WO2024202200A1 - 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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WO2024202200A1
WO2024202200A1 PCT/JP2023/040962 JP2023040962W WO2024202200A1 WO 2024202200 A1 WO2024202200 A1 WO 2024202200A1 JP 2023040962 W JP2023040962 W JP 2023040962W WO 2024202200 A1 WO2024202200 A1 WO 2024202200A1
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sic
substrate
layer
biaxially oriented
single crystal
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English (en)
French (fr)
Japanese (ja)
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真也 松川
陽平 岡田
潔 松島
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NGK Insulators Ltd
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NGK Insulators Ltd
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Priority to EP23930828.1A priority Critical patent/EP4692430A1/en
Priority to CN202380080022.0A priority patent/CN120858208A/zh
Priority to JP2025509693A priority patent/JPWO2024202200A1/ja
Publication of WO2024202200A1 publication Critical patent/WO2024202200A1/ja
Priority to US19/339,550 priority patent/US20260022494A1/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
    • 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
    • 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
    • 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
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/18—Epitaxial-layer growth characterised by the substrate
    • C30B25/20—Epitaxial-layer growth characterised by the substrate the substrate being of the same materials as the epitaxial layer
    • 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
    • C30B33/02—Heat treatment

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 smaller, consume less power, and are more efficient than those using Si semiconductors, and are therefore expected to be used in a variety of applications.
  • the adoption of SiC power devices can make it possible to miniaturize converters, inverters, on-board chargers, etc. for electric vehicles (EVs) and plug-in hybrid vehicles (PHEVs) and increase their efficiency.
  • EVs electric vehicles
  • PHEVs plug-in hybrid vehicles
  • the resulting SiC single crystal substrate contains many dislocations, which are roughly divided into three types: basal plane dislocations (BPDs), threading screw dislocations (TSDs), and edge dislocations (TEDs).
  • BPDs basal plane dislocations
  • TSDs threading screw dislocations
  • TEDs edge dislocations
  • basal plane dislocations are inherited by the epitaxially grown film, and if they are present in the driving region of the device, they expand into stacking faults by current application, adversely affecting the reliability of the SiC device.
  • Patent Document 1 Japanese Patent No.
  • Patent Document 2 Japanese Patent No. 5750363 discloses a SiC single crystal including a low dislocation density region in which the volume density of dislocations (mainly basal plane dislocations and threading edge dislocations) having a Burgers vector in the ⁇ 0001 ⁇ in-plane direction is 3700 cm/ cm3 or less. It is also known that breaks and cracks occur when processing a SiC single crystal substrate.
  • Non-Patent Document 1 Y.
  • Non-Patent Document 1 SiC is extremely hard and difficult to process, and reduced yields due to fractures and cracks that occur during grinding, polishing, cutting, etc. of wafers are an issue. Although the direct cause has not been clarified, it is possible that distortion within the crystal, such as plastic deformation due to dislocations, is involved. In this regard, the dislocations present in SiC single crystals as disclosed in Patent Documents 1 and 2, are thought to be distributed unevenly, in which case fractures and cracks are more likely to occur during substrate processing such as grinding, polishing, and cutting of SiC substrates.
  • the inventors have now discovered that by providing a SiC substrate with a biaxially oriented SiC layer with few regions with extremely high BPDs (i.e., a uniform distribution of BPDs), the distortion within the crystals in the SiC substrate is reduced, and fractures and cracks during substrate processing such as grinding, polishing, and cutting can be reduced.
  • the object of the present invention is therefore to provide a SiC substrate that can reduce breakage and cracks during substrate processing.
  • a SiC substrate having a biaxially textured SiC layer A SiC substrate in which, when an entire area of an XRT image obtained by XRT measurement of the biaxially oriented SiC layer is partitioned into a lattice pattern with each square being an area of 4 mm length ⁇ 4 mm width ⁇ 28 ⁇ m depth, and when the average value of the volume density of basal plane dislocations (BPDs) per square is X (cm/ cm3 ), there are no areas with a density of 5X (cm/ cm3 ) or more per square that are consecutive in a straight line vertically or horizontally for 10 squares or more.
  • BPDs basal plane dislocations
  • Aspect 3 The SiC substrate according to aspect 1 or 2 , wherein when the entire area of the XRT image is divided into a lattice shape with each square being an area of 4 mm in length and 4 mm in width, and the average number density of threading screw dislocations (TSDs) per square is Y (/ cm2 ), there are no areas with 10 or more consecutive squares in a straight line in either the vertical or horizontal direction.
  • FIG. 2 is a longitudinal sectional view of the SiC composite substrate 10.
  • 1 is a manufacturing process diagram of a SiC composite substrate 10.
  • FIG. 1 is a conceptual diagram showing the configuration of an aerosol deposition (AD) device 50.
  • FIG. 1 is a schematic diagram showing regions in the sample of Example 1 where one square has a density of 5X (cm/cm 3 ) or more, analyzed from the XRT image, and the regions are displayed with black squares.
  • the SiC substrate according to the present invention includes a biaxially oriented SiC layer.
  • an XRT image obtained by measuring the biaxially oriented SiC layer with an XRT when the entire XRT image is divided into a lattice shape with an area of 4 mm length x 4 mm width x 28 ⁇ m depth per square, the average value of the volume density of basal plane dislocations (BPDs) per square is X (cm/cm 3 ).
  • BPDs basal plane dislocations
  • no consecutive areas of 10 squares or more in either direction refers to counting only the number of squares consecutive in a straight line vertically and the number of squares consecutive in a straight line horizontally, and not the number of squares consecutive in a straight line diagonally.
  • SiC is extremely hard and difficult to process, and the reduction in yield due to fractures and cracks that occur during grinding, polishing, cutting, etc. of the wafer is an issue.
  • the dislocations present in the SiC substrate are unevenly distributed, fractures and cracks are likely to occur during substrate processing such as grinding, polishing, and cutting of the SiC substrate.
  • the present invention conveniently solves such problems, and as a result, it is possible to improve the yield during the manufacture of SiC substrates.
  • the region with 5X (cm/cm 3 ) or more per square does not extend vertically or horizontally in a straight line for 10 or more squares, preferably 5 or more squares, more preferably 2 or more squares.
  • the region with 3X (cm/cm 3 ) or more per square does not extend vertically or horizontally in a straight line for 5 or more squares, more preferably 4 or more squares, even more preferably 3 or more squares.
  • the average value X of the volume density of BPDs per square is preferably 200 to 5000 cm/cm 3 .
  • the average value of the number density of TSDs per square is Y (/cm 2 )
  • the number of consecutive squares with a density of 2Y (/cm 2 ) or more per square does not extend in a straight line of 10 squares or more vertically and horizontally, and more preferably does not extend in a straight line of 6 squares or more.
  • the average value Y of the number density of TSDs per square is preferably 100 to 800/cm 2 .
  • the average value of the number density of TEDs per square is Z (/cm 2 )
  • the number of consecutive squares with a density of 2Z (/cm 2 ) or more per square does not extend in a straight line of 10 squares or more vertically and horizontally, and more preferably does not extend in a straight line of 4 squares or more.
  • the average value Z of the number density of TEDs per square is preferably 1000 to 8000/cm 2 .
  • the SiC substrate or the biaxially oriented SiC layer may have an off-angle, in which case the off-angle is preferably 0.1 to 12°, more preferably 1 to 5°, from the [0001] axis of the SiC substrate or the biaxially oriented SiC layer.
  • the biaxially oriented SiC layer preferably contains a rare earth element, examples of which include Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Sc, and combinations thereof. From the standpoint of reducing breakage and cracking, the rare earth element is preferably Y.
  • the rare earth element concentration in the biaxially textured SiC layer is preferably 2.0 ⁇ 10 14 to 5.0 ⁇ 10 15 atoms/cm 3 , and more preferably 5.0 ⁇ 10 14 to 2.0 ⁇ 10 15 atoms/cm 3.
  • the rare earth element concentration in the biaxially textured SiC layer is preferably 2.0 ⁇ 10 14 to 5.0 ⁇ 10 15 atoms/cm 3 , and more preferably 5.0 ⁇ 10 14 to 2.0 ⁇ 10 15 atoms/cm 3.
  • the biaxially oriented SiC layer is preferably oriented in the c-axis direction and the a-axis direction.
  • the SiC substrate is preferably composed of a biaxially oriented SiC layer.
  • the biaxially oriented SiC layer may be a SiC single crystal, a SiC polycrystal, or a mosaic crystal, as long as it is oriented in the two axes of the c-axis and the a-axis.
  • a mosaic crystal is a collection of crystals that do not have clear grain boundaries but have slightly different orientations in either or both of the c-axis and the a-axis.
  • the method for evaluating the orientation is not particularly limited, but known analytical methods such as the EBSD (Electron Back Scatter Diffraction Patterns) method and X-ray pole figures can be used.
  • EBSD Electro Back Scatter Diffraction Patterns
  • X-ray pole figures can be used.
  • the EBSD method 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 SiC layer when the following four conditions are satisfied, (A) the SiC layer is oriented in a specific direction (first axis) approximately normal to the plate surface, (B) the SiC layer is oriented in a specific direction (second axis) approximately in the plate surface direction perpendicular to the first axis, (C) the inclination angle from the first axis is distributed within ⁇ 10°, and (D) the inclination angle from the second axis is distributed within ⁇ 10°, the SiC layer can be defined as being oriented in two axes, the approximately normal direction and the approximately plate surface direction.
  • the SiC layer is determined to be oriented in two axes, the c-axis and the a-axis.
  • the approximately normal direction of the plate surface is oriented to the c-axis
  • the approximately in-plane direction may be oriented in a specific direction (e.g., the a-axis) perpendicular to the c-axis.
  • the biaxially oriented SiC layer may be oriented in two axes, the approximately normal direction and the approximately in-plane direction, but it is preferable that the approximately normal direction is oriented to the c-axis.
  • the tilt angle distribution in the approximately normal direction and/or the approximately in-plane direction the smaller the mosaic property of the biaxially oriented SiC layer, and the closer it is to zero, the closer it is to a single crystal. Therefore, from the viewpoint of the crystallinity of the biaxially oriented SiC layer, it is preferable that the tilt angle distribution is small in both the approximately normal direction and the approximately in-plane direction, for example, ⁇ 5° or less is more preferable, and ⁇ 3° or less is even more preferable.
  • the SiC substrate of the present invention is preferably in the form of a SiC composite substrate. That is, according to a preferred embodiment of the present invention, there is provided a SiC composite substrate comprising a SiC single crystal substrate and the above-mentioned SiC substrate on the SiC single crystal substrate. In this way, by providing the SiC composite substrate with a SiC substrate having a biaxially oriented SiC layer with few regions with extremely high BPDs (i.e., with a uniform distribution of BPDs), it is possible to reduce breakage and cracks during substrate processing.
  • the SiC single crystal substrate is typically a layer composed of a SiC single crystal, and has a crystal growth surface.
  • the SiC single crystal substrate preferably has an off angle.
  • the polytype, off angle, and polarity of the SiC single crystal are not particularly limited, but the polytype is preferably 4H or 6H, the off angle is preferably 0.1 to 12° from the [0001] axis of the single crystal SiC, and the polarity may be either the Si face or the C face. It is more preferable that the polytype is 4H, the off angle is 1 to 5° from the [0001] axis of the single crystal SiC, and the polarity may be either the Si face or the C face.
  • the SiC substrate of the present invention may be in the form of a free-standing substrate of a biaxially oriented SiC layer alone, or in the form of a SiC composite substrate accompanied by a SiC single crystal substrate. Therefore, if necessary, the biaxially oriented SiC layer may finally be separated from the SiC single crystal substrate.
  • the 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 the biaxially oriented SiC layer using a wire saw, a method of separating the biaxially oriented SiC layer using electric discharge machining, a method of separating the biaxially oriented SiC layer using a laser, etc. may be mentioned.
  • the biaxially oriented SiC layer may be placed on another support substrate.
  • the material of the other support substrate is not particularly limited, and a suitable one may be selected from the viewpoint of material properties.
  • a metal substrate such as Cu, a ceramic substrate such as SiC or AlN, etc. may be mentioned.
  • the SiC composite substrate having the SiC substrate of the present invention can be preferably manufactured by (a) forming a predetermined oriented precursor layer on a SiC single crystal substrate, (b) heat-treating the oriented precursor layer on the SiC single crystal substrate to convert at least the portion near the SiC single crystal substrate into a SiC substrate (biaxially oriented SiC layer), and optionally (c) performing processing such as grinding or polishing to expose the surface of the biaxially oriented SiC layer.
  • processing such as grinding or polishing to expose the surface of the biaxially oriented SiC layer.
  • there is no limitation on the manufacturing method of the SiC composite substrate and it is sufficient to obtain a SiC substrate having a biaxially oriented SiC layer with few regions with extremely high BPD as described above.
  • a gas phase method such as CVD or sublimation method or a liquid phase method such as a solution method may be used.
  • a gas phase method such as CVD or sublimation method
  • a liquid phase method such as a solution method
  • this manufacturing method it is possible to preferably produce a SiC substrate having a biaxially oriented SiC layer with few regions with extremely high BPDs, and it is possible to effectively reduce breakage and cracks during processing of the SiC substrate or a SiC composite substrate using the same.
  • Figure 1 is a longitudinal cross-sectional view of a SiC composite substrate 10 (a cross-sectional view of the SiC composite substrate 10 cut longitudinally along a plane including the central axis of the SiC composite substrate 10), and Figure 2 is a manufacturing process diagram for the SiC composite substrate 10.
  • the SiC composite substrate 10 of this embodiment includes a SiC single crystal substrate 20 and a SiC substrate 30 (corresponding to the SiC substrate of the present invention) on the SiC single crystal substrate.
  • the textured precursor layer 40 becomes the SiC substrate (biaxially textured SiC layer) 30 by a heat treatment described later.
  • the textured precursor layer 40 is formed on the crystal growth surface of the SiC single crystal substrate 20.
  • the method of forming the oriented precursor layer 40 can employ known methods.
  • the method of forming the oriented precursor layer 40 can be, for example, a solid-phase film formation method such as an AD (aerosol deposition) method or an HPPD (supersonic plasma particle deposition) method, a gas-phase film formation method such as a sputtering method, a vapor deposition method, a sublimation method, or various CVD (chemical vapor deposition) methods, or a liquid-phase film formation method such as a solution growth method.
  • a method of forming the oriented precursor layer 40 directly on the SiC single crystal substrate 20 can be used.
  • a thermal CVD method for example, a thermal CVD method, a plasma CVD method, a mist CVD method, an MO (metal organic) CVD method, or the like can be used.
  • a method of using a polycrystalline body prepared in advance by a sublimation method, various CVD methods, sintering, or the like as the oriented precursor layer 40 and placing it on the SiC single crystal substrate 20 can also be used.
  • a method of preparing a molded body of the oriented precursor layer 40 in advance and placing this molded body on the SiC single crystal substrate 20 may be used.
  • Such an orientation precursor layer 40 may be a tape molded body produced by tape casting, or a green compact produced by pressure molding such as a uniaxial press.
  • the raw material of the oriented precursor layer 40 contains a rare earth compound.
  • the rare earth compound is not particularly limited, but includes oxides, nitrides, carbides, and fluorides of at least one element of the above-mentioned 17 types of rare earth elements.
  • oxides of rare earth elements are preferable, and oxides of Y (yttrium oxide) are more preferable.
  • the flow rate of the carrier gas (e.g., N 2 ) used when forming the oriented precursor layer 40 can effectively control the distribution of dislocations in the biaxially oriented SiC layer.
  • the oriented precursor layer 40 In the method of forming the oriented precursor layer 40 directly on the SiC single crystal substrate 20, when various CVD methods, sublimation methods, solution growth methods, etc. are used, epitaxial growth may occur on the SiC single crystal substrate 20 without going through the heat treatment process described below, and the SiC substrate 30 may be formed.
  • the oriented precursor layer 40 is in an unoriented state when formed, that is, it is an amorphous or unoriented polycrystal, and it is preferable to orient it using the SiC single crystal as a seed in the subsequent heat treatment process. In this way, it is possible to effectively reduce crystal defects that reach the surface of the SiC substrate 30.
  • the re-arrangement of the crystal structure of the solid-phase oriented precursor layer once formed using the SiC single crystal as a seed may also be effective in eliminating crystal defects. Therefore, when various CVD methods, sublimation methods, solution growth methods, etc. are used, it is preferable to select conditions that do not cause epitaxial growth in the formation process of the oriented precursor layer 40.
  • the method of forming the oriented precursor layer 40 directly on the SiC single crystal substrate 20 by the AD method or various CVD methods, or the method of placing a polycrystalline body separately prepared by sublimation, various CVD methods, sintering, etc. on the SiC single crystal substrate 20 is preferable.
  • the AD method is particularly preferable because it does not require a high vacuum process and the film formation speed is relatively fast.
  • the method of directly forming the oriented precursor layer 40 is preferable.
  • the method of placing a pre-prepared molded body on the SiC single crystal substrate 20 is also preferable as a simple method, but since the oriented precursor layer 40 is made of powder, a sintering process is required in the heat treatment step described later. Both methods can use known conditions, but below we will describe a method of forming an orientation precursor layer 40 directly on a SiC single crystal substrate 20 by the AD method or thermal CVD method, and a method of placing a previously prepared molded body on a SiC single crystal substrate 20.
  • the AD method is a technique in which fine particles or fine particle raw material is mixed with a 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 has the characteristic that a coating can be formed at room temperature.
  • An example of a film forming apparatus (AD apparatus) used in such an AD method is shown in FIG. 3.
  • the AD apparatus 50 shown in FIG. 3 is configured as an apparatus used in the AD method in which raw material powder is sprayed onto a substrate under an atmosphere with a pressure lower than atmospheric pressure.
  • This AD apparatus 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 sprays the raw material powder onto a SiC single crystal substrate 20 to form a film containing the raw material components.
  • the aerosol generating section 52 includes an aerosol generating chamber 53 that contains raw material powder and generates an aerosol by receiving a carrier gas from a gas cylinder (not shown), a raw material supply pipe 54 that supplies the generated aerosol to the film forming section 60, and a vibrator 55 that applies vibrations at a frequency of 10 to 100 Hz to the aerosol generating chamber 53 and the aerosol therein.
  • the carrier gas include N2 .
  • the film forming section 60 includes a film forming chamber 62 that sprays an aerosol onto the SiC single crystal substrate 20, a substrate holder 64 that is disposed inside the film forming chamber 62 and fixes the SiC single crystal substrate 20, and an XY stage 63 that moves the substrate holder 64 in the X-axis and Y-axis directions.
  • the film forming unit 60 also includes an injection nozzle 66 having a slit 67 formed at its tip for injecting the 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 may cause pores in the film or the film may become a compact depending on the deposition conditions. For example, it is easily affected by the impact speed of the raw material powder with the substrate, the particle size of the raw material powder, the agglomeration state of the raw material powder in the aerosol, the amount sprayed per unit time, etc.
  • the impact speed of the raw material powder with the substrate is affected by the pressure difference between the deposition chamber 62 and the spray nozzle 66, the opening area of the spray nozzle, etc. Therefore, in order to obtain a dense oriented precursor layer, it is necessary to appropriately control these factors. In particular, in order to effectively control the distribution of dislocation density in the biaxially oriented SiC layer, it is preferable to control, for example, the opening area of the spray nozzle (nozzle size).
  • the source gas is not particularly limited, but silicon tetrachloride (SiCl 4 ) gas or silane (SiH 4 ) gas can be used as a Si source, and methane (CH 4 ) gas or propane (C 3 H 8 ) gas can be used as a C source.
  • the film forming temperature is preferably 1000 to 2200°C, more preferably 1100 to 2000°C, and even more preferably 1200 to 1900°C.
  • the oriented precursor layer 40 is not oriented when it is produced, that is, it is amorphous or unoriented polycrystalline, and it is preferable to use a SiC single crystal as a seed crystal during the heat treatment process to cause crystal rearrangement. It is known that the film formation temperature, the gas flow rate of the Si source and the C source and their ratio, the film formation pressure, etc. have an effect on the formation of an amorphous or polycrystalline layer on a SiC single crystal using a thermal CVD method.
  • the film formation temperature has a large effect, and from the viewpoint of forming an amorphous or polycrystalline layer, a low film formation temperature is preferable, preferably less than 1700°C, more preferably 1500°C or less, and even more preferably 1400°C or less. However, if the film formation temperature is too low, the film formation rate itself also decreases, so from the viewpoint of the film formation rate, a high film formation temperature is preferable.
  • the orientation precursor layer 40 can be prepared by molding the raw material powder of the orientation precursor.
  • the orientation precursor layer 40 is a press molded body.
  • the press molded body can be prepared by press molding the raw material powder of the orientation precursor based on a known method, for example, by putting the raw material powder into a mold and pressing it at a pressure of preferably 100 to 400 kgf/cm 2 , more preferably 150 to 300 kgf/cm 2.
  • there is no particular limitation on the molding method and in addition to press molding, tape molding, extrusion molding, casting molding, doctor blade method, and any combination thereof can be used.
  • additives such as binders, plasticizers, dispersants, and dispersion media are appropriately added to the raw material powder to make a slurry, and the slurry is preferably discharged and molded into a sheet by passing it through a thin slit-shaped discharge port.
  • the thickness of the molded body molded into a sheet there is no limitation on the thickness of the molded body molded into a sheet, but from the viewpoint of handling, it is preferable that it is 5 to 500 ⁇ m.
  • a number of these sheet molded bodies may be stacked and used to obtain the desired thickness. These molded bodies are then heat-treated on the SiC single crystal substrate 20, and the portions near the SiC single crystal substrate 20 become the SiC substrate 30.
  • the molded body it is necessary to sinter the molded body in the heat treatment process described below. It is preferable to form the SiC substrate 30 after the molded body is sintered and integrated with the SiC single crystal substrate 20 as a polycrystalline body. If the molded body does not go through the sintered state, epitaxial growth using the SiC single crystal as a seed may not occur sufficiently. For this reason, the molded body may contain additives such as sintering aids in addition to the SiC raw material.
  • the SiC substrate 30 is generated by heat treating a laminate in which the orientation precursor layer 40 is laminated or placed on the 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 can be performed in a known heat treatment furnace such as a tubular furnace or a hot plate. In addition to these normal pressure (pressless) heat treatments, pressurized heat treatments such as hot pressing and HIP, and combinations of normal pressure heat treatment and pressurized heat treatment can also be used.
  • the heat treatment atmosphere can be selected from vacuum, nitrogen, inert gas, and combinations thereof.
  • the heat treatment temperature is preferably 1700 to 2700° C.
  • the heat treatment temperature is preferably 1700°C or higher, more preferably 1800°C or higher, even more preferably 1900°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 concentration of rare earth elements in the biaxially oriented SiC layer and the distribution of dislocation density in the biaxially oriented SiC layer
  • the heat treatment temperature is preferably 2200 to 2600°C, more preferably 2390 to 2500°C, even more preferably 2400 to 2500°C, and particularly preferably 2400 to 2450°C.
  • the holding time is preferably 2 to 30 hours, more preferably 4 to 20 hours.
  • the heat treatment may be performed in multiple stages. Even in such a case, the heat treatment temperature and the total holding time are preferably within the above ranges.
  • the heat treatment temperature and the holding time are related to the thickness of the SiC substrate 30 produced by epitaxial growth, and can be appropriately adjusted.
  • the orientation precursor layer 40 when a molded body prepared in advance is used as the orientation precursor layer 40, it is necessary to sinter it during the heat treatment, and high-temperature atmospheric sintering, 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, and even more preferably 200 kgf/cm 2 or more, and there is no particular upper limit.
  • the sintering temperature is also not particularly limited as long as sintering and epitaxial growth occur.
  • the sintering conditions affect the concentration of rare earth elements in the biaxially oriented SiC layer and the distribution of dislocations in the biaxially oriented SiC layer
  • the conditions for example, the sintering temperature and holding time.
  • the sintering temperature is preferably 1700 to 2700 ° C.
  • the holding time is preferably 2 to 18 hours.
  • the atmosphere during sintering can be selected from vacuum, nitrogen, inert gas atmosphere, or a mixed gas of nitrogen and inert gas.
  • the firing may be performed in a plurality of stages, and the firing temperature and the total holding time are preferably within the above ranges.
  • the crystals in the oriented precursor layer 40 preferably grow from the crystal growth surface of the SiC single crystal substrate 20 while being oriented along the c-axis and a-axis, so that the oriented precursor layer 40 gradually changes from the crystal growth surface into the SiC substrate 30.
  • the SiC composite substrate including the resulting SiC substrate 30 has reduced breakage and cracks during substrate processing.
  • Example 1 (1) Preparation of Oriented Precursor Layer
  • Raw material powders containing 90.8% by weight of commercially available fine ⁇ -SiC powder (volume-based D50 particle size: 0.7 ⁇ m) and 9.2% by weight of yttrium oxide powder (volume-based D50 particle size: 0.1 ⁇ m) were prepared. These raw material powders were mixed in ethanol for 24 hours using SiC balls in a ball mill, and then dried to obtain a mixed powder.
  • the nozzle scan conditions were a scan speed of 0.5 mm/s, a 155 mm movement perpendicular to the long side of the slit in the forward direction, a 5 mm movement in the long side direction of the slit, a 155 mm movement perpendicular to the long side of the slit in the return direction, and a 5 mm movement in the long side direction of the slit in the opposite direction to the initial position, and a scan was repeated at the point where the slit moved 155 mm from the initial position in the long side direction, and a cycle of returning to the initial position was defined as one cycle, and this was repeated 4000 times.
  • the thickness of the AD film formed in this way was about 400 ⁇ m.
  • the occurrence rate P C (%) of cracks and cracks was calculated by determining the number of SiC substrates with cracks and cracks with a length of 100 ⁇ m or more among 100 SiC substrates produced under the same conditions as the SiC substrate produced as described above. The yield of the substrate was evaluated by determining this P C. The results are shown in Table 1.
  • Polishing (5-1) Surface Polishing
  • the (0001) surface of the SiC substrate obtained in (3) above was polished with diamond abrasive grains and then finished by chemical mechanical polishing (CMP) to achieve the target thickness and surface condition.
  • CMP chemical mechanical polishing
  • X-Ray Topography (XRT) Measurement of Heat-Treated Layer The SiC substrate produced in (5) above was used as an evaluation sample, and an XRT image of the evaluation sample was obtained under the conditions shown below.
  • basal plane dislocations BPDs
  • the entire XRT image of the entire surface of the obtained sample was partitioned into a grid pattern that gave an area of 4 mm length x 4 mm width x 28 ⁇ m depth per square.
  • the "depth” refers to the penetration depth of X-rays.
  • the entire length of the BPDs was measured using image processing software (manufactured by Rigaku Corporation) to determine the volume density (cm/cm 3 ) of the BPDs per square.
  • the average value of the volume density in the entire XRT image area was calculated to determine the average value X (cm/cm 3 ) of the volume density of the BPDs per square.
  • Example 1 In the sample of Example 1, the area where the density per cell is 5X (cm/cm 3 ) or more was analyzed from the XRT image, and a schematic diagram showing the area with blackened cells is shown in Figure 4. In Figure 4, the part A corresponding to C 5X is also shown.
  • TSDs threading screw dislocations
  • TEDs edge dislocations
  • the entire XRT image of the entire surface of the obtained sample was divided into a grid pattern with an area of 4 mm vertical x 4 mm horizontal per square.
  • the number of TEDs was measured using image processing software (manufactured by Rigaku Corporation), and the number density (/cm 2 ) of TEDs per square was obtained.
  • the average value of the number density in the entire XRT image area was calculated to obtain the average value Z (/cm 2 ) of the number density of TEDs per square.
  • the maximum number of squares C 2Z (mass) in which areas with 2Z or more per square are continuous in a straight line vertically and horizontally was also confirmed.
  • Example 3 (Comparison) In the above (1), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that the flow rate of the carrier gas N2 was set to 3.5 L/min. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 4 In the above (1), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that the flow rate of the carrier gas N2 was set to 6.5 L/min. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 5 In the above (1), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that the flow rate of the carrier gas N2 was set to 6.0 L/min. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 6 Comparison
  • a raw material powder containing 80.8% by weight of fine ⁇ -SiC powder (volume-based D50 particle size: 0.7 ⁇ m) and 19.2% by weight of yttrium oxide powder (volume-based D50 particle size: 0.1 ⁇ m) was used, and the flow rate of N2, which is a carrier gas, was set to 2.0 L/min.
  • N2 which is a carrier gas
  • a SiC substrate was produced and evaluated in the same manner as in Example 1. It was confirmed that the obtained heat-treated layer was a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 7 In the above (1), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that the flow rate of the carrier gas N2 was set to 4.5 L/min. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 8 In the above (1), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that the flow rate of the carrier gas N2 was set to 5.0 L/min. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 10 (Comparative) In the above (1), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that the flow rate of the carrier gas N2 was set to 2.5 L/min. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 11 In the above (1), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that a ceramic nozzle with a slit of 5 mm long side x 0.5 mm short side was used for deposition. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 12 In the above (1), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that a ceramic nozzle with a slit of 5 mm long side x 0.6 mm short side was used for deposition. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 13 (Comparative) In the above (1), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that a ceramic nozzle with a slit of 5 mm long side x 0.9 mm short side was used for deposition. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 14 In the above (1), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that a ceramic nozzle with a slit of 5 mm long side x 0.2 mm short side was used for deposition. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 15 In the above (1), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that a ceramic nozzle with a slit of 5 mm long side x 0.3 mm short side was used for deposition. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 16 (Comparative) In the above (1), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that a ceramic nozzle with a slit of 5 mm long side x 1.0 mm short side was used for deposition. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 17 In the above (1), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that a ceramic nozzle with a slit of 5 mm long side x 0.8 mm short side was used for deposition. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 18 In the above (1), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that a ceramic nozzle with a slit of 5 mm long side x 0.7 mm short side was used for deposition. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 19 (Comparative) In the above (1), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that a ceramic nozzle with a slit of 5 mm long side x 1.1 mm short side was used for deposition. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 20 (Comparative) In the above (1), a raw material powder containing 80.8% by weight of fine ⁇ -SiC powder (volume-based D50 particle size: 0.7 ⁇ m) and 19.2% by weight of yttrium oxide powder (volume-based D50 particle size: 0.1 ⁇ m) was used, and a ceramic nozzle with a slit of 5 mm long side x 1.2 mm short side was used for deposition.
  • the SiC substrate was produced and evaluated in the same manner as in Example 1. It was confirmed that the obtained heat-treated layer was a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 21 In the above (2), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that annealing was performed in an argon atmosphere at 2410° C. for 10 hours. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 22 In the above (2), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that annealing was performed in an argon atmosphere at 2420° C. for 10 hours. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 23 (Comparative) In the above (2), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that annealing was performed in an argon atmosphere at 2370° C. for 10 hours. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 24 In the above (2), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that annealing was performed in an argon atmosphere at 2430° C. for 10 hours. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 25 In the above (2), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that annealing was performed in an argon atmosphere at 2440° C. for 10 hours. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 26 (Comparative) In the above (1), a raw material powder containing 94.9% by weight of fine ⁇ -SiC powder (volume-based D50 particle size: 0.7 ⁇ m) and 5.1% by weight of yttrium oxide powder (volume-based D50 particle size: 0.1 ⁇ m) was used, and in the above (2), annealing was performed for 10 hours at 2460° C. in an argon atmosphere. Except for this, a SiC substrate was produced and evaluated in the same manner as in Example 1. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 27 In the above (2), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that annealing was performed in an argon atmosphere at 2450° C. for 10 hours. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 28 In the above (2), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that annealing was performed in an argon atmosphere at 2390° C. for 10 hours. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 29 (Comparative) In the above (2), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that annealing was performed in an argon atmosphere at 2470° C. for 10 hours. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • Example 30 (Comparative) In the above (2), a SiC substrate was produced and evaluated in the same manner as in Example 1, except that annealing was performed in an argon atmosphere at 2480° C. for 10 hours. The obtained heat-treated layer was confirmed to be a biaxially oriented SiC layer. The results are shown in Table 1.
  • the distribution of BPDs and the like can be controlled by the film formation conditions (carrier gas flow rate, etc.) in the AD method and the rare earth element concentration in the SiC substrate.
  • the film formation conditions carrier gas flow rate, etc.
  • the rare earth element concentration in the SiC substrate when the entire XRT image of the biaxially oriented SiC layer is divided into a lattice shape that gives an area of 4 mm length x 4 mm width x 28 ⁇ m depth per square, when the average value of the volume density of BPDs per square is X (cm/cm 3 ), it was found that in a SiC substrate in which the area of 5X (cm/cm 3 ) or more per square is not continuous for 10 squares or more in a straight line vertically and horizontally, it is possible to reduce cracks and breakage during processing.

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JP6192948B2 (ja) 2013-02-20 2017-09-06 株式会社豊田中央研究所 ＳｉＣ単結晶、ＳｉＣウェハ、ＳｉＣ基板、及び、ＳｉＣデバイス
WO2021149235A1 (ja) * 2020-01-24 2021-07-29 日本碍子株式会社 希土類含有ＳｉＣ基板及びＳｉＣエピタキシャル層の製法
WO2021149598A1 (ja) * 2020-01-24 2021-07-29 日本碍子株式会社 二軸配向ＳｉＣ複合基板及び半導体デバイス用複合基板
WO2022168372A1 (ja) * 2021-02-05 2022-08-11 日本碍子株式会社 希土類含有ＳｉＣ基板及びそれを用いたＳｉＣ複合基板
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See also references of EP4692430A1
Y. QIUSHENGC. SENKAIP. JISHENG: "Surface and subsurface cracks characteristics of single crystal SiC wafer in surface machining", AIP CONFERENCE PROCEEDINGS, vol. 1653, 2015, pages 020091

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