WO2021149598A1 - 二軸配向ＳｉＣ複合基板及び半導体デバイス用複合基板 - Google Patents

二軸配向ＳｉＣ複合基板及び半導体デバイス用複合基板 Download PDF

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WO2021149598A1
WO2021149598A1 PCT/JP2021/001148 JP2021001148W WO2021149598A1 WO 2021149598 A1 WO2021149598 A1 WO 2021149598A1 JP 2021001148 W JP2021001148 W JP 2021001148W WO 2021149598 A1 WO2021149598 A1 WO 2021149598A1
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biaxially oriented
oriented sic
sic layer
layer
composite substrate
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French (fr)
Japanese (ja)
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守道 渡邊
潔 松島
吉川　潤
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NGK Insulators Ltd
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Priority to JP2021573119A priority Critical patent/JP7628968B2/ja
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Publication of WO2021149598A1 publication Critical patent/WO2021149598A1/ja
Priority to US17/663,229 priority patent/US12125883B2/en
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    • C—CHEMISTRY; METALLURGY
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    • 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
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/005—Epitaxial layer growth
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    • H10D—INORGANIC ELECTRIC SEMICONDUCTOR DEVICES
    • H10D62/00—Semiconductor bodies, or regions thereof, of devices having potential barriers
    • H10D62/40—Crystalline structures
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    • 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
    • H10P14/24—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials using chemical vapour deposition [CVD]
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    • 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
    • H10P14/26—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials using liquid deposition
    • H10P14/265—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials using liquid deposition using solutions
    • 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
    • H10P14/2901—Materials
    • H10P14/2902—Materials being Group IVA materials
    • H10P14/2904—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
    • H10P14/2926—Crystal orientations
    • H—ELECTRICITY
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    • 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
    • H10P14/34—Deposited materials, e.g. layers
    • H10P14/3402—Deposited materials, e.g. layers characterised by the chemical composition
    • H10P14/3404—Deposited materials, e.g. layers characterised by the chemical composition being Group IVA materials
    • H10P14/3408—Silicon carbide
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    • 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
    • H10P14/34—Deposited materials, e.g. layers
    • H10P14/3438—Doping during depositing
    • H10P14/3441—Conductivity type
    • H10P14/3446—Transition metal elements; Rare earth elements
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    • 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
    • H10P14/34—Deposited materials, e.g. layers
    • H10P14/3466—Crystal orientation
    • 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
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    • 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
    • H10P14/38—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials characterised by treatments done after the formation of the materials
    • H10P14/3802—Crystallisation or recrystallisation of non-monocrystalline semiconductor materials, e.g. regrowth

Definitions

  • the present invention relates to a biaxially oriented SiC composite substrate and a composite substrate for a semiconductor device.
  • SiC Silicon Carbide
  • SiC Silicon Carbide
  • all the dislocation density of the current commercially available SiC single crystal substrate is approximately 10 3 ⁇ 10 4 cm It is said to be -2 (for example, Patent Document 1). Therefore, in contrast to Si, in which dislocation-free crystals are industrially realized, SiC is a single crystal material in which an element must be manufactured from a region having a constant dislocation density. It is also known that these dislocations have different effects on device performance.
  • Patent Document 2 discloses a SiC single crystal substrate produced by using a method of forming a macro step on a seed crystal during film formation, and the height of the SiC single crystal on the crystal growth surface of the seed crystal is high. It is said that by forming a macrostep having a large size, a SiC single crystal having few penetrating spiral dislocations can be obtained by crystal growth due to the subsequent progress of the macrostep.
  • the method disclosed in Patent Document 2 has a feature that the stacking defects propagate in the progress direction of the macrosteps because the penetrating spiral dislocations are converted into stacking defects and discharged to the outside of the crystal as the macrostep progresses.
  • Patent Document 3 by adding a predetermined amount of Nb, Ta, Mo, W, Ir to the SiC single crystal, dislocations due to thermal stress generated during the growth of the SiC single crystal are less likely to occur, and SiC is generated by epitaxial growth. It is disclosed that dislocations are less likely to occur when a SiC layer is formed on a single crystal.
  • Patent Document 2 the SiC single crystal produced by the method of Patent Document 2 has a problem that the warp becomes large. The cause of this is not clear, but it is probable that the warpage occurred as a result of some stress distribution occurring inside the substrate due to the stacking defects lining up in one direction (the direction in which the macrosteps propagated). Further, Patent Document 2 focuses on the reduction of the penetrating spiral dislocations by converting the penetrating spiral dislocations into stacking defects, and has not made a concrete study on the reduction of the basal plane dislocations. If there are many through-helical dislocations, the long-term reliability of the insulating film is lowered and leak fracture is likely to occur, so that the life of the device is shortened.
  • the present invention has been made to solve such a problem, and an object of the present invention is to provide a biaxially oriented SiC composite substrate having a low defect density reaching the surface and a small warp.
  • the biaxially oriented SiC composite substrate of the present invention is A first biaxially oriented SiC layer containing penetrating spiral dislocations and basal plane dislocations, Second biaxial orientation A second biaxial orientation that is continuously formed on one surface of the first biaxially oriented SiC layer and contains rare earth elements of 1 ⁇ 10 16 atoms / cm 3 or more and 1 ⁇ 10 19 atoms / cm 3 or less. SiC layer and With The defect density on the surface of the second biaxially oriented SiC layer is smaller than the defect density of the first biaxially oriented SiC layer. It is a thing.
  • the second biaxially oriented SiC layer has a rare earth element concentration set within the range of 1 ⁇ 10 16 atoms / cm 3 or more and 1 ⁇ 10 19 atoms / cm 3 or less. There is. Therefore, the defect density reaching the surface of the second biaxially oriented SiC layer can be reduced as compared with the first biaxially oriented SiC layer. Since such a biaxially oriented SiC composite substrate has a small warp and a low defect density reaching the surface of the second biaxially oriented SiC layer, a functional layer is formed on the surface by epitaxial growth or the like to manufacture a semiconductor device. Suitable for. Further, since the second biaxially oriented SiC layer does not contain Nb, Ta, etc., it can be used even in a situation where components such as Nb, Ta, etc. affect the semiconductor characteristics.
  • the biaxially oriented SiC layer is a SiC layer whose orientations are aligned on two axes, the a-axis and the c-axis.
  • the defect density is the sum of the density of penetrating spiral dislocations (TSD) and the density of basal plane dislocations (BPD).
  • the first cause of defect formation is the case where defects existing in the underlying layer propagate. That is, when the second biaxially oriented SiC layer is formed on the first biaxially oriented SiC layer, the defects existing in the first biaxially oriented SiC layer propagate to the second biaxially oriented SiC layer. there is a possibility.
  • the effect of suppressing the propagation of defects can be considered. Although this mechanism is not clear, the formation of the biaxially oriented SiC layer around the defect is suppressed by the accumulation of rare earth elements, Al, and N in the defect propagated in the biaxially oriented SiC layer, and a healthy region without defects.
  • the biaxially oriented SiC layer from the above grows preferentially, and as a result, the defects reaching the surface of the second biaxially oriented SiC layer are reduced. Further, it is also considered that the defects propagated in the second biaxially oriented SiC layer are likely to cause pair annihilation between the defects at an early stage by containing a predetermined amount and a predetermined ratio of rare earth elements, Al, and N.
  • the second cause of defect formation is considered to be a lattice mismatch with the base substrate for forming the first biaxially oriented SiC layer.
  • lattice mismatch may occur.
  • the stress of lattice mismatch in the film can be relaxed and the defect density can be reduced by containing a predetermined amount and a predetermined ratio of rare earth elements, Al, and N in the second biaxially oriented SiC layer.
  • pair annihilation between defects is likely to occur.
  • the second biaxially oriented SiC layer contains a predetermined amount and a predetermined ratio of rare earth elements, Al and N, so that the stress of the lattice mismatch is relaxed and the second biaxially oriented SiC layer has desired characteristics (for example, electrical characteristics).
  • a biaxially oriented SiC layer can be obtained.
  • the third cause of defect formation is considered to be thermal stress due to the temperature distribution when the second biaxially oriented SiC layer is formed or when the temperature is lowered to room temperature after the formation. At this time, it is considered that the thermal stress is relaxed and the generation of new defects can be suppressed by containing the rare earth elements, Al and N in a predetermined amount and a predetermined ratio in the second biaxially oriented SiC layer.
  • the rare earth elements contained in the second biaxially oriented SiC layer are Sc, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, It contains at least one element selected from the group consisting of 17 elements of Ho, Er, Tm, Yb, and Lu.
  • the rare earth element is preferably at least one selected from the group consisting of Y, Sm, Ho, Dy and Yb. In this way, the defect density reaching the surface of the second biaxially oriented SiC layer can be further reduced.
  • the defect density reaching the surface of the second biaxially oriented SiC layer is not particularly limited, but the defect density is preferably 1.0 ⁇ 10 2 / cm 2 or less. more preferably 0 ⁇ 10 1 / cm 2 or less, more preferably 1.0 ⁇ 10 0 / cm 2 or less.
  • the second biaxially oriented SiC layer preferably contains Al, and the concentration of Al in the second biaxially oriented SiC layer is 1 ⁇ 10. It is preferably 16 atoms / cm 3 or more and 1 ⁇ 10 21 atoms / cm 3 or less. In this way, the defect density reaching the surface of the second biaxially oriented SiC layer can be further reduced. It is preferred second biaxially oriented SiC layer of the (concentration of Al) / (concentration of rare earth elements) is 1 ⁇ 10 5 or less 1 ⁇ 10 -2 or more.
  • the second biaxially oriented SiC layer preferably contains N in addition to Al, and the concentration of N in the second biaxially oriented SiC layer is It is preferably 1 ⁇ 10 17 atoms / cm 3 or more and 1 ⁇ 10 22 atoms / cm 3 or less. In this way, the defect density reaching the surface of the second biaxially oriented SiC layer can be further reduced. It is preferred second biaxially oriented SiC layer of the (concentration of N) / (concentration of rare earth elements) is 1 ⁇ 10 5 or less 1 ⁇ 10 -2 or more.
  • the (N concentration) / (Al concentration) in the second biaxially oriented SiC layer is preferably 3 or more and 5 or less, and the second biaxial orientation is described. It is preferable that the concentrations of rare earth elements, Al and N in the oriented SiC layer have a relationship of N> Al> rare earth elements, and the concentrations of rare earth elements, Al and N in the second biaxially oriented SiC layer are the first. It is preferably higher than in the biaxially oriented SiC layer of.
  • the first biaxially oriented SiC layer and the second biaxially oriented SiC layer It is preferable that Ar is contained in the vicinity of the interface between the two, and the defect density of the first biaxially oriented SiC layer is preferably low.
  • the composite substrate for a semiconductor device of the present invention With any of the above-mentioned biaxially oriented SiC composite substrates, A functional layer for a semiconductor device provided on the second biaxially oriented SiC composite substrate of the biaxially oriented SiC composite substrate, and a functional layer for a semiconductor device. It is equipped with.
  • Examples of such a composite substrate for a semiconductor device include MOSFETs, IGBTs, LEDs, HEMTs, and the like.
  • FIG. 3 is a manufacturing process diagram of a biaxially oriented SiC composite substrate 10.
  • FIG. 1 is a schematic view of the biaxially oriented SiC composite substrate 10 of the present embodiment.
  • the biaxially oriented SiC composite substrate 10 includes a first biaxially oriented SiC layer 20 and a second biaxially oriented SiC layer 30.
  • the biaxially oriented SiC layer means a layer having the same orientation on both the a-axis and the c-axis.
  • the first biaxially oriented SiC layer 20 contains penetrating spiral dislocations (TSD) and basal plane dislocations (BPD).
  • the second biaxially oriented SiC layer 30 is continuously formed on one surface of the first biaxially oriented SiC layer 20 and contains rare earth elements of 1 ⁇ 10 16 atoms / cm 3 or more and 1 ⁇ 10 19 atoms / cm. Contains 3 or less.
  • the defect density of the second biaxially oriented SiC layer is smaller than the defect density of the first biaxially oriented SiC layer 20.
  • the substrate surface refers to the surface of the second biaxially oriented SiC layer 30 opposite to the surface in contact with the first biaxially oriented SiC layer 20.
  • the rare earth element is at least selected from the group consisting of 17 kinds of elements Sc, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu. Contains one or more elements.
  • the rare earth element is preferably at least one selected from the group consisting of Y, Sm, Ho, Dy and Yb.
  • the first biaxially oriented SiC layer 20 has a crystal growth plane.
  • the first biaxially oriented SiC layer 20 is preferably a layer composed of a SiC single crystal.
  • 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 the SiC single crystal.
  • the temperature is preferably °, and the surface on which the second biaxially oriented SiC layer 30 is formed is preferably a Si surface. It is more preferable that the polytype is 4H, the off angle is 1 to 5 ° from the [0001] axis of the SiC single crystal, and the surface on which the second biaxially oriented SiC layer 30 is formed is the Si surface.
  • the second biaxially oriented SiC layer 30 is formed on the crystal growth plane of the first biaxially oriented SiC layer 20.
  • the second biaxially oriented SiC layer 30 is a SiC layer oriented in the biaxial directions of the a-axis and the c-axis.
  • 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 biaxial directions of the c-axis and the a-axis. good.
  • a mosaic crystal is a group of crystals that do not have clear grain boundaries but have slightly different orientations of the crystals on one or both of the c-axis and the a-axis.
  • the method for evaluating the orientation is not particularly limited, but for example, a known analysis method such as an EBSD (Electron Backscatter Diffraction Patterns) method or an X-ray pole figure can be used.
  • EBSD Electro Backscatter Diffraction Patterns
  • X-ray pole figure the reverse pole figure mapping of the surface (plate surface) of the biaxially oriented SiC layer or the cross section orthogonal to the plate surface is measured.
  • the obtained reverse pole map mapping (A) it is oriented in a specific direction (first axis) in the approximate normal direction of the plate surface, and (B) it is orthogonal to the first axis and is approximately inward to the plate surface.
  • the orientation is oriented in two axes, the normal normal direction and the substantially plate surface direction. In other words, when the above four conditions are satisfied, it is determined that the orientation is in the two axes of the c-axis and the a-axis.
  • the direction in the plate surface 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 in two axes, a substantially normal direction and a substantially in-plane direction, but it is preferable that the substantially normal direction is oriented in the c-axis.
  • the smaller the inclination angle distribution in the substantially normal direction and / or the substantially in-plane direction of the plate the smaller the mosaic property of the biaxially oriented SiC layer, and the closer to zero, the closer to a single crystal.
  • the inclination angle distribution is preferably small in both the substantially normal direction and the substantially plate surface direction, for example, ⁇ 5 ° or less, and more preferably ⁇ 3 ° or less.
  • the second biaxially oriented SiC layer 30 has a defect density of 1.0 ⁇ 10 2 / cm 2 or less, which is defined as the number of basal plane dislocations and penetrating spiral dislocations reaching the surface per unit area. is typical, preferably 1.0 ⁇ 10 1 / cm 2 or less, more preferably 1.0 ⁇ 10 0 / cm 2 or less.
  • the lower limit of the defect density is not particularly limited, but is typically 1.0 ⁇ 10 -3 / cm 2 or more, and more typically 1.0 ⁇ 10 ⁇ 2 / cm 2 or more.
  • a known etch pit evaluation by KOH melt etching shall be used. When etch pit evaluation by KOH melt etching is not possible, PL mapping, X-ray topography, CL mapping, etc. may be performed. The defect density can also be evaluated by using such a method.
  • the density of crystal defects propagating to the surface of the second biaxially oriented SiC layer 30 can be significantly reduced.
  • the biaxially oriented SiC composite substrate 10 of the present embodiment has a low crystal defect density and can also reduce the warpage. The reason for this is not clear, but it is considered that the in-plane distribution of crystal defects inside the second biaxially oriented SiC layer 30 is small or absent, and there is no stress bias in the substrate surface.
  • the first biaxially oriented SiC layer 20 and the second biaxially oriented SiC layer 30 are preferably layers having a low resistivity. It is typically 20 m ⁇ cm or less.
  • the low-resistance biaxially oriented SiC layer a layer made of n-type SiC is preferable.
  • a biaxially oriented SiC composite substrate provided with such a conductive biaxially oriented SiC layer has conductivity in the thickness direction and can be used as a substrate for a vertical device (for example, a power device). Further, depending on the application, the biaxially oriented SiC composite substrate may be a p-type SiC.
  • the first biaxially oriented SiC layer 20 and the second biaxially oriented SiC layer 30 are preferably layers having high resistivity. Typically, it is 1 ⁇ 10 7 ⁇ cm or more.
  • some high-resistance biaxially oriented SiC layers do not contain a doping element. Further, such a high resistance can be obtained even when both the n-type dopant and the p-type dopant are contained.
  • the biaxially oriented SiC composite substrate provided with the biaxially oriented SiC layer imparted with such insulating properties has insulating properties, and a horizontal device (for example, a GaN layer, an AlGaN layer, etc. are formed on the biaxially oriented SiC composite substrate). It can be used as a base substrate for a filmed high-frequency power device).
  • the biaxially oriented SiC composite substrate 10 of the present embodiment can be manufactured by various manufacturing methods, but here, a SiC single crystal layer is used as the first biaxially oriented SiC layer 20, and a second silicon single crystal layer is used on the surface thereof. The case where the biaxially oriented SiC layer 30 is produced will be described.
  • the method for forming the second biaxially oriented SiC layer is particularly limited as long as a second biaxially oriented SiC layer containing a rare earth element and having a smaller defect density than the first biaxially oriented SiC layer can be obtained. do not have.
  • a vapor phase method such as CVD or sublimation method may be used, a liquid phase method such as a solution method may be used, or a solid phase method may be used.
  • the process of forming the orientation precursor layer and obtaining the biaxially oriented SiC layer by the heat treatment step will be described below. Specifically, it includes (a) a step of forming the orientation precursor layer 40, (b) a heat treatment step, and (c) a grinding step.
  • the orientation precursor layer 40 becomes the second biaxially oriented SiC layer 30 by the heat treatment described later.
  • these steps will be described in order with reference to FIG.
  • (A) Formation step of orientation precursor layer 40 (see FIG. 2A)
  • a SiC single crystal layer is used as the first biaxially oriented SiC layer 20, and the alignment precursor layer 40 is formed on the crystal growth surface of the SiC single crystal layer.
  • the SiC single crystal layer it is preferable to use a 4H or 6H polytype.
  • the crystal growth plane of the SiC single crystal layer a Si plane having an off angle of 0.1 to 12 ° from the SiC [0001] axis is preferable. The off angle is more preferably 1 to 5 °.
  • the first biaxially oriented SiC layer 20 is not particularly limited to the SiC single crystal layer, and any SiC layer oriented in the biaxial directions of the a-axis and the c-axis can be used.
  • the method for forming the alignment precursor layer 40 includes, for example, a solid phase deposition method such as an AD (aerosol deposition) method and an HPPD (supersonic plasma particle deposition) method, a sputtering method, a vapor deposition method, a sublimation method, and various CVD methods.
  • a solid phase deposition method such as an AD (aerosol deposition) method and an HPPD (supersonic plasma particle deposition) method
  • a sputtering method a vapor deposition method, a sublimation method, and various CVD methods.
  • Examples include a vapor phase deposition method such as a chemical vapor deposition method and a liquid phase deposition method such as a solution growth method, in which the alignment precursor layer 40 is directly formed on the first biaxially oriented SiC layer 20. Can be used.
  • the CVD method for example, a thermal CVD method, a plasma CVD method, a mist CVD method, an MO (organic metal) CVD method and the like can be used.
  • the orientation precursor layer 40 a method of using a polycrystalline material prepared in advance by a sublimation method, various CVD methods, sintering, or the like and placing it on the first biaxially oriented SiC layer 20 can also be used. .. Alternatively, a method may be used in which a molded body of the alignment precursor layer 40 is prepared in advance and the molded body is placed on the first biaxially oriented SiC layer 20.
  • Such an orientation precursor layer 40 may be a tape molded product produced by tape molding, or a green compact produced by pressure molding such as a uniaxial press.
  • the raw material powder of the alignment precursor layer 40 contains a rare earth compound according to the concentration of the rare earth element in the second biaxially oriented SiC layer 30.
  • the rare earth compound is not particularly limited, and examples thereof include oxides, nitrides, carbides, and fluorides of at least one of the 17 types of rare earth elements described above.
  • Al is contained in the second biaxially oriented SiC layer 30
  • the Al compound is contained in the raw material powder of the oriented precursor layer 40 according to the Al concentration in the second biaxially oriented SiC layer 30.
  • the Al compound is not particularly limited, and examples thereof include aluminum oxide, aluminum nitride, aluminum carbide, and aluminum fluoride.
  • N when N is contained in the second biaxially oriented SiC layer 30, a nitrogen compound is contained in the raw material powder of the oriented precursor layer 40 according to the N concentration in the second biaxially oriented SiC layer 30.
  • the nitrogen compound is not particularly limited, and examples thereof include aluminum nitride.
  • N can be added by the following method.
  • N is also contained by synthesizing a second biaxially oriented SiC layer from the raw material powder of the oriented precursor layer 40 in a nitrogen atmosphere, or by annealing the synthesized second biaxially oriented SiC layer in a nitrogen atmosphere. Can be made to.
  • the first method does not go through the heat treatment step described later.
  • Epitaxial growth may occur on the biaxially oriented SiC layer 20 of the above, and a second biaxially oriented SiC layer 30 may be formed.
  • the orientation precursor layer 40 is in a non-oriented state at the time of formation, that is, an amorphous or non-oriented polycrystal, and it is preferable to orient the SiC single crystal as a seed in the subsequent heat treatment step. By doing so, it is possible to effectively reduce the crystal defects that reach the surface of the second biaxially oriented SiC layer 30.
  • a method of forming a direct orientation precursor layer 40 on the first biaxially oriented SiC layer 20 by an AD method or various CVD methods, or a polycrystal separately prepared by a sublimation method, various CVD methods, or sintering is first.
  • the method of placing on the biaxially oriented SiC layer 20 is preferable.
  • the AD method is particularly preferable because it does not require a high vacuum process and the film formation rate is relatively high.
  • the surface of the polycrystal is sufficiently smoothed in order to improve the adhesion between the polycrystal and the first biaxially oriented SiC layer 20.
  • the method of directly forming the orientation precursor layer 40 is preferable. Further, a method of placing the molded product prepared in advance on the first biaxially oriented SiC layer 20 is also preferable as a simple method, but since the orientation precursor layer 40 is composed of powder, in the heat treatment step described later. Requires a sintering process.
  • known conditions can be used for any of the methods, in the following, a method of directly forming the orientation precursor layer 40 on the first biaxially oriented SiC layer 20 by the AD method or the thermal CVD method and a prefabricated molded product. Will be described on the method of placing the above on the first biaxially oriented SiC layer 20.
  • the AD method is a technology in which fine particles and fine particle raw materials are mixed with a gas to form an aerosol, and this aerosol is jetted at high speed from a nozzle to collide with a substrate to form a film.
  • FIG. 3 shows an example of a film forming apparatus (AD apparatus) used in such an AD method.
  • the AD device 50 shown in FIG. 3 is configured as a device used in the AD method of injecting raw material powder onto a substrate in an atmosphere having a pressure lower than atmospheric pressure.
  • the AD device 50 includes an aerosol generation unit 52 that generates an aerosol of the raw material powder containing the raw material component, and a film forming unit that injects the raw material powder onto the first biaxially oriented SiC layer 20 to form a film containing the raw material component.
  • the aerosol generation unit 52 includes an aerosol generation chamber 53 that stores raw material powder and receives a carrier gas from a gas cylinder (not shown) to generate an aerosol, and a raw material supply pipe 54 that supplies the generated aerosol to the film forming unit 60.
  • the aerosol generation chamber 53 and the aerosol in the aerosol are provided with a vibration exciter 55 that vibrates at a frequency of 10 to 100 Hz.
  • the film forming section 60 includes a film forming chamber 62 that injects aerosol into the first biaxially oriented SiC layer 20, and a substrate holder that is arranged inside the film forming chamber 62 and fixes the first biaxially oriented SiC layer 20.
  • the film forming section 60 includes an injection nozzle 66 in which a slit 67 is formed at the tip thereof and ejects an aerosol to the first biaxially oriented SiC layer 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 causes pores in the film depending on the film forming conditions, or the film becomes a green compact. For example, it is easily affected by the collision rate of the raw material powder with the substrate, the particle size of the raw material powder, the aggregated 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 with the substrate is affected by the differential pressure between the film forming 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 densely oriented precursor layer.
  • the raw material gas is not particularly limited, but the source of Si is silicon tetrachloride (SiCl 4 ) gas or silane (SiH 4 ) gas, and the source of C is methane (CH 4 ) gas or propane (C). 3 H 8 ) Gas or the like can be used.
  • the film formation temperature is preferably 1000 to 2200 ° C, more preferably 1100 to 2000 ° C, and even more preferably 1200 to 1900 ° C.
  • the orientation precursor layer 40 is in a non-oriented state at the time of its production, that is, it is an amorphous or non-oriented polycrystal, and the SiC single crystal may be used as a seed crystal to cause crystal rearrangement during the heat treatment step. preferable.
  • the film formation temperature, Si source, gas flow rate of C source and their ratio, film formation pressure, etc. have an effect.
  • the film forming temperature is preferably low, preferably less than 1700 ° C., further preferably 1500 ° C. or lower, and particularly preferably 1400 ° C. or lower.
  • the film formation temperature is too low, the film formation rate itself also decreases, so that the film formation temperature is preferably high from the viewpoint of the film formation rate.
  • the raw material powder of the orientation precursor can be molded and prepared.
  • the orientation precursor layer 40 is a press molded product.
  • the press-molded product can be produced by press-molding the raw material powder of the orientation precursor based on a known method.
  • the raw material powder is placed in a mold, preferably 100 to 400 kgf / cm 2 , more preferably 150. It may be produced by pressing at a pressure of about 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 narrow slit-shaped discharge port to form a sheet. It is preferable to discharge and mold.
  • the thickness of the molded product formed into a sheet is not limited, but is preferably 5 to 500 ⁇ m from the viewpoint of handling. Further, when a thick orientation precursor layer is required, a large number of these sheet molded products may be stacked and used as a desired thickness.
  • the portion near the first biaxially oriented SiC layer 20 becomes the second biaxially oriented SiC layer 30 by the subsequent heat treatment on the first biaxially oriented SiC layer 20.
  • the second biaxially oriented SiC layer 30 is generated by heat-treating the laminated body in which the oriented precursor layer 40 is laminated or placed on the first biaxially oriented SiC layer 20.
  • the heat treatment method is not particularly limited as long as epitaxial growth using the first biaxially oriented SiC layer 20 as a seed occurs, and the heat treatment method can be carried out in a known heat treatment furnace such as a tube furnace or a hot plate. Further, in addition to these heat treatments under normal pressure (pressless), pressure heat treatments such as hot press and HIP, and combinations of normal pressure heat treatments and pressure heat treatments can also be used.
  • the atmosphere of the heat treatment can be selected from vacuum, nitrogen, and an inert gas atmosphere.
  • the heat treatment temperature is preferably 1700 to 2700 ° C.
  • the 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 temperature is excessively high, a part of SiC may be lost due to sublimation, or the SiC may be plastically deformed to cause problems such as warpage.
  • the temperature is preferably 2700 ° C. or lower, more preferably 2500 ° C. or lower.
  • the heat treatment temperature and holding time are related to the thickness of the second biaxially oriented SiC layer 30 generated by epitaxial growth and can be appropriately adjusted.
  • the orientation precursor layer 40 when a molded product prepared in advance is used as the orientation precursor layer 40, it is necessary to sinter during heat treatment, and atmospheric firing at high temperature, 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, particularly preferably preferably 200 kgf / cm 2 or more, there is no particular upper limit.
  • the firing temperature is not particularly limited as long as sintering and epitaxial growth occur. 1700 ° C. or higher is preferable, 1800 ° C. or higher is more preferable, 2000 ° C. or higher is further preferable, and 2200 ° C. or higher is particularly preferable.
  • the atmosphere at the time of firing can be selected from vacuum, nitrogen, an inert gas atmosphere, or a mixed gas of nitrogen and an inert gas.
  • the SiC powder as a raw material may be either ⁇ -SiC or ⁇ -SiC.
  • the SiC powder is preferably composed of SiC particles having an average particle size of 0.01 to 5 ⁇ m.
  • the average particle size refers to the average value obtained by observing the powder with a scanning electron microscope and measuring the maximum diameter in the constant direction for 100 primary particles.
  • the crystals in the alignment precursor layer 40 grow while being oriented from the crystal growth plane of the first biaxially oriented SiC layer 20 to the c-axis and the a-axis, so that the alignment precursor layer 40 is a crystal. From the growth surface, it gradually changes to the second biaxially oriented SiC layer 30.
  • the generated second biaxially oriented SiC layer 30 has a low defect density (for example, 1 ⁇ 10 2 / cm 2 or less).
  • the method for growing the SiC epitaxial layer is not particularly limited, and a known method can be adopted.
  • a biaxially oriented SiC composite substrate 10 is arranged on a susceptor in a CVD apparatus so that the surface of the second biaxially oriented SiC layer 30 faces up, silane and propane are used as raw material gases, and hydrogen is used as a carrier gas. May be supplied to carry out epitaxial growth.
  • the growth temperature is preferably set within the range of 1570 ° C. or higher and 1610 ° C. or lower.
  • the concentration ratio C / Si is preferably set within the range of 0.7 or more and 1.2 or less.
  • the second biaxially oriented SiC layer 30 has a rare earth element concentration of 1 ⁇ 10 16 atoms / cm 3 or more and 1 ⁇ 10 19 atoms /. It is set within the range of cm 3 or less. Therefore, the defect density reaching the surface of the second biaxially oriented SiC layer 30 can be reduced as compared with the first biaxially oriented SiC layer 20. Since such a biaxially oriented SiC composite substrate 10 has a small warp and a low defect density reaching the surface of the second biaxially oriented SiC layer 30, a functional layer is formed on the surface by epitaxial growth or the like to manufacture a semiconductor device. Suitable for Further, since the second biaxially oriented SiC layer 30 does not contain Nb, Ta, etc., it can be used even in a situation where components such as Nb, Ta, etc. affect the semiconductor characteristics.
  • the rare earth element contained in the second biaxially oriented SiC layer 30 is preferably at least one selected from the group consisting of Y, Sm, Ho, Dy and Yb. In this way, the defect density reaching the surface of the second biaxially oriented SiC layer 30 can be further reduced.
  • the defect density reaching the surface of the second biaxially oriented SiC layer 30 is preferably 1.0 ⁇ 10 2 / cm 2 or less, more preferably 1.0 ⁇ 10 1 / cm 2 or less, and 1.0. ⁇ more preferably 10 0 / cm 2 or less.
  • the second biaxially oriented SiC layer 30 preferably contains Al, and the concentration of Al in the second biaxially oriented SiC layer 30 is 1 ⁇ 10 16 atoms / cm 3 or more 1 ⁇ . It is preferably 10 21 atoms / cm 3 or less. In this way, the defect density reaching the surface of the second biaxially oriented SiC layer 30 can be further reduced. It is preferred second biaxially oriented SiC layer 30 in the (concentration of Al) / (concentration of rare earth elements) is 1 ⁇ 10 5 or less 1 ⁇ 10 -2 or more.
  • the second biaxially oriented SiC layer 30 preferably contains N in addition to Al, and the concentration of N in the second biaxially oriented SiC layer 30 is 1 ⁇ 10 17 atoms / cm 3 or more. It is preferably 1 ⁇ 10 22 atoms / cm 3 or less. In this way, the defect density reaching the surface of the second biaxially oriented SiC layer 30 can be further reduced. It is preferred second biaxially oriented SiC layer 30 in the (concentration of N) / (concentration of rare earth elements) is 1 ⁇ 10 5 or less 1 ⁇ 10 -2 or more.
  • the (concentration of N) / (concentration of Al) in the second biaxially oriented SiC layer 30 is preferably 3 or more and 5 or less, and the rare earth element in the second biaxially oriented SiC layer 30. It is preferable that the concentrations of Al and N are N> Al> rare earth elements, and the concentrations of the rare earth elements in the second biaxially oriented SiC layer 30 and the concentrations of Al and N are higher than those in the first biaxially oriented SiC layer. High is preferable.
  • the defect density reaching the surface of the second biaxially oriented SiC layer 30 near the interface between the first biaxially oriented SiC layer 20 and the second biaxially oriented SiC layer 30. It is preferable that Ar is contained, and the defect density of the first biaxially oriented SiC layer 20 is preferably low.
  • the biaxially oriented SiC composite substrate 10 is made into a semiconductor device composite substrate by providing a functional layer for semiconductor devices on the second biaxially oriented SiC composite substrate 30 of the biaxially oriented SiC composite substrate 10. You can also do it.
  • the functional layer for semiconductor devices include a SiC epitaxial layer.
  • the SiC epitaxial layer is formed by supplying a raw material gas for producing SiC to the surface of the second biaxially oriented SiC layer 30 (the surface opposite to the surface in contact with the first biaxially oriented SiC layer 20). , Formed on its surface.
  • the composite substrate for a semiconductor device include MOSFETs, IGBTs, LEDs, HEMTs, and the like.
  • the orientation precursor layer 40 is laminated on the second biaxially oriented SiC layer 30 of the biaxially oriented SiC composite substrate 10, and heat treatment, annealing, and grinding are performed in this order to perform the second biaxially oriented SiC layer 30.
  • a second biaxially oriented SiC layer 30 as a second layer can be provided on the SiC layer 30.
  • a commercially available SiC single crystal substrate (n-type 4H-SiC, diameter 50.8 mm (2 inches), Si plane, (0001) plane, off angle 4 °, thickness 0.35 mm, orientation flat None) was prepared, and the mixed powder was sprayed onto the SiC single crystal substrate by the AD apparatus 50 shown in FIG. 1 to form an AD film (alignment precursor layer).
  • the AD film formation conditions were as follows. First, the carrier gas was N 2, and a film was formed using a ceramic nozzle having slits having a long side of 5 mm and a short side of 0.4 mm.
  • the scanning conditions of the nozzle are 0.5 mm / s, movement of 55 mm perpendicular to the long side of the slit and in the forward direction, movement of 5 mm in the direction of the long side of the slit, and vertical and return to the long side of the slit. Repeated scanning of moving 55 mm in the direction, moving 5 mm in the long side direction of the slit and in the direction opposite to the initial position, and when moving 55 mm from the initial position in the long side direction of the slit, scan in the opposite direction. The cycle of returning to the initial position was set as one cycle, and this was repeated for 1200 cycles.
  • the thickness of the AD film thus formed was about 120 ⁇ m.
  • polishing part 1 After polishing with diamond abrasive grains so that the entire surface of the obtained heat-treated layer is parallel to the back surface (bottom surface of the SiC single crystal substrate), a chemical mechanical polishing (CMP) finish is performed to obtain a composite substrate. rice field.
  • CMP chemical mechanical polishing
  • Polishing part 2 A sample separately prepared by the same method as in (1) and (2) was prepared and cut so as to pass through the center of the substrate in the direction orthogonal to the plate surface. The cross section of the cut sample was smoothed by lapping with diamond abrasive grains, and mirror-finished by chemical mechanical polishing (CMP).
  • CMP chemical mechanical polishing
  • Example 2 Using a raw material powder containing 89.1% by weight of ⁇ -SiC powder, 7.1% by weight of yttrium oxide powder, and 3.8% by weight of aluminum oxide powder, and annealing at 1950 ° C. in an N 2 atmosphere. The experiment was carried out in the same manner as in Experimental Example 1 except that it was not carried out. It was confirmed that the obtained heat treatment layer was a second biaxially oriented SiC layer. Table 1 shows the concentrations of Y and Al in the second biaxially oriented SiC layer, the Al / Y concentration ratio, and the defect density on the surface of the biaxially oriented SiC layer.
  • Example 3 The experiment was carried out in the same manner as in Experimental Example 1 except that the raw material powder containing 92.9% by weight of ⁇ -SiC powder and 7.1% by weight of yttrium oxide powder was used. It was confirmed that the obtained heat treatment layer was a second biaxially oriented SiC layer. Table 1 shows the concentrations of Y and N in the second biaxially oriented SiC layer, the N / Y concentration ratio, and the defect density on the surface of the biaxially oriented SiC layer.
  • the present invention can be used, for example, in semiconductor devices.
  • biaxially oriented SiC composite substrate 20 first biaxially oriented SiC layer, 30 second biaxially oriented SiC layer, 40 oriented precursor layer, 50 AD device, 52 aerosol generator, 53 aerosol generator, 54 raw materials Supply pipe, 55 shaker, 60 film forming part, 62 film forming chamber, 63 XY stage, 64 substrate holder, 66 injection nozzle, 67 slit, 68 vacuum pump.

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