WO2021149235A1 - 希土類含有ＳｉＣ基板及びＳｉＣエピタキシャル層の製法 - Google Patents

希土類含有ＳｉＣ基板及びＳｉＣエピタキシャル層の製法 Download PDF

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WO2021149235A1
WO2021149235A1 PCT/JP2020/002447 JP2020002447W WO2021149235A1 WO 2021149235 A1 WO2021149235 A1 WO 2021149235A1 JP 2020002447 W JP2020002447 W JP 2020002447W WO 2021149235 A1 WO2021149235 A1 WO 2021149235A1
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sic
layer
rare earth
single crystal
concentration
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French (fr)
Japanese (ja)
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潔 松島
守道 渡邊
吉川　潤
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NGK Insulators Ltd
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NGK Insulators Ltd
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Priority to JP2021572228A priority Critical patent/JP7282214B2/ja
Priority to PCT/JP2020/002447 priority patent/WO2021149235A1/ja
Priority to CN202080089055.8A priority patent/CN114901875B/zh
Publication of WO2021149235A1 publication Critical patent/WO2021149235A1/ja
Priority to US17/805,234 priority patent/US12424440B2/en
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    • 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
    • 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
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/36—Carbides
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • 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]
    • 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
    • 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
    • H10P14/3402—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
    • 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
    • H10P14/34—Deposited materials, e.g. layers
    • H10P14/3438—Doping during depositing
    • H10P14/3441—Conductivity type
    • H10P14/3446—Transition metal elements; Rare earth elements
    • 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
    • H10P14/34—Deposited materials, e.g. layers
    • H10P14/3466—Crystal orientation
    • 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
    • H10P14/38—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 method for producing a rare earth-containing SiC substrate and a SiC epitaxial layer.
  • SiC Silicon Carbide
  • SiC power devices power semiconductor devices (SiC power devices) using SiC materials are expected to be used in various applications because they are superior in miniaturization, low power consumption, and high efficiency to those using Si semiconductors.
  • SiC power devices converters, inverters, in-vehicle chargers and the like for electric vehicles (EV) and plug-in hybrid vehicles (PHEV) can be miniaturized and efficiency can be improved.
  • EV electric vehicles
  • PHEV plug-in hybrid vehicles
  • Patent Documents 1 and 2 study a method of converting harmful BPD into harmless blade-shaped dislocations (TED) when SiC is epitaxially grown on a SiC single crystal substrate.
  • 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.
  • JP-A-2018-113303 Japanese Patent No. 6122704 Japanese Unexamined Patent Publication No. 2019-218229
  • Patent Documents 1 and 2 the conversion rate from BPD to TED is still insufficient, and it cannot be said that the quality of the SiC epitaxial layer is high. Further, in Patent Document 3, when the components such as Nb and Ta added to the SiC single crystal have an unfavorable effect on the characteristics of the semiconductor, Nb and Ta and the like could not be added.
  • the present invention has been made to solve such a problem, and an object of the present invention is to provide a SiC substrate capable of growing a high-quality SiC epitaxial layer.
  • the rare earth-containing SiC substrate of the present invention It contains a rare earth element, and the concentration of the rare earth element is 1 ⁇ 10 16 atoms / cm 3 or more and 1 ⁇ 10 19 atoms / cm 3 or less. It is a thing.
  • the concentration of the rare earth element is set within the range of 1 ⁇ 10 16 atoms / cm 3 or more and 1 ⁇ 10 19 atoms / cm 3 or less. Therefore, the BPD density of the SiC epitaxial growth layer grown on the rare earth-containing SiC substrate can be sufficiently reduced as compared with the BPD density of the rare earth-containing SiC substrate.
  • the SiC epitaxial growth layer thus obtained is suitable for manufacturing a SiC device (for example, SiC-MOSFET, SiC-SBD, etc.) by laminating a functional layer on the surface thereof. Further, since the rare earth-containing SiC substrate 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-containing SiC substrate of the present invention preferably contains Al, and the concentration of Al in that case is preferably 1 ⁇ 10 16 atoms / cm 3 or more and 1 ⁇ 10 21 atoms / cm 3 or less. In this way, the BPD density of the SiC epitaxial growth layer grown on the rare earth-containing SiC substrate can be further reduced. (Concentration of rare earth elements) (Al concentration) / is preferably not 1 ⁇ 10 5 or less 1 ⁇ 10 -2 or more.
  • the rare earth-containing SiC substrate of the present invention preferably contains N in addition to Al, and the concentration of N in that case is 1 ⁇ 10 17 atoms / cm 3 or more and 1 ⁇ 10 22 atoms / cm 3 or less. Is preferable. In this way, the BPD density of the SiC epitaxial growth layer grown on the rare earth-containing SiC substrate can be further reduced.
  • the concentration of rare earth elements) (N concentrations) / is preferably not 1 ⁇ 10 5 or less 1 ⁇ 10 -2 or more.
  • the rare earth element is preferably at least one selected from the group consisting of Y, Sm, Ho, Dy and Yb.
  • the rare earth-containing SiC substrate of the present invention is preferably oriented in both the c-axis direction and the a-axis direction.
  • the variation in the depth direction of the rare earth element is 0.9 or more in terms of coefficient of variation. In this way, the BPD density of the SiC epitaxial growth layer grown on the rare earth-containing SiC substrate can be further reduced.
  • the method of obtaining the coefficient of variation of the variation in the depth direction of the rare earth element will be described in Example (Experimental Example 1) described later.
  • the method for producing a SiC epitaxial layer of the present invention is By supplying a raw material gas for producing SiC to the surface of any of the above-mentioned rare earth-containing SiC substrates, a SiC epitaxial layer is formed on the surface. It is a thing.
  • the BPD density of the SiC epitaxial growth layer grown on the rare earth-containing SiC substrate can be sufficiently reduced.
  • FIG. 3 is a manufacturing process diagram of the SiC composite substrate 10.
  • FIG. 1 is a vertical cross-sectional view of the SiC composite substrate 10 (a cross-sectional view when the SiC composite substrate 10 is cut on a surface including the central axis of the SiC composite substrate 10), and
  • FIG. 2 is a manufacturing process diagram of the SiC composite substrate 10.
  • the SiC composite substrate 10 of the present embodiment includes a SiC single crystal layer 20 and a rare earth-containing SiC layer 30 (corresponding to the rare earth-containing SiC substrate of the present invention).
  • the SiC single crystal layer 20 is a layer made of a SiC single crystal and has a crystal growth surface.
  • the polytype, off-angle, and polarity of the SiC single crystal are not particularly limited, but the polytype is preferably 4H or 6H, and the off-angle is 0.1 to 12 ° from the [0001] axis of the single crystal SiC. It is preferable that the polarity is Si surface. More preferably, the polytype is 4H, the off angle is 1 to 5 ° from the [0001] axis of single crystal SiC, and the polarity is the Si plane.
  • the rare earth-containing SiC layer 30 is provided on the crystal growth surface of the SiC single crystal layer 20, and the SiC is oriented in both the c-axis direction and the a-axis direction. That is, the rare earth-containing SiC layer 30 is preferably 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 biaxial directions of the c-axis and the a-axis. ..
  • 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 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 SiC single crystal layer 20 contains BPD.
  • the BPD density of the SiC single crystal layer 20 is not particularly limited , but is preferably 1 ⁇ 10 5 / cm 2 or less, and more preferably 1 ⁇ 10 3 / cm 2 or less.
  • the rare earth-containing SiC layer 30 contains a rare earth element, and the concentration of the rare earth element is in the range of 1 ⁇ 10 16 atoms / cm 3 or more and 1 ⁇ 10 19 atoms / cm 3 or less. Since the concentration of the rare earth element is set within this range, the BPD density of the SiC epitaxial layer grown on the rare earth-containing SiC layer 30 can be sufficiently reduced as compared with the BPD density of the rare earth-containing SiC layer 30.
  • the rare earth-containing SiC layer 30 contains 17 types of rare earth elements such as scandium, ytterbium, lantern, cerium, praseodymium, neodymium, promethium, samarium, urobium, gadolinium, terbium, disprosium, formium, erbium, thulium, ytterbium and lutetium. It contains at least one element selected from the group consisting of elements. As the rare earth element, at least one of Y and Yb is preferable.
  • the rare earth-containing SiC layer 30 preferably contains Al.
  • the concentration of Al is preferably in the range of 1 ⁇ 10 16 atoms / cm 3 or more and 1 ⁇ 10 21 atoms / cm 3 or less.
  • the BPD density of the SiC epitaxial layer grown on the rare earth-containing SiC layer 30 can be further reduced.
  • Al concentration (Al concentration) / is preferably at 1 ⁇ 10 5 or less 1 ⁇ 10 -2 or more.
  • the rare earth-containing SiC layer 30 preferably contains N in addition to Al. In that case, the concentration of N is preferably 1 ⁇ 10 17 atoms / cm 3 or more and 1 ⁇ 10 22 atoms / cm 3 or less.
  • the concentration of rare earth elements (N concentrations) / is preferably not 1 ⁇ 10 5 or less 1 ⁇ 10 -2 or more.
  • the SiC composite substrate 10 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 a rare earth-containing SiC layer 30 by the heat treatment described later.
  • the method for producing the SiC composite substrate 10 is not limited, and is not particularly limited as long as the SiC layer 30 containing a rare earth element can be obtained.
  • it may be a vapor phase method such as CVD or sublimation method, or a liquid phase method such as a solution method.
  • the alignment precursor layer 40 is formed on the crystal growth surface of the SiC single crystal layer 20.
  • the SiC single crystal layer 20 it is preferable to use a 4H or 6H polytype.
  • the crystal growth plane of the SiC single crystal layer 20 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 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, and a method of directly forming the alignment precursor layer 40 on the SiC single crystal 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 SiC single crystal layer 20 can also be used.
  • a method may be used in which a molded product of the orientation precursor layer 40 is prepared in advance and the molded product is placed on the SiC single crystal 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 is made to contain a rare earth compound according to the concentration of the rare earth element in the rare earth-containing 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 rare earth-containing SiC layer 30
  • the Al compound is contained in the raw material powder of the orientation precursor layer 40 according to the Al concentration in the rare earth-containing 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 rare earth-containing SiC layer 30, a nitrogen compound is contained in the raw material powder of the orientation precursor layer 40 according to the N concentration in the rare earth-containing 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 can also be contained by synthesizing a rare earth-containing SiC layer from the raw material powder of the orientation precursor layer 40 in a nitrogen atmosphere, or by annealing the synthesized rare earth-containing SiC layer in a nitrogen atmosphere.
  • the SiC single crystal layer 20 is laid on the SiC single crystal layer 20 without going through the heat treatment step described later.
  • 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 rare earth-containing SiC layer 30.
  • a method of forming the orientation precursor layer 40 directly on the SiC single crystal 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 formed on the SiC single crystal layer 20.
  • the method of placing in 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. is necessary.
  • 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 SiC single crystal layer 20 is also preferable as a simple method, but since the alignment precursor layer 40 is composed of powder, a process of sintering in a heat treatment step described later. Needs. Although known conditions can be used for any of the methods, in the following, a method of forming the orientation precursor layer 40 directly on the SiC single crystal layer 20 by an AD method or a thermal CVD method and a prefabricated molded product are used as a SiC single crystal. The method of placing on the layer 20 will be described.
  • 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 a raw material powder containing a raw material component, and a film forming unit 60 that injects the raw material powder onto a SiC single crystal 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 SiC single crystal layer 20, a substrate holder 64 that is arranged inside the film forming chamber 62 and fixes the SiC single crystal layer 20, and a substrate holder 64. It is provided with an XY stage 63 that moves in the axis-Y axis direction.
  • the film forming section 60 includes an injection nozzle 66 in which a slit 67 is formed at the tip thereof to inject aerosol into the SiC single crystal 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. It has been known.
  • 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. In these molded bodies, the portion near the SiC single crystal layer 20 becomes the rare earth-containing SiC layer 30 by the subsequent heat treatment on the SiC single crystal layer 20.
  • the molded product it is necessary to sinter the molded product in the heat treatment step described later. It is preferable to form the rare earth-containing SiC layer 30 after the molded product is sintered and undergoes a step of being integrated with the SiC single crystal layer 20 as a polycrystal. If the molded product does not pass through the sintered state, epitaxial growth using the SiC single crystal as a seed may not occur sufficiently. Therefore, the molded product may contain additives such as a sintering aid in addition to the SiC raw material.
  • (B) Heat treatment step (see FIG. 2 (b))
  • the rare earth-containing SiC layer 30 is generated by heat-treating the laminate in which the orientation precursor layer 40 is laminated or placed on the SiC single crystal layer 20.
  • the heat treatment method is not particularly limited as long as epitaxial growth using the SiC single crystal 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 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 rare earth-containing 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 SiC single crystal layer 20 to the c-axis and the a-axis, so that the orientation precursor layer 40 gradually grows from the crystal growth plane. It changes to the rare earth-containing SiC layer 30.
  • the generated rare earth-containing SiC layer 30 has a low BPD density (for example, 1 ⁇ 10 2 / cm 2 or less). The reason why the BPD density decreases in this way is unknown, but it is thought that it is related to the bending of defects due to crystal growth, the conversion to laminated defects that extend in the direction orthogonal to the c-axis, and the pair annihilation of defects. ..
  • the BPD density is measured by etch pit evaluation using known KOH melt etching.
  • the method for growing the SiC epitaxial layer is not particularly limited, and a known method can be adopted.
  • a SiC composite substrate 10 is arranged on a susceptor in a CVD apparatus so that the surface of the rare earth-containing SiC layer 30 faces up, silane and propane are used as raw material gases, and hydrogen is supplied as a carrier gas for epitaxial growth. You may do so.
  • 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 concentration of the rare earth element is set within the range of 1 ⁇ 10 16 atoms / cm 3 or more and 1 ⁇ 10 19 atoms / cm 3 or less.
  • the BPD density of the SiC epitaxial growth layer grown on the rare earth-containing SiC layer 30 can be sufficiently reduced as compared with the BPD density of the rare earth-containing SiC layer 30.
  • the SiC epitaxial growth layer thus obtained is suitable for manufacturing a SiC device (for example, SiC-MOSFET, SiC-SBD, etc.) by laminating a functional layer on the surface thereof.
  • the rare earth-containing 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-containing SiC layer 30 preferably contains Al, and the concentration of Al in that case is preferably 1 ⁇ 10 16 atoms / cm 3 or more and 1 ⁇ 10 21 atoms / cm 3 or less. In this way, the BPD density of the SiC epitaxial growth layer grown on the rare earth-containing SiC layer 30 can be further reduced.
  • the rare earth-containing SiC layer 30 preferably contains N in addition to Al, and the concentration of N in that case is 1 ⁇ 10 17 atoms / cm 3 or more and 1 ⁇ 10 22 atoms / cm 3 or less. Is preferable. In this way, the BPD density of the SiC epitaxial growth layer grown on the rare earth-containing SiC layer 30 can be further reduced.
  • the SiC epitaxial layer is formed on the surface of the rare earth-containing SiC layer 30 by supplying a raw material gas for producing SiC. According to this production method, the BPD density of the SiC epitaxial growth layer grown on the rare earth-containing SiC layer 30 can be sufficiently reduced as compared with the BPD density of the rare earth-containing SiC layer 30.
  • argon is contained in the vicinity of the interface between the SiC single crystal layer 20 and the rare earth-containing SiC layer 30 from the viewpoint of reducing the BPD density in the SiC epitaxial growth layer.
  • the orientation precursor layer 40 is laminated on the rare earth-containing SiC layer 30 of the SiC composite substrate 10, and heat treatment, annealing, and grinding are performed in this order to obtain a second layer of rare earth on the rare earth-containing SiC layer 30.
  • the containing SiC layer 30 can be provided.
  • SiC single crystal substrate as a SiC single crystal layer (n-type 4H-SiC, diameter 50.8 mm (2 inches), Si plane, (0001) plane, off angle 4 °, thickness 0.35 mm, no orientation, BPD density 1.0 ⁇ 10 5 / cm 2 ) 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
  • the average value of a total of 224 points of data in a range of 10 ⁇ m in the direction) was determined.
  • the Y / Al concentration ratio and the N / Y concentration ratio were also determined.
  • the coefficient of variation was calculated in order to represent the concentration variation in the range of 10 ⁇ m in the depth direction of Y. That is, after calculating the standard deviation and the average value of the total number of data of 224 points in the depth direction of 10 ⁇ m, the coefficient of variation was obtained by dividing the standard deviation by the average value. The results obtained are shown in Table 1.
  • SiC epitaxial layer 1 The composite substrate produced by the same method as in (1) to (3) (3-1) is placed in the CVD apparatus, silane and propane are used as the raw material gas, and hydrogen is supplied as the carrier gas to supply the composite substrate. Epitaxial growth was carried out on the biaxially oriented SiC layer. At this time, the growth temperature was 1600 ° C. and the concentration ratio C / Si was 1.2. A SiC epitaxial layer (single crystal layer) was formed on the biaxially oriented SiC layer until the film thickness became 10 ⁇ m to obtain a SiC epitaxial substrate.
  • the surface BPD density of the SiC epitaxial substrate obtained in 1 was evaluated by the following method.
  • the composite substrate was placed in a nickel crucible together with KOH crystals and etched at 500 ° C. for 10 minutes in an electric furnace.
  • the evaluation sample after the etching treatment was washed, observed with an optical microscope, and the number of pits showing BPD was counted by a known method.
  • a field of view of 2.3 mm in length ⁇ 3.6 mm in width was photographed for 100 images at a magnification of 50 times, the total number of pits was counted, and the total number of counted pits was counted.
  • the BPD density was calculated by dividing by the total area of 8.05 cm 2. The results were as shown in Table 1.
  • the obtained heat treatment layer was a biaxially oriented SiC layer.
  • Table 1 shows the concentrations of Y, Al, and N in the biaxially oriented SiC layer, the variation in the depth direction of Y, the Al / Y concentration ratio, the N / Y concentration ratio, and the BPD density on the surface of the SiC epitaxial layer.
  • Example 3 Using a raw material powder containing 99.95% by weight of ⁇ -SiC powder, 0.05% by weight of yttrium oxide powder, and 0.0002% by weight of aluminum nitride 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 biaxially oriented SiC layer. Table 1 shows the concentrations of Y, Al, and N in the biaxially oriented SiC layer, the variation in the depth direction of Y, the Al / Y concentration ratio, the N / Y concentration ratio, and the BPD density on the surface of the SiC epitaxial layer.
  • Example 4 The experiment was carried out in the same manner as in Experimental Example 1 except that a raw material powder containing 98.65% by weight of ⁇ -SiC powder, 0.05% by weight of yttrium oxide powder and 1.3% by weight of aluminum nitride powder was used. carried out. It was confirmed that the obtained heat treatment layer was a biaxially oriented SiC layer. Table 1 shows the concentrations of Y, Al, and N in the biaxially oriented SiC layer, the variation in the depth direction of Y, the Al / Y concentration ratio, the N / Y concentration ratio, and the BPD density on the surface of the SiC epitaxial layer.
  • Example 5 Using a raw material powder containing 92.90% by weight of ⁇ -SiC powder, 7.1% by weight of yttrium oxide powder, and 0.0002% by weight of aluminum nitride 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 biaxially oriented SiC layer.
  • Table 1 shows the concentrations of Y, Al, and N in the biaxially oriented SiC layer, the variation in the depth direction of Y, the Al / Y concentration ratio, the N / Y concentration ratio, and the BPD density on the surface of the SiC epitaxial layer.
  • Example 6 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 biaxially oriented SiC layer. Table 1 shows the concentrations of Y, Al, and N in the biaxially oriented SiC layer, the variation in the depth direction of Y, the Al / Y concentration ratio, and the BPD density on the surface of the SiC epitaxial layer.
  • Example 7 Using a raw material powder containing 99.95% by weight of ⁇ -SiC powder, 0.05% by weight of yttrium oxide powder, and 0.0003% 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 biaxially oriented SiC layer. Table 1 shows the concentrations of Y, Al, and N in the biaxially oriented SiC layer, the variation in the depth direction of Y, the Al / Y concentration ratio, and the BPD density on the surface of the SiC epitaxial layer.
  • Example 8 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 biaxially oriented SiC layer. Table 1 shows the concentrations of Y, Al, and N in the biaxially oriented SiC layer, the variation in the depth direction of Y, the N / Y concentration ratio, and the BPD density on the surface of the SiC epitaxial layer.
  • Table 1 shows the concentrations of Y, Al, and N in the biaxially oriented SiC layer, the variation in the depth direction of Y, the Al / Y concentration ratio, the N / Y concentration ratio, and the BPD density on the surface of the SiC epitaxial layer.
  • Example 12 Using a raw material powder containing 99.92% by weight of ⁇ -SiC powder, 0.08% by weight of samarium oxide powder, and 0.0002% by weight of aluminum nitride 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 biaxially oriented SiC layer. Table 1 shows the concentrations of Sm, Al, and N in the biaxially oriented SiC layer, the variation in the depth direction of Y, the Al / Sm concentration ratio, the N / Sm concentration ratio, and the BPD density on the surface of the SiC epitaxial layer.
  • Example 15 Using a raw material powder containing 99.995% by weight of ⁇ -SiC powder, 0.005% by weight of yttrium oxide powder, and 0.0001% 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 biaxially oriented SiC layer. Table 1 shows the concentrations of Y, Al, and N in the biaxially oriented SiC layer, the variation in the depth direction of Y, the Al / Y concentration ratio, and the BPD density on the surface of the SiC epitaxial layer.
  • Example 16 Using a raw material powder containing 60.0% by weight of ⁇ -SiC powder, 20.0% by weight of yttrium oxide powder, and 20.0% 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 biaxially oriented SiC layer. Table 1 shows the concentrations of Y, Al, and N in the biaxially oriented SiC layer, the variation in the depth direction of Y, the Al / Y concentration ratio, and the BPD density on the surface of the SiC epitaxial layer.
  • Example 17 Using a raw material powder containing 99.995% by weight of ⁇ -SiC powder, 0.005% by weight of yttrium oxide powder, and 0.0001% by weight of aluminum nitride 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 biaxially oriented SiC layer. Table 1 shows the concentrations of Y, Al, and N in the biaxially oriented SiC layer, the variation in the depth direction of Y, the Al / Y concentration ratio, the N / Y concentration ratio, and the BPD density on the surface of the SiC epitaxial layer.
  • Example 18 The experiment was carried out in the same manner as in Experimental Example 1 except that a raw material powder containing 60.0% by weight of ⁇ -SiC powder, 20.0% by weight of yttrium oxide powder and 20.0% by weight of aluminum nitride powder was used. did. It was confirmed that the obtained heat treatment layer was a biaxially oriented SiC layer.
  • Table 1 shows the concentrations of Y, Al, and N in the biaxially oriented SiC layer, the variation in the depth direction of Y, the Al / Y concentration ratio, the N / Y concentration ratio, and the BPD density on the surface of the SiC epitaxial layer.
  • the concentration of rare earth elements such as yttrium and samarium in the biaxially oriented SiC layer is 1 ⁇ 10 16
  • a range of ⁇ 1 ⁇ 10 19 atoms / cm 3 was found to be suitable.
  • aluminum is contained in the range of 1 ⁇ 10 16 to 1 ⁇ 10 21 atoms / cm 3 , the effect of reducing BPD is further enhanced, and nitrogen is further increased to 1 ⁇ 10.
  • the (Al concentration) / (rare earth element concentration) is preferably 1 ⁇ 10 ⁇ 2 to 1 ⁇ 10 5 (Experimental Examples 1 to 7), and (N concentration) / (rare earth element concentration) is 1. It was found that ⁇ 10 ⁇ 2 to 1 ⁇ 10 5 is preferable (Experimental Examples 1 to 5 and Experimental Example 8). On the other hand, from Experimental Examples 13 to 18, it was found that when the contents of yttrium, aluminum and nitrogen were out of the above range, the BPD density in the SiC epitaxial layer was clearly increased.
  • the present invention can be used, for example, in a power semiconductor device (SiC power device).
  • SiC power device SiC power device
  • SiC composite substrate 10 SiC composite substrate, 20 SiC single crystal layer, 30 rare earth-containing SiC layer, 40 orientation precursor layer, 50 AD device, 52 aerosol generator, 53 aerosol generation chamber, 54 raw material supply pipe, 55 vibrator, 60 film formation Part, 62 film forming chamber, 63 XY stage, 64 substrate holder, 66 injection nozzle, 67 slit, 68 vacuum pump.

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