WO2024254789A1 - 一种晶体制备方法 - Google Patents

一种晶体制备方法 Download PDF

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Publication number
WO2024254789A1
WO2024254789A1 PCT/CN2023/100230 CN2023100230W WO2024254789A1 WO 2024254789 A1 WO2024254789 A1 WO 2024254789A1 CN 2023100230 W CN2023100230 W CN 2023100230W WO 2024254789 A1 WO2024254789 A1 WO 2024254789A1
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Prior art keywords
crystal
wafer
seed
cut
treatment
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PCT/CN2023/100230
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English (en)
French (fr)
Inventor
王宇
顾鹏
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Meishan Boya Advanced Materials Co Ltd
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Meishan Boya Advanced Materials Co Ltd
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Priority to PCT/CN2023/100230 priority Critical patent/WO2024254789A1/zh
Priority to CN202380097484.3A priority patent/CN121057849A/zh
Priority to TW113115531A priority patent/TWI911720B/zh
Publication of WO2024254789A1 publication Critical patent/WO2024254789A1/zh
Priority to US19/412,791 priority patent/US20260092396A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • C30B23/02—Epitaxial-layer growth
    • C30B23/025—Epitaxial-layer growth characterised by the substrate
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B19/00—Liquid-phase epitaxial-layer growth
    • C30B19/02—Liquid-phase epitaxial-layer growth using molten solvents, e.g. flux
    • C30B19/04—Liquid-phase epitaxial-layer growth using molten solvents, e.g. flux the solvent being a component of the crystal composition
    • 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
    • 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
    • C30B29/02—Elements
    • C30B29/06—Silicon
    • 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
    • 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
    • C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • C30B29/403—AIII-nitrides
    • 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
    • C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • C30B33/06—Joining of crystals
    • 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
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/005—Epitaxial layer growth

Definitions

  • the present invention relates to the technical field of crystal preparation, and in particular to a method for preparing a crystal.
  • PVT Physical Vapor Transport
  • the top seeded solution growth method can be used to prepare high-quality silicon carbide crystals because of its low growth temperature and close to thermodynamic equilibrium conditions.
  • the thickness of crystals prepared by the TSSG method is limited and cannot meet the needs of industrial production.
  • One or more embodiments of the present specification provide a crystal preparation method, the method comprising: obtaining a first wafer after a first treatment; using the first wafer after the first treatment as a first seed crystal, and growing a prefabricated crystal based on a top seed crystal solution growth method; performing a second treatment on the prefabricated crystal; using the prefabricated crystal after the second treatment as a second seed crystal, and growing a target crystal based on a physical vapor transport method.
  • One or more embodiments of the present specification provide a method for preparing a seed crystal, the method comprising: radially cutting an off-axis seed crystal to obtain at least two seed crystals; splicing the at least two seed crystals so that the step directions of the at least two seed crystals after splicing are opposite to each other, to obtain a target seed crystal.
  • FIG. 1 is an exemplary flow chart of a crystal preparation method according to some embodiments of the present specification.
  • FIG. 2 is an exemplary schematic diagram of a crystal preparation method according to some embodiments of the present specification.
  • FIG. 3A is an exemplary schematic diagram of performing a first process on an off-axis wafer according to some embodiments of the present specification.
  • FIG. 3B is an exemplary top view of the first wafer 2 after being cut in FIG. 3A .
  • FIG. 3C is an exemplary schematic diagram showing that a step direction of a first seed crystal is opposite to a solution flow direction according to some embodiments of the present specification.
  • FIG. 4A is an exemplary cross-sectional view of a second wafer according to some embodiments of the present disclosure.
  • FIG. 4B is an exemplary cross-sectional view of a second wafer according to some other embodiments of the present specification.
  • FIG. 4C is an exemplary cross-sectional view of a second wafer according to some other embodiments of the present specification.
  • FIG. 5 is an exemplary schematic diagram of an immersion angle according to some embodiments of the present specification.
  • 210 is the first wafer after the first treatment
  • 220 is the crystal growth layer
  • 230 is the crystal growth layer after the second treatment
  • 240 is the target crystal growth layer
  • 310 is the off-axis wafer
  • 320 is the first wafer after cutting
  • 321, 321-1 are the first wafer one after cutting
  • 322, 322-1, 322-2, 322-3 are the first wafer two after cutting
  • 330 is the first seed crystal
  • 400 is the second wafer
  • 410 is the groove.
  • Some embodiments of the present specification provide a crystal preparation method, in which a first wafer after a first treatment is used as a first seed crystal, and a high-quality prefabricated crystal is grown based on a top seed crystal solution growth method; and a prefabricated crystal after a second treatment is used as a second seed crystal, and a large-sized, high-quality target crystal is grown based on a physical vapor transport method.
  • FIG. 1 is an exemplary flow chart of a crystal preparation method according to some embodiments of this specification.
  • process 100 can be performed by one or more components.
  • process 100 can be automatically performed by a control system.
  • process 100 can be implemented by a control instruction, and the control system controls each component to complete each operation of process 100 based on the control instruction.
  • process 100 can be performed semi-automatically.
  • one or more operations of process 100 can be performed manually by an operator.
  • one or more additional operations not described can be added, and/or one or more operations discussed herein can be deleted.
  • process 100 can include the following steps.
  • Step 110 obtaining a first wafer after a first process.
  • the first treatment may include, but is not limited to, grinding and/or polishing the first wafer.
  • grinding may refer to processing the surface of the first wafer by relative movement of a grinding tool and the first wafer under a preset pressure.
  • the surface of the grinding tool may be coated with or pressed with abrasive particles.
  • polishing may refer to processing the surface of the first wafer using a polishing medium to reduce its roughness so as to make its surface flat.
  • the polishing medium may be a polishing medium. Gloss powder.
  • the first process may further include cutting, etc.
  • the first wafer may be grown by a PVT method.
  • the first wafer may include, but is not limited to, a silicon carbide wafer, an aluminum nitride wafer, or the like.
  • the defect density of the first wafer prepared by the PVT method is relatively high, so the first wafer needs to be subjected to a first treatment to make the surface of the first wafer obtained after the first treatment smoother and reduce the defect density of the first wafer.
  • the material of the seed crystal holder may include but is not limited to graphite.
  • the thickness of the first wafer after the first treatment needs to be greater than the first thickness threshold.
  • the first thickness threshold and the second thickness threshold can be empirical values or preset values.
  • the thickness of the first wafer after the first treatment may be 0.35mm-10mm. In some embodiments, the thickness of the first wafer after the first treatment may be 0.5mm-9.5mm. In some embodiments, the thickness of the first wafer after the first treatment may be 1mm-9mm. In some embodiments, the thickness of the first wafer after the first treatment may be 1.5mm-8.5mm. In some embodiments, the thickness of the first wafer after the first treatment may be 2mm-8mm. In some embodiments, the thickness of the first wafer after the first treatment may be 2.5mm-7.5mm. In some embodiments, the thickness of the first wafer after the first treatment may be 3mm-7mm. In some embodiments, the thickness of the first wafer after the first treatment may be 3.5mm-6.5mm. In some embodiments, the thickness of the first wafer after the first treatment may be 4mm-6mm. In a In some embodiments, the thickness of the first wafer after the first processing may be 4.5 mm-5.5 mm.
  • the thickness of the first wafer after the first treatment by controlling the thickness of the first wafer after the first treatment, it can not only ensure that it has a certain thickness for the dissolution of the first seed crystal during the process of preparing prefabricated crystals by the TSSG method as the first seed crystal, but also prevent the solution from climbing to the back of the first seed crystal and reacting with the seed crystal holder, and can also ensure that the first seed crystal will not fall off the seed crystal holder due to its heavy weight.
  • the first treatment may also include radial cutting of the first wafer to obtain at least two cut first wafers; and splicing the at least two cut first wafers so that the steps of the at least two cut first wafers after splicing are opposite in direction. In this way, when the at least two cut first wafers after splicing are used as the first seed crystal for preparing prefabricated crystals by the TSSG method, the solution flow direction is opposite to the step direction of the first seed crystal.
  • FIG. 2 is an exemplary schematic diagram of a crystal preparation method according to some embodiments of the present specification.
  • FIG. 3A is an exemplary schematic diagram of a first treatment of an off-axis wafer according to some embodiments of the present specification.
  • FIG. 3B is an exemplary top view of the first wafer 2 after cutting in FIG. 3A.
  • FIG. 3C is an exemplary schematic diagram of a step direction of a first seed crystal opposite to a solution flow direction according to some embodiments of the present specification.
  • the off-axis wafer 310 can be radially cut to obtain two cut first wafers 320.
  • radial cutting can refer to cutting along the diameter direction or the direction perpendicular to the axis. As shown in FIG2, radial cutting can be represented by double arrows ab.
  • An off-axis wafer refers to a wafer in which the crystallographic c-axis (longest axis) is deflected by a preset angle in the crystal direction. In some embodiments, the off-axis wafer can be obtained by machining the wafer (for example, cutting or beveling).
  • the step direction of the off-axis wafer is always along a single direction. As shown in FIG3A, the off-axis wafer 310 The steps are in the same direction and all point to one side. Therefore, in order to achieve a solution flow direction opposite to the direction of all the steps of the first seed crystal, at least two cut first wafers 320 need to be spliced.
  • At least two cut first wafers 320 can be spliced in a variety of ways, so that the steps of the at least two cut first wafers 320 after splicing are in opposite directions.
  • one of the cut first wafers for example, the cut first wafer 1 321 shown in FIG. 3A
  • the other cut first wafer for example, the cut first wafer 2 322 shown in FIG. 3A
  • the mirror transformation can include a 180° rotation with a certain axis (for example, a certain side line, a vertical central axis, or a horizontal central axis of the cut first wafer 2) as the axis.
  • the first process may further include rotating and/or flipping at least one of the at least two cut first wafers 320.
  • the rotation process and/or flipping process may include rotating at a preset angle with a certain axis (e.g., a certain edge line, a vertical center axis, or a horizontal center axis of the cut first wafer) as the rotation axis.
  • a certain axis e.g., a certain edge line, a vertical center axis, or a horizontal center axis of the cut first wafer
  • the off-axis wafer 310 may be radially cut to obtain a cut first wafer 1 321 and a cut first wafer 2 322.
  • the step directions of the cut first wafer 1 321 and the cut first wafer 2 322 in the two spliced cut first wafers are opposite.
  • the two spliced cut first wafers are used as
  • the step direction is opposite to the solution flow direction (it can be understood that step B blocks the solution flow or the solution flow collides with step B).
  • Step B can be understood as a cut parallel to the axis of the first seed crystal 330.
  • the embodiment of this specification does not limit the shape of the eccentric wafer 310, for example, it can be a cuboid, a cube, a cylinder, etc.
  • the eccentric wafer 310 can be a cuboid.
  • the cross-section of the eccentric wafer 310 can be a regular or irregular shape such as a polygon (for example, a rectangle, a square), a circle, an ellipse, etc.
  • the shape can also be changed by cutting the edges of at least two cut first wafers after splicing.
  • the cuboid first seed crystal 330 shown in Figure 3A can be cut to obtain a cylindrical seed crystal.
  • the first chip (also referred to herein as the eccentric chip 310) is a cylinder
  • two cylindrical first chips with opposite step directions can be radially cut respectively, and then the two cut first chips with opposite step directions can be spliced together to obtain two cut first chips with opposite step directions, and the two spliced cut first chips are cylinders.
  • the first wafer is radially cut and at least two cut first wafers are spliced so that the steps of the at least two spliced first wafers are in opposite directions.
  • the step direction of the first seed crystal is opposite to the flow direction of the solution, and the step aggregation behavior can be significantly suppressed, which is beneficial to reduce microscopic defects and macroscopic defects, improve the quality of the prepared prefabricated crystal, and make the overall morphology of the crystal smoother.
  • the solution will rise along the splicing gap under the action of capillary force until it contacts the seed crystal holder and reacts, resulting in a lower quality of the prepared prefabricated crystal.
  • the at least two cut first wafers can be bonded to the second crystal holder.
  • the cut first wafer 1 321 and the cut first wafer 2 322 are spliced to obtain two spliced cut first wafers (also referred to as first seed crystals 330 ), and the first seed crystals 330 can be bonded to one side of the second wafer 400 , and the other side of the second wafer 400 can be bonded to the seed crystal holder A .
  • the second wafer 400 may be located between the first seed crystal 330 and the seed crystal holder A, and is used to bond the first seed crystal 330 and the seed crystal holder A.
  • the second wafer 400 may include an equiaxial wafer or an eccentric wafer, etc.
  • the material of the second wafer 400 may be the same as or different from that of the first seed crystal 330.
  • the shape of the second wafer 400 may be the same as or different from that of the first seed crystal 330.
  • the at least two cut first wafers after splicing can be bonded to the second wafer by thermal bonding.
  • the bonding of the at least two cut first wafers after splicing and the second wafer can also be achieved by other methods. For example, adhesive bonding, etc.
  • the bonding method of the second wafer and the seed crystal holder can be the same as or different from the bonding method of the at least two cut first wafers (also referred to as first seed crystals) after splicing and the second wafer.
  • first seed crystals also referred to as first seed crystals
  • second wafer by bonding at least two cut first wafers (also referred to as first seed crystals) after splicing to one side of a second wafer, and then bonding the other side of the second wafer to a seed crystal holder, it is possible to avoid direct contact and reaction between the solution and the seed crystal holder through the splicing gap during the process of preparing a prefabricated crystal from the first seed crystal based on the TSSG method, which is beneficial to improving the quality of the prepared prefabricated crystal.
  • a groove may be provided at a preset height on the second wafer to further reduce the amount of solution climbing to the surface of the seed crystal holder.
  • the preset height may refer to the distance between the lowest end of the groove of the second wafer and the lower bottom surface of the second wafer.
  • the preset height may be a preset value or a default value, etc.
  • the groove may include a variety of structures, for example, an annular structure.
  • the longitudinal section of the groove may be of any shape, for example, a regular or irregular shape such as a polygon or a circle.
  • the groove depth may refer to the distance between the farthest end of the groove and the side of the second wafer.
  • the groove inclination may refer to the angle between the inclined edge of the groove and the horizontal plane.
  • the second wafer 400 is provided at a preset height (shown as h1 in FIG. 4A )
  • a preset height shown as h1 in FIG. 4A
  • annular groove 410 with a rectangular longitudinal section The depth of the groove 410 (which can be understood as the length of the rectangle) can be expressed as L1 in Figure 4A.
  • an annular groove 410 with a parallelogram longitudinal section is provided at a preset height of the second wafer 400 (as shown in h2 in Figure 4B).
  • the depth of the groove 410 can be expressed as L2 in Figure 4B, and the inclination of the groove 410 is ⁇ .
  • annular groove 410 with a semicircular longitudinal section is provided at a preset height of the second wafer 400 (as shown in h3 in Figure 4C).
  • the depth of the groove 410 (which can also be understood as the radius of the semicircle) can be expressed as L3 in Figure 4C.
  • the at least two cut first wafers after splicing are used as the first seed crystal, in order to allow the solution to better infiltrate the entire splicing gap under the action of surface tension, the solution is allowed to grow crystals at the splicing gap to close the entire splicing gap.
  • the first treatment may also include performing a third treatment on the at least two cut first wafers after splicing, so that the at least two cut first wafers form an immersion angle near one end of the splicing gap.
  • the third treatment may include cutting at least two cut first wafers at one end (e.g., growth end) close to the joint gap to form an immersion angle.
  • the cut first wafer 1 321 and the cut first wafer 2 322 may be cut at one end (e.g., growth end) close to the joint gap to obtain the cut first wafer 1 321-1 after the third treatment and the cut first wafer 2 322-3 after the third treatment, which may then be spliced to form the first seed crystal 330.
  • the immersion angle ⁇ may be formed at the joint gap of the first seed crystal 330.
  • the immersion angle is to allow the solution of the first seed crystal to better penetrate into the splicing gap during the TSSG method of growing crystals, so that the splicing gap grows and closes.
  • the immersion angle can be a variety of structures. For example, a cylinder, a cone, a polyhedron, etc.
  • the longitudinal section of the immersion angle can be a polygon, a triangle (as shown in Figure 5), etc.
  • the longitudinal section of the immersion angle can also be any other shape that can increase the capillary force of the solution at the splicing gap.
  • the splicing gap can be a cone, and the bottom circle of the cone is close to one end of the step.
  • the radius of the splicing gap can be understood as the radius of the bottom circle of the cone, and the immersion angle can be understood as the top angle of the cone.
  • the length of the solution immersed in the splicing gap can be calculated by the formula Calculated.
  • H is the length of the splicing gap (i.e., The thickness of the first wafer after the first treatment);
  • ⁇ is the surface tension of the liquid (which can be understood as the raw material melt) in the TSSG method;
  • ⁇ is the density of the liquid;
  • g is the gravitational acceleration;
  • r is the radius of the splicing gap;
  • ⁇ is the wetting angle between the liquid and the seed crystal (for example, the first seed crystal).
  • the immersion angle ⁇ may be greater than 0° and less than 20°. In some embodiments, the immersion angle ⁇ may be greater than 2° and less than 18°. In some embodiments, the immersion angle ⁇ may be greater than 4° and less than 16°. In some embodiments, the immersion angle ⁇ may be greater than 6° and less than 14°. In some embodiments, the immersion angle ⁇ may be greater than 8° and less than 12°. In some embodiments, the immersion angle ⁇ may be greater than 9° and less than 10°.
  • an immersion angle is formed at one end of the at least two cut first wafers after splicing close to the splicing gap, which is beneficial to enhancing the capillary force of the solution, allowing the solution to better penetrate the splicing gap and close the splicing gap through crystal growth.
  • Step 120 using the first wafer after the first treatment as a first seed crystal, and growing a prefabricated crystal based on a top seed crystal solution growth method.
  • the top seed solution growth method refers to a method in which the raw material for preparing the crystal (for example, silicon carbide powder) is dissolved in a low melting point flux at high temperature to form a uniform saturated solution, and then a supersaturated melt is formed by slowly cooling the temperature to precipitate the crystal on the seed crystal.
  • the raw material for preparing the crystal for example, silicon carbide powder
  • Preformed crystal refers to an intermediate crystal prepared by the TSSG method.
  • the other side of the second wafer is bonded to the seed crystal holder, and a prefabricated crystal is grown by a top seed solution growth method.
  • a top seed solution growth method As an example only, as shown in FIG2 , the first wafer 210 after the first treatment is used as the first seed crystal, and a crystal growth layer 220 with a preset thickness is prepared based on the TSSG method.
  • the first wafer 210 after the first treatment and the crystal growth layer 220 can be referred to as a prefabricated crystal.
  • the TSSG method is used to prepare the crystal growth layer by using a TSSG method.
  • the TSSG method is used to prepare the crystal growth layer by using a TSSG method.
  • the TSSG method is used to prepare the crystal growth layer by using a TSSG method.
  • the TSSG method is used to prepare the crystal growth layer by using a TSSG method.
  • the TSSG method is used to prepare the crystal growth layer by using a TSSG method.
  • the TSSG method is used to prepare the crystal growth layer by using a TSSG method.
  • the TSSG method is used to prepare the crystal growth layer by using a TSSG method.
  • the TSSG method is used to prepare the crystal growth layer by using a TSSG method.
  • the TSSG method is used to prepare the crystal growth layer by using a TSSG method.
  • the TSSG method is used to prepare the crystal growth layer by using a TSSG method.
  • the TSSG method is used to prepare the crystal growth layer by using a TSSG method.
  • the TSSG method is used to prepare the crystal growth layer by using a TSSG method.
  • the TSSG method is used to prepare the crystal growth layer by using a TSSG method.
  • the TSSG method is used to prepare the crystal growth layer by using a TSSG method.
  • the prefabricated crystal with a preset thickness can ensure that the prefabricated crystal can be subsequently subjected to a second treatment.
  • Step 130 performing a second treatment on the prefabricated crystal.
  • the second treatment may include, but is not limited to, grinding and/or polishing the prefabricated crystal or its crystal growth layer.
  • the prefabricated crystal or its crystal growth layer can be subjected to a second treatment in a variety of ways.
  • the surface of the crystal growth layer 220 can be processed by relative movement of the grinding tool and the crystal growth layer 220 under a preset pressure to improve its surface smoothness and flatness, reduce surface defects, and obtain a crystal growth layer 230 after the second treatment.
  • the second treatment method may be the same as or different from the first treatment method.
  • the first wafer 210 after the first treatment and the crystal growth layer 230 after the second treatment can be referred to as a prefabricated crystal after the second treatment.
  • the surface roughness of the second seed crystal may be no greater than 0.2 nm. In some embodiments, the surface roughness of the second seed crystal may be no greater than 0.15 nm. In some embodiments, the surface of the second seed crystal may be no greater than 0.15 nm. The roughness may be no greater than 0.1 nm. In some embodiments, the surface roughness of the second seed crystal may be no greater than 0.05 nm.
  • the smoothness of the surface of the second seed crystal can be ensured, the quality of the second seed crystal can be improved, and it is beneficial to further improve the quality of the target crystal subsequently prepared by the PVT method.
  • Step 140 Use the prefabricated crystal after the second treatment as a second seed crystal and grow the target crystal based on the physical vapor transport method.
  • the physical vapor transport method refers to a method in which the material decomposes and sublimates into gaseous components under high temperature conditions, and the gaseous components are transported to the seed crystal in the low temperature zone driven by the axial temperature gradient, and deposited on the surface of the seed crystal to form crystals.
  • the target crystal can be grown by physical vapor transport method based on the second seed crystal.
  • the first wafer 210 after the first treatment and the crystal growth layer 230 after the second treatment can be used as a second seed crystal (which can be called a prefabricated crystal after the second treatment) as a whole, and the target crystal growth layer 240 can be prepared by PVT method based on the second seed crystal.
  • the target crystal can include the first wafer 210 after the first treatment, the crystal growth layer 230 after the second treatment, and the target crystal growth layer 240.
  • high-quality prefabricated crystals are prepared by the TSSG method, and are subjected to a second treatment to obtain high-quality second seed crystals, which are used to prepare target crystals by the PVT method. This not only can obtain large-sized target crystals, but also can ensure the high quality of the target crystals and reduce micro- and macro-defects in the target crystals.
  • the present specification also provides a method for preparing a seed crystal, the method comprising: Perform radial cutting to obtain at least two seed chips; splice the at least two seed chips so that the step directions of the at least two seed chips after splicing are opposite to obtain the target seed crystal.
  • the method may also include rotating and/or flipping at least one of the at least two seed chips.
  • off-axis seed crystals and off-axis chips can be used interchangeably.
  • splicing may include splicing at least two seed chips by bonding them to a chip.
  • a groove may be provided at a preset height on the wafer.
  • the groove please refer to the description of other parts of this specification (for example, FIG. 4A to FIG. 4C ), which will not be repeated here.
  • the method further comprises processing the at least two seed wafers after splicing so that an immersion angle is formed at one end of the at least two seed wafers close to the splicing gap.
  • an immersion angle please refer to the description of other parts of this specification (for example, FIG. 5 ), which will not be repeated here.
  • the off-axis seed crystal is radially cut, and at least two seed crystals obtained by cutting are spliced, so that the steps of the at least two spliced seed crystals are in opposite directions, thereby obtaining a target seed crystal.
  • the target seed crystal is used to grow a crystal based on the TSSG method, since the step direction of the target seed crystal is opposite to the flow direction of the solution, the step aggregation behavior can be significantly suppressed, which is beneficial to reducing microscopic defects and macroscopic defects, improving the quality of the prepared crystal, and making the overall morphology of the crystal smoother.
  • numbers describing the number of components and attributes are used. It should be understood that such numbers used in the description of the embodiments are modified by the modifiers "about”, “approximately” or “substantially” in some examples. Unless otherwise specified, “about”, “approximately” or “substantially” indicate that the numbers are allowed to vary by ⁇ 20%. Accordingly, in some embodiments, the numerical parameters used in the specification and claims are approximate values, which may change according to the required features of individual embodiments. In some embodiments, the numerical parameters should take into account the specified significant digits and adopt the general method of retaining digits. Although the numerical domains and parameters used to confirm the breadth of their range in some embodiments of this specification are approximate values, in specific embodiments, the setting of such numerical values is as accurate as possible within the feasible range.

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Abstract

一种晶体制备方法，该方法包括：获取经过第一处理后的第一晶片；将经过第一处理后的第一晶片作为第一籽晶，基于顶部籽晶溶液生长法生长得到预制晶体；对预制晶体进行第二处理；将经过第二处理后的预制晶体作为第二籽晶，基于物理气相传输法生长得到目标晶体。

Description

一种晶体制备方法 技术领域
本说明书涉及晶体制备技术领域，特别涉及一种晶体制备方法。
背景技术
碳化硅单晶具有优异的物理化学性能，因此成为制造高频率和大功率器件的重要材料。物理气相传输法(Physical Vapor Transport，PVT)是一种用于制备半导体晶体的方法。然而，由于缺乏优质的籽晶，导致PVT法生长晶体的过程中，籽晶的固有缺陷会延伸至外延层中，导致制备的晶体的缺陷密度较大。
顶部籽晶溶液生长法(Top Seeded Solution Growth，TSSG)因其生长温度较低且接近热力学平衡条件，可以用于制备高质量的碳化硅晶体。但是TSSG法制备的晶体厚度有限，无法满足工业生产需求。
因此，有必要提供一种晶体制备方法，以制备大尺寸、高质量的晶体。
发明内容
本说明书一个或多个实施例提供一种晶体制备方法，所述方法包括：获取经过第一处理后的第一晶片；将所述经过第一处理后的第一晶片作为第一籽晶，基于顶部籽晶溶液生长法生长得到预制晶体；对所述预制晶体进行第二处理；将经过所述第二处理后的预制晶体作为第二籽晶，基于物理气相传输法生长得到目标晶体。
本说明书一个或多个实施例提供一种籽晶制备方法，所述方法包括：对偏轴籽晶进行径向切割，得到至少两个籽晶片；将所述至少两个籽晶片进行拼接，使拼接后的所述至少两个籽晶片的台阶方向相反，得到目标籽晶。
附图说明
本说明书将以示例性实施例的方式进一步说明，这些示例性实施例将通过附图进行详细描述。这些实施例并非限制性的，在这些实施例中，相同的编号表示相同的结构，其中：
图1是根据本说明书一些实施例所示的晶体制备方法的示例性流程图。
图2是根据本说明书一些实施例所示的晶体制备方法的示例性示意图。
图3A是根据本说明书一些实施例所示的对偏轴晶片进行第一处理的示例性示意图。
图3B是图3A中切割后的第一晶片二的示例性俯视图。
图3C是根据本说明书一些实施例所示的第一籽晶的台阶方向与溶液流向相反的示例性示意图。
图4A根据本说明书一些实施例所示的第二晶片的示例性剖面图。
图4B根据本说明书另一些实施例所示的第二晶片的示例性剖面图。
图4C根据本说明书另一些实施例所示的第二晶片的示例性剖面图。
图5是根据本说明书一些实施例所示的浸入角的示例性示意图。
图中，210为经过第一处理后的第一晶片；220为晶体生长层；230为经第二处理后的晶体生长层；240为目标晶体生长层；310为偏轴晶片；320为切割后的第一晶片；321、321-1为切割后的第一晶片一；322、322-1、322-2、322-3为切割后的第一晶片二；330为第一籽晶；400为第二晶片，410为凹槽。
具体实施方式
为了更清楚地说明本说明书实施例的技术方案，下面将对实施例描述中所需要使用的附图作简单的介绍。显而易见地，下面描述中的附图仅仅是本说明书的一些示例或实施例，对于本领域的普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图将本说明书应用于其它类似情景。除非从语言环境中显而易见或另做说明，图中相同标号代表相同结构或操作。
如本说明书和权利要求书中所示，除非上下文明确提示例外情形，“一”、 “一个”、“一种”和/或“该”等词并非特指单数，也可包括复数。一般说来，术语“包括”与“包含”仅提示包括已明确标识的步骤和元素，而这些步骤和元素不构成一个排它性的罗列，方法或者设备也可能包含其它的步骤或元素。
本说明书中使用了流程图用来说明根据本说明书的实施例的系统所执行的操作。应当理解的是，前面或后面操作不一定按照顺序来精确地执行。相反，可以按照倒序或同时处理各个步骤。同时，也可以将其他操作添加到这些过程中，或从这些过程移除某一步或数步操作。
本说明书一些实施例提供一种晶体制备方法，该方法将经过第一处理后的第一晶片作为第一籽晶，基于顶部籽晶溶液生长法生长可以得到高质量的预制晶体；将经过第二处理后的预制晶体作为第二籽晶，基于物理气相传输法生长可以得到大尺寸、高质量的目标晶体。
图1是根据本说明书一些实施例所示的晶体制备方法的示例性流程图。在一些实施例中，流程100可以由一个或多个组件执行。在一些实施例中，流程100可以由控制系统自动执行。例如，流程100可以通过控制指令实现，控制系统基于控制指令，控制各个组件完成流程100的各个操作。在一些实施例中，流程100可以半自动执行。例如，流程100的一个或多个操作可以由操作者手动执行。在一些实施例中，在完成流程100时，可以添加一个或以上未描述的附加操作，和/或删减一个或以上此处所讨论的操作。如图1所示，流程100可以包括以下步骤。
步骤110，获取经过第一处理后的第一晶片。
在一些实施例中，第一处理可以包括但不限于对第一晶片进行研磨和/或抛光。在一些实施例中，研磨可以指通过研具与第一晶片在预设压力下的相对运动，对第一晶片表面进行加工。在一些实施例中，研具表面可以涂覆或压嵌磨料颗粒。在一些实施例中，抛光可以指利用抛光介质对第一晶片的表面进行加工，降低其粗糙度以使其表面平整。在一些实施例中，抛光介质可以是抛 光粉。
在一些实施例中，对第一晶片进行研磨和/或抛光之前，第一处理还可以包括切割等。在一些实施例中，第一晶片可以是通过PVT法生长得到。
在一些实施例中，第一晶片可以包括但不限于碳化硅晶片、氮化铝晶片等。
应当理解的是，PVT法制备的第一晶片的缺陷密度较高，所以需要对第一晶片进行第一处理，使得到的经过第一处理后的第一晶片表面更加平整，降低第一晶片的缺陷密度。
在一些实施例中，籽晶托的材质可以包括但不限于石墨等。将经过第一处理后的第一晶片作为第一籽晶，基于顶部籽晶溶液生长法生长预制晶体时，为了避免在晶体生长过程中，溶液通过表面张力的作用攀爬到第一籽晶的背面，并与籽晶托发生反应，导致制备的预制晶体的质量下降，经过第一处理后的第一晶片的厚度需要大于第一厚度阈值。但是第一籽晶的厚度太大又会导致在TSSG法制备预制晶体的过程中，可能会因为第一籽晶重量过大，导致第一籽晶与籽晶托之间由于粘接强度问题发生脱落，所以经过第一处理后的第一晶片的厚度需要小于第二厚度阈值。其中，第一厚度阈值和第二厚度阈值可以是经验值或预设值等。
在一些实施例中，经过第一处理后的第一晶片的厚度可以为0.35mm-10mm。在一些实施例中，经过第一处理后的第一晶片的厚度可以为0.5mm-9.5mm。在一些实施例中，经过第一处理后的第一晶片的厚度可以为1mm-9mm。在一些实施例中，经过第一处理后的第一晶片的厚度可以为1.5mm-8.5mm。在一些实施例中，经过第一处理后的第一晶片的厚度可以为2mm-8mm。在一些实施例中，经过第一处理后的第一晶片的厚度可以为2.5mm-7.5mm。在一些实施例中，经过第一处理后的第一晶片的厚度可以为3mm-7mm。在一些实施例中，经过第一处理后的第一晶片的厚度可以为3.5mm-6.5mm。在一些实施例中，经过第一处理后的第一晶片的厚度可以为4mm-6mm。在一 些实施例中，经过第一处理后的第一晶片的厚度可以为4.5mm-5.5mm。
本说明书一些实施例中，通过控制经第一处理后的第一晶片的厚度，不仅可以保证其作为第一籽晶用于TSSG法制备预制晶体的过程中，有一定的厚度用于第一籽晶的回溶，还可以避免溶液攀爬到第一籽晶背面与籽晶托发生反应，而且可以保证第一籽晶不会因为重量太大从籽晶托上发生脱落现象。
将经过第一处理后的第一晶片作为第一籽晶，用于TSSG法制备预制晶体时，由于溶液在离心力作用下会呈现从中心向四周扩散的流向，若第一晶片为偏轴晶片，偏轴晶片的部分台阶方向会与溶液的流向相同，导致该部分生长的晶体的缺陷较多。在一些实施例中，第一晶片为偏轴晶片时，第一处理还可以包括对第一晶片进行径向切割，得到至少两个切割后的第一晶片；以及将至少两个切割后的第一晶片进行拼接，使拼接后的至少两个切割后的第一晶片的台阶方向相反。这样可以实现将拼接后的至少两个切割后的第一晶片作为第一籽晶用于TSSG法制备预制晶体时，溶液流向和第一籽晶的台阶方向相反。
图2是根据本说明书一些实施例所示的晶体制备方法的示例性示意图。图3A是根据本说明书一些实施例所示的对偏轴晶片进行第一处理的示例性示意图。图3B是图3A中切割后的第一晶片二的示例性俯视图。图3C是根据本说明书一些实施例所示的第一籽晶的台阶方向与溶液流向相反的示例性示意图。
在一些实施例中，如图3A所示，第一晶片为偏轴晶片310时，可以对偏轴晶片310进行径向切割得到两个切割后的第一晶片320。在一些实施例中，径向切割可以指沿着直径方向或与轴线垂直的方向进行切割。如图2所示，径向切割可以用双箭头ab表示。偏轴晶片是指晶体学上的c轴(最长轴)向晶向方向偏转预设角度的晶片。在一些实施例中，偏轴晶片可以通过对晶片进行机械加工(例如，切割或斜切)得到。应当理解的是，由于机械加工的限制，偏轴晶片的台阶方向总是沿着单一方向。如图3A所示，偏轴晶片310的 台阶方向一致，均指向一侧。因此，为了实现溶液流向与第一籽晶的所有台阶方向相反，需要对至少两个切割后的第一晶片320进行拼接。
可以通过多种方式将至少两个切割后的第一晶片320进行拼接，使拼接后的至少两个切割后的第一晶片320的台阶方向相反。例如，对两个切割后的第一晶片320进行拼接时，可以使其中一个切割后的第一晶片(例如，如图3A所示的切割后的第一晶片一321)保持不动，另一个切割后的第一晶片(例如，如图3A所示的切割后的第一晶片二322)做至少一次镜像变换，将镜像变换后的切割后的第一晶片二322与保持不动的切割后的第一晶片一321进行拼接，使拼接后的两个切割后的第一晶片的台阶方向相反。其中，镜像变换可以包括以某一轴线(例如，切割后的第一晶片二的某条边线、垂直中轴线或水平中轴线)为轴进行180°旋转。
在一些实施例中，第一处理还可以包括对至少两个切割后的第一晶片320中的至少一个进行旋转处理和/或翻转处理。其中，旋转处理和/或翻转处理可以包括以某一轴线(例如，切割后的第一晶片的某条边线、垂直中轴线或水平中轴线)为旋转轴进行预设角度的旋转。仅作为示例，如图3A所示，当第一晶片为偏轴晶片310时，可以对偏轴晶片310进行径向切割得到切割后的第一晶片一321和切割后的第一晶片二322。保持切割后的第一晶片一321不动，对切割后的第一晶片二322以其边线(如图3B中m所示的边线)为旋转轴线顺时针(如图3A中箭头b所示的方向)旋转180°得到如图3A所示的切割后的第一晶片二322-1，然后对切割后的第一晶片二322-1以其边线(如图3A中n所示的边线)为旋转轴线旋转180°得到切割后的第一晶片二322-2，然后将切割后的第一晶片二322-2与切割后的第一晶片一321进行拼接，如图3A所示，可以得到拼接后的两个切割后的第一晶片(也可以称为第一籽晶330)。如图3A和图3C所示，拼接后的两个切割后的第一晶片(也可以称为第一籽晶330)中切割后的切割后的第一晶片一321与切割后的第一晶片二322的台阶方向相反。如图3C所示，以拼接后的两个切割后的第一晶片作 为第一籽晶330用于TSSG法制备预制晶体时，台阶方向与溶液流向相反(可以理解为台阶B阻碍溶液流动或溶液流动与台阶B相碰撞)。其中，台阶B可以理解为与第一籽晶330的轴线平行的切痕。
本说明书实施例对偏轴晶片310的形状不做限定，例如，可以为长方体、正方体、圆柱体等。例如，如图3A-图3B所示，偏轴晶片310可以为长方体。在一些实施例中，偏轴晶片310的横截面可以为多边形(例如，矩形、正方形)、圆形、椭圆形等规则或不规则形状。在一些实施例中，还可以通过对拼接后的至少两个切割后的第一晶片的边缘进行切割来改变其形状。例如，可以对图3A所示的长方体第一籽晶330进行切割得到圆柱体籽晶。
在一些实施例中，第一晶片(此处也可以称为偏轴晶片310)为圆柱体时，可以对台阶方向相反的两个圆柱体第一晶片分别进行径向切割，然后取台阶方向相反的两个切割后的第一晶片进行拼接，可以得到台阶方向相反的拼接后的两个切割后的第一晶片，且该拼接后的两个切割后的第一晶片为圆柱体。
本说明书一些实施例中，通过对第一晶片进行径向切割，将切割得到的至少两个切割后的第一晶片进行拼接，使拼接后的至少两个切割后的第一晶片的台阶方向相反，将其作为第一籽晶基于TSSG法生长预制晶体时，第一籽晶的台阶方向与溶液的流向相反，台阶聚集行为可以得到显著的抑制，有利于降低微观缺陷和宏观缺陷，提高制备的预制晶体的质量，使得晶体整体形貌更加平整光滑。
应当理解的是，由于对第一晶片进行了径向切割和拼接处理，如果直接将拼接后的至少两个切割后的第一晶片粘接在籽晶托上，将其作为第一籽晶基于TSSG法制备预制晶体，在生长晶体过程中，对于拼接后的至少两个切割后的第一晶片的拼接缝隙处，溶液会在毛细管力的作用下，沿着拼接缝隙上升至与籽晶托接触并发生反应，导致制备的预制晶体的质量较低。在一些实施例中，为了避免上述情况，可以将至少两个切割后的第一晶片通过粘接在第二晶 片上进行拼接。仅作为示例，如图3A和图3C所示，切割后的第一晶片一321和切割后的第一晶片二322拼接后得到拼接后的两个切割后的第一晶片(也可以称为第一籽晶330)，经第一籽晶330可以与第二晶片400的一面进行粘接，第二晶片400的另一面可以与籽晶托A进行粘接。
如图3A和图3C所示，第二晶片400可以位于第一籽晶330与籽晶托A之间，用于粘接第一籽晶330和籽晶托A。在一些实施例中，第二晶片400可以包括等轴晶片或偏轴晶片等。在一些实施例中，第二晶片400的材质可以与第一籽晶330相同或不同。在一些实施例中，第二晶片400的形状可以与第一籽晶330相同或不同。
可以通过热键合的方式将拼接后的至少两个切割后的第一晶片粘接在第二晶片上。还可以通过其他方式实现拼接后的至少两个切割后的第一晶片和第二晶片的粘接。例如，胶粘接等。第二晶片与籽晶托的粘接方式可以与拼接后的至少两个切割后的第一晶片(也可以称为第一籽晶)与第二晶片的粘接方式相同或不同。
本说明书一些实施例中，通过将拼接后的至少两个切割后的第一晶片(也可以称为第一籽晶)粘接在第二晶片的一面，再将第二晶片的另一面粘接在籽晶托上，可以避免第一籽晶基于TSSG法制备预制晶体的过程中，溶液通过拼接缝隙与籽晶托直接接触发生反应，有利于提高制备的预制晶体的质量。
在一些实施例中，第二晶片上预设高度处可以设有凹槽，以进一步减少攀爬到籽晶托表面的溶液量。在一些实施例中，预设高度可以指第二晶片的凹槽的最低端与第二晶片的下底面的距离。预设高度可以是预设值或默认值等。在一些实施例中，凹槽可以包括多种结构，例如，环形结构。在一些实施例中，凹槽的纵截面可以为任意形状，例如，多边形、圆形等规则或不规则形状。在一些实施例中，凹槽深度可以指凹槽的最远端与第二晶片侧面的间距。在一些实施例中，凹槽倾斜度可以指凹槽的倾斜边与水平面的夹角。
如图4A所示，第二晶片400的预设高度(如图4A中h1所示)处设 有纵截面为矩形的环形凹槽410。凹槽410深度(可以理解为矩形的长度)可以表示为图4A中L1。如图4B所示，第二晶片400的预设高度(如图4B中h2所示)处设有纵截面为平行四边形的环形凹槽410。凹槽410深度可以表示为图4B中的L2，且凹槽410倾斜度为α。如图4C所示，第二晶片400的预设高度(如图4C中h3所示)处设有纵截面为半圆形的环形凹槽410。凹槽410深度(也可以理解为半圆的半径)可以表示为图4C中L3。
将拼接后的至少两个切割后的第一晶片作为第一籽晶，基于TSSG法制备预制晶体时，为了能够让溶液在表面张力的作用下更好地浸润整个拼接缝隙，使溶液在拼接缝隙处进行晶体生长，以闭合整个拼接缝隙。在一些实施例中，第一处理还可以包括对拼接后的至少两个切割后的第一晶片进行第三处理，使至少两个切割后的第一晶片靠近拼接缝隙的一端形成浸入角。
第三处理可以包括对至少两个切割后的第一晶片靠近拼接缝隙的一端(例如，生长端)进行切割处理，形成浸入角。仅作为示例，如图5所示，可以分别对切割后的第一晶片一321和切割后的第一晶片二322靠近拼接缝隙的一端(例如，生长端)进行切割处理，得到经第三处理后的切割后的第一晶片一321-1和经第三处理后的切割后的第一晶片二322-3，然后将其拼接后可以形成第一籽晶330。如图5所示，第一籽晶330的拼接缝隙处可以形成浸入角θ。
应当理解的是，浸入角是为了让第一籽晶在TSSG法生长晶体过程中，溶液更好地浸入拼接缝隙，使拼接缝隙生长闭合。浸入角可以是多种结构。例如，圆柱体、圆锥体、多面体等。相应地，浸入角的纵截面可以是多边形、三角形(如图5所示)等。在一些实施例中，浸入角的纵截面还可以是其他能够增加拼接缝隙处溶液的毛细管力的任何形状。作为示例，如图5所示，拼接缝隙可以为圆锥体，圆锥体的底面圆靠近台阶的一端。拼接缝隙的半径可以理解为圆锥体的底面圆半径，浸入角可以理解为圆锥体的顶角。溶液浸入拼接缝隙的长度可以通过公式计算得到。其中，H为拼接缝隙的长度(即， 经第一处理后第一晶片的厚度)；γ为TSSG法中液体(可以理解为原料熔体)的表面张力；ρ为液体的密度；g为重力加速度；r为拼接缝隙的半径；θ为液体与籽晶(例如，第一籽晶)的浸润角。
在一些实施例中，浸入角太大会导致生长的晶体出现裂纹。因此，浸入角需小于预设阈值。在一些实施例中，浸入角θ可以大于0°小于20°。在一些实施例中，浸入角θ可以大于2°小于18°。在一些实施例中，浸入角θ可以大于4°小于16°。在一些实施例中，浸入角θ可以大于6°小于14°。在一些实施例中，浸入角θ可以大于8°小于12°。在一些实施例中，浸入角θ可以大于9°小于10°。
本说明书一些实施例中，通过对至少两个切割后的第一晶片进行第三处理，在拼接后的至少两个切割后的第一晶片靠近拼接缝隙的一端形成浸入角，有利于增强溶液的毛细管力，使得溶液能够更好地浸入拼接缝隙，通过晶体生长让拼接缝隙闭合。
步骤120，将经过第一处理后的第一晶片作为第一籽晶，基于顶部籽晶溶液生长法生长得到预制晶体。
顶部籽晶溶液生长法是指将制备晶体的原料(例如，碳化硅粉末)在高温下溶解于低熔点助熔剂中，形成均匀的饱和溶液，然后通过缓慢降温等方法，形成过饱和熔液，使其在籽晶上析出制备晶体的方法。
预制晶体是指通过TSSG法制备的中间晶体。
将第一籽晶与第二晶片的一面粘接后，再将第二晶片的另一面与籽晶托粘接，通过顶部籽晶溶液生长法生长得到预制晶体。仅作为示例，如图2所示，将经过第一处理后的第一晶片210作为第一籽晶，基于TSSG法制备得到具有预设厚度的晶体生长层220。经过第一处理后的第一晶片210与晶体生长层220可以称为预制晶体。
应当理解的是，基于第一籽晶，通过顶部籽晶溶液生长法生长得到预制晶体时，由于受到TSSG法的限制，当制备的晶体生长层的厚度过大时，会导 致晶体生长层出现大量的宏观缺陷(例如，溶剂包裹)，因此TSSG法制备的晶体生长层的厚度需要满足预设条件。在一些实施例中，在预制晶体的晶体生长层的生长过程中，需要控制基于顶部籽晶溶液生长法生长的晶体生长层220的厚度在1mm-1.5mm范围内。在一些实施例中，在预制晶体的生长过程中，可以控制基于顶部籽晶溶液生长法生长的晶体生长层220的厚度在1.1mm-1.4mm范围内。在一些实施例中，在预制晶体的生长过程中，可以控制基于顶部籽晶溶液生长法生长的晶体生长层220的厚度在1.2mm-1.3mm范围内。
本说明书一些实施例中，通过控制TSSG法制备的晶体生长层的厚度，不仅能够减少制备的预制晶体因为生长厚度过大导致的各种缺陷问题，而且预设厚度的预制晶体可以保证后续可以对预制晶体进行第二处理。
步骤130，对预制晶体进行第二处理。
第二处理可以包括但不限于对预制晶体或其晶体生长层进行研磨和/或抛光。
应当理解的是，由于通过TSSG法制备的预制晶体的晶体生长层表面会附着一定量的溶剂和/或结晶颗粒，所以需要对预制晶体或其晶体生长层进行第二处理。在一些实施例中，可以通过多种方式对预制晶体或其晶体生长层进行第二处理。仅作为示例，如图2所示，可以通过研具与晶体生长层220在预设压力下的相对运动，对晶体生长层220表面进行加工，提高其表面光滑度和平整度，降低表面缺陷，得到经过第二处理后的晶体生长层230。在一些实施例中，第二处理的方式可以和第一处理的方式相同或不相同。如图2所示，经过第一处理后的第一晶片210与经过第二处理后的晶体生长层230可以称为经过第二处理后的预制晶体。
为了能够制备高质量的目标晶体，将经过第二处理后的预制晶体作为第二籽晶时，需要保证第二籽晶的表面足够光滑平整，且尽量没有缺陷。在一些实施例中，第二籽晶的表面粗糙度可以不大于0.2nm。在一些实施例中，第二籽晶的表面粗糙度可以不大于0.15nm。在一些实施例中，第二籽晶的表面 粗糙度可以不大于0.1nm。在一些实施例中，第二籽晶的表面粗糙度可以不大于0.05nm。
本说明书一些实施例中，通过对预制晶体进行第二处理，使其作为PVT法的第二籽晶时的表面粗糙度不大于0.2nm，可以保证第二籽晶表面的光滑平整，提高第二籽晶的质量，有利于进一步提高后续通过PVT法制备的目标晶体的质量。
步骤140，将经过第二处理后的预制晶体作为第二籽晶，基于物理气相传输法生长得到目标晶体。
物理气相传输法是指物料在高温条件下分解升华为气相组分，气相组分在轴向温度梯度驱动下传输至低温区的籽晶处，并在籽晶表面沉积生成晶体的方法。
可以基于第二籽晶，通过物理气相传输法生长得到目标晶体。仅作为示例的，如图2所示，经过第一处理后的第一晶片210与经过第二处理后的晶体生长层230作为一个整体可以作为第二籽晶(可以称为经过第二处理后的预制晶体)，基于第二籽晶通过PVT法制备可以得到目标晶体生长层240。其中，目标晶体可以包括经过第一处理后的第一晶片210、经第二处理后的晶体生长层230和目标晶体生长层240。
本说明书一些实施例中，通过TSSG法制备高质量的预制晶体，并对其进行第二处理，得到优质的第二籽晶，将其用于PVT法制备目标晶体，不仅可以得到大尺寸的目标晶体，而且可以保证目标晶体的高质量，降低目标晶体中的微观缺陷和宏观缺陷。
应当注意的是，上述有关流程100的描述仅仅是为了示例和说明，而不限定本说明书的适用范围。对于本领域技术人员来说，在本说明书的指导下可以对流程100进行各种修正和改变。然而，这些修正和改变仍在本说明书的范围之内。
本说明书实施例还提供一种籽晶制备方法，所述方法包括：对偏轴籽晶 进行径向切割，得到至少两个籽晶片；将至少两个籽晶片进行拼接，使拼接后的至少两个籽晶片的台阶方向相反，得到目标籽晶。在一些实施例中，所述方法还可以包括对至少两个籽晶片中的至少一个进行旋转处理和/或翻转处理。本说明书实施例中，偏轴籽晶与偏轴晶片可以互换使用。在一些实施例中，拼接可以包括将至少两个籽晶片通过粘接在晶片上进行拼接。关于径向切割及拼接的相关说明可以参见本说明书其他部分(例如，图3A-图3C)的相关描述，在此不再赘述。
在一些实施例中，晶片上预设高度处可以设有凹槽。关于凹槽的相关描述可以参见本说明书其他部分(例如，图4A-图4C)的相关描述，在此不再赘述。
在一些实施例中，所述方法还包括对拼接后的至少两个籽晶片进行处理，使至少两个籽晶片靠近拼接缝隙的一端形成浸入角。关于浸入角的相关描述可以参见本说明书其他部分(例如，图5)的相关描述，在此不再赘述。
本说明书一些实施例中，通过对偏轴籽晶进行径向切割，将切割得到的至少两个籽晶片进行拼接，使拼接后的至少两个籽晶片的台阶方向相反，得到目标籽晶。将该目标籽晶基于TSSG法生长晶体时，由于目标籽晶的台阶方向与溶液的流向相反，台阶聚集行为可以得到显著的抑制，有利于降低微观缺陷和宏观缺陷，提高制备的晶体的质量，使得晶体整体形貌更加平整光滑。
上文已对基本概念做了描述，显然，对于本领域技术人员来说，上述详细披露仅仅作为示例，而并不构成对本说明书的限定。虽然此处并没有明确说明，本领域技术人员可能会对本说明书进行各种修改、改进和修正。该类修改、改进和修正在本说明书中被建议，所以该类修改、改进、修正仍属于本说明书示范实施例的精神和范围。
同时，本说明书使用了特定词语来描述本说明书的实施例。如“一个实施例”、“一实施例”、和/或“一些实施例”意指与本说明书至少一个实施例相关的某一特征、结构或特点。因此，应强调并注意的是，本说明书中在不同 位置两次或多次提及的“一实施例”或“一个实施例”或“一个替代性实施例”并不一定是指同一实施例。此外，本说明书的一个或多个实施例中的某些特征、结构或特点可以进行适当的组合。
此外，除非权利要求中明确说明，本说明书所述处理元素和序列的顺序、数字字母的使用、或其他名称的使用，并非用于限定本说明书流程和方法的顺序。尽管上述披露中通过各种示例讨论了一些目前认为有用的发明实施例，但应当理解的是，该类细节仅起到说明的目的，附加的权利要求并不仅限于披露的实施例，相反，权利要求旨在覆盖所有符合本说明书实施例实质和范围的修正和等价组合。例如，虽然以上所描述的系统组件可以通过硬件设备实现，但是也可以只通过软件的解决方案得以实现，如在现有的服务器或移动设备上安装所描述的系统。
同理，应当注意的是，为了简化本说明书披露的表述，从而帮助对一个或多个发明实施例的理解，前文对本说明书实施例的描述中，有时会将多种特征归并至一个实施例、附图或对其的描述中。但是，这种披露方法并不意味着本说明书对象所需要的特征比权利要求中提及的特征多。实际上，实施例的特征要少于上述披露的单个实施例的全部特征。
一些实施例中使用了描述成分、属性数量的数字，应当理解的是，此类用于实施例描述的数字，在一些示例中使用了修饰词“大约”、“近似”或“大体上”来修饰。除非另外说明，“大约”、“近似”或“大体上”表明所述数字允许有±20％的变化。相应地，在一些实施例中，说明书和权利要求中使用的数值参数均为近似值，该近似值根据个别实施例所需特点可以发生改变。在一些实施例中，数值参数应考虑规定的有效数位并采用一般位数保留的方法。尽管本说明书一些实施例中用于确认其范围广度的数值域和参数为近似值，在具体实施例中，此类数值的设定在可行范围内尽可能精确。
针对本说明书引用的每个专利、专利申请、专利申请公开物和其他材料，如文章、书籍、说明书、出版物、文档等，特此将其全部内容并入本说明书作 为参考。与本说明书内容不一致或产生冲突的申请历史文件除外，对本说明书权利要求最广范围有限制的文件(当前或之后附加于本说明书中的)也除外。需要说明的是，如果本说明书附属材料中的描述、定义、和/或术语的使用与本说明书所述内容有不一致或冲突的地方，以本说明书的描述、定义和/或术语的使用为准。
最后，应当理解的是，本说明书中所述实施例仅用以说明本说明书实施例的原则。其他的变形也可能属于本说明书的范围。因此，作为示例而非限制，本说明书实施例的替代配置可视为与本说明书的教导一致。相应地，本说明书的实施例不仅限于本说明书明确介绍和描述的实施例。

Claims (15)

  1. 一种晶体制备方法，其特征在于，所述方法包括：
    获取经过第一处理后的第一晶片；
    将所述经过第一处理后的第一晶片作为第一籽晶，基于顶部籽晶溶液生长法生长得到预制晶体；
    对所述预制晶体进行第二处理；
    将经过所述第二处理后的预制晶体作为第二籽晶，基于物理气相传输法生长得到目标晶体。
  2. 根据权利要求1所述的晶体制备方法，其特征在于，
    所述经过第一处理后的第一晶片的厚度为0.35mm-10mm。
  3. 根据权利要求1所述的晶体制备方法，其特征在于，所述方法还包括：
    在所述预制晶体的生长过程中，控制基于顶部籽晶溶液生长法生长的晶体生长层的厚度在1mm-1.5mm范围内。
  4. 根据权利要求1所述的晶体制备方法，其特征在于，所述第二籽晶的表面粗糙度不大于0.2nm。
  5. 根据权利要求1所述的晶体制备方法，其特征在于，所述第一处理和/或所述第二处理包括研磨和/或抛光。
  6. 根据权利要求1所述的晶体制备方法，其特征在于，所述第一晶片为偏轴晶片时，所述第一处理还包括：
    对所述第一晶片进行径向切割，得到至少两个切割后的第一晶片；
    将所述至少两个切割后的第一晶片进行拼接，使拼接后的所述至少两个切割后的第一晶片的台阶方向相反。
  7. 根据权利要求6所述的晶体制备方法，其特征在于，所述第一处理还包括：对所述至少两个切割后的第一晶片中的至少一个进行旋转处理和/或翻转处理。
  8. 根据权利要求6所述的晶体制备方法，其特征在于，所述将所述至少两个切割后的第一晶片进行拼接包括：将所述至少两个切割后的第一晶片通过粘接在第二晶片上进行拼接。
  9. 根据权利要求8所述的晶体制备方法，其特征在于，所述第二晶片上预设高度处设有凹槽。
  10. 根据权利要求6所述的晶体制备方法，其特征在于，所述第一处理还包括：
    对所述拼接后的至少两个切割后的第一晶片进行第三处理，使所述至少两个切割后的第一晶片靠近拼接缝隙的一端形成浸入角。
  11. 一种籽晶制备方法，其特征在于，所述方法包括：
    对偏轴籽晶进行径向切割，得到至少两个籽晶片；
    将所述至少两个籽晶片进行拼接，使拼接后的所述至少两个籽晶片的台阶方向相反，得到目标籽晶。
  12. 根据权利要求11所述的籽晶制备方法，其特征在于，所述方法还包括：对所述至少两个籽晶片中的至少一个进行旋转处理和/或翻转处理。
  13. 根据权利要求11所述的籽晶制备方法，其特征在于，所述将所述至少两个籽晶片进行拼接包括：将所述至少两个籽晶片通过粘接在晶片上进行拼接。
  14. 根据权利要求13所述的籽晶制备方法，其特征在于，所述晶片上预设高度处设有凹槽。
  15. 根据权利要求11所述的籽晶制备方法，其特征在于，所述方法还包括：
    对所述拼接后的至少两个籽晶片进行处理，使所述至少两个籽晶片靠近拼接缝隙的一端形成浸入角。
PCT/CN2023/100230 2023-06-14 2023-06-14 一种晶体制备方法 Ceased WO2024254789A1 (zh)

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CN110541199A (zh) * 2019-10-11 2019-12-06 山东大学 一种直径8英寸及以上尺寸高质量SiC籽晶的制备方法
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