of the plurality of coils (60) may be 5 mm to 20 mm, and the spacing (d1) between the plurality of coils (60) may be 10 mm to 30 mm.
  • the spacing (d1) refers to the distance between the center lines of the coils (60) adjacent to each other vertically.
  • the induced current of the coil (60) may be 1 ⁇ 10 4 A to 2 ⁇ 10 6 A.
  • the induced current of the coil (60) may be 1.5 ⁇ 10 4 A to 2 ⁇ 10 6 A.
  • the induced current of the coil (60) may be 1.5 ⁇ 10 4 A to 1.5 ⁇ 10 6 A.
  • the induced current of the coil (60) may be 1 ⁇ 10 5 A to 1.5 ⁇ 10 6 A.
  • the reaction vessel (10) and the insulation material (40) can be positioned in the reaction chamber (50).
  • the reaction chamber (50) is connected to the interior of the reaction chamber (50) and can include a vacuum exhaust device that controls the vacuum level of the interior of the reaction chamber (50).
  • the reaction chamber (50) is connected to the interior of the reaction chamber (50) and can include a pipe that introduces gas into the interior of the reaction chamber (50) and a mass flow controller that controls the introduction of the gas.
  • the above manufacturing method includes a first temperature-raising step (S20).
  • the S20 step is a step of raising the temperature of the internal space by the heating means (60) surrounding the reaction vessel (10).
  • step S20 may include a step of adjusting to a high vacuum atmosphere (S21), a step of injecting an inert gas into the internal space (S22), and a step of increasing the temperature of the internal space using a heating means (60) (S23).
  • the above S21 step can adjust the internal space of the reaction vessel (10) to a high vacuum atmosphere.
  • the S21 step can reduce the pressure of the internal space to 50 torr or less.
  • the S21 step can reduce the pressure of the internal space to 10 torr or less.
  • the S21 step can reduce the pressure of the internal space to 5 torr or less.
  • the S21 step can reduce the pressure of the internal space to 1 torr to 5 torr.
  • the above step S22 can inject an inert gas into the internal space of the reaction vessel (10).
  • the internal space can be substantially adjusted to the inert gas atmosphere.
  • the type of the inert gas may be argon (Ar), helium (He), nitrogen (N 2 ), or a mixed gas thereof.
  • the pressure of the internal space in the step S22 can be 500 torr to 800 torr.
  • the pressure of the internal space in the step S22 can be 600 torr to 800 torr.
  • the pressure of the internal space in the step S22 can be 650 torr to 800 torr.
  • the above step S23 may be a step of first increasing the temperature of the internal space using the heating means (60).
  • the first temperature increasing may be performed until the depressurization of the internal space begins.
  • the first temperature increasing may be performed at a rate of 1 °C/min to 10 °C/min.
  • the first temperature increasing may be performed at a rate of 3 °C/min to 10 °C/min.
  • the first temperature increasing may be performed at a rate of 5 °C/min to 10 °C/min.
  • the step S23 may be performed to increase the temperature so that the lower temperature (T2) of the internal space becomes about 1,500 °C to 1,700 °C.
  • the step S23 may be performed to increase the temperature so that the lower temperature (T2) of the internal space becomes about 1,550 °C to 1,700 °C.
  • the above step S23 can be performed by increasing the temperature so that the lower temperature (T2) of the internal space becomes about 1,550° C. to 1,650° C.
  • the difference between the upper temperature (T1) of the internal space and the lower temperature (T2) of the internal space can be maintained at 40° C. to 60° C.
  • the difference between the upper temperature (T1) of the internal space and the lower temperature (T2) of the internal space can be maintained at 45° C. to 60° C.
  • the difference between the upper temperature (T1) of the internal space and the lower temperature (T2) of the internal space can be maintained at 45° C. to 55° C.
  • the above manufacturing method includes a second temperature-elevating step (S30).
  • the S30 step is a step of secondarily heating the temperature of the internal space by the heating means (60) while depressurizing the internal space.
  • the meaning of the second temperature-elevating step may mean a temperature-elevating step that is distinct from the first temperature-elevating step in the S20 step.
  • the S30 step may be performed until the depressurization of the internal space is completed.
  • the S30 step may be a step of depressurizing the pressure of the internal space to reach a growth pressure and heating the temperature of the internal space to reach a growth temperature. By the S30 step, the ratio of carbon and silicon of the silicon carbide gas may be stabilized.
  • the above S30 step can be decompressed to a growth pressure of 1 torr to 50 torr.
  • the above S30 step can be decompressed to a growth pressure of 1 torr to 30 torr.
  • the above S30 step can be decompressed to a growth pressure of 1 torr to 10 torr.
  • the above S30 step can apply a difference between the upper temperature (T1) of the internal space and the lower temperature (T2) of the internal space by the coil (60).
  • Fig. 7 schematically illustrates the positions of the coils at step S30.
  • the plurality of coils (60) can be moved in the height direction of the reaction vessel (10).
  • the H0 is the total height of the reaction vessel (10)
  • the H1 refers to the height of the reaction vessel at a position corresponding to the center of the plurality of coils (60) based on the height direction of the reaction vessel (10).
  • the internal space of the reaction vessel (10) corresponding to the center of the plurality of coils (60) can be the maximum heating area.
  • the upper temperature (T1) of the internal space and the lower temperature (T2) of the internal space can be controlled according to the central positions of the plurality of coils (60).
  • the difference between the upper temperature (T1) of the internal space and the lower temperature (T2) of the internal space can be controlled by adjusting the central position of the plurality of coils (60).
  • the internal space includes an upper part where the seed crystal (30) is arranged and a lower part where the silicon carbide raw material (20) is arranged, and in the step S30, a difference between the upper temperature (T1) of the internal space and the lower temperature (T2) of the internal space is maintained at 50° C. to 100° C.
  • T1 of the internal space the upper temperature of the internal space
  • T2 of the internal space is maintained at 50° C. to 100° C.
  • the above S30 step may be performed at a heating rate of 1°C/min to 5°C/min.
  • the above S30 step may be performed at a heating rate of 2°C/min to 5°C/min.
  • the above S30 step may be performed at a heating rate of 2°C/min to 4°C/min.
  • the upper temperature (T1) of the internal space may be 2,200°C to 2,250°C. In the step S30, the upper temperature (T1) of the internal space may be 2,220°C to 2,250°C. In the step S30, the upper temperature (T1) of the internal space may be 2,225°C to 2,250°C. In the step S30, the upper temperature (T1) of the internal space may be 2,230°C to 2,250°C.
  • the lower temperature (T2) of the internal space may be 2,250 °C to 2,350 °C. In the step S30, the lower temperature (T2) of the internal space may be 2,270 °C to 2,350 °C. In the step S30, the lower temperature (T2) of the internal space may be 2,280 °C to 2,350 °C. In the step S30, the lower temperature (T2) of the internal space may be 2,280 °C to 2,320 °C.
  • step S30 the center position of the coil (60) according to the following equation 1 can satisfy 40% to 60%.
  • H0 is the total height of the reaction vessel
  • H1 is the height of the reaction vessel at a position corresponding to the center of the plurality of coils based on the height direction of the reaction vessel.
  • the center position of the coil (60) according to the above formula 1 can satisfy 41% to 59%, 45% to 59%, 45% to 58%, or 53% to 57%.
  • the phenomenon of seed crystal loss can be minimized, so that a silicon carbide ingot and wafer having substantially no defects and improved crystal quality can be manufactured.
  • the above manufacturing method includes a step of inducing growth of a silicon carbide ingot (S40).
  • the step S40 is a step of inducing growth of a silicon carbide ingot (31) under the decompressed pressure after the depressurization of the internal space is completed.
  • the step S40 may be a step of maintaining the internal space at a constant temperature and a constant pressure and inducing growth of the silicon carbide ingot (31).
  • the step S40 is performed by sublimating the silicon carbide raw material (20) after the temperature is increased to the temperature of the step S30, thereby forming the silicon carbide ingot (31).
  • Fig. 8 schematically illustrates the positions of the coils at step S40. Referring to Fig. 8, after step S30, the plurality of coils (60) can be moved downwards in the reaction vessel (10).
  • step S40 the plurality of coils (60) are moved downward in the reaction vessel (10), so that the difference between the upper temperature (T1) of the internal space and the lower temperature (T2) of the internal space can increase compared to the step S30.
  • the difference between the upper temperature (T1) of the internal space and the lower temperature (T2) of the internal space can be maintained at 50 °C to 200 °C.
  • the temperature in the step S40 is adjusted to a specific temperature range different from that in the step S30, thereby increasing the deposition rate of the silicon carbide gas in the seed crystal (30), and thus the growth rate of the silicon carbide ingot (31) can be improved.
  • the above S40 step can be performed for 5 hours to 180 hours.
  • the above S40 step can be performed for 30 hours to 160 hours.
  • the above S40 step can be performed for 50 hours to 150 hours.
  • the upper temperature (T1) of the internal space may be 2,000 °C to 2,250 °C. In the step S40, the upper temperature (T1) of the internal space may be 2,050 °C to 2,250 °C. In the step S40, the upper temperature (T1) of the internal space may be 2,100 °C to 2,250 °C. In the step S40, the upper temperature (T1) of the internal space may be 2,100 °C to 2,220 °C.
  • the lower temperature (T2) of the internal space may be 2,250 °C to 2,350 °C. In the step S40, the lower temperature (T2) of the internal space may be 2,270 °C to 2,350 °C. In the step S40, the lower temperature (T2) of the internal space may be 2,280 °C to 2,350 °C. In the step S40, the lower temperature (T2) of the internal space may be 2,280 °C to 2,320 °C.
  • the center position of the coil according to the above formula 1 can satisfy 20% to 50%, 22% to 50%, or 22% to 48%.
  • the deposition rate of the silicon carbide gas on the seed crystal (30) increases, so that the growth rate of the silicon carbide ingot (31) can be improved.
  • the above manufacturing method includes a cooling step (S50).
  • Fig. 4 is a flowchart specifically showing step S50.
  • the S50 step may include a step of first cooling while pressurizing the internal space (S51), a step of second cooling the temperature of the internal space to room temperature (S52), and a step of recovering the silicon carbide ingot (S53).
  • the above S51 step can be performed while pressurizing the internal space of the reaction vessel (10) to a maximum pressure of 800 torr.
  • the S51 step can be performed while pressurizing the internal space of the reaction vessel (10) to a pressure higher than atmospheric pressure.
  • the S51 step can be performed at a cooling rate of 1°C/min to 10°C/min.
  • the S51 step can be performed at a cooling rate of 3°C/min to 9°C/min.
  • the S51 step can be performed at a cooling rate of 5°C/min to 8°C/min.
  • the above step S51 can add a predetermined flow rate of an inert gas into the reaction vessel (10).
  • the inert gas can flow in the internal space of the reaction vessel (10), and the flow can be formed in the direction of the silicon carbide raw material (20) toward the seed (30).
  • the above step S52 may be a step of cooling the temperature of the internal space of the reaction vessel (10) to room temperature.
  • the recovery of the silicon carbide ingot (31) in the above step S53 may be performed by cutting the rear surface of the silicon carbide ingot (31) in contact with the seed hole (30).
  • the above silicon carbide ingot (31) may contain 4H SiC.
  • the surface of the above silicon carbide ingot (31) may have a convex shape or a flat shape.
  • the surface of the above silicon carbide ingot (31) is formed in a concave shape, other polymorphs such as 6H-SiC may be mixed in addition to the intended 4H-SiC crystal, which may deteriorate the quality of the silicon carbide ingot (31). If the surface of the above silicon carbide ingot (31) is formed in an excessively convex shape, cracks may occur in the silicon carbide ingot (31) itself, or the crystal may be broken when processed into a wafer.
  • the warpage of the silicon carbide ingot (31) manufactured according to the manufacturing method of the present invention may be 20 mm or less.
  • the above warpage can be evaluated by placing a sample of the silicon carbide ingot (31) on which growth is completed on a platen and measuring the height of the center and edge of the ingot based on the rear surface of the ingot with a height gauge (center height - edge height).
  • a positive value of the warpage value indicates convexity, a value of 0 indicates flatness, and a negative value indicates concaveness.
  • the above silicon carbide ingot (31) may have a convex or flat surface and may have a warpage of 0 mm to 14 mm.
  • the above silicon carbide ingot (31) may have a warpage of 0 mm to 11 mm.
  • the above silicon carbide ingot (31) may have a warpage of 0 mm to 8 mm.
  • the above silicon carbide ingot (31) may be a substantially single crystal 4H SiC ingot with minimal defects or polymorphism.
  • the above silicon carbide ingot (31) is substantially made of 4H SiC, and its surface may have a convex shape or a flat shape.
  • the above silicon carbide ingot (31) can provide a silicon carbide wafer of higher quality by reducing defects that may occur in the silicon carbide ingot.
  • the silicon carbide ingot (31) manufactured according to the manufacturing method of the present invention can reduce pits on its surface, and for example, in an ingot having a diameter of 4 inches or more, the pits included in its surface can be 10 k/cm2 or less.
  • the surface pit measurement of the above silicon carbide ingot (31) can be evaluated by observing a total of five locations, one location in the central portion of the surface of the ingot excluding the facets, and four locations in the 3 o'clock, 6 o'clock, 9 o'clock, and 12 o'clock directions located about 10 mm inside the central portion from the edge of the ingot, using an optical microscope, and measuring the pit per unit area (1 cm2) at each location, and then taking the average value.
  • the above silicon carbide ingot (31) may have a wafer whose locking angle is obtained by applying an off-angle of 0 degrees to the (0001) plane from the ingot to a reference angle of -1.0 to +1.0 degrees, -0.5 to +0.5 degrees, or -0.1 to +0.1 degrees. When the above range is satisfied, the silicon carbide ingot (31) may have excellent crystal characteristics.
  • the above rocking angle is measured by applying a high-resolution X-ray diffraction analysis system (HR-XRD system) to align the wafer [11-20] direction to the X-ray path, setting the angle between the X-ray source optic and the X-ray detector optic to 2 ⁇ (35 to 36 degrees), and then adjusting the omega ( ⁇ ) or theta ( ⁇ ) angle to match the off-angle of the wafer to measure the rocking curve, and setting the difference between the peak angle, which is the reference angle, and the two FWHM values as the rocking angle, respectively, so that the crystallinity can be evaluated.
  • HR-XRD system high-resolution X-ray diffraction analysis system
  • the silicon carbide ingot (31) can be processed by applying external grinding equipment to trim the outer edge of the ingot (External Grinding), cutting it to a certain thickness (Slicing), and then edge grinding, surface grinding, and polishing.
  • the above cutting step may be a step of slicing the silicon carbide ingot (31) to have a certain off-angle to prepare a sliced crystal.
  • the off-angle is based on the [0001] plane in 4H SiC.
  • the off-angle may be an angle selected from 0 to 15 degrees.
  • the off-angle may be an angle selected from 0 to 12 degrees.
  • the off-angle may be an angle selected from 0 to 8 degrees.
  • the above cutting step can be applied without limitation to any slicing method that is commonly applied to wafer manufacturing. For example, cutting using a diamond wire or a wire to which diamond slurry is applied, cutting using a blade or wheel to which diamond is partially applied, etc. can be applied.
  • the thickness of the above-mentioned sliced crystal can be adjusted in consideration of the thickness of the wafer to be manufactured, and can be sliced to an appropriate thickness in consideration of the thickness after polishing in the polishing step described later.
  • the above polishing step may be a step of polishing the sliced crystal to a thickness of 300 um to 800 um to form a silicon carbide wafer.
  • the above polishing step may be applied to a polishing method that is typically applied to wafer manufacturing.
  • a method in which polishing is performed after processes such as lapping and/or grinding are performed may be applied.
  • silicon carbide raw material (20) was charged into the inner space of a reaction vessel (10) having a height of 220 mm, and a seed hole (30) was placed on the upper part of the inner space.
  • the seed hole (30) was made of a 6-inch 4H-SiC crystal, and was fixed so that the C plane ((0001) plane) faced the silicon carbide raw material (20).
  • the crucible body (11) was covered using a crucible cover (12), and the outside was surrounded with an insulating material (40), and then a coil (60), which is a heating means, was placed on the outside.
  • a coil which is a heating means
  • the coil (60) was placed such that the distance (d2) from the reaction vessel was about 60 mm, the diameter (r) was about 20 mm, and the spacing (d1) between the coils was about 25 mm. Additionally, the induced current of the coil (60) was set to about 1.5 ⁇ 10 5 A.
  • the internal space of the above reaction vessel (10) was depressurized to adjust to a vacuum atmosphere, and argon (Ar) gas was injected so that the internal space reached 760 torr. Thereafter, the temperature was first increased at a rate of 10 °C/min to approximately 1600 °C based on the lower temperature (T2) of the internal space.
  • the internal space was depressurized and the temperature was increased for the second time at a rate of 4°C/min to 5°C/min, and at this time, the center position of the coil (60), the upper temperature (T1) of the internal space, the lower temperature (T2) of the internal space, and the difference between the upper temperature (T1) and the lower temperature (T2) of the internal space were set to the conditions shown in Table 1 below.
  • the central position of the coil (60) was changed to grow a silicon carbide ingot (31) on the surface of the seed cell (30) for about 100 hours.
  • the central position of the coil (60), the upper temperature (T1) of the internal space, the lower temperature (T2) of the internal space, and the difference between the upper temperature (T1) and the lower temperature (T2) of the internal space were set to the conditions shown in Table 1 below.
  • the temperature of the internal space was cooled to 25°C at a rate of 5°C/min, and at the same time, argon (Ar) gas was injected so that the pressure of the internal space became 760 torr, and the silicon carbide ingot formed in the seed hole (30) was recovered.
  • the outer surface of the silicon carbide ingot was ground to about 5% of the maximum outer diameter to process it into a cylindrical shape with a uniform outer diameter, and then cut to have an off angle of about 4° with respect to the (0001) plane of the silicon carbide ingot, to manufacture a wafer sample with a thickness of 360 ⁇ m.
  • Silicon carbide ingot and wafer samples were manufactured by the same process as Example 1, except that the silicon carbide ingot was manufactured under the conditions shown in Table 1 below.
  • Example 1 The surfaces of the silicon carbide ingots manufactured in Example 1 and Comparative Examples 1 and 2 were photographed using an optical microscope (Eclipse LV150, Nikon). The photograph of Example 1 is shown in Fig. 9, the photograph of Comparative Example 1 is shown in Fig. 10, and the photograph of Comparative Example 2 is shown in Fig. 11.
  • each of the wafer samples manufactured in Examples 1 to 6 and Comparative Examples 1 to 4 was cut to a size of 50 mm ⁇ 50 mm, and then etched by immersing in potassium hydroxide (95%) at a temperature of 600 ° C. for 3 minutes. Thereafter, the surface of the etched wafer sample was photographed using the optical microscope (Eclipse LV150, Nikon).
  • the photograph of Example 1 is shown in FIG. 12, the photograph of Comparative Example 1 is shown in FIG. 13, and the photograph of Comparative Example 2 is shown in FIG. 14.
  • an area of 500 ⁇ 500 ⁇ m on the surface of the wafer sample was arbitrarily designated 12 times, and the number of defects in each area was determined, and the average number of defects per unit area was calculated, and the results are shown in Table 2 below.
  • EPD 1 Growth rate Seed loss assessment unit Number of defects/cm 2 ⁇ m/h - Example 1 8,560 240 Good Example 2 8,230 240 Good Example 3 8,540 240 Good Example 4 8,630 245 Good Example 5 8,620 245 Good Example 6 8,960 250 Good Comparative Example 1 35,880 175 error Comparative Example 2 25,660 250 error Comparative Example 3 29,810 180 error Comparative Example 4 55,340 265 error 1)
  • Examples 1 to 6 in which the difference between the upper temperature of the internal space and the lower temperature of the internal space was set to 50 °C to 100 °C showed significantly reduced defects and no loss of seed crystals compared to Comparative Examples 1 to 4. More specifically, looking at the surface photograph of the silicon carbide ingot of Example 1 (Fig. 9), it was confirmed that the defects were significantly reduced compared to the surface photograph of the silicon carbide ingot of Comparative Example 1 (Fig. 10) and the surface photograph of the silicon carbide ingot of Comparative Example 2 (Fig. 11).
  • the embodiment can be applied to a method for manufacturing a silicon carbide ingot.

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Abstract

La présente invention comprend les étapes consistant à : agencer une matière première de carbure de silicium et un germe cristallin dans une cuve de réaction présentant un espace interne ; premièrement, élever la température de l'espace interne par un moyen de chauffage entourant la cuve de réaction ; deuxièmement, élever la température de l'espace interne par le moyen de chauffage tout en décompressant l'espace interne ; induire la croissance d'un lingot de carbure de silicium dans la condition de pression réduite après la fin de la réduction de pression de l'espace interne ; refroidir la température de l'espace interne à la température ambiante, l'espace interne comprenant une partie supérieure dans laquelle le germe cristallin est disposé et une partie inférieure dans laquelle la matière première de carbure de silicium est disposée et, dans la deuxième étape d'élévation de température, une différence entre la température supérieure de l'espace interne et la température inférieure de l'espace interne étant maintenue à 50 °C jusqu'à 100 °C.
PCT/KR2024/012391 2023-10-25 2024-08-21 Procédé de fabrication d'un lingot de carbure de silicium Pending WO2025089583A1 (fr)

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Citations (5)

* Cited by examiner, † Cited by third party
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