WO2023068309A1 - ＳｉＣ基板及びＳｉＣ複合基板 - Google Patents

ＳｉＣ基板及びＳｉＣ複合基板 Download PDF

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Publication number
WO2023068309A1
WO2023068309A1 PCT/JP2022/039004 JP2022039004W WO2023068309A1 WO 2023068309 A1 WO2023068309 A1 WO 2023068309A1 JP 2022039004 W JP2022039004 W JP 2022039004W WO 2023068309 A1 WO2023068309 A1 WO 2023068309A1
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sic
substrate
point
intensity
biaxially oriented
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French (fr)
Japanese (ja)
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勇輝 浦田
潔 松島
潤 吉川
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NGK Insulators Ltd
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NGK Insulators Ltd
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Priority to CN202280043244.0A priority Critical patent/CN117529584A/zh
Priority to JP2023514848A priority patent/JP7587688B2/ja
Priority to EP22883613.6A priority patent/EP4421221A4/en
Publication of WO2023068309A1 publication Critical patent/WO2023068309A1/ja
Priority to US18/441,303 priority patent/US20240186380A1/en
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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
    • C30B1/00—Single-crystal growth directly from the solid state
    • C30B1/02—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing
    • 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
    • C30B28/00—Production of homogeneous polycrystalline material with defined structure
    • C30B28/02—Production of homogeneous polycrystalline material with defined structure directly from the solid state
    • 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
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10D—INORGANIC ELECTRIC SEMICONDUCTOR DEVICES
    • H10D62/00—Semiconductor bodies, or regions thereof, of devices having potential barriers
    • H10D62/50—Physical imperfections
    • H10D62/57—Physical imperfections the imperfections being on the surface of the semiconductor body, e.g. the body having a roughened surface
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10D—INORGANIC ELECTRIC SEMICONDUCTOR DEVICES
    • H10D62/00—Semiconductor bodies, or regions thereof, of devices having potential barriers
    • H10D62/80—Semiconductor bodies, or regions thereof, of devices having potential barriers characterised by the materials
    • H10D62/83—Semiconductor bodies, or regions thereof, of devices having potential barriers characterised by the materials being Group IV materials, e.g. B-doped Si or undoped Ge
    • H10D62/832—Semiconductor bodies, or regions thereof, of devices having potential barriers characterised by the materials being Group IV materials, e.g. B-doped Si or undoped Ge being Group IV materials comprising two or more elements, e.g. SiGe
    • H10D62/8325—Silicon carbide
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
    • H10P14/20—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials
    • H10P14/29—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials characterised by the substrates
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/6489—Photoluminescence of semiconductors

Definitions

  • the present invention relates to SiC substrates and SiC composite substrates.
  • SiC silicon carbide
  • SiC power devices power semiconductor devices using SiC materials
  • SiC power devices are superior to those using Si semiconductors in terms of miniaturization, low power consumption, and high efficiency, so they are expected to be used in various applications.
  • SiC power devices converters, inverters, on-board chargers, etc. for electric vehicles (EV) and plug-in hybrid vehicles (PHEV) can be made smaller and more efficient.
  • EV electric vehicles
  • PHEV plug-in hybrid vehicles
  • the solution growth method is known as a method for reducing defects in the wafer, particularly threading screw dislocations (TSD) which are said to cause breakdown voltage deterioration.
  • TSD threading screw dislocations
  • Patent Document 1 Japanese Patent Application Laid-Open No. 2014-043369
  • a macrostep made of a SiC single crystal and having a height of more than 70 nm is formed to obtain a second seed crystal.
  • a method for manufacturing a SiC single crystal comprising: According to this manufacturing method, it is described that a SiC single crystal with few threading screw dislocations can be obtained.
  • problems such as macro defects such as solvent inclusions and heterogeneous polymorphs due to surface roughening.
  • Non-Patent Document 1 Lixia Zhao et al. "Surface defects in 4H-SiC homoepitaxial layers” Nanotechnology and Precision Engineering 3 (2020) 229-234
  • a SiC epitaxial layer is obtained by chemical vapor deposition, It discloses that the morphology and structure of this surface defect were investigated, and generally the TSD density of the SiC substrate is 300 to 500 cm ⁇ 2 .
  • Non-Patent Document 1 most of the TSD on the substrate is propagated to the epitaxial layer, so it is difficult to reduce the TSD density on the substrate surface significantly below 300 cm ⁇ 2 . Therefore, further reduction of the TSD density on the SiC substrate surface is desired.
  • the present inventors have recently found that a biaxially oriented SiC layer that satisfies predetermined conditions when analyzed by photoluminescence (PL) results in a SiC substrate with a very low TSD density on the surface.
  • PL photoluminescence
  • an object of the present invention is to provide a SiC substrate having a very low surface TSD density.
  • a SiC substrate comprising a biaxially oriented SiC layer, wherein the surface of the biaxially oriented SiC layer is analyzed by photoluminescence (PL), and the horizontal axis is the distance ( ⁇ m) in the [11-20] direction, and , PL intensity I plotted on the vertical axis, (i) the graph has a shape that repeats maxima and minima, where the maxima are the first, second and third closest points on the left and right of the graph, totaling 6 points; is defined as a point that gives a higher PL intensity I than each of the PL intensity I of , and the local minimum point is a total of 6 points consisting of the first closest point, the second closest point, and the third closest point on the left and right defined as the point giving a lower PL intensity I than each of the PL intensities I of (ii) Let M be the maximum value of the PL intensity I at a certain maximum point PM , and a minimum point located
  • a SiC substrate provided with a biaxially oriented SiC layer wherein in an image obtained by analyzing the surface of the biaxially oriented SiC layer by photoluminescence (PL), Previtt about the [11-20] direction of the image
  • a graph is obtained by processing with a filter and plotting the distance ( ⁇ m) in the [11-20] direction on the horizontal axis and the PL intensity IF on the vertical axis
  • the graph has a shape that repeats a plurality of local maxima, where the local maxima are the first, second and third closest points on the left and right of the graph, totaling six points; defined as the point giving a higher PL intensity IF than each of the PL intensity IF ,
  • the biaxially oriented SiC layer is oriented in the c-axis direction and the a-axis direction.
  • the graph shows a constant as the depth decreases.
  • FIG. 1 is a longitudinal sectional view of a SiC composite substrate 10;
  • FIG. 4 is a manufacturing process diagram of the SiC composite substrate 10.
  • FIG. It is a schematic cross section showing the configuration of an aerosol deposition (AD) apparatus.
  • 2 is a photoluminescence (PL) imaging image in the (0001) plane of the biaxially oriented SiC layer obtained in Example 1.
  • FIG. The horizontal axis represents the distance ( ⁇ m) in the [11-20] direction, and the vertical axis represents the PL intensity I, which was created based on the PL imaging image of the (0001) plane of the biaxially oriented SiC layer obtained in Example 1.
  • FIG. 4 is a graph plotted on 4 is an image obtained by processing a PL imaging image on the (0001) plane of the biaxially oriented SiC layer obtained in Example 1 with a Prewitt filter.
  • the distance in the [11-20] direction ( ⁇ m) is plotted on the horizontal axis and the PL intensity IF is plotted on the vertical axis.
  • the horizontal axis represents the depth ( ⁇ m) from the (0001) plane to the arbitrary (000-1) plane of the biaxially oriented SiC layer obtained in Example 1, and the threading screw dislocation (TSD) density (cm ⁇ 2 ). is plotted on the vertical axis.
  • 4 is an optical microscope image showing a step-terrace structure on the substrate surface of a SiC substrate obtained by a solution growth method, published in Non-Patent Document 2.
  • the SiC substrate according to the invention is a SiC substrate with a biaxially oriented SiC layer.
  • the surface of this biaxially oriented SiC layer is analyzed by photoluminescence (PL), and a graph plotted with the distance ( ⁇ m) in the [11-20] direction as the horizontal axis and the PL intensity I as the vertical axis is shown.
  • PL photoluminescence
  • FIG. 5 which will be described later, (i) it has a peculiar shape in which local maximum points and local minimum points are repeated.
  • the maximum point is defined as a point that gives a higher PL intensity I than each of the 6 points in total consisting of the first, second and third closest points on the left and right sides of the maximum point.
  • the local minimum point is defined as a point that gives a lower PL intensity I than each of the 6 PL intensities I in total consisting of the first, second and third closest points on the left and right. be.
  • this graph is under the following conditions: (ii) Let M be the maximum value of the PL intensity I at a certain maximum point PM , and the minimum point P that is longer in the horizontal axis direction than that maximum point PM and that is closest to that maximum point PM When the minimum value of the PL intensity I at m is m, the ratio of M/m is 1.05 or more, and (iii) [11-20] between the maximum point P M and the minimum point P m It satisfies that the directional distance L is 15 to 150 ⁇ m.
  • the [11-20] direction of the image is processed with a Prewitt filter, and the [11-20] direction
  • a graph is obtained by plotting the distance ( ⁇ m) on the horizontal axis and the PL intensity IF on the vertical axis, for example, as shown in FIG. have.
  • the maximum point is a point that gives a higher PL intensity IF than each of the total 6 points consisting of the first, second and third closest points on the left and right sides of the PL intensity IF . Defined.
  • a biaxially oriented SiC layer that satisfies predetermined conditions can provide a SiC substrate with a very low TSD density on the surface. Moreover, since such a SiC substrate can be produced without using a solution growth method, macro defects on the substrate surface are less likely to occur.
  • the surface of the biaxially oriented SiC layer is analyzed by PL, the horizontal axis is the distance ( ⁇ m) in the [11-20] direction, and the PL intensity
  • M be the maximum value of the PL intensity I at a certain maximum point PM
  • the ratio of M/ m is 1.05 or more, where m is the minimum value of the PL intensity I at the minimum point Pm closest to the maximum point PM (hereinafter referred to as condition (ii)).
  • condition (ii) the upper limit of the M/m ratio is not particularly limited, it is preferably 1.05 to 1.80.
  • the distance L in the [11-20] direction between the maximum point PM and the minimum point Pm is 15 to 150 ⁇ m (hereinafter, condition (iii )), preferably 50 to 150 ⁇ m, more preferably 50 to 120 ⁇ m, even more preferably 50 to 100 ⁇ m.
  • the above graph typically has a regular pattern in which waveforms including local maximum points and local minimum points are repeated at regular intervals, as shown in FIG. 5, which will be described later.
  • at least one of a plurality of maximum points (and a corresponding minimum point) on a predetermined measurement line segment parallel to the [11-20] direction meets the above conditions (ii) and If (iii) is satisfied, the SiC substrate is assumed to satisfy the above conditions (ii) and (iii). More preferably, however, at least two of the local maxima (and their corresponding local minima) satisfy conditions (ii) and (iii) above, and even more preferably at least three of the local maxima.
  • the biaxially oriented SiC layer constituting the SiC substrate of the present invention is an image obtained by PL analysis of the surface of the biaxially oriented SiC layer, Prewitt filter for the [11-20] direction of the image to obtain a graph in which the distance ( ⁇ m) in the [11-20] direction is plotted on the horizontal axis and the PL intensity IF is plotted on the vertical axis.
  • the distance in the [11-20] direction is longer than M1 , and the distance L F in the [11-20] direction between the local maximum point P M1 and the closest local maximum point P M2 is 30 to 300 ⁇ m (
  • condition (v)) the thickness is preferably 100 to 300 ⁇ m, more preferably 100 to 240 ⁇ m, further preferably 100 to 200 ⁇ m.
  • the graph obtained by processing with the Prewitt filter repeats a plurality of maximum points, as shown in FIG. 7, which will be described later.
  • a predetermined measurement line segment eg, a line segment of 500 ⁇ m
  • the SiC substrate satisfies the above condition (v). More preferably, however, there are at least two such combinations, and even more preferably three.
  • the biaxially oriented SiC layer is preferably oriented in the c-axis direction and the a-axis direction. It is also preferred that the SiC substrate consists of a biaxially oriented SiC layer.
  • the biaxially oriented SiC layer may be a SiC single crystal or a mosaic crystal as long as it is oriented in the biaxial directions of the c-axis and the a-axis.
  • Mosaic crystals are aggregates of crystals that do not have distinct grain boundaries but have slightly different crystal orientations in one or both of the c-axis and a-axis.
  • the orientation evaluation method is not particularly limited, but for example, a known analysis method such as an EBSD (Electron Back Scatter Diffraction Patterns) method or an X-ray pole figure can be used.
  • EBSD Electro Back Scatter Diffraction Patterns
  • X-ray pole figure inverse pole figure mapping of the surface (plate surface) of the biaxially oriented SiC layer or a cross section perpendicular to the plate surface is measured.
  • the substantially in-plane direction of the plate may be oriented in a specific direction (for example, the a-axis) orthogonal to the c-axis.
  • the biaxially oriented SiC layer may be oriented biaxially in the substantially normal direction and the substantially in-plane direction, but the substantially normal direction is preferably oriented in the c-axis. The smaller the tilt angle distribution in the substantially normal direction and/or the substantially in-plane direction, the smaller the mosaic property of the biaxially oriented SiC layer.
  • the tilt angle distribution is preferably small both in the normal direction and in the plate surface direction, for example ⁇ 5° or less, and more preferably ⁇ 3° or less. .
  • the biaxially oriented SiC layer oriented in the c-axis direction and the a-axis direction has a depth ( ⁇ m) on the horizontal axis and the TSD density (cm ⁇ 2 ) on the vertical axis, the graph preferably includes at least a part of the TSD gradient region.
  • This TSD graded region effectively contributes to the realization of a SiC substrate with a very low surface TSD density.
  • This TSD slope region is a region in which the TSD density decreases with a constant slope a as the depth decreases.
  • the absolute value of the slope a is 5.0 cm ⁇ 2 / ⁇ m or more, preferably 5.0 to 25 cm ⁇ 2 / ⁇ m, more preferably 10 to 25 cm ⁇ 2 / ⁇ m, still more preferably 15 to 25 cm ⁇ 2 / ⁇ m. ⁇ m.
  • This slope a can be calculated, for example, by obtaining an approximate straight line using the least squares method in the TSD slope region of the above graph.
  • "The depth from the (0001) plane, which is the substrate surface, to an arbitrary (000-1) plane” is the (0001) plane of the biaxially oriented SiC layer surface in the biaxially oriented SiC layer on the SiC single crystal substrate. to the back surface direction of the biaxially oriented SiC layer on the side of the SiC single crystal substrate.
  • the biaxially oriented SiC layer preferably contains boron in a concentration of 1.0 ⁇ 10 16 to 1.0 ⁇ 10 17 atoms/cm 3 , more preferably 1.0 ⁇ 10 16 to 9.5 ⁇ 10 16 . atoms/ cm3 .
  • boron content it is possible to preferably control the PL intensity distribution in the above-described PL graph, and effectively obtain a SiC substrate with a reduced TSD density on the substrate surface. can be done.
  • the SiC substrate of the present invention may be a self-supporting substrate consisting of only a SiC substrate, or may be in the form of a SiC composite substrate.
  • the SiC composite substrate may include a SiC single crystal substrate and the above-described SiC substrate on the SiC single crystal substrate.
  • a SiC single crystal substrate is typically a layer composed of SiC single crystal and has a crystal growth surface.
  • the polytype, off angle, and polarity of the SiC single crystal are not particularly limited, but the polytype is preferably 4H or 6H, and the off angle is 0.1 to 12° from the [0001] axis of single crystal SiC.
  • the polarity is the Si face. More preferably, the polytype is 4H, the off angle is 1 to 5° from the [0001] axis of the single crystal SiC, and the polarity is the Si plane.
  • the SiC substrate of the present invention may be in the form of a self-supporting substrate with a single biaxially oriented SiC layer, or may be in the form of a SiC composite substrate accompanied by a SiC single crystal substrate. Therefore, if desired, the biaxially oriented SiC layer may finally be separated from the SiC single crystal substrate. Separation of the SiC single crystal substrate may be performed by a known method, and is not particularly limited. For example, a method of separating a biaxially oriented SiC layer by a wire saw, a method of separating a biaxially oriented SiC layer by electrical discharge machining, a method of separating a biaxially oriented SiC layer by using a laser, and the like can be mentioned.
  • the biaxially oriented SiC layer may be placed on another support substrate after separating the SiC single crystal substrate.
  • the material of the other support substrate is not particularly limited, but a suitable material may be selected from the viewpoint of material properties.
  • metal substrates such as Cu, ceramic substrates such as SiC and AlN, and the like can be used.
  • a SiC composite substrate comprising the SiC substrate of the present invention is produced by (a) forming a predetermined orientation precursor layer on a SiC single crystal substrate, and (b) forming an orientation precursor layer on the SiC single crystal substrate. is heat treated to convert at least a portion near the SiC single crystal substrate to a SiC substrate (biaxially oriented SiC layer), and if desired, (c) processing such as grinding or polishing is performed to expose the surface of the biaxially oriented SiC layer.
  • the manufacturing method may be a vapor phase method such as CVD or sublimation, a liquid phase method such as a solution method, or a solid phase method utilizing grain growth.
  • the distribution of the PL intensity in the graph obtained by PL can be obtained by controlling the heat treatment conditions in (b) above, or by adding boron or a boron compound (e.g., boron carbide, etc.) when forming the alignment precursor layer in (a) above.
  • a SiC substrate having a biaxially oriented SiC layer is analyzed by PL, a SiC substrate having a specific analysis result as described above can be manufactured. can significantly reduce the TSD density on the surface of the SiC composite substrate.
  • FIG. 1 is a vertical cross-sectional view of SiC composite substrate 10 (a cross-sectional view when SiC composite substrate 10 is cut vertically along a plane including the central axis of SiC composite substrate 10), and FIG. It is a diagram.
  • the SiC composite substrate 10 of this embodiment includes a SiC single crystal substrate 20 and a SiC substrate 30 on the SiC single crystal substrate (corresponding to the SiC substrate of the present invention).
  • the orientation precursor layer 40 becomes the SiC substrate (biaxially oriented SiC layer) 30 by heat treatment described later.
  • the orientation precursor layer 40 is formed on the crystal growth surface of the SiC single crystal substrate 20 .
  • a known method can be adopted as a method for forming the alignment precursor layer 40 .
  • the method of forming the alignment precursor layer 40 includes, for example, solid-phase deposition methods such as AD (aerosol deposition) method and HPPD (supersonic plasma particle deposition method) method, sputtering method, vapor deposition method, sublimation method, various CVD ( Chemical vapor deposition) method and other vapor deposition methods, and solution deposition methods and other liquid phase deposition methods can be mentioned, and a method of directly forming the orientation precursor layer 40 on the SiC single crystal substrate 20 can be used. .
  • solid-phase deposition methods such as AD (aerosol deposition) method and HPPD (supersonic plasma particle deposition method) method
  • sputtering method vapor deposition method, sublimation method
  • various CVD ( Chemical vapor deposition) method and other vapor deposition methods and solution deposition methods and other liquid phase deposition methods can be mentioned
  • the CVD method for example, a thermal CVD method, a plasma CVD method, a mist CVD method, an MO (organometal) CVD method, or the like can be used.
  • the orientation precursor layer 40 a polycrystalline body previously prepared by sublimation, various CVD methods, sintering, or the like may be used and placed on the SiC single crystal substrate 20.
  • a method of preparing a molded body of the orientation precursor layer 40 in advance and placing the molded body on the SiC single crystal substrate 20 may be used.
  • Such an orientation precursor layer 40 may be a tape compact produced by tape molding, or may be a powder compact produced by pressure molding such as uniaxial pressing.
  • the raw material of the alignment precursor layers 40 contains a boron compound.
  • the boron compound include, but are not limited to, boron carbide.
  • the concentration of boron in the finally obtained biaxially oriented SiC layer can be controlled by controlling the amount of the boron compound added.
  • the SiC single crystal substrate 20 can be formed without going through the heat treatment process described later. , epitaxial growth occurs, and the SiC substrate 30 may be deposited.
  • the orientation precursor layer 40 is in an unoriented state at the time of formation, that is, amorphous or non-oriented polycrystal, and is preferably oriented using a SiC single crystal as a seed in a subsequent heat treatment step. By doing so, crystal defects reaching the surface of the SiC substrate 30 can be effectively reduced.
  • a method of forming the directly oriented precursor layer 40 on the SiC single crystal substrate 20 by the AD method or various CVD methods, or a polycrystalline body separately prepared by a sublimation method, various CVD methods, sintering or the like is used as the SiC single crystal substrate. 20 is preferred.
  • the alignment precursor layer 40 can be formed in a relatively short time.
  • the AD method is particularly preferred because it does not require a high-vacuum process and its film formation speed is relatively high.
  • it is necessary to sufficiently smooth the surface of the polycrystal. is necessary.
  • the technique of directly forming the alignment precursor layer 40 is preferable.
  • a method of placing a prefabricated compact on the SiC single crystal substrate 20 is also preferable as a simple method. need.
  • known conditions can be used for either method, the following describes a method of forming a directly aligned precursor layer 40 on a SiC single crystal substrate 20 by an AD method or a thermal CVD method, and a method of forming a prefabricated molded body into a SiC single crystal. A method of mounting on the crystal substrate 20 will be described.
  • the AD method is a technique in which fine particles or fine particle raw materials are mixed with gas to form an aerosol, and the aerosol is sprayed at high speed from a nozzle to collide with a substrate to form a coating, and is characterized by being able to form a coating at room temperature.
  • FIG. 3 shows an example of a film forming apparatus (AD apparatus) used in such an AD method.
  • the AD apparatus 50 shown in FIG. 3 is configured as an apparatus used for the AD method in which raw material powder is jetted onto a substrate under an atmosphere of pressure lower than the atmospheric pressure.
  • the AD device 50 includes an aerosol generating section 52 that generates an aerosol of raw material powder containing raw material components, and a film forming section 60 that injects the raw material powder onto the SiC single crystal substrate 20 to form a film containing the raw material components.
  • the aerosol generation unit 52 includes an aerosol generation chamber 53 that contains raw material powder and receives carrier gas supplied from a gas cylinder (not shown) to generate an aerosol, a raw material supply pipe 54 that supplies the generated aerosol to the film formation unit 60, It has an aerosol generation chamber 53 and a vibrator 55 for applying vibrations to the aerosol therein at a frequency of 10 to 100 Hz.
  • the film forming section 60 includes a film forming chamber 62 for injecting an aerosol onto the SiC single crystal substrate 20, a substrate holder 64 arranged inside the film forming chamber 62 for fixing the SiC single crystal substrate 20, and the substrate holder 64 being arranged in an X direction. and an XY stage 63 that moves in the axial-Y direction.
  • the film forming section 60 includes an injection nozzle 66 having a slit 67 formed at its tip for injecting an aerosol onto the SiC single crystal substrate 20 and a vacuum pump 68 for reducing the pressure in the film forming chamber 62 .
  • the injection nozzle 66 is attached to the tip of the raw material supply pipe 54 .
  • the AD method it is known that depending on the film formation conditions, pores may be generated in the film or the film may become a compact. For example, it is easily affected by the collision speed of the raw material powder against the substrate, the particle size of the raw material powder, the aggregation state of the raw material powder in the aerosol, the injection amount per unit time, and the like.
  • the collision speed of the raw material powder against the substrate is affected by the differential pressure between the film formation chamber 62 and the injection nozzle 66, the opening area of the injection nozzle, and the like. Therefore, it is necessary to appropriately control these factors in order to obtain a dense alignment precursor layer.
  • the raw material gas is not particularly limited, but silicon tetrachloride (SiCl 4 ) gas and silane (SiH 4 ) gas are used as Si supply sources, and methane (CH 4 ) gas and propane (C 3 H 8 ) gas or the like can be used.
  • the film formation temperature is preferably 1000 to 2200.degree. C., more preferably 1100 to 2000.degree. C., even more preferably 1200 to 1900.degree.
  • the orientation precursor layer 40 when the orientation precursor layer 40 is formed on the SiC single crystal substrate 20 using the thermal CVD method, epitaxial growth may occur on the SiC single crystal substrate 20 to form the SiC substrate 30. .
  • the orientation precursor layer 40 is not oriented at the time of its fabrication, that is, is amorphous or non-oriented polycrystal, and crystal rearrangement may occur during the heat treatment process using a SiC single crystal as a seed crystal. preferable.
  • the film formation temperature, Si source and C source gas flow rates and their ratios, film formation pressure, etc. are affected. It has been known.
  • the film formation temperature is preferably low, preferably less than 1700° C., more preferably 1500° C. or less, and even more preferably 1400° C. or less.
  • the film formation temperature is too low, the film formation rate itself will also decrease, so from the viewpoint of the film formation rate, a higher film formation temperature is preferable.
  • the orientation precursor layer 40 can be produced by molding raw material powder of the orientation precursor.
  • the orientation precursor layer 40 is a press molding.
  • the press-formed body can be produced by press-molding the raw material powder of the orientation precursor based on a known technique. It may be produced by pressing with a pressure of up to 300 kgf/cm 2 .
  • the molding method is not particularly limited, and in addition to press molding, tape molding, extrusion molding, cast molding, doctor blade method, and any combination thereof can be used.
  • additives such as a binder, a plasticizer, a dispersant, and a dispersion medium are appropriately added to the raw material powder to form a slurry, and the slurry is passed through a thin slit-shaped discharge port to form a sheet.
  • Dispensing and molding are preferred.
  • the thickness of the sheet-shaped molding is not limited, it is preferably 5 to 500 ⁇ m from the viewpoint of handling. Further, when a thick orientation precursor layer is required, a large number of such sheet moldings may be stacked to obtain a desired thickness.
  • the compact may contain additives such as a sintering aid in addition to the SiC raw material.
  • a SiC substrate 30 is produced by heat-treating a laminate obtained by laminating or placing an orientation precursor layer 40 on a SiC single crystal substrate 20.
  • the heat treatment method is not particularly limited as long as epitaxial growth occurs using the SiC single crystal substrate 20 as a seed, and a known heat treatment furnace such as a tubular furnace or a hot plate can be used.
  • a known heat treatment furnace such as a tubular furnace or a hot plate
  • pressure heat treatments such as hot pressing and HIP, and combinations of normal pressure heat treatments and pressure heat treatments can also be used.
  • the heat treatment atmosphere can be selected from vacuum, nitrogen, and inert gas atmospheres.
  • the heat treatment temperature is preferably 1700-2700°C.
  • the heat treatment temperature is preferably 1700° C. or higher, more preferably 1850° C. or higher, still more preferably 2000° C. or higher, and particularly preferably 2200° C. or higher.
  • the heat treatment temperature is preferably 2700° C. or lower, more preferably 2500° C. or lower.
  • the heat treatment conditions affect the PL intensity distribution in the graph obtained from the PL of the surface of the biaxially oriented SiC layer, so it is preferable to appropriately control the conditions (for example, heat treatment temperature and holding time).
  • the heat treatment temperature is preferably 2000 to 2700°C, more preferably 2200 to 2600°C, still more preferably 2400 to 2500°C.
  • the holding time is preferably 2 to 30 hours, more preferably 4 to 20 hours.
  • the heat treatment temperature and holding time are also related to the thickness of the SiC substrate 30 produced by epitaxial growth, and can be appropriately adjusted.
  • the alignment precursor layer 40 when using a pre-fabricated molded body as the alignment precursor layer 40, it is necessary to sinter it during the heat treatment, and high-temperature normal pressure firing, hot pressing, HIP, or a combination thereof is suitable.
  • the surface pressure is preferably 50 kgf/cm 2 or more, more preferably 100 kgf/cm 2 or more, still more preferably 200 kgf/cm 2 or more, with no particular upper limit.
  • the sintering temperature is not particularly limited as long as sintering and epitaxial growth occur.
  • the firing conditions affect the PL intensity distribution in the graph obtained from the PL of the surface of the biaxially oriented SiC layer, it is preferable to appropriately control the conditions (for example, firing temperature and holding time).
  • the firing temperature is preferably 1700 to 2700°C.
  • the holding time is preferably 2 to 18 hours.
  • the atmosphere during firing can be selected from vacuum, nitrogen, inert gas atmosphere, or mixed gas of nitrogen and inert gas.
  • SiC powder as a raw material may be either ⁇ -SiC powder or ⁇ -SiC powder, but ⁇ -SiC powder is preferable.
  • the SiC powder preferably consists of SiC particles with an average particle size of 0.01 to 100 ⁇ m. Note that the average particle diameter refers to the average value obtained by observing the powder with a scanning electron microscope and measuring the unidirectional maximum diameter of 100 primary particles.
  • the crystals in the orientation precursor layer 40 grow from the crystal growth surface of the SiC single crystal substrate 20 while being oriented along the c-axis and the a-axis. , it changes to the SiC substrate 30 .
  • a SiC composite substrate including the produced SiC substrate 30 has a reduced TSD density on the substrate surface. The reason for this is unknown, but it is believed that the distribution of the PL intensity reflects the step-terrace structure that occurs during crystal growth, and the TSDs were converted to stacking faults along with the crystal growth.
  • the present invention is by no means limited to the above-described embodiments, and can be implemented in various forms as long as they fall within the technical scope of the present invention.
  • only one layer of SiC substrate 30 is provided on SiC single crystal substrate 20, but two or more layers may be provided.
  • the alignment precursor layer 40 is laminated on the SiC substrate 30 of the SiC composite substrate 10, and heat treatment and grinding are performed in this order, so that the SiC substrate 30 as the second layer can be provided on the SiC substrate 30. can.
  • Example 1 Preparation of Orientation Precursor Layer 90.8% by weight of commercially available fine ⁇ -SiC powder (volume-based D50 particle size: 0.7 ⁇ m) and yttrium oxide powder (volume-based D50 particle size: 0.1 ⁇ m)8.
  • Raw material powder containing 1% by weight and 1.1% by weight of silicon dioxide powder (volume-based D50 particle size: 0.7 ⁇ m) is mixed by ball mill mixing for 24 hours in ethanol using SiC balls and drying. A powder was obtained.
  • a commercially available SiC single crystal substrate n-type 4H—SiC, diameter 100 mm (4 inches), Si plane, (0001) plane, off angle 4°, thickness 0.35 mm, no orientation flat
  • An AD film orientation precursor layer was formed by injecting the mixed powder onto the SiC single crystal substrate by the device 50 .
  • AD film forming conditions were as follows. First, N2 was used as a carrier gas, and a film was formed using a ceramic nozzle having a slit with a long side of 5 mm and a short side of 0.4 mm.
  • the nozzle scanning conditions were a scan speed of 0.5 mm/s, a movement of 105 mm in the forward direction perpendicular to the long side of the slit, a 5 mm movement in the long side of the slit, and a return perpendicular to the long side of the slit.
  • the thickness of the AD film thus formed was about 400 ⁇ m.
  • the (0001) plane (that is, the surface of the heat-treated layer) of the SiC composite substrate in which the heat-treated layer is formed on the SiC single crystal substrate is polished with diamond abrasive grains (particle size: 3.0 ⁇ m, 1.0 ⁇ m, 0.5 ⁇ m, and 0.1 ⁇ m) were used in descending order of particle size and polished to achieve the target thickness and surface condition.
  • the (000-1) plane of the SiC composite substrate having a heat-treated layer formed on the SiC single crystal substrate is ground with a grinder (1000 to 6000 diamond wheel). It was surface-ground to a predetermined thickness. Subsequently, diamond abrasive grains (particle sizes of 3.0 ⁇ m, 1.0 ⁇ m, 0.5 ⁇ m and 0.1 ⁇ m) were used in descending order of particle size for polishing. As a result, the entire SiC single crystal substrate was ground to obtain a substrate (SiC substrate) consisting only of the heat-treated layer.
  • a graph was created in which the distance ( ⁇ m) in the [11-20] direction was plotted on the horizontal axis and the PL intensity I was plotted on the vertical axis.
  • the graph had a shape of repeating maxima and minima.
  • the maximum point is a point that gives a higher PL intensity I than each of the six PL intensities I in total consisting of the first, second and third closest points on the left and right, and , confirm that the minimum point is a point that gives a lower PL intensity I than each of the total 6 points consisting of the 1st, 2nd and 3rd closest points on the left and right bottom. Also, from FIG.
  • the maximum value of the PL intensity I at a certain maximum point PM is defined as M, and the distance in the horizontal axis direction is longer than this maximum point PM , and the local minimum at the position closest to this maximum point PM M/m was calculated, where m is the minimum value of PL intensity I at point Pm . Furthermore, the distance L in the [11-20] direction between the maximum point P M and the minimum point P m was measured. The results were as shown in Table 1. The measurement conditions at this time were as shown below. From FIG. 4, it was found that the step width of the step-terrace structure on the surface of the heat-treated layer was as wide as about 100 to 200 ⁇ m.
  • image processing software (product name: WinROOF2015) was used to process 5 ⁇ 5 in the [11-20] direction. was processed by a Prewitt filter with a kernel of The results are shown in FIG.
  • a line segment of 500 ⁇ m parallel to the [11-20] direction (indicated by the lower left line segment in FIG. 6) was drawn at an arbitrary position in the filtered image.
  • a graph was prepared by plotting the distance ( ⁇ m) in the [11-20] direction on the horizontal axis and the PL intensity IF on the vertical axis in the line segment area. The graph is shown in FIG. This graph had a shape in which multiple maximum points were repeated.
  • the maximum point is the point that gives a higher PL intensity IF than each of the total 6 PL intensity IF points consisting of the first, second and third closest points on the left and right. It was confirmed.
  • a maximum point P M1 and a maximum point P M2 that is at a longer distance in the horizontal axis direction than this maximum point P M1 and that is closest to this maximum point P M1 [ 11- 20] direction distance L F was measured. The results were as shown in Table 1.
  • Threading screw dislocation (TSD) density of heat-treated layer (biaxially oriented SiC layer) SiC composite substrate obtained by above (1) to (3-1) was processed into chips by above (4) Using the sample as an evaluation sample, the TSD density (cm ⁇ 2 ) of the biaxially oriented SiC layer was measured. An evaluation sample was placed in a crucible made of nickel together with a KOH crystal, and etched in an electric furnace at 500° C. for 10 minutes. After the etching treatment, the evaluation sample was washed, the surface was observed with an optical microscope, and the type of dislocation was determined from the shape of the pits.
  • the TSD density was measured with a shell-shaped pit as a basal plane dislocation, a small hexagonal pit as a threading edge dislocation, and a medium or large hexagonal pit as a TSD.
  • the surface of this evaluation sample is polished in the same procedure as in (3-1) above, and the etching process and TSD density measurement are repeated multiple times in the same manner as described above to obtain the TSD density at multiple depths. bottom.
  • the horizontal axis represents the depth (polishing thickness) ( ⁇ m) from the (0001) plane, which is the substrate surface of the evaluation sample, to an arbitrary (000-1) plane, and the TSD density ( cm ⁇ 2 ) was plotted on the vertical axis.
  • the area where the TSD density increases from the (0001) plane to the (000-1) plane (the area where the polishing thickness is about 380 to 400 ⁇ m), that is, from the (0001) plane to any (000-1)
  • a region where the TSD density decreases with a constant slope a as the depth to the surface decreases is defined as a TSD gradient region.
  • a TSD gradient region In this graph of the TSD gradient area, an approximate straight line was obtained by the method of least squares, and the absolute value of the gradient a of the TSD density with respect to the polishing thickness was obtained.
  • the TSD density of the (0001) plane of the evaluation sample with a polishing thickness of 50 ⁇ m was regarded as the TSD density of the SiC substrate surface and measured. The results were as shown in Table 1.
  • Example 2 (Comparison) A SiC substrate was produced and evaluated in the same manner as in Example 1, except that the annealing temperature was set to 2200° C. in (2) above. It was confirmed that the heat-treated layer of the obtained SiC substrate was a biaxially oriented SiC layer. The results were as shown in Table 1.
  • Example 3 8. In (1) above, 85.8% by weight of fine ⁇ -SiC powder (volume-based D50 particle size: 0.7 ⁇ m) and yttrium oxide powder (volume-based D50 particle size: 0.1 ⁇ m)8. A powder containing 1% by weight, 1.1% by weight of silicon dioxide powder (volume-based D50 particle size: 0.7 ⁇ m), and 5.0% by weight of boron carbide powder (volume-based D50 particle size: 0.5 ⁇ m) was used. A SiC substrate was produced and evaluated in the same manner as in Example 1 except for the above. It was confirmed that the heat-treated layer of the obtained SiC substrate was a biaxially oriented SiC layer. The results were as shown in Table 1.
  • Example 4 8. In (1) above, 80.8% by weight of fine ⁇ -SiC powder (volume-based D50 particle size: 0.7 ⁇ m) and yttrium oxide powder (volume-based D50 particle size: 0.1 ⁇ m)8. A powder containing 1% by weight, 1.1% by weight of silicon dioxide powder (volume-based D50 particle size: 0.7 ⁇ m), and 10.0% by weight of boron carbide powder (volume-based D50 particle size: 0.5 ⁇ m) was used. A SiC substrate was produced and evaluated in the same manner as in Example 1 except for the above. It was confirmed that the heat-treated layer of the obtained SiC substrate was a biaxially oriented SiC layer. The results were as shown in Table 1.
  • example 5 8.
  • fine ⁇ -SiC powder volume-based D50 particle size: 0.7 ⁇ m
  • yttrium oxide powder volume-based D50 particle size: 0.1 ⁇ m
  • a powder containing 1% by weight, 1.1% by weight of silicon dioxide powder volume-based D50 particle size: 0.7 ⁇ m
  • 20.0% by weight of boron carbide powder volume-based D50 particle size: 0.5 ⁇ m
  • a SiC substrate was produced and evaluated in the same manner as in Example 1 except for the above. It was confirmed that the heat-treated layer of the obtained SiC substrate was a biaxially oriented SiC layer. The results were as shown in Table 1.
  • Example 6 (Comparison) 8.
  • 60.8% by weight of fine ⁇ -SiC powder volume-based D50 particle size: 0.7 ⁇ m
  • yttrium oxide powder volume-based D50 particle size: 0.1 ⁇ m
  • a powder containing 1% by weight, 1.1% by weight of silicon dioxide powder volume-based D50 particle size: 0.7 ⁇ m
  • 30.0% by weight of boron carbide powder volume-based D50 particle size: 0.5 ⁇ m
  • a SiC substrate was produced and evaluated in the same manner as in Example 1 except for the above. It was confirmed that the heat-treated layer of the obtained SiC substrate was a biaxially oriented SiC layer. The results were as shown in Table 1.
  • Example 7 A SiC substrate was produced and evaluated in the same manner as in Example 1, except that the annealing temperature was set to 2350° C. in (2) above. It was confirmed that the heat-treated layer of the obtained SiC substrate was a biaxially oriented SiC layer. The results were as shown in Table 1.
  • the distribution of the PL intensity with respect to the distance in the [11-20] direction can be controlled by the annealing temperature and the boron content.
  • the ratio of M / m is 1.05 or more and the distance L is 15 to 150 ⁇ m, or
  • the distance LF is 30 to 300 ⁇ m, so that the TSD density of the (0001) plane of the evaluation sample with a polishing thickness of 50 ⁇ m, that is, biaxial orientation It was found that the TSD density on the SiC layer surface can be reduced.
  • a SiC substrate provided with a biaxially oriented SiC layer having a TSD gradient region in which the TSD density is reduced in a and the absolute value of the gradient a is 5.0 cm ⁇ 2 / ⁇ m or more is the biaxially oriented SiC layer It has been found that the surface TSD density can be effectively reduced.
  • the step width of the step-terrace structure on the surface of the biaxially oriented SiC layer of the SiC substrate showing an example of the present invention is as wide as about 100 to 200 ⁇ m.
  • Non-Patent Document 2 (Toru Ujihara et al. “Conversion Mechanism of Threading Screw Dislocation during SiC Solution Growth” Materials Science Forum Vols. 717-720, pp. 351-354 (2012)), shown in FIG.
  • the step width on the surface of the SiC substrate produced by the solution growth method is as narrow as 20 ⁇ m or less. It is considered that such a step-terrace structure difference affects the TSD density on the SiC substrate surface.

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JPH11228295A (ja) * 1998-02-04 1999-08-24 Nippon Pillar Packing Co Ltd 単結晶ＳｉＣ及びその製造方法
JP2004533720A (ja) * 2001-05-11 2004-11-04 クリー　インコーポレイテッド 高い降伏電圧を有する半導体デバイスのための高抵抗率炭化珪素基板
JP2014043369A (ja) 2012-08-26 2014-03-13 Nagoya Univ ＳｉＣ単結晶の製造方法およびＳｉＣ単結晶

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JPH11228295A (ja) * 1998-02-04 1999-08-24 Nippon Pillar Packing Co Ltd 単結晶ＳｉＣ及びその製造方法
JP2004533720A (ja) * 2001-05-11 2004-11-04 クリー　インコーポレイテッド 高い降伏電圧を有する半導体デバイスのための高抵抗率炭化珪素基板
JP2014043369A (ja) 2012-08-26 2014-03-13 Nagoya Univ ＳｉＣ単結晶の製造方法およびＳｉＣ単結晶

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See also references of EP4421221A4
TORU UJIHARA ET AL.: "Conversion Mechanism of Threading Screw Dislocation during SiC Solution Growth", MATERIALS SCIENCE FORUM, vol. 717-720, 2012, pages 351 - 354

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