SiC seed crystals and their manufacturing methods, SiC ingots grown from said SiC seed crystals and their manufacturing methods, SiC wafers manufactured from said SiC ingots, SiC wafers with epitaxial films, and their manufacturing methods

Abstract

The present invention addresses the problem of providing a novel technique whereby it becomes possible to provide a high-quality SiC seed crystal, a SiC ingot, a SiC wafer and a SiC wafer with an epitaxial film. The present invention is a method for producing a SiC seed crystal for growing a SiC ingot, the method including a heat treatment step S1 of heat-treating a SiC single crystal body 10 under an atmosphere containing a Si element and a C element. It becomes possible to produce a high-quality SiC seed crystal 11 by heat-treating the SiC single crystal body 10 under an atmosphere containing a Si element and a C element.

Description

[Technical Field]

[0001] The present invention relates to a SiC seed crystal from which strain and dislocation defects have been removed and a manufacturing method thereof, a SiC ingot grown from the SiC seed crystal and a manufacturing method thereof, and a SiC wafer manufactured from the SiC ingot, a SiC wafer with an epitaxial film, and manufacturing methods thereof. [Background technology]

[0002] SiC (silicon carbide) semiconductor devices are capable of higher voltage resistance, higher efficiency, and higher temperature operation than Si (silicon) and GaAs (gallium arsenide) semiconductor devices, and development is underway with a view to industrialization.

[0003] Typically, SiC wafers are manufactured by slicing SiC ingots, which are obtained by growing single-crystal SiC on a SiC seed crystal using a method such as sublimation.

[0004] In the production of SiC ingots, there is a problem that dislocation defects (threading edge dislocations, threading screw dislocations, basal plane dislocations, etc.) remain in the ingot. Various methods have been proposed to solve this problem.

[0005] Patent Document 1 discloses a method for producing a SiC ingot, including a first growth step of growing single crystal SiC on a first growth plane and an nth growth step of growing single crystal SiC on an nth growth plane different from the first growth plane. The manufacturing method described in Patent Document 1 is said to be able to provide high-quality single crystal SiC that is almost free of micropipe defects, screw dislocations, edge dislocations, and stacking faults. It is therefore disclosed that the resulting SiC can be used in high-performance power devices.

[0006] Patent Document 2 describes a technique for emitting threading dislocations from the side surfaces of an epitaxial film by adjusting the impurity concentration of the epitaxial film being grown. It also discloses that by using this epitaxial film as a seed crystal to grow single-crystal SiC in bulk by sublimation, it is possible to further suppress crystal defects. [Prior art documents] [Patent documents]

[0007] [Patent Document 1] Japanese Patent Application Laid-Open No. 2003-321298 [Patent Document 2] Japanese Patent Application Laid-Open No. 2010-184829 Summary of the Invention [Problem to be solved by the invention]

[0008] An object of the present invention is to provide a new technique that can realize high-quality SiC seed crystals, SiC ingots, SiC wafers, and SiC wafers with epitaxial films. [Means for solving the problem]

[0009] The present invention, which solves the above-mentioned problems, is a method for producing a SiC seed crystal for growing a SiC ingot, which comprises a heat treatment step of heat treating a SiC single crystal body in an atmosphere containing Si element and C element. In this way, by heat treating the SiC single crystal mass in an atmosphere containing Si and C elements, it is possible to produce a high-quality SiC seed crystal in which distortion and crystal defects are suppressed.

[0010] In a preferred embodiment of the present invention, the heat treatment step is a step of heat treating the SiC single crystal body in a semi-closed space in which the SiC material is exposed. In this way, by heat treating the SiC single crystal body in a semi-closed space where the SiC material is exposed, it is possible to produce a higher quality SiC seed crystal.

[0011] In a preferred embodiment of the present invention, the heat treatment step is a step of heat treating the SiC single crystal body in a main body container made of SiC material. In this way, by heat treating the SiC single crystal body in the main body container made of SiC material, it is possible to produce a higher quality SiC seed crystal.

[0012] In a preferred embodiment of the present invention, the heat treatment step includes an etching step of etching the SiC single crystal body and / or a crystal growth step of growing a crystal of the SiC single crystal body. In this way, by including the etching step of etching the SiC single crystal body, it is possible to manufacture a SiC seed crystal having a surface with reduced distortion and macrostep bunching. Furthermore, by including a crystal growth step of growing a SiC single crystal, it is possible to manufacture a SiC seed crystal having a growth layer with reduced basal plane dislocations and macrostep bunching.

[0013] In a preferred embodiment of the present invention, the etching step and / or the crystal growth step is a step of placing the SiC single crystal body and the SiC material opposite each other and heating them so as to form a temperature gradient between the SiC single crystal body and the SiC material. In this way, by placing the SiC single crystal body and the SiC material opposite each other in an atmosphere containing Si and C elements and heating them so as to form a temperature gradient between them, etching and crystal growth of the SiC single crystal body can be easily performed.

[0014] In a preferred embodiment of the present invention, the etching step is a step of heating the SiC single crystal body to a high temperature side and the SiC material to a low temperature side. In this way, by heating the SiC single crystal so that the SiC material is on the low temperature side and the SiC single crystal is on the high temperature side, the SiC single crystal can be easily etched.

[0015] In a preferred embodiment of the present invention, the crystal growth step is a step of heating the SiC single crystal body to a low temperature side and the SiC material to a high temperature side. In this way, by heating the SiC single crystal so that the SiC single crystal is on the low temperature side and the SiC material is on the high temperature side, crystal growth of the SiC single crystal can be easily achieved.

[0016] In a preferred embodiment of the present invention, the etching step and / or the crystal growth step includes a step of heating the SiC single crystal body in an SiC-C equilibrium vapor pressure environment. In this way, by including an etching step in which the SiC single crystal mass is etched in an SiC-C equilibrium vapor pressure environment, a high-quality SiC seed crystal from which the strained layer has been removed can be produced. Furthermore, by including a crystal growth step in which a growth layer is grown under a SiC-C equilibrium vapor pressure environment, it is possible to produce a high-quality SiC seed crystal having a surface with reduced basal plane dislocations.

[0017] In a preferred embodiment of the present invention, the etching step and / or the crystal growth step includes a step of placing and heating the SiC single crystal body in a semi-closed space having an atomic ratio Si / C of 1 or less. In this way, by placing and heating a SiC single crystal body in a semi-closed space with an atomic ratio Si / C of 1 or less, it is possible to produce a high-quality SiC seed crystal having a surface with reduced distortion and basal plane dislocations.

[0018] In a preferred embodiment of the present invention, the etching step and / or the crystal growth step includes a step of heating the SiC single crystal body in an SiC-Si equilibrium vapor pressure environment. In this way, by performing etching and crystal growth of a SiC single crystal body in an SiC-Si equilibrium vapor pressure environment, it is possible to produce a high-quality SiC seed crystal having a surface with reduced macrostep bunching.

[0019] In a preferred embodiment of the present invention, the etching step and / or the crystal growth step includes a step of placing the SiC single crystal body in a semi-closed space in which the atomic ratio Si / C exceeds 1, and heating the SiC single crystal body. In this way, by placing and heating a SiC single crystal body in a quasi-closed space with an atomic ratio Si / C exceeding 1, it is possible to produce a high-quality SiC seed crystal having a surface with reduced macrostep bunching.

[0020] In a preferred embodiment of the present invention, the etching step and / or the crystal growth step includes a step of accommodating and heating the SiC single crystal body and a Si vapor supply source in the semi-closed space. In this way, by accommodating and heating a SiC single crystal body and a Si vapor supply source in a semi-closed space, it is possible to easily produce a high-quality SiC seed crystal having a surface with reduced macrostep bunching.

[0021] In a preferred embodiment of the present invention, the heat treatment step includes a planarization step of planarizing the surface of the SiC single crystal body. By including such a planarization step, it is possible to produce a high-quality SiC seed crystal having a surface with reduced macrostep bunching.

[0022] In a preferred embodiment of the present invention, the heat treatment step includes a basal plane dislocation reduction step of forming a growth layer with reduced basal plane dislocations on the SiC single crystal body. In this way, by forming a growth layer on a SiC single crystal body in which basal plane dislocations are removed or reduced, it is possible to suppress the propagation of basal plane dislocations to the SiC ingot in the subsequent ingot growth process.

[0023] In a preferred embodiment of the present invention, the heat treatment step includes a strained layer removal step of removing the strained layer of the SiC single crystal body. In this way, by removing the strained layer from the SiC single crystal, it is possible to obtain a SiC seed crystal from which a higher quality SiC ingot can be produced.

[0024] In a preferred embodiment of the present invention, the heat treatment step includes a basal plane dislocation reduction step of forming a growth layer with reduced basal plane dislocations on the SiC single crystal body after the planarization step. In this way, by forming a growth layer on a SiC single crystal body in which basal plane dislocations are eliminated or reduced, a SiC seed crystal that can be used to produce a higher quality SiC ingot can be obtained.

[0025] In a preferred embodiment of the present invention, the heat treatment step includes a planarization step of planarizing the surface of the SiC single crystal body after the strained layer removal step. In this way, by further planarizing the surface after the strained layer removal step, it is possible to obtain a SiC seed crystal that can be used to produce a higher quality SiC ingot.

[0026] In a preferred embodiment of the present invention, the heat treatment step further includes the planarization step after the basal plane dislocation reduction step. In this way, by further planarizing the surface after the basal plane dislocation reduction step, it is possible to obtain a SiC seed crystal that can be used to produce a higher quality SiC ingot.

[0027] In a preferred embodiment of the present invention, the heat treatment step includes the basal plane dislocation reduction step after the strained layer removal step. In this way, by forming a growth layer with reduced basal plane dislocations on the surface after the strained layer removal step, it is possible to obtain a SiC seed crystal that can be used to produce a higher quality SiC ingot.

[0028] In a preferred embodiment of the present invention, the heat treatment step includes the strained layer removal step, the planarization step, the basal plane dislocation reduction step, and the planarization step in this order. By carrying out the heat treatment in this order, it is possible to obtain a SiC seed crystal that is free from strained layers, basal plane dislocations, and macrostep bunching.

[0029] In a preferred embodiment of the present invention, the strained layer removal step is a step of placing the SiC single crystal body and the SiC material opposite each other and heating them so that the SiC single crystal body is on the high temperature side and the SiC material is on the low temperature side. In this way, by etching the SiC single crystal body using the temperature gradient as a driving force, a SiC seed crystal with a reduced strain layer can be obtained.

[0030] In a preferred embodiment of the present invention, the planarization step includes a step of placing the SiC single crystal body and a SiC material opposite each other, and heating them in a SiC-Si equilibrium vapor pressure environment so as to form a temperature gradient between the SiC single crystal body and the SiC material. In this way, by heating in a SiC-Si equilibrium vapor pressure environment so as to form a temperature gradient between the SiC single crystal body and the SiC material, a SiC seed crystal having a surface with reduced macrostep bunching can be obtained.

[0031] In a preferred embodiment of the present invention, the planarization step includes a step of placing a SiC single crystal body and a SiC material opposite each other in a quasi-closed space in which the atomic ratio Si / C exceeds 1, and heating the SiC single crystal body and the SiC material so as to form a temperature gradient between the SiC single crystal body and the SiC material. In this way, by placing a SiC single crystal body and a SiC material in a quasi-closed space with an atomic ratio Si / C exceeding 1 and heating them so as to form a temperature gradient between the SiC single crystal body and the SiC material, a SiC seed crystal having a surface with reduced macrostep bunching can be obtained.

[0032] In a preferred embodiment of the present invention, the planarization step includes a step of housing the SiC single crystal body and a Si vapor supply source in a main body container made of SiC material, and heating the main body container so as to form a temperature gradient within the main body container. In this way, by housing and heating a SiC single crystal body and a Si vapor supply source in a main body container made of SiC material, it is possible to easily obtain a SiC seed crystal having a surface with reduced macrostep bunching.

[0033] In a preferred embodiment of the present invention, the planarization step includes a step of arranging a SiC single crystal body and a SiC material so that they face each other, and heating the SiC single crystal body to a high temperature side and the SiC material to a low temperature side in a SiC-Si equilibrium vapor pressure environment. In this way, by etching the SiC single crystal body in an SiC-Si equilibrium vapor pressure environment, it is possible to obtain a SiC seed crystal having a surface with reduced macrostep bunching (etching planarization step).

[0034] In a preferred embodiment of the present invention, the planarization step includes a step of arranging a SiC single crystal body and a SiC material so that they face each other in a quasi-closed space in which the atomic ratio Si / C exceeds 1, and heating the SiC single crystal body so that it is on the high-temperature side and the SiC material is on the low-temperature side. In this way, by placing a SiC single crystal body in a quasi-closed space with an atomic ratio Si / C of 1 or more and etching it, a SiC seed crystal having a surface with reduced macrostep bunching can be obtained (etching planarization process).

[0035] In a preferred embodiment of the present invention, the planarization step includes a step of arranging a SiC single crystal body and a SiC material so that they face each other, and heating the SiC single crystal body to a low temperature side and the SiC material to a high temperature side in a SiC-Si equilibrium vapor pressure environment. In this way, by growing a SiC single crystal mass under a SiC-Si equilibrium vapor pressure environment, it is possible to obtain a SiC seed crystal having a growth layer with reduced macrostep bunching (growth flattening step).

[0036] In a preferred embodiment of the present invention, the planarization step includes a step of arranging a SiC single crystal body and a SiC material opposite each other in a quasi-closed space in which the atomic ratio Si / C exceeds 1, and heating the SiC single crystal body so that it is on the low-temperature side and the SiC material is on the high-temperature side. In this way, by placing a SiC single crystal body in a quasi-closed space with an atomic ratio Si / C of 1 or more and growing the crystal, a SiC seed crystal having a growth layer with reduced macrostep bunching can be obtained (growth flattening process).

[0037] In a preferred embodiment of the present invention, the basal plane dislocation reduction step is a step of arranging a SiC single crystal body and a SiC material opposite each other and heating them in a SiC-C equilibrium vapor pressure environment so that the SiC single crystal body is on the low temperature side and the SiC material is on the high temperature side. In this way, by growing a SiC single crystal mass under a SiC-C equilibrium vapor pressure environment, basal plane dislocations can be converted to other dislocations with high efficiency, thereby producing a SiC seed crystal with a surface that does not expose basal plane dislocations.

[0038] In a preferred embodiment of the present invention, the basal plane dislocation reduction step is a step of arranging a SiC single crystal body and a SiC material opposite each other in a quasi-closed space having an atomic ratio Si / C of 1 or less, and heating the SiC single crystal body so that it is on the low temperature side and the SiC material is on the high temperature side. In this way, by placing a SiC single crystal in a space where the atomic ratio Si / C is 1 or less and growing the crystal, it is possible to convert basal plane dislocations into other dislocations with high efficiency. This makes it possible to produce a SiC seed crystal with a good surface where basal plane dislocations are not exposed.

[0039] The present invention also relates to a SiC seed crystal for growing a SiC ingot, produced by the above-described production method. The SiC seed crystal of the present invention has a good surface with reduced strain, basal plane dislocations, or macrostep bunching, and therefore, by growing the SiC seed crystal of the present invention, a high-quality SiC ingot can be produced.

[0040] The present invention also relates to a SiC seed crystal for growing a SiC ingot, the seed crystal having a basal plane dislocation-free layer on its surface. Basal plane dislocations are known to be defects that adversely affect SiC semiconductor devices. The SiC seed crystal of the present invention has a growth layer on its surface that does not contain basal plane dislocations, so that basal plane dislocations do not propagate in the SiC ingot during the subsequent ingot growth process.

[0041] In a preferred embodiment of the invention, the SiC seed crystal has a diameter of 6 inches or greater.

[0042] The present invention also relates to a method for producing a SiC ingot, which includes an ingot growing step of growing single crystal SiC on the above-mentioned SiC seed crystal. The above-described SiC seed crystal has a good surface with reduced distortion, basal plane dislocations, or macrostep bunching, and therefore can produce high-quality SiC ingots.

[0043] The present invention also relates to a SiC ingot produced by the above-described production method.

[0044] The present invention also relates to a method for producing a SiC wafer, which includes a slicing step of slicing the SiC ingot into SiC wafers so as to expose the film-formed surface.

[0045] The present invention also relates to a SiC wafer manufactured by the above-described manufacturing method.

[0046] The present invention also relates to a method for producing an epitaxially-filmed SiC wafer, which includes an epitaxial growth step of forming an epitaxial film on the film-forming surface of the above-mentioned SiC wafer. [Effects of the Invention]

[0047] According to the present invention, it is possible to produce a SiC seed crystal having a good surface in which at least one of distortion, basal plane dislocations, and macrostep bunching is reduced, and accordingly, it is possible to provide a high-quality SiC ingot, SiC wafer, and SiC wafer with an epitaxial film.

[0048] Other objects, features and advantages will become apparent from a reading of the following detailed description when taken in conjunction with the drawings and claims. [Brief explanation of the drawings]

[0049] [Figure 1] 1 is a schematic diagram of a manufacturing process of an SiC wafer with an epitaxial film according to an embodiment. [Figure 2] FIG. 1 is a conceptual diagram showing a preferred embodiment of the heat treatment step of the present invention. [Figure 3] FIG. 2 is an explanatory diagram illustrating an outline of an etching mechanism in a heat treatment step of the present invention. [Figure 4] FIG. 2 is an explanatory diagram illustrating an outline of the growth mechanism in the heat treatment step of the present invention. [Figure 5] 1 is a schematic diagram of a main container and a high-melting-point container according to an embodiment. [Figure 6] FIG. 1 is an explanatory diagram of an apparatus for manufacturing a SiC seed crystal according to an embodiment. [Figure 7] FIG. 2 is a schematic diagram showing a vessel configuration in a preferred embodiment of the heat treatment step of the present invention. [Figure 8] FIG. 10 is a diagram illustrating an outline of a strained layer removing step. [Figure 9] FIG. 10 is a diagram showing an apparatus configuration for implementing a strained layer removal step. [Figure 10] FIG. 1 is a diagram illustrating an outline of an etching planarization process. [Figure 11] FIG. 1 is a diagram showing an apparatus configuration for implementing an etching planarization process. [Figure 12] FIG. 1 is an explanatory diagram showing an outline of a growth and flattening step. [Figure 13] FIG. 1 is a diagram showing an apparatus configuration and overview for realizing a growth planarization process. [Figure 14] FIG. 1 is an explanatory diagram illustrating an overview of a basal plane dislocation reduction step. [Figure 15] FIG. 1 is a diagram showing an apparatus configuration and overview for implementing a basal plane dislocation reduction process. [Figure 16] A preferred embodiment of a process for producing a SiC ingot is presented. [Figure 17] 2 is an explanatory diagram of a SiC seed crystal obtained in the strained layer removal step of the present invention. FIG. [Figure 18] FIG. 2 is an explanatory diagram of a SiC seed crystal obtained in the etching planarization step of the present invention. [Figure 19]FIG. 2 is an explanatory diagram of a SiC seed crystal obtained in the growth and flattening step of the present invention. [Figure 20] FIG. 1 is an explanatory diagram of a method for determining the BPD conversion rate in the basal plane dislocation reduction step of the present invention. [Figure 21] 1 is an Arrhenius plot of the etching process and the crystal growth process of the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0050] <1> Summary of the Invention The following describes in detail preferred embodiments of the present invention with reference to the accompanying drawings. The technical scope of the present invention is not limited to the embodiments shown in the accompanying drawings, and can be modified as appropriate within the scope of the claims.

[0051] First, referring to FIG. 1, an outline of one embodiment of the method of the present invention for producing a SiC seed crystal 11, a SiC ingot 12, a SiC wafer 13, and an epitaxially coated SiC wafer 14 will be described.

[0052] A feature of the present invention is that a high-quality SiC seed crystal 11 is obtained by subjecting a SiC single crystal mass 10 to a heat treatment step S1 (FIG. 1). By subjecting a SiC single crystal mass 10 to the heat treatment step S1, a high-quality SiC seed crystal 11 can be obtained in which distortion (strained layer 101), basal plane dislocations (BPD), and macro step bunching (MSB) are eliminated or reduced.

[0053] In this specification, the term "SiC single crystal mass" broadly includes single crystal SiC in a state prior to being subjected to the ingot growth step S2 as the SiC seed crystal 11. The term "SiC single crystal mass" does not limitatively refer to single crystal SiC in a particular state.

[0054] After the heat treatment step S1, at least one of distortion, BPD, and MSB is removed or reduced from the SiC seed crystal 11, making it suitable for growing a high-quality SiC ingot. In the present invention, a high-quality SiC ingot 12 can be obtained by performing an ingot growth step S2 in which single-crystal SiC is grown on the SiC seed crystal 11 (see FIG. 1).

[0055] The SiC ingot 12 thus obtained is suppressed from inheriting defects caused by distortion, BPD, MSB, etc., that were present in the SiC single crystal mass 10. Therefore, the SiC wafers 13 cut out from the ingot 12 in the slicing step S3 are also of high quality (see FIG. 1).

[0056] Normally, when BPDs exist on the surface of a SiC wafer, the BPDs may propagate to the epitaxial film formed by epitaxially growing the SiC wafer. However, in the present invention, neither strain nor BPDs are exposed on the surface of the SiC wafer 13. Therefore, propagation of BPDs to the epitaxial film formed on the SiC wafer 13 can be suppressed. In other words, according to the present invention, it is possible to manufacture a SiC wafer 14 with an epitaxial film, which can be used to manufacture high-performance SiC semiconductor devices (see FIG. 1). Each of the components of the present invention will be described in further detail below.

[0057] <2> SiC single crystal 10 An example of the SiC single crystal body 10 is a SiC substrate obtained by processing single crystal SiC into a thin plate. More specifically, an example is a SiC wafer obtained by slicing a SiC ingot produced by a sublimation method or the like into a disk shape. Note that any polytype of single crystal SiC can be used.

[0058] Typically, a SiC single crystal mass 10 that has undergone mechanical processing (e.g., slicing, grinding, and polishing) or laser processing has a strained layer 101 in which processing damage such as scratches 1011, latent scratches 1012, and distortions 1013 has been introduced, and a bulk layer 102 in which such processing damage has not been introduced (see FIG. 8).

[0059] The presence or absence of this strained layer 101 can be confirmed by SEM-EBSD, TEM, μXRD, Raman spectroscopy, etc. In order to grow a high-quality SiC ingot, it is preferable to remove the strained layer 101 and expose the bulk layer 102 that has not been subjected to processing damage.

[0060] A step-terrace structure is observed on the atomically flattened surface of SiC single crystal 10. This step-terrace structure is a staircase structure in which steps 103, which are step portions of one molecular layer or more, and terraces 104, which are flat portions where the {0001} plane is exposed, are arranged alternately (see FIGS. 10 and 12).

[0061] The step 103 has a minimum height (minimum unit) of one molecular layer (0.25 nm), and various step heights are formed by stacking multiple layers of this one molecular layer. In the description herein, the steps 103 bunch together to become huge and have a height exceeding one unit cell of each polytype, and are referred to as MSBs.

[0062] That is, an MSB refers to a step 103 bunched beyond four molecular layers (five molecular layers or more) in the case of 4H—SiC, and refers to a step 103 bunched beyond six molecular layers (seven molecular layers or more) in the case of 6H—SiC.

[0063] If defects caused by these MSBs are inherited by the SiC ingot, this will lead to a deterioration in the performance of the SiC semiconductor device. Therefore, it is desirable that no MSBs are formed on the surface of the SiC seed crystal 11.

[0064] <3> Heat treatment process S1 The heat treatment step S1 is a step of heat treating the SiC single crystal mass 10 in an atmosphere containing Si and C elements. The SiC seed crystal 11 that has undergone the heat treatment step S1 has a surface in which at least one of strain (strained layer 101), BPDs, and MSBs has been reduced. Therefore, in the subsequent ingot growth step S2, defects caused by the strain, BPDs, and MSBs of the SiC seed crystal 11 can be prevented from being inherited by the SiC ingot 12. In other words, a high-quality SiC ingot 12 can be produced.

[0065] Specifically, the heat treatment step S1 can be exemplified by heating the SiC single crystal mass 10 and a SiC material while they are facing each other. That is, the heat treatment step S1 can include an etching step of transporting Si and C elements from the SiC single crystal mass 10 to the SiC material to etch the SiC single crystal mass 10, and a crystal growth step of transporting Si and C elements from the SiC material to the SiC single crystal mass 10 to grow the SiC single crystal mass 10. The specific form of heat treatment step S1 is not particularly limited as long as it is a step that can remove or reduce strained layer 101, BPDs, and MSBs contained in SiC single crystal mass 10.

[0066] The driving force for transporting the Si and C elements in the etching and crystal growth steps can be the temperature gradient or chemical potential difference between the SiC single crystal mass 10 and the SiC material.

[0067] The SiC material is made of SiC that can receive or transfer Si and C elements between the SiC single crystal mass 10 and the SiC single crystal mass 10 when heated while facing the SiC material. For example, a SiC container (main container 20) or a SiC substrate (SiC member) can be used. Note that any polytype can be used as the crystalline polymorph of this SiC material, and polycrystalline SiC may also be used.

[0068] The SiC single crystal body 10 and the SiC material are preferably placed in a semi-closed space and heated. By receiving or transferring Si and C elements in the semi-closed space, the surface of the SiC single crystal body 10 can be etched and grown to form a surface in which at least one of the strained layer 101, BPDs, and MSBs is reduced. In this specification, the term "semi-closed space" refers to a space in which the container can be evacuated but in which at least a portion of the vapor generated in the container can be confined.

[0069] A preferred embodiment of the heat treatment step S1 will be described in detail below with reference to FIGS. A preferred embodiment of the heat treatment step S1 can be broadly divided into an etching step for etching the surface of the SiC single crystal mass 10, and a crystal growth step for growing single crystal SiC on the SiC single crystal mass 10 (see FIG. 2).

[0070] (etching process) According to the etching step (the step located on the left side of FIG. 2), strained layer 101 and MSBs present on the surface of SiC single crystal mass 10 can be removed or reduced.

[0071] 3 is an explanatory diagram showing an outline of the etching process. In this etching process, SiC single crystal mass 10 is placed in a semi-closed space in which the SiC material is exposed, and is heated at a temperature range of 1400°C to 2300°C, whereby the following reactions 1) to 5) are continuously carried out, resulting in the progress of etching.

[0072] 1) SiC(s) → Si(v) + C(s) 2) 2C(s) + Si(v) → SiC2(v) 3) C(s) + 2Si(v) → SiC(v) 4) Si(v) + SiC2(v) → 2SiC(s) 5) SiC(v) → Si(v) + SiC(s)

[0073] Explanation of 1): When SiC single crystal 10 (SiC(s)) is heated, Si atoms (Si(v)) are desorbed from the surface of SiC single crystal 10 by thermal decomposition (Si atom sublimation process). Explanation of 2) and 3): When Si atoms (Si(v)) are released, C (C(s)) remaining on the surface of SiC single crystal 10 reacts with Si vapor (Si(v)) in the semi-closed space. As a result, C (C(s)) becomes SiC, SiC, etc., and sublimes from the surface of SiC single crystal 10 (C atom sublimation process). Explanation of 4) and 5): Sublimated Si2C or SiC2 etc. reaches the SiC material in the semi-closed space due to the temperature gradient and grows.

[0074] Thus, the etching process includes a Si atom sublimation process in which Si atoms are thermally sublimated from the surface of the SiC single crystal body 10, and a C atom sublimation process in which C atoms remaining on the surface of the SiC single crystal body 10 are sublimated from the surface of the SiC single crystal body 10 by reacting them with Si vapor in the quasi-closed space.

[0075] Preferably, the etching step involves heating the SiC single crystal body 10 so that it is positioned on the high temperature side of the temperature gradient, and the SiC material so that it is positioned on the low temperature side of the temperature gradient, thereby forming an etching space X between the SiC single crystal body 10 and the SiC material, and the surface of the SiC single crystal body 10 can be etched using the temperature gradient as a driving force.

[0076] (Crystal growth process) According to the crystal growth step (the step located on the right side of FIG. 2), BPDs present on the surface of SiC single crystal mass 10 can be converted into other dislocations, and BPDs exposed on the surface of SiC seed crystal 11 can be removed or reduced. Moreover, the MSB on the surface of the SiC seed crystal 11 can be removed or reduced.

[0077] 4 is an explanatory diagram showing an overview of the crystal growth process. In this crystal growth process, SiC single crystal mass 10 is placed in a semi-closed space where the SiC material is exposed, and is heated at a temperature range of 1400°C to 2300°C, whereby the following reactions 1) to 5) are continuously carried out, which is thought to result in the progress of crystal growth.

[0078] 1) Poly-SiC(s) → Si(v) + C(s) 2) 2C(s) + Si(v) → SiC2(v) 3) C(s) + 2Si(v) → SiC(v) 4) Si(v) + SiC2(v) → 2SiC(s) 5) SiC(v) → Si(v) + SiC(s)

[0079] Explanation of 1): When SiC material (Poly-SiC(s)) is heated, Si atoms (Si(v)) are released from the SiC due to thermal decomposition. Explanation of 2) and 3): When Si atoms (Si(v)) are released, the remaining C (C(s)) reacts with the Si vapor (Si(v)) in the semi-closed space. As a result, the C (C(s)) becomes Si2C or SiC2, etc., and sublimes into the semi-closed space. Explanation of 4) and 5): The sublimated SiC or SiC, etc. reaches and diffuses onto the terraces of the SiC single crystal 10 due to the temperature gradient (or chemical potential difference), and when it reaches the steps, it grows while inheriting the polytype of the underlying SiC single crystal 10 (step flow growth).

[0080] Thus, the crystal growth process includes a Si atom sublimation process in which Si atoms are thermally sublimated from the surface of the SiC material, a C atom sublimation process in which C atoms remaining on the surface of the SiC material are sublimated by reacting with Si vapor in a semi-closed space, a raw material transport process in which raw materials (Si atoms and C atoms) are transported to the surface of the SiC single crystal body 10 using a temperature gradient or a chemical potential difference as a driving force, and a step flow growth process in which the raw materials reach the steps of the SiC single crystal body 10 and grow.

[0081] Preferably, the crystal growth step involves heating the SiC material so that it is positioned on the high temperature side of the temperature gradient, and the SiC single crystal mass 10 so that it is positioned on the low temperature side of the temperature gradient. This forms a source material supply space Y between the SiC single crystal mass 10 and the SiC material, and the temperature gradient can be used as a driving force to grow the SiC single crystal mass 10.

[0082] When single crystal SiC is used for the SiC single crystal mass 10 and polycrystalline SiC is used for the SiC material, the partial pressure difference (chemical potential difference) generated at the surfaces of the polycrystalline SiC and single crystal SiC can be used as the driving force for transporting the raw material to grow the crystal. In this case, a temperature gradient may or may not be provided.

[0083] Up to this point, the heat treatment step S1 has been broadly divided into an etching step and a crystal growth step. However, the heat treatment step S1 can also be divided into two types from the perspective of the environment in which the SiC single crystal mass 10 is heated.

[0084] That is, as shown in the vertical direction of FIG. 2, the heat treatment step S1 can be classified into a form in which the SiC single crystal mass 10 is heated in a SiC-Si equilibrium vapor pressure environment, and a form in which the SiC-C equilibrium vapor pressure environment is heated.

[0085] Here, the SiC-Si equilibrium vapor pressure environment refers to a vapor pressure environment in which SiC (solid) and Si (liquid phase) are in phase equilibrium via the gas phase. The SiC-C equilibrium vapor pressure environment refers to a vapor pressure environment in which SiC (solid phase) and C (solid phase) are in phase equilibrium via the gas phase.

[0086] In this specification, the SiC-Si equilibrium vapor pressure environment and the SiC-C equilibrium vapor pressure environment include a near-thermal equilibrium vapor pressure environment that satisfies the relationship between growth rate and growth temperature derived from a theoretical thermal equilibrium environment.

[0087] The atomic ratio Si / C in the gas phase of the SiC-Si equilibrium vapor pressure environment is larger than the atomic ratio Si / C in the gas phase of the SiC-C equilibrium vapor pressure environment.

[0088] The SiC-Si equilibrium vapor pressure environment can be formed by placing and heating the SiC single crystal mass 10 in a semi-closed space in which the atomic ratio Si / C exceeds 1. For example, when the SiC single crystal mass 10 satisfying the stoichiometric ratio of 1:1, a SiC material satisfying the stoichiometric ratio of 1:1, and a Si vapor supply source (Si pellets, etc.) are placed in a SiC container (main container 20) that satisfies the stoichiometric ratio of 1:1, the atomic ratio Si / C in the semi-closed space exceeds 1.

[0089] On the other hand, a SiC-C equilibrium vapor pressure environment can be formed by placing and heating the SiC single crystal mass 10 in a semi-closed space in which the atomic ratio Si / C is 1 or less. For example, when a SiC single crystal mass 10 satisfying a stoichiometric ratio of 1:1 and a SiC material satisfying a stoichiometric ratio of 1:1 are placed in a SiC container (main container 20) that also satisfies a stoichiometric ratio of 1:1, the atomic ratio Si / C in the main container 20 will be 1. Alternatively, a C vapor supply source (C pellets, etc.) may be placed to make the atomic ratio Si / C 1 or less.

[0090] As described above, the heat treatment step S1 can be classified according to whether it is an etching step or a crystal growth step, and whether it is a heat treatment in a SiC-Si equilibrium vapor pressure environment or a SiC-C equilibrium vapor pressure environment. When these classification combinations are linked to effects, they can be classified into the following four types.

[0091] In the case of performing the etching step under a SiC-C equilibrium vapor pressure environment, it is possible to remove the strained layer 101 of the SiC single crystal mass 10 by etching, and MSBs are formed on the surface after etching. For this reason, this step is classified as an etching bunching step S111 (lower left of FIG. 2).

[0092] In the embodiment where the etching step is performed under a SiC-Si equilibrium vapor pressure environment, it is possible to remove the strained layer 101 of the SiC single crystal mass 10 by etching, and no MSB is formed on the surface after etching. For this reason, this step is classified as an etching planarization step S121 (upper left in FIG. 2).

[0093] In the etching bunching step S111 and the etching planarization step S121, the strained layer 101 of the SiC single crystal mass 10 can be removed or reduced, and so these steps are collectively classified as the strained layer removal step S11 (left side of FIG. 2).

[0094] In a form in which the crystal growth step is performed under a SiC-Si equilibrium vapor pressure environment, it is possible to form a growth layer 105 in which MSBs are reduced or removed on the SiC single crystal mass 10. For this reason, this step is classified as a growth flattening step S122 (upper right in FIG. 2).

[0095] In addition, the etching planarization step S121 and the growth planarization step S122 can remove or reduce MSBs, and therefore are collectively classified as the planarization step S12 (upper side of FIG. 2).

[0096] In the case where the crystal growth step is performed under a SiC-C equilibrium vapor pressure environment, it is possible to remove or reduce BPDs in the growth layer 105. Therefore, this step is classified as a basal plane dislocation reduction step S13 (bottom right of FIG. 2).

[0097] (manufacturing equipment) Next, the configuration of a manufacturing device that can realize the above four types of classification will be described. Hereinafter, as a preferred embodiment, a configuration using a main body vessel 20 capable of heat-treating a SiC single crystal body 10 in an atmosphere containing Si and C elements will be described. Naturally, any apparatus configuration that forms an environment similar to that of main body vessel 20 can be adopted. Specifically, any apparatus configuration that can form an atmosphere of Si and C elements in a semi-closed space can be adopted.

[0098] The main container 20 preferably has a configuration in which the SiC material is exposed to the internal space. In this embodiment, the entire main container 20 is made of a SiC material (polycrystalline SiC). By heating the main container 20 made of such a material, an atmosphere containing Si and C elements can be generated inside (semi-closed space).

[0099] The environment inside the heat-treated main container 20 is preferably a vapor pressure environment of a mixture of gaseous species containing Si element and gaseous species containing C element. Examples of the gaseous species containing Si element include Si, Si2, Si3, Si2C, SiC2, and SiC. Examples of the gaseous species containing C element include Si2C, SiC2, SiC, and C. In other words, a state is reached in which SiC-based gas exists inside the main container 20.

[0100] Any configuration can be employed as long as it generates vapor pressure of gaseous species containing Si element and gaseous species containing C element in the internal space during heat treatment of main container 20. For example, a configuration in which SiC material is exposed on a part of the inner surface, or a configuration in which a separate SiC material (such as a substrate made of SiC) is placed inside main container 20 can be shown.

[0101] Heat treatment step S1 is preferably performed by accommodating SiC single crystal body 10 inside main body container 20 and heating main body container 20 so as to form a temperature gradient inside. Below, the apparatus configuration (main body container 20, heating furnace 30, high-melting-point container 40) when main body container 20 is heated so as to form a temperature gradient inside will be described with reference to FIGS. 5 and 6.

[0102] 5, the main container 20 is a fitting container comprising an upper container 21 and a lower container 22 that can fit together. A minute gap 23 is formed at the fitting portion between the upper container 21 and the lower container 22, and the main container 20 is configured so that the inside of the main container 20 can be evacuated (vacuumed) through this gap 23. In other words, the inside of the main container 20 is a semi-closed space.

[0103] Heating furnace 30 has a configuration capable of heating main container 20 with a temperature gradient in an atmosphere containing Si element. Specifically, as shown in Fig. 6, heating furnace 30 includes main heating chamber 31 capable of heating the workpiece (such as SiC single crystal body 10) to a temperature of 1000°C or more and 2300°C or less, preheating chamber 32 capable of preheating the workpiece to a temperature of 500°C or more, high-melting-point container 40 capable of accommodating main container 20, and moving means 33 (moving stage) capable of moving high-melting-point container 40 from preheating chamber 32 to main heating chamber 31.

[0104] The main heating chamber 31 is formed in a regular hexagonal shape in a planar cross section, and a high-melting-point container 40 is placed inside the main heating chamber 31. A heater 34 (mesh heater) is provided inside the main heating chamber 31. In addition, a multilayer heat-reflecting metal plate (not shown) is fixed to the side walls and ceiling of the main heating chamber 31. This multilayer heat-reflecting metal plate is configured to reflect heat from the heater 34 toward approximately the center of the main heating chamber 31.

[0105] As a result, within the main heating chamber 31, a heating heater 34 is arranged to surround the high-melting-point container 40 in which the workpiece is housed, and a multilayer heat-reflecting metal plate is further arranged on the outside of that, allowing the temperature to be raised to a temperature of 1000°C or higher and 2300°C or lower. The heater 34 may be, for example, a resistance heating heater or a high-frequency induction heating heater.

[0106] The heater 34 may also be configured to be capable of forming a temperature gradient within the high-melting-point container 40. For example, the heater 34 may be configured so that more heaters are arranged on the upper side (or lower side). The heater 34 may also be configured so that its width increases toward the upper side (or lower side). Alternatively, the heater 34 may be configured so that the power supplied to it can increase toward the upper side (or lower side).

[0107] In addition, the main heating chamber 31 is connected to a vacuum forming valve 35 for evacuating the main heating chamber 31, an inert gas injection valve 36 for introducing an inert gas into the main heating chamber 31, and a vacuum gauge 37 for measuring the degree of vacuum within the main heating chamber 31.

[0108] The vacuum forming valve 35 is connected to a vacuum pump (not shown) that evacuates the main heating chamber 31 to create a vacuum. By using the vacuum forming valve 35 and the vacuum pump, the degree of vacuum in the main heating chamber 31 can be set to, for example, 10 Pa or less, more preferably 1 Pa or less, and even more preferably 10 -3 The pressure can be adjusted to below Pa. An example of the vacuum pump is a turbo molecular pump.

[0109] The inert gas injection valve 36 is connected to an inert gas supply source (not shown). The inert gas is injected into the heating chamber 31 by the inert gas injection valve 36 and the inert gas supply source. -5 It can be introduced at a pressure in the range of up to 10,000 Pa. As this inert gas, Ar, He, N2, etc. can be selected.

[0110] Preheating chamber 32 is connected to main heating chamber 31, and is configured so that high-melting-point container 40 can be moved by moving means 33. Note that preheating chamber 32 in this embodiment is configured so that it can be heated by residual heat from heater 34 of main heating chamber 31. For example, when main heating chamber 31 is heated to 2000°C, preheating chamber 32 is heated to about 1000°C, and degassing of the workpiece (SiC single crystal body 10, main container 20, high-melting-point container 40, etc.) can be performed.

[0111] The moving means 33 is configured to be able to place the high-melting-point container 40 and move it between the main heating chamber 31 and the preheating chamber 32. The transfer between the main heating chamber 31 and the preheating chamber 32 by the moving means 33 can be completed in as little as one minute, making it possible to achieve a temperature increase and decrease rate of 1 to 1000°C / min. In this way, the present manufacturing apparatus is capable of rapid temperature increase and decrease, making it possible to observe surface shapes that do not have a history of low-temperature growth during temperature increase and decrease, which was difficult with conventional apparatuses. In addition, in FIG. 6, the preheating chamber 32 is arranged below the main heating chamber 31, but this is not limitative and the chamber may be arranged in any direction.

[0112] Furthermore, the moving means 33 according to this embodiment is a moving stage on which the high-melting-point container 40 is placed. A small amount of heat is released from the contact area between the moving stage and the high-melting-point container 40. This allows a temperature gradient to be formed within the high-melting-point container 40.

[0113] In the heating furnace 30 of this embodiment, the bottom of the high-melting-point container 40 is in contact with the moving stage, so a temperature gradient is created such that the temperature decreases from the upper container 41 to the lower container 42 of the high-melting-point container 40. The direction of this temperature gradient can be set to any direction by changing the position of the contact point between the moving stage and the high-melting-point container 40. For example, if a hanging type moving stage is used and the contact point is provided on the ceiling of the high-melting-point container 40, heat will escape upward. Therefore, the temperature gradient is set so that the temperature increases from the upper container 41 to the lower container 42 of the high-melting-point container 40. It is desirable that this temperature gradient be formed along the front-to-back direction of the SiC single crystal mass 10. As described above, the heater 34 may be configured to create a temperature gradient.

[0114] The atmosphere containing Si element in heating furnace 30 is formed using high-melting-point container 40 and Si vapor supply source 44. For example, any method capable of forming an atmosphere containing Si element around main body container 20 can be adopted in the manufacturing apparatus for SiC seed crystal 11.

[0115] The high-melting-point container 40 is configured to contain a high-melting-point material, such as C, which is a general-purpose heat-resistant member; W, Re, Os, Ta, and Mo, which are high-melting-point metals; Ta9C8, HfC, TaC, NbC, ZrC, Ta2C, TiC, WC, and MoC, which are carbides; HfN, TaN, BN, Ta2N, ZrN, and TiN, which are nitrides; HfB2, TaB2, ZrB2, Nb2, and TiB2, which are borides; and polycrystalline SiC.

[0116] Like the main container 20, the high-melting-point container 40 is a fitting container comprising an upper container 41 and a lower container 42 that can fit together, and is configured to be able to house the main container 20. A minute gap 43 is formed at the fitting portion between the upper container 41 and the lower container 42, and the high-melting-point container 40 is configured to be able to be evacuated (vacuumed) through this gap 43. In other words, like the main container 20, the interior of the high-melting-point container 40 is preferably a semi-closed space.

[0117] The high-melting-point container 40 has a Si vapor supply source 44 capable of supplying Si vapor into the high-melting-point container 40. The Si vapor supply source 44 may be configured to generate Si vapor in the high-melting-point container 40 during heat treatment. Examples of the Si vapor supply source 44 include solid Si (single-crystal Si pieces, Si pellets such as Si powder, etc.) and Si compounds.

[0118] In the manufacturing apparatus for SiC seed crystal 11 according to this embodiment, TaC is used as the material for high-melting-point container 40, and tantalum silicide is used as Si vapor supply source 44. That is, as shown in Fig. 5, a tantalum silicide layer is formed inside high-melting-point container 40, and Si vapor is supplied from the tantalum silicide layer into the container during heat treatment. This creates a Si vapor pressure environment within high-melting-point container 40, and main container 20 can be heated in an atmosphere containing Si elements. Other configurations may be adopted as long as an atmosphere containing Si elements is formed in the high-melting-point container 40 during the heat treatment.

[0119] According to the manufacturing apparatus for SiC seed crystal 11 of this embodiment, main container 20 is heated in an atmosphere containing Si element (for example, a Si vapor pressure environment), thereby making it possible to prevent gaseous species containing Si element from being exhausted from inside main container 20. That is, by balancing the vapor pressure of the gaseous species containing Si element inside main container 20 and the vapor pressure of the gaseous species containing Si element outside main container 20, the environment inside main container 20 can be maintained.

[0120] Furthermore, in the manufacturing apparatus for SiC seed crystal 11 according to this embodiment, main container 20 is made of polycrystalline SiC. With this configuration, when main container 20 is heated using heating furnace 30, vapor of a gas phase species containing Si element and a gas phase species containing C element can be generated inside main container 20.

[0121] (Device configuration for implementing heat treatment process S1) The outline of the equipment configuration that realizes the above-mentioned four types of etching (etching under a SiC-C equilibrium vapor pressure environment (lower left in Figure 2), etching under a SiC-Si equilibrium vapor pressure environment (upper left in Figure 2), crystal growth under a SiC-C equilibrium vapor pressure environment (lower right in Figure 2), and crystal growth under a SiC-Si equilibrium vapor pressure environment (upper right in Figure 2)) will be described in detail with reference to Figure 7.

[0122] An outline of the apparatus configuration for implementing the etching step is shown on the left side of Fig. 7. As shown on the left side of Fig. 7, main body vessel 20 has etching space X in which SiC single crystal body 10 is located on the high temperature side of the temperature gradient and SiC material (part of main body vessel 20) is located on the low temperature side of the temperature gradient. That is, etching space X is formed by arranging SiC single crystal body 10 at a position where it is hotter than the SiC material (e.g., the bottom surface of lower vessel 22) due to the temperature gradient formed by heating furnace 30.

[0123] Etching space X is a space that transports Si atoms and C atoms on the surface of SiC single crystal body 10 to main body vessel 20 using the temperature difference between SiC single crystal body 10 and main body vessel 20 as a driving force. For example, main vessel 20 is heated so that, when the temperature of the surface of SiC single crystal body 10 is compared with the temperature of the bottom of lower vessel 22 facing this surface, the temperature on the surface side of SiC single crystal body 10 is higher and the temperature on the bottom side of lower vessel 22 is lower (see the left side of FIG. 7). In this way, by forming a space (etching space X) with a temperature difference between the surface of SiC single crystal body 10 and the bottom of lower vessel 22, it is possible to transport Si atoms and C atoms using the temperature difference as a driving force and etch the surface of SiC single crystal body 10 (the open arrow on the right side of FIG. 7 indicates the direction of transport).

[0124] The main body vessel 20 may have a substrate holder 24 provided between the SiC single crystal mass 10 and the main body vessel 20 .

[0125] The heating furnace 30 according to this embodiment is configured to be capable of heating by forming a temperature gradient such that the temperature decreases from the upper vessel 21 to the lower vessel 22 of the main vessel 20. Therefore, a substrate holder 24 capable of holding the SiC single crystal mass 10 may be provided between the SiC single crystal mass 10 and the lower vessel 22, thereby forming an etching space X between the SiC single crystal mass 10 and the lower vessel 22.

[0126] The substrate holder 24 may be configured to hold at least a portion of the SiC single crystal mass 10 in the hollow of the main body container 20. Naturally, any conventional supporting means may be employed, such as one-point support, three-point support, a configuration that supports the outer periphery, or a configuration that clamps a portion. The substrate holder 24 may be made of SiC or a high-melting-point metal material.

[0127] Substrate holder 24 may not be provided depending on the direction of the temperature gradient in heating furnace 30. For example, if heating furnace 30 forms a temperature gradient such that the temperature decreases from lower vessel 22 to upper vessel 21, SiC single crystal mass 10 may be placed on the bottom surface of lower vessel 22 (without substrate holder 24).

[0128] Next, an outline of the apparatus configuration for implementing the crystal growth step is illustrated on the right side of Fig. 7. As shown on the right side of Fig. 7, main vessel 20 has a source material supply space Y in which SiC single crystal body 10 is located on the low temperature side of the temperature gradient and the SiC material (part of main vessel 20) is located on the high temperature side of the temperature gradient. That is, the source material supply space Y is formed by arranging SiC single crystal body 10 at a position where its temperature is lower than that of the SiC material (for example, the top surface of upper vessel 21) due to the temperature gradient formed by heating furnace 30.

[0129] That is, in addition to the SiC single crystal mass 10, a Si atom supply source and a C atom supply source, which are the raw materials, are present within the raw material supply space Y. These are heated to supply the Si atoms and C atoms, which are the raw materials for the SiC single crystal mass 10, into the raw material supply space Y. These Si atoms and C atoms are transported to the surface of the SiC single crystal mass 10 and recrystallized, thereby forming a growth layer 105 (the black arrow on the right side of FIG. 7 indicates the direction of transport).

[0130] In this embodiment, at least a portion of main vessel 20 is made of polycrystalline SiC (Poly-SiC), so that main vessel 20 itself serves as a Si atom supply source and a C atom supply source. As the Si atom source and the C atom source, a material capable of supplying Si atoms, such as a Si substrate, a material capable of supplying C atoms, such as graphite, or a material capable of supplying Si atoms and C atoms, such as a SiC substrate, can be used.

[0131] The arrangement of the Si atom supply source and the C atom supply source is not limited to this form, and any form capable of supplying Si atoms and C atoms into the raw material supply space Y may be used. When polycrystalline SiC is used as the source material, the vapor pressure difference (chemical potential difference) between polycrystalline SiC (source material) and single-crystal SiC (SiC single-crystal mass 10) can be used as the growth driving force.

[0132] Furthermore, a temperature gradient is provided within the source supply space Y such that the temperature decreases toward the SiC single crystal mass 10. This temperature gradient serves as a growth driving force for transporting Si atoms and C atoms to the SiC single crystal mass 10, thereby increasing the growth rate of the growth layer 105 (the black arrow on the right side of FIG. 7 indicates the direction of transport).

[0133] Furthermore, in order to allow Si atoms and C atoms to efficiently reach the SiC single crystal body 10, the Si atom supply source and the C atom supply source may be located close to the SiC single crystal body 10. In the configuration on the right side of Fig. 7, an upper vessel 21 made of polycrystalline SiC, which serves as the Si atom supply source and the C atom supply source, may be located close to and parallel to the SiC single crystal body 10.

[0134] The distance between the surface of SiC single crystal body 10 and the top surface of upper vessel 21 is preferably set to 100 mm or less, more preferably 10 mm or less, and even more preferably 2.7 mm or less, and is preferably set to 0.7 mm or more, more preferably 1.2 mm or more, and even more preferably 1.7 mm or more.

[0135] It is desirable that the etching space X and the raw material supply space Y are evacuated (vacuumed) via the Si vapor pressure space Z. That is, it is desirable that a main body vessel 20 having the etching space X and / or the raw material supply space Y is placed in a high-melting-point vessel 40 having the Si vapor pressure space Z, and that a SiC single crystal mass 10 is further placed in this main body vessel 20.

[0136] Next, an outline of the apparatus configuration for realizing the SiC-Si equilibrium vapor pressure environment is shown in the upper part of Fig. 7. The SiC-Si equilibrium vapor pressure environment can be created by placing and heating a SiC single crystal mass 10 in a semi-closed space in which the atomic ratio Si / C exceeds 1, as shown in the upper part of Fig. 7.

[0137] 7, for example, if SiC single crystal mass 10 satisfying a stoichiometric ratio of 1:1, SiC substrate holder 24 satisfying a stoichiometric ratio of 1:1, and Si vapor source 25 (Si pellets, etc.) are placed in main container 20 made of polycrystalline SiC satisfying a stoichiometric ratio of 1:1, the atomic ratio Si / C within main container 20 will exceed 1. By heating this main container 20, the inside of main container 20 will approach a SiC-Si equilibrium vapor pressure environment.

[0138] An outline of the apparatus configuration for realizing the SiC-C equilibrium vapor pressure environment is shown in the lower part of Fig. 7. As shown in the lower part of Fig. 7, the SiC-C equilibrium vapor pressure environment can be created by placing and heating a SiC single crystal mass 10 in a semi-closed space with an atomic ratio Si / C of 1 or less.

[0139] 7, for example, when SiC single crystal mass 10 satisfying a 1:1 stoichiometric ratio and SiC substrate holder 24 satisfying a 1:1 stoichiometric ratio are placed in main container 20 made of polycrystalline SiC satisfying a 1:1 stoichiometric ratio, the atomic ratio Si / C within main container 20 is 1 or less. By heating main container 20, the inside of main container 20 approaches a SiC-C equilibrium vapor pressure environment.

[0140] Furthermore, in order to reduce the atomic ratio Si / C in main vessel 20, a C vapor supply source may be separately arranged, or main vessel 20 or substrate holder 24 including a C vapor supply source may be employed. Examples of this C vapor supply source include solid C (C substrate or C pellets such as C powder) and C compounds.

[0141] If the heat treatment step S1 is performed in an SiC-C equilibrium vapor pressure environment, it is possible to obtain a SiC seed crystal 11 from which the strained layer 101 of the SiC single crystal mass 10 has been removed. Furthermore, if the heat treatment step S1 for growing the crystal is performed under a SiC-C equilibrium vapor pressure environment, a high-quality SiC seed crystal 11 having a growth layer 105 in which BPDs are removed or reduced can be obtained.

[0142] This can prevent defects caused by strain (strained layer 101) in SiC single crystal body 10 and the inheritance of BPD of SiC single crystal body 10 in the subsequent ingot growth step S2.

[0143] On the other hand, if the heat treatment step S1 in which etching or crystal growth is performed in a SiC-Si equilibrium vapor pressure environment is performed, the surface of the SiC single crystal mass 10 can be flattened. That is, a SiC seed crystal 11 in which MSBs have been removed or reduced can be obtained. As a result, defects caused by MSBs and the like can be prevented from being inherited by the SiC ingot in the subsequent ingot growth step S2.

[0144] Next, the strained layer removing step S11, the planarizing step S12, and the basal plane dislocation reducing step S13, which are performed using the manufacturing apparatus according to this embodiment, will be described in detail with reference to FIGS.

[0145] <3-1> Strained layer removal process S11 8, the strained layer removal step S11 is a step of removing the strained layer 101 introduced into the SiC single crystal mass 10. The strained layer removal step S11 will be explained below, but explanations that overlap with the general explanation of the heat treatment step S1 given above will be omitted.

[0146] As shown in FIG. 9, the strained layer removal step S11 is a step of arranging a SiC single crystal body 10 and a SiC material (an upper container 21 made of polycrystalline SiC) facing each other in a semi-closed space in which the atomic ratio Si / C is 1 or less, and heating the SiC single crystal body 10 to be on the high temperature side and the SiC material to be on the low temperature side (etching bunching step S111).

[0147] Alternatively, the strained layer removal step S11 is a step of arranging the SiC single crystal body 10 and the SiC material (upper container 21 made of polycrystalline SiC) facing each other in a semi-closed space in which the atomic ratio Si / C exceeds 1, and heating them so that the SiC single crystal body 10 is on the high temperature side and the SiC material is on the low temperature side (etching planarization step S121).

[0148] In other words, this is a process in which the SiC single crystal body 10 and the SiC material are arranged opposite each other and heated in a SiC-Si equilibrium vapor pressure environment or a SiC-C equilibrium vapor pressure environment so that the SiC single crystal body 10 is on the high temperature side and the SiC material is on the low temperature side.

[0149] In this way, by placing the SiC single crystal body 10, which is located on the high temperature side of the temperature gradient, opposite a part of the main body container 20, which is located on the low temperature side of the temperature gradient, and performing heat treatment, atoms are transported from the SiC single crystal body 10 to the main body container 20, thereby achieving etching of the SiC single crystal body 10.

[0150] That is, the surface of SiC single crystal body 10 and the bottom surface of main body container 20, which has a lower temperature than the surface, are arranged opposite to each other, thereby forming an etching space X between them. In this etching space X, atomic transport occurs using the temperature gradient created by heating furnace 30 as a driving force, and as a result, SiC single crystal body 10 can be etched.

[0151] On the other hand, on the opposite side (back side) of the SiC single crystal mass 10 from the surface to be etched, the back side of the SiC single crystal mass 10 and the top surface of the main body vessel 20, which has a higher temperature than the back side, may be arranged facing each other, thereby forming a raw material supply space Y between them. In this raw material supply space Y, raw material transport occurs using the temperature gradient created by the heating furnace 30 as a driving force, and as a result, a growth layer 105 can be formed on the back side of the SiC single crystal mass 10. Note that in this strained layer removal step S11, a configuration may be adopted in which the raw material supply space Y is not formed, for example, by bringing the back side of the SiC single crystal mass 10 into contact with the top surface of the main body vessel 20.

[0152] Furthermore, main body container 20 is placed in Si vapor pressure space Z, in which an atmosphere containing Si elements is formed. In this way, main body container 20 is placed in Si vapor pressure space Z, and the inside of main body container 20 is evacuated (evacuated) through the space of the Si vapor pressure environment, thereby preventing the loss of Si atoms from inside main body container 20. This makes it possible to maintain a preferable atomic ratio Si / C inside the main body container for a long period of time.

[0153] That is, when exhausting directly from the etching space X and the raw material supply space Y without passing through the Si vapor pressure space Z, Si atoms are exhausted from the gap 23. In this case, the atomic ratio Si / C in the etching space X and the raw material supply space Y decreases significantly. On the other hand, when the inside of the main body vessel is evacuated through the Si vapor pressure space Z in the Si vapor pressure environment, the exhaust of Si atoms from the etching space X and the raw material supply space Y can be suppressed, and the atomic ratio Si / C inside the main body vessel 20 can be maintained.

[0154] The etching temperature in the strained layer removing step S11 is preferably set in the range of 1400 to 2300°C, and more preferably in the range of 1600 to 2000°C. The etching rate in the strained layer removing step S11 can be controlled by the temperature range described above, and can be selected within the range of 0.001 to 2 μm / min. The etching amount in the strained layer removal step S11 can be any amount that can remove the strained layer 101 of the SiC single crystal mass 10. This etching amount can be, for example, between 0.1 μm and 20 μm, but can be adjusted as needed. The etching time in the strained layer removal step S11 can be set to any time so as to obtain a desired etching depth. For example, when the etching rate is 1 μm / min and the etching depth is desired to be 1 μm, the etching time is set to 1 minute. The temperature gradient in the strained layer removing step S11 is set in the etching space X in the range of 0.1 to 5° C. / mm.

[0155] The case where etching is performed by placing SiC single crystal mass 10 and a SiC material opposite each other in a semi-closed space in which the atomic ratio Si / C is 1 or less (etching bunching step S111) has been described above with reference to FIG. It should be noted that even when etching is performed by placing the SiC single crystal body 10 and the SiC material opposite each other in a semi-closed space in which the atomic ratio Si / C exceeds 1 (etching planarization step S121), it is possible to remove the strained layer 101 in a similar manner.

[0156] By carrying out the strained layer removing step S11 described above, it is possible to manufacture SiC seed crystal 11 in which strained layer 101 has been removed or reduced, as shown in FIG.

[0157] <3-2> Flattening process S12 10 and 12, the planarization step S12 is a step of decomposing and removing MSB formed on the surface of SiC seed crystal 11. As described above, preferred examples of the planarization step S12 include the etching planarization step S121 and the growth planarization step S122. The planarization step S12 will be explained below, but explanations that overlap with the general explanation of the heat treatment step S1 will be omitted.

[0158] <3-2-1> Etching planarization step S121 As shown in FIG. 10, the etching planarization step S121 is a step of reducing or removing the MSBs by etching the surface of the SiC single crystal mass 10 on which the MSBs have been formed.

[0159] As shown in FIG. 11, the etching planarization step S121 is a step in which the SiC single crystal body 10 and the SiC material (lower container 22 made of polycrystalline SiC) are arranged facing each other in a semi-closed space in which the atomic ratio Si / C exceeds 1, and heated so that the SiC single crystal body 10 is on the high temperature side and the SiC material is on the low temperature side. In other words, this is a process in which SiC single crystal mass 10 and a SiC material are arranged opposite each other and heated in a SiC-Si equilibrium vapor pressure environment so that SiC single crystal mass 10 is on the high temperature side and the SiC material is on the low temperature side.

[0160] The apparatus configuration for implementing this etching planarization step S121 is configured such that a Si vapor supply source 25 is further disposed within the main vessel 20 of the strained layer removal step S11. By disposing this Si vapor supply source 25, the SiC single crystal mass 10 can be heated in a SiC-Si equilibrium vapor pressure environment. The explanation of the parts that overlap with the general explanation of the strained layer removing step S11 will be omitted as appropriate.

[0161] The etching temperature in the etching planarization step S121 is preferably set in the range of 1400 to 2300°C, and more preferably in the range of 1600 to 2000°C. The etching rate in the etching planarization step S121 can be controlled by the temperature range described above, and can be selected within the range of 0.001 to 2 μm / min. The etching amount used in the etching planarization step S121 can be any amount that can decompose the MSB of the SiC single crystal mass 10. Examples of this etching amount include 0.1 μm or more and 20 μm or less. The etching time in the etching planarization step S121 can be set to any time so as to obtain a desired etching amount. For example, if the etching rate is 1 μm / min and the etching amount is desired to be 1 μm, the etching time is set to 1 minute. The temperature gradient in the etching planarization step S121 is set in the etching space X in the range of 0.1 to 5° C. / mm.

[0162] According to the etching planarization step S121, as shown in FIG. 10, by etching the surface of the SiC single crystal mass 10, it is possible to produce a SiC seed crystal 11 in which MSBs have been removed or reduced.

[0163] <3-2-2> Growth flattening step S122 As shown in FIG. 12, the growth and flattening step S122 is a step of growing a crystal on the surface of the SiC single crystal mass 10 on which the MSBs have been formed, thereby forming a growth layer 105 in which the MSBs have been reduced or removed.

[0164] As shown in FIG. 13, the growth flattening step S122 is a step of arranging the SiC single crystal body 10 and the SiC material (upper container 21 made of polycrystalline SiC) facing each other in a quasi-closed space in which the atomic ratio Si / C exceeds 1, and heating the SiC single crystal body 10 so that it is on the low temperature side and the SiC material is on the high temperature side. In other words, this is a process in which SiC single crystal mass 10 and a SiC material are arranged opposite each other and heated in a SiC-Si equilibrium vapor pressure environment so that SiC single crystal mass 10 is on the low temperature side and the SiC material is on the high temperature side.

[0165] In this way, by placing SiC single crystal body 10, which is located on the low temperature side of the temperature gradient, opposite a part of main body container 20, which is located on the high temperature side of the temperature gradient, and performing heat treatment, raw material is transported from main body container 20 to SiC single crystal body 10, and growth layer 105 is formed.

[0166] That is, the surface of SiC single crystal body 10 and the top surface of main body vessel 20, which has a higher temperature than this surface, are arranged opposite to each other, thereby forming a raw material supply space Y between them. In this raw material supply space Y, the raw material is transported using the temperature gradient created by heating furnace 30 and the chemical potential difference between SiC single crystal body 10 and the SiC material as driving forces, and as a result, a growth layer 105 can be formed on the surface of SiC single crystal body 10.

[0167] Similarly to the etching planarization step S121, the apparatus configuration for realizing this growth planarization step S122 is configured such that a Si vapor supply source 25 is further disposed within main body vessel 20. Note that explanations that overlap with the general explanation of the etching planarization step S121 described above will be omitted.

[0168] The heating temperature in the growth and flattening step S122 is preferably set in the range of 1400 to 2200°C, and more preferably in the range of 1600 to 2000°C. The growth rate in the growth and flattening step S122 can be controlled by the temperature range described above, and can be selected within the range of 0.001 to 1 μm / min. The amount of growth in the growth and flattening step S122 is preferably 5 μm or more, and more preferably 8 μm or more. The growth time in the growth and flattening step S122 can be set to any time to achieve a desired growth amount. For example, if the growth rate is 10 nm / min and the growth amount is desired to be 10 μm, the growth time is 100 minutes. The degree of vacuum (main heating chamber 31) in the growth and flattening step S122 is 10 -5 ~10 Pa, more preferably 10 -3 ~1Pa. In the growth and flattening step S122, an inert gas can be introduced during growth. The inert gas can be selected from Ar and the like. -5 By introducing a pressure in the range of 10,000 Pa or less, the degree of vacuum in the heating furnace 30 (main heating chamber 31) can be adjusted.

[0169] According to the growth flattening step S122, as shown in FIG. 12, a growth layer 105 having no MSBs is grown on the surface of SiC single crystal mass 10, thereby producing a SiC seed crystal 11 in which MSBs have been removed or reduced.

[0170] <3-3> Basal plane dislocation reduction step S13 14, the basal plane dislocation reduction step S13 is a step of forming a growth layer 105 in which BPDs have been removed or reduced by growing the crystal under conditions that increase the terrace width W of the SiC single crystal mass 10. Explanations that overlap with the general explanation of the heat treatment step S1 described above will be omitted.

[0171] As shown in FIG. 15, the basal plane dislocation reduction step S13 is a step of arranging a SiC single crystal body 10 and a SiC material (an upper container 21 made of polycrystalline SiC) facing each other in a quasi-closed space in which the atomic ratio Si / C is 1 or less, and heating the SiC single crystal body 10 so that it is on the low temperature side and the SiC material is on the high temperature side. In other words, this is a process in which SiC single crystal mass 10 and a SiC material are arranged opposite to each other and heated in a SiC-C equilibrium vapor pressure environment so that SiC single crystal mass 10 is on the low temperature side and the SiC material is on the high temperature side.

[0172] The apparatus configuration for realizing this basal plane dislocation reduction step S13 is similar to that of the growth flattening step S122, in that SiC single crystal body 10 placed on the low temperature side of the temperature gradient and a part (SiC material) of main body container 20 placed on the high temperature side of the temperature gradient are placed opposite each other and heat treated, thereby transporting raw material from main body container 20 to SiC single crystal body 10 to form growth layer 105.

[0173] On the other hand, unlike the growth and planarization step S122, the basal plane dislocation reduction step S13 does not include the Si vapor supply source 25. Note that a description of parts that overlap with the general description of the growth and planarization step S122 described above will be omitted.

[0174] The heating temperature in the basal plane dislocation reducing step S13 is preferably set in the range of 1400 to 2200°C, and more preferably in the range of 1600 to 2000°C. The growth rate in the basal plane dislocation reduction step S13 can be controlled by the temperature range and growth environment, and can be selected within the range of 0.001 to 1 μm / min. The growth amount in the basal plane dislocation reducing step S13 is preferably 5 μm or more, and more preferably 8 μm or more. The growth time in the basal plane dislocation reduction step S13 can be set to any time to achieve the desired growth amount. For example, if the growth rate is 10 nm / min and the growth amount is desired to be 10 μm, the growth time is 100 minutes. The degree of vacuum (main heating chamber 31) in the basal plane dislocation reduction step S13 is 10 -5 ~10 Pa, more preferably 10 -3 ~1Pa. In the basal plane dislocation reduction step S13, an inert gas can be introduced during growth. The inert gas can be selected from Ar and the like. -5 By introducing a pressure in the range of 10,000 Pa or less, the degree of vacuum in the heating furnace 30 (main heating chamber 31) can be adjusted.

[0175] According to the basal plane dislocation reduction step S13, growth is performed under conditions that increase the width (terrace width W) of the terraces 104, thereby improving the conversion rate (BPD conversion rate) at which BPDs are converted into other defects or dislocations, and reducing or eliminating the BPD density in the growth layer 105. The conditions that increase the terrace width W are conditions that increase the terrace width W2 after growth compared to the terrace width W1 before growth, and this can be achieved, for example, by growing the layer in a SiC-C equilibrium vapor pressure environment or a C-rich environment.

[0176] The value of the terrace width W (including terrace width W1 and terrace width W2) may be determined by, for example, drawing a line perpendicular to the steps 103 in the captured SEM image and counting the number of steps 103 present on this line, thereby adopting the average value of the terrace width (terrace width W = line length / number of steps on the line).

[0177] Preferably, the basal plane dislocation reduction step S13 is performed after the planarization step S12. That is, when the width of the terrace 104 on the surface where MSBs are not formed is compared with the width of the terrace 104 on the surface where MSBs are formed, the width of the terrace 104 on the surface where MSBs are not formed is narrower. Therefore, by growing the growth layer 105 under conditions where MSBs are formed after decomposition of the MSBs, the BPD conversion rate can be improved.

[0178] <3-4> Preferred form of heat treatment step S1 FIG. 16 shows a preferred embodiment of the steps of treating SiC single crystal body 10 in heat treatment step S1 to produce SiC seed crystal 11, and then performing ingot growth step S2 to produce SiC ingot 12.

[0179] FIG. 16(a) shows a form in which a strained layer removing step S11 is performed as the heat treatment step S1, and the SiC seed crystal 11 thus obtained is subjected to an ingot growing step S2. 16(a), an SiC seed crystal 11 is obtained from which the strained layer 101 has been removed. That is, defects caused by the strained layer 101 can be prevented from being inherited by the SiC ingot 12.

[0180] As the strained layer removing step S11 in the embodiment shown in FIG. 16, either an etching bunching step S111 or an etching planarizing step S121 can be adopted. When the etching planarization step S121 is employed, the MSB can be removed or reduced at the same time as the strained layer 101 is removed.

[0181] 16(b) shows a configuration in which the planarization step S12 is performed after the strained layer removal step S11. According to this configuration, it is possible to produce a SiC seed crystal 11 that does not include a strained layer 101 or an MSB on the surface. This allows a high-quality SiC ingot 12 to be produced.

[0182] 16(c) shows a configuration in which the basal plane dislocation reduction step S13 is performed after the strained layer removal step S11 and the planarization step S12. By performing the strained layer removal step S11 and the planarization step S12 in advance as in this configuration, the conversion rate at which BPDs are converted to other defects / dislocations (BPD conversion rate) can be improved in the subsequent basal plane dislocation reduction step S13, and a growth layer 105 with a reduced BPD density can be formed.

[0183] 16(d) shows an embodiment in which the planarization step S12 is further performed after the basal plane dislocation reduction step S13 in the embodiment shown in FIG. 16(c). By performing the planarization step S12 after the basal plane dislocation reduction step S13 in this manner, it is possible to produce a SiC seed crystal 11 that is free of not only strained layer 101 and BPDs but also MSBs on its surface.

[0184] As the planarization step S12 in the embodiment shown in FIG. 16, either the etching planarization step S121 or the growth planarization step S122 can be adopted.

[0185] When the heat treatment process S1 includes two or more processes selected from the strained layer removal process S11 (etching bunching process S111 or etching planarization process S121), the planarization process S12 (etching planarization process S121 or growth planarization process S122), and the basal plane dislocation reduction process S13, the two or more processes can be heat treated using the same apparatus configuration.

[0186] The container in which the plurality of heat treatment steps S1 are performed may be a container that generates an atmosphere of Si elements and C elements in its internal space, specifically, main container 20. In this way, by using the main vessel 20, etc., even if the heat treatment step S1 includes multiple steps, all of the steps can be completed in the same vessel, which is expected to simplify the work. Furthermore, since etching and crystal growth can be performed in the same equipment system, there is no need to introduce multiple devices, which is extremely advantageous industrially.

[0187] <4> SiC seed crystal 11 The present invention also relates to a SiC seed crystal 11 manufactured through the heat treatment step S1. The SiC seed crystal 11 of the present invention does not contain factors that adversely affect ingot growth, such as a strained layer 101, BPD, or MSB, on its surface due to the heat treatment step S1. Therefore, the SiC seed crystal 11 of the present invention can grow a higher quality SiC ingot.

[0188] SiC seed crystal 11 is preferably characterized by having a BPD-free growth layer 105 on its surface. The thickness of BPD-free growth layer 105 is preferably 0.001 μm or more, more preferably 0.01 μm or more, and even more preferably 0.1 μm or more. When the thickness of the BPD-free layer is within the above range, propagation of BPDs present in SiC seed crystal 11 to the ingot can be suppressed during the growth step of growing SiC on SiC seed crystal 11.

[0189] The diameter of the SiC seed crystal 11 of the present invention is not particularly limited, and is preferably 6 inches or more, more preferably 8 inches or more, and even more preferably 12 inches or more. By growing the SiC seed crystal 11 of such a size to produce the SiC ingot 12, it is possible to obtain a large-diameter yet high-quality SiC wafer 13.

[0190] <5> Ingot growth process S2 The ingot growth step S2 is a step of growing single crystal SiC on a SiC seed crystal 11 to produce a SiC ingot 12. Any known growth method may be used for the ingot growth step S2, and examples of the method include sublimation and CVD.

[0191] <6> SiC ingot 12 The present invention also relates to a SiC ingot 12 produced by the ingot growing step S2 described above. The SiC ingot 12 of the present invention contains almost no BPD and is of high quality.

[0192] <7> Slicing process S3 The slicing step S3 is a step of slicing SiC wafers 13 from the SiC ingot 12. Examples of slicing means used in the slicing step S3 include multi-wire saw cutting, which cuts the SiC ingot 12 at predetermined intervals by reciprocating multiple wires, electric discharge machining, which cuts the SiC ingot 12 by intermittently generating plasma discharges, and laser cutting, which irradiates and focuses a laser into the SiC ingot 12 to form a layer that serves as the starting point for cutting.

[0193] <8> SiC wafer 13 The present invention also relates to a SiC wafer 13 obtained through the above-described steps. The SiC wafer 13 of the present invention is manufactured from a SiC ingot 12 derived from a SiC seed crystal 11 in which strain and dislocations are suppressed. Therefore, the SiC wafer 13 of the present invention can significantly reduce defects that propagate to an epitaxial layer formed in the subsequent epitaxial growth step S5.

[0194] In the SiC wafer 13, the surface on which a semiconductor element is formed (specifically, the surface on which an epitaxial layer is deposited) is referred to as the main surface. The surface opposite to the main surface is referred to as the back surface. The main surface and the back surface together are referred to as the front surface.

[0195] The main surface of the SiC wafer 13 can be, for example, a surface having an off-angle of several degrees (for example, 0.4 to 8°) from the (0001) plane or the (000-1) plane (in this specification, in the notation of Miller indices, "-" means a bar attached to the index immediately following it).

[0196] <9> Surface processing process S4 The surface processing step S4 is a step of processing the surface of the SiC wafer 13 so that it is in a state (epi-ready) that can be subjected to the subsequent epitaxial growth step S5. For the surface processing step S4, any known SiC wafer processing method can be applied without any restrictions.Typically, a rough grinding step such as a loose abrasive method (such as lapping polishing) in which processing is performed while fine abrasive grains are applied to a surface plate is performed, followed by a finish grinding step using abrasive grains with a smaller grain size than the abrasive grains used in the rough grinding step, and finally a chemical mechanical polishing (CMP) step in which polishing is performed using a combination of the mechanical action of a polishing pad and the chemical action of a slurry.

[0197] <10> Epitaxial growth step S5 The epitaxial growth step S5 is a step of forming an epitaxial film on the main surface of the SiC wafer 13 by epitaxial growth to form an epitaxial film-coated SiC wafer 14 to be used for applications such as power devices.

[0198] As the epitaxial growth method in the epitaxial growth step S5, any known method can be used without limitation, such as chemical vapor deposition (CVD), physical vapor transport (PVT), metastable solvent epitaxy (MSE), etc.

[0199] <11> Epitaxial SiC wafer 14 The present invention also relates to an epitaxially-coated SiC wafer 14 manufactured by the above-described process. As described above, the epitaxial film-provided SiC wafer 14 of the present invention is derived from the SiC wafer 13 in which distortion, BPD, and MSB are suppressed, and therefore the propagation of defects to the epitaxial layer is suppressed. Therefore, the epitaxial film-provided SiC wafer 14 of the present invention can provide a high-performance SiC semiconductor device. [Example]

[0200] The present invention will be described more specifically below with reference to Examples 1, 2, 3 and 4. Example 1 is an example that specifically describes the etching bunching step S111. Example 2 is an example that specifically describes the etching planarization step S121. Example 3 is an example that specifically describes the growth planarization step S122. Example 4 is an example that specifically describes the basal plane dislocation reduction step S13.

[0201] <Example 1: Etching bunching process> The SiC single crystal body 10 was housed in the main container 20 and the high-melting-point container 40 (see FIG. 9), and was heat-treated under the following heat treatment conditions to remove the strained layer 101 of the SiC single crystal body 10.

[0202] [SiC single crystal 10] Polymorphism: 4H-SiC Board size: 10mm wide x 10mm long x 0.45mm thick Off direction and off angle: 4° off in the <11-20> direction Etched surface: (0001) surface Depth of strain layer 101: 5 μm The depth of the strained layer 101 was confirmed by SEM-EBSD. The strained layer 101 can also be confirmed by TEM, μXRD, or Raman spectroscopy.

[0203] [Main container 20] Material: Polycrystalline SiC Container size: diameter 60mm x height 4mm Material of substrate holder 24: Single crystal SiC Distance between the bottom of the SiC single crystal 10 and the main container 20: 2 mm Atomic ratio Si / C in the container: 1 or less

[0204] [High melting point container 40] Material: TaC Container size: diameter 160mm x height 60mm Si vapor source 44 (Si compound): TaSi2

[0205] [Heat treatment conditions] The SiC single crystal mass 10 arranged under the above conditions was subjected to a heat treatment under the following conditions. Heating temperature: 1800℃ Heating time: 20min Etching amount: 5 μm Temperature gradient: 1°C / mm Etching speed: 0.25 μm / min Main heating chamber vacuum degree: 10 -5 Pa

[0206] [Measurement of strained layer using SEM-EBSD method] The lattice strain of the SiC single crystal body 10 can be determined by comparing it with a reference crystal lattice. For example, the SEM-EBSD method can be used to measure this lattice strain. The SEM-EBSD method is a technique (Electron Backscattering Diffraction (EBSD)) that can measure strain in a microscopic area based on a Kikuchi diffraction pattern obtained by backscattering electron beams in a scanning electron microscope (SEM). This technique can determine the amount of lattice strain by comparing the diffraction pattern of the measured crystal lattice with the diffraction pattern of the reference crystal lattice.

[0207] For the reference crystal lattice, for example, a reference point is set in a region where lattice distortion is not considered to occur. That is, it is desirable to place the reference point in the region of the bulk layer 102 in FIG. 8. It is generally accepted that the depth of the strained layer 101 is about 10 μm. Therefore, it is sufficient to set the reference point at a depth of about 20 to 35 μm, which is considered to be sufficiently deeper than the strained layer 101.

[0208] Next, the diffraction pattern of the crystal lattice at this reference point is compared with the diffraction pattern of the crystal lattice in each measurement area measured at a pitch on the order of nanometers, allowing the amount of lattice strain in each measurement area relative to the reference point to be calculated.

[0209] In addition, although the case where a reference point where no lattice distortion is thought to occur is set as the reference crystal lattice has been shown, it is of course also possible to use an ideal crystal lattice of single crystal SiC as the reference, or to use a crystal lattice that occupies the majority (e.g., more than half) of the surface of the measurement area as the reference.

[0210] By measuring whether or not lattice strain exists using this SEM-EBSD method, it is possible to determine the presence or absence of strained layer 101. That is, when processing damage such as scratches 1011, latent scratches 1012, or strain 1013 is introduced, lattice strain occurs in SiC single crystal mass 10, and therefore stress can be observed using SEM-EBSD.

[0211] The strained layer 101 present in the SiC single crystal mass 10 before heat treatment step S1 and the strained layer 101 present in the SiC single crystal mass 10 after heat treatment step S1 were observed by SEM-EBSD. The results are shown in Figures 17(a) and 17(b).

[0212] In this measurement, a cross section obtained by cleaving SiC single crystal body 10 before and after heat treatment step S1 was measured using a scanning electron microscope under the following conditions. SEM equipment: Zeiss Merline EBSD analysis: TSL Solutions OIM crystal orientation analyzer Accelerating voltage: 15 kV Probe current: 15nA Step size: 200nm Reference point R depth: 20 μm

[0213] FIG. 17(a) is a cross-sectional SEM-EBSD image of SiC single crystal mass 10 before heat treatment step S1. As shown in Fig. 17(a), before heat treatment step S1, lattice strain was observed to a depth of 5 µm within SiC single crystal mass 10. This is lattice strain introduced during machining, and it is clear that there is strained layer 101. Note that compressive stress is observed in Fig. 17(a).

[0214] FIG. 17(b) is a cross-sectional SEM-EBSD image of SiC single crystal mass 10 after heat treatment step S1. 17(b), after heat treatment step S1, no lattice strain was observed within SiC single crystal mass 10. In other words, it can be seen that heat treatment step S1 removed strained layer 101. After heat treatment step S1, MSBs were formed on the surface of SiC single crystal mass 10.

[0215] Thus, according to the etching bunching step S111, the strained layer 101 can be removed or reduced by etching the SiC single crystal mass 10 in a semi-closed space in which the atomic ratio Si / C is 1 or less. This makes it possible to manufacture a SiC seed crystal 11 in which the strained layer 101 has been removed or reduced.

[0216] <Example 2: Etching planarization process> The SiC single crystal 10 was housed in the main container 20 and the high-melting-point container 40 (see FIG. 11), and the MSBs on the surface of the SiC single crystal 10 were removed by heat treatment under the following heat treatment conditions.

[0217] [SiC single crystal 10] Polymorphism: 4H-SiC Board size: 10mm wide x 10mm long x 0.3mm thick Off direction and off angle: 4° off in the <11-20> direction Etched surface: (0001) surface MSB: Yes

[0218] The step height, terrace width, and presence or absence of MSB can be confirmed by an atomic force microscope (AFM) or a method for evaluating the contrast of a scanning electron microscope (SEM) image described in JP 2015-179082 A.

[0219] [Main container 20] Material: Polycrystalline SiC Container size: diameter 60mm x height 4mm Material of substrate holder 24: Single crystal SiC Distance between SiC single crystal 10 and the bottom of main container 20: 2 mm Si vapor source 25: single crystal Si piece The atomic ratio in the container is Si / C: more than 1

[0220] In this way, by accommodating Si pieces together with SiC single crystal body 10 in main body container 20, the atomic ratio Si / C within the container exceeds 1.

[0221] [High melting point container 40] Material: TaC Container size: diameter 160mm x height 60mm Si vapor source 44 (Si compound): TaSi2

[0222] [Heat treatment conditions] The SiC single crystal mass 10 arranged under the above conditions was subjected to a heat treatment under the following conditions. Heating temperature: 1900℃ Heating time: 60min Temperature gradient: 1°C / mm Etching speed: 300nm / min Main heating chamber vacuum degree: 10 -5 Pa

[0223] The steps 103 of the SiC single crystal mass 10 before the heat treatment step S1 and the steps 103 of the SiC single crystal mass 10 after the heat treatment step S1 were observed by SEM. The results are shown in Figures 18(a) and 18(b). The height of the steps 103 was measured by an atomic force microscope (AFM). The width of the terraces 104 was also measured by SEM.

[0224] 18(a) is an SEM image of the surface of SiC single crystal mass 10 before heat treatment step S1. MSBs with a height of 3 nm or more are formed on the surface of SiC single crystal mass 10 before heat treatment step S1.

[0225] 18(b) is an SEM image of the surface of SiC single crystal mass 10 after heat treatment step S1. It can be seen that no MSBs are formed on the surface of SiC single crystal mass 10 after heat treatment step S1, and that steps of 1.0 nm (full unit cell) are regularly arranged.

[0226] Thus, according to the etching planarization step S121, it is possible to remove or reduce MSBs by etching SiC single crystal mass 10 in a semi-closed space in which the atomic ratio Si / C exceeds 1. This makes it possible to produce SiC seed crystal 11 in which MSBs have been removed or reduced.

[0227] Furthermore, when SiC single crystal mass 10 after heat treatment step S1 was observed by SEM-EBSD, no strained layer 101 was observed, as in Example 1. That is, strained layer 101 can also be removed in etching planarization step S121.

[0228] Example 3: Growth and Planarization Process The SiC single crystal body 10 was housed in the main container 20 and the high-melting-point container 40 (see FIG. 13), and the MSBs on the surface of the SiC single crystal body 10 were removed by heat treatment under the following heat treatment conditions.

[0229] [SiC single crystal 10] Polymorphism: 4H-SiC Board size: 10mm wide x 10mm long x 0.3mm thick Off direction and off angle: 4° off in the <11-20> direction Etched surface: (0001) surface MSB: Yes

[0230] [Main container 20] Material: Polycrystalline SiC Container size: diameter 60mm x height 4mm Distance between SiC single crystal 10 and the bottom of main container 20: 2 mm Si vapor source 25: single crystal Si piece The atomic ratio in the container is Si / C: more than 1

[0231] By accommodating Si pieces together with SiC single crystal body 10 in main body container 20 in this manner, the atomic ratio Si / C within the container exceeds 1.0.

[0232] [High melting point container 40] Material: TaC Container size: diameter 160mm x height 60mm Si vapor source 44 (Si compound): TaSi2

[0233] [Heat treatment conditions] The SiC single crystal mass 10 arranged under the above conditions was subjected to a heat treatment under the following conditions. Heating temperature: 1800℃ Heating time: 60min Temperature gradient: 1°C / mm Growth rate: 68nm / min Main heating chamber 31 degree of vacuum: 10 -5 Pa

[0234] Steps 103 on the surface of SiC single crystal mass 10 after heat treatment step S1 were observed by SEM, and the results are shown in Figure 19. The height of steps 103 was measured by atomic force microscope (AFM), and the width of terraces 104 was measured by SEM.

[0235] Fig. 19 is an SEM image of the surface of SiC single crystal mass 10 after heat treatment step S1. Similar to Fig. 18(a), MSBs with a height of 3 nm or more were formed on the surface of SiC single crystal mass 10 before heat treatment step S1. As shown in Fig. 19, no MSBs were formed on the surface of SiC single crystal mass 10 after heat treatment step S1 in Example 3, and steps of 1.0 nm (full unit cell) were found to be regularly arranged.

[0236] Thus, according to the growth flattening step S122, it is possible to form a growth layer 105 free of MSBs by growing SiC single crystal mass 10 in a quasi-closed space in which the atomic ratio Si / C exceeds 1. This makes it possible to produce a SiC seed crystal 11 in which MSBs are removed or reduced.

[0237] Example 4: Basal Plane Dislocation Reduction Process BPDs can be eliminated or reduced by housing SiC single crystal body 10 in main body container 20 and high-melting-point container 40 (see FIG. 15) and subjecting it to heat treatment under the following heat treatment conditions.

[0238] [SiC single crystal 10] Polymorphism: 4H-SiC Board size: 10mm wide x 10mm long x 0.3mm thick Off direction and off angle: 4° off in the <11-20> direction Growth plane: (0001) plane MSB: None Presence or absence of strain layer 101: None

[0239] [Main container 20] Material: Polycrystalline SiC Container size: diameter 60mm x height 4mm Distance between SiC single crystal 10 and SiC material: 2 mm Atomic ratio Si / C in the container: 1 or less

[0240] [High melting point container 40] Material: TaC Container size: diameter 160mm x height 60mm Si vapor source 44 (Si compound): TaSi2

[0241] [Heat treatment conditions] The SiC single crystal mass 10 arranged under the above conditions was subjected to a heat treatment under the following conditions. Heating temperature: 1700℃ Heating time: 300min Temperature gradient: 1°C / mm Growth rate: 5nm / min Main heating chamber 31 degree of vacuum: 10 -5 Pa

[0242] [BPD conversion rate in the growing layer] FIG. 20 is an explanatory diagram of a method for determining the conversion rate of BPDs into other defects / dislocations (TEDs, etc.) in the growth layer 105. In FIG. 20(a) shows the state of growth layer 105 grown by heat treatment step S1. In this heating step, BPDs present in SiC single crystal mass 10 are converted to TEDs with a certain probability. Therefore, unless 100% conversion is achieved, TEDs and BPDs will be present mixedly on the surface of growth layer 105. Figure 20(b) shows the state of defects in the growth layer 105 confirmed using the KOH dissolution etching method. This KOH dissolution etching method involves immersing the SiC substrate in molten salt (such as KOH) heated to approximately 500°C, forming etch pits at dislocations and defects, and identifying the type of dislocation based on the size and shape of the etch pits. This method allows us to obtain the number of BPDs present on the surface of the growth layer 105. 20(c) shows the removal of growth layer 105 after KOH dissolution etching. In this method, after planarization to the depth of the etch pits by mechanical polishing, CMP, or the like, growth layer 105 is removed by thermal etching to expose the surface of SiC single crystal body 10. 20(d) shows the state in which defects in the SiC single crystal 10 are confirmed using a KOH dissolution etching method for the SiC single crystal 10 from which the growth layer 105 has been removed. By this method, the number of BPDs present on the surface of the SiC single crystal 10 is obtained.

[0243] By comparing the number of BPDs present on the surface of growth layer 105 (see FIG. 20(b)) with the number of BPDs present on the surface of SiC single crystal mass 10 (see FIG. 20(d)) according to the sequence shown in FIG. 20, the BPD conversion rate of BPDs converted to other defects and dislocations during heat treatment step S1 can be obtained.

[0244] The number of BPDs present on the surface of the growth layer 105 in Example 4 was 0 cm -2 The number of BPDs present on the surface of the SiC single crystal 10 is approximately 1000 cm -2 It was. That is, it can be seen that BPDs can be eliminated or reduced by placing SiC single crystal 10, which does not have MSBs on its surface, in a semi-closed space where the atomic ratio Si / C is 1 or less and growing the crystal.

[0245] Thus, according to basal plane dislocation reduction step S13, it is possible to form growth layer 105 on the surface from which BPDs have been removed or reduced by growing SiC single crystal mass 10 in a quasi-closed space having an atomic ratio Si / C of 1 or less. This makes it possible to manufacture SiC seed crystal 11 having growth layer 105 from which BPDs have been removed or reduced.

[0246] [Thermodynamic calculation] 21(a) is a graph showing the relationship between the heating temperature and the etching rate in the etching process of the present invention, where the horizontal axis of the graph represents the reciprocal of the temperature, and the vertical axis of the graph represents the logarithmic etching rate. 21(b) is a graph showing the relationship between heating temperature and growth rate in the crystal growth process of the present invention. The horizontal axis of this graph represents the reciprocal of temperature, and the vertical axis of this graph represents the logarithmic growth rate.

[0247] 21, the results of heat treatment of SiC single crystal body 10 placed in a space (inside main container 20) where the atomic ratio Si / C exceeds 1 are indicated by circles, and the results of heat treatment of SiC single crystal body 10 placed in a space (inside main container 20) where the atomic ratio Si / C is 1 or less are indicated by crosses.

[0248] No MSBs were formed on the surface of the SiC single crystal 10 at any of the locations marked with a circle, and the steps 103 had a height of one unit cell. On the other hand, MSBs were formed on the surface of the SiC single crystal 10 at any of the locations marked with an x.

[0249] In addition, in the graph of FIG. 21, the results of thermodynamic calculations in a SiC-Si equilibrium vapor pressure environment are shown by a dashed line (Arrhenius plot), and the results of thermodynamic calculations in a SiC-C equilibrium vapor pressure environment are shown by a two-dot chain line (Arrhenius plot). The thermodynamic calculations for the etching process and the crystal growth process will be explained in detail below.

[0250] (Thermodynamic calculation of the etching process) In thermodynamic calculations of the etching step, the amount of vapor (vapor phase species containing Si element and vapor phase species containing C element) generated from SiC single crystal body 10 when main body vessel 20 is heated can be converted into an etching amount. In this case, the etching rate of SiC single crystal body 10 can be calculated using the following equation 1.

[0251]

number

[0252] where T is the temperature of the SiC single crystal 10, m i is the gas phase species (Si x Cy ) and k is the Boltzmann constant. Also, P i is the sum of the vapor pressures generated in the main body container 20 when the SiC single crystal body 10 is heated. i The gas phase species are expected to be SiC, Si2C, SiC2, etc.

[0253] The dashed line in Figure 21(a) shows the results of thermodynamic calculations performed when etching single-crystal SiC in a vapor pressure environment where SiC (solid) and Si (liquid) are in phase equilibrium via the gas phase. Specifically, using Equation 1, the thermodynamic calculations were performed under the following conditions (i) to (iv): (i) a constant-volume SiC-Si equilibrium vapor pressure environment, (ii) the etching driving force is the temperature gradient within the main vessel 20, (iii) the source gases are SiC, SiC, and SiC, and (iv) the desorption coefficient for the source material sublimating from step 103 is 0.001.

[0254] The two-dot chain line in Figure 21(a) represents the results of a thermodynamic calculation of etching single-crystal SiC in a vapor pressure environment where SiC (solid phase) and C (solid phase) are in phase equilibrium via the gas phase. Specifically, using Equation 1, the thermodynamic calculation was performed under the following conditions (i) to (iv): (i) a constant-volume SiC-C equilibrium vapor pressure environment, (ii) the etching driving force is the temperature gradient within the main vessel 20, (iii) the source gases are SiC, Si2C, and SiC2, and (iv) the desorption coefficient for the source material sublimating from step 103 is 0.001. The data for each chemical species used in the thermodynamic calculations were taken from the JANAF thermochemical tables.

[0255] According to the graph in Figure 21(a), it can be seen that the results (marked with circles) of etching SiC single crystal body 10 when it is placed in a space (inside main body container 20) where the atomic ratio Si / C exceeds 1 are consistent with the results of thermodynamic calculations of single crystal SiC etching in a SiC-Si equilibrium vapor pressure environment. Furthermore, the SiC single crystal body 10 was placed in a space (inside the main body container 20) where the atomic ratio Si / C was 1 or less, and the results of etching the SiC single crystal body 10 (marked with an x) showed a trend consistent with the results of thermodynamic calculations of single crystal SiC etching in a SiC-C equilibrium vapor pressure environment.

[0256] It can be seen that under the conditions of the circled areas etched under a SiC-Si equilibrium vapor pressure environment, the formation of MSBs is decomposed and suppressed, and steps 103 with a height of 1 nm (1 unit cell) are aligned on the surface of the SiC single crystal body 10. On the other hand, it can be seen that MSBs are formed under the conditions of the x marks, which are etched under the SiC-C equilibrium vapor pressure environment.

[0257] (Thermodynamic calculation of the crystal growth process) Next, in the thermodynamic calculation of the crystal growth process, the partial pressure difference between the SiC raw material and the vapor generated from the SiC substrate when the inside of the main vessel 20 is heated can be converted into the growth amount. At this time, the growth driving force can be assumed to be a chemical potential difference or a temperature gradient. Note that this chemical potential difference can be assumed to be the partial pressure difference between the gas phase species generated on the surface of the polycrystalline SiC (SiC material) and the single crystal SiC (SiC single crystal mass 10). In this case, the growth rate of SiC can be calculated using the following equation 2.

[0258]

number

[0259] where T is the temperature of the SiC raw material side, m i is the gas phase species (Si x C y ) and k is the Boltzmann constant. Also, P 原料 -P 基板 is the amount of SiC deposited when the source gas becomes supersaturated, and the source gas is assumed to be SiC, Si2C, or SiC2.

[0260] That is, the dashed line in Figure 21(b) is the result of a thermodynamic calculation when single-crystal SiC is grown using polycrystalline SiC as a raw material in a vapor pressure environment where SiC (solid) and Si (liquid phase) are in phase equilibrium via the gas phase. Specifically, thermodynamic calculations were performed using Equation 2 under the following conditions (i) to (iv): (i) a SiC-Si equilibrium vapor pressure environment with a constant volume, (ii) the growth driving force was the temperature gradient within the main vessel 20 and the vapor pressure difference (chemical potential difference) between polycrystalline SiC and single-crystal SiC, (iii) the source gases were SiC, SiC, and SiC, and (iv) the adsorption coefficient of the source material adsorbed to the steps of the SiC single crystal mass 10 was 0.001.

[0261] The dashed double-dashed line in Figure 21(b) represents the results of thermodynamic calculations when single-crystal SiC is grown using polycrystalline SiC as a raw material in a vapor pressure environment where SiC (solid phase) and C (solid phase) are in phase equilibrium via the gas phase. Specifically, thermodynamic calculations were performed using Equation 2 under the following conditions (i) to (iv): (i) a SiC-C equilibrium vapor pressure environment with a constant volume, (ii) the growth driving force was the temperature gradient within the main vessel 20 and the vapor pressure difference (chemical potential difference) between polycrystalline SiC and single-crystal SiC, (iii) the source gases were SiC, SiC, and SiC, and (iv) the adsorption coefficient of the source material adsorbed to the steps of the SiC single crystal mass 10 was 0.001. The data for each chemical species used in the thermodynamic calculations were taken from the JANAF thermochemical tables.

[0262] According to the graph in Figure 21(b), it can be seen that the results (marked with circles) of placing SiC single crystal body 10 in a space (inside main body container 20) where the atomic ratio Si / C exceeds 1 and growing growth layer 105 on SiC single crystal body 10 show a trend consistent with the results of thermodynamic calculations of SiC growth in a SiC-Si equilibrium vapor pressure environment. Furthermore, the results (marked with an x) of placing the SiC single crystal 10 in a space (inside the main container 20) where the atomic ratio Si / C is 1 or less and growing a growth layer 105 on the SiC single crystal 10 show a trend consistent with the results of thermodynamic calculations of SiC growth in a SiC-C equilibrium vapor pressure environment.

[0263] In a SiC-Si equilibrium vapor pressure environment, it is estimated that a growth rate of 1.0 μm / min or more can be achieved at a heating temperature of 1960°C, and a growth rate of 2.0 μm / min or more can be achieved at a heating temperature of 2000°C or higher. On the other hand, under a SiC-C equilibrium vapor pressure environment, it is estimated that a growth rate of 1.0 μm / min or more can be achieved at a heating temperature of 2000°C, and a growth rate of 2.0 μm / min or more can be achieved at a heating temperature of 2030°C or higher. [Explanation of symbols]

[0264] 10 SiC single crystal 101 Strain layer 1011 Scratch 1012 Latent injury 1013 Distortion 102 Bulk layer 103 steps 104 Terrace 105 Growth layer 11 SiC seed crystal 12 SiC ingot 13 SiC wafers 14 SiC wafer with epitaxial film 20 Main container 21 Upper container 22 Lower container 23 Gap 24 PCB holder 25 Si vapor source 30 Furnace 31 main heating chamber 32 Pre-heating chamber 33 Transportation 34 Heater 35 Vacuum forming valve 36 Inert gas injection valve 37 Vacuum gauge 40 High-melting-point container 41 Upper container 42 Lower container 43 Gap 44 Si vapor source X Etching Space Y Raw material supply space Z Si vapor pressure space S1 Heat treatment process S11 Strained layer removal process S111 Etching bunching process S12 Flattening process S121 Etching planarization process S122 Growth flattening process S13 Basal plane dislocation reduction process S2 Ingot growth process S3 Slicing process S4 Surface processing process S5 Epitaxial growth process

Claims

1. a heat treatment step of heat treating a SiC single crystal body in an atmosphere containing Si element and C element, the heat treatment step is a step of placing the SiC single crystal body in a main body container made of a SiC material, facing the SiC material constituting the main body container or another SiC material, and performing the heat treatment; The heat treatment step includes: a planarization step for reducing macrostep bunching of the SiC single crystal body; a basal plane dislocation reduction step of forming a growth layer with reduced basal plane dislocations on the SiC single crystal body; a strained layer removal step of removing the strained layer of the SiC single crystal body; The method includes at least two steps selected from the following: the planarization step is an etching step of etching the SiC single crystal body by heating the SiC single crystal body in a SiC-Si equilibrium vapor pressure environment so that the SiC material constituting the main body container or the other SiC material is on the high temperature side and the SiC material constituting the main body container or the other SiC material is on the low temperature side, and / or a crystal growth step of growing the SiC single crystal body by heating the SiC single crystal body in a SiC-Si equilibrium vapor pressure environment so that the SiC material is on the low temperature side and the SiC material constituting the main body container or the other SiC material is on the high temperature side, the basal plane dislocation reduction step is a crystal growth step in which the SiC single crystal is grown by heating in a SiC-C equilibrium vapor pressure environment such that the SiC single crystal is on the low temperature side and the SiC material constituting the main body container or the other SiC material is on the high temperature side; the strained layer removal step is an etching step of etching the SiC single crystal body by heating the SiC single crystal body in a SiC-Si equilibrium vapor pressure environment or a SiC-C equilibrium vapor pressure environment so that the SiC material constituting the main body container or the other SiC material is on the low temperature side. A method for producing a SiC seed crystal for growing a SiC ingot.

2. The method for producing a SiC seed crystal for growing a SiC ingot according to claim 1 , wherein the heat treatment step includes the planarization step performed after the basal plane dislocation reduction step.

3. The method for producing a SiC seed crystal for growing a SiC ingot according to claim 1 , wherein the heat treatment step includes the basal plane dislocation reduction step performed after the planarization step.

4. The method for producing a SiC seed crystal for growing a SiC ingot according to claim 1 , wherein the heat treatment step includes the flattening step after the strained layer removal step.

5. The method for producing a SiC seed crystal according to claim 1 , wherein the heat treatment step includes the basal plane dislocation reduction step performed after the strained layer removal step.

6. The method for producing a SiC seed crystal according to claim 1 , wherein the heat treatment step includes the strained layer removal step, the planarization step, the basal plane dislocation reduction step, and the planarization step in this order.

7. 7. The method for producing a SiC seed crystal according to claim 1, wherein the planarization step includes: arranging the SiC single crystal body and the SiC material constituting the main body container or another SiC material so as to face each other in a quasi-closed space having an atomic ratio Si / C exceeding 1; and heating the SiC single crystal body and the SiC material constituting the main body container or the other SiC material so as to form a temperature gradient between the SiC single crystal body and the SiC material constituting the main body container or the other SiC material, thereby forming a SiC-Si equilibrium vapor pressure environment.

8. 7. The method for producing a SiC seed crystal according to claim 1, wherein the planarization step includes accommodating a SiC single crystal body and a Si vapor supply source in a main body container made of a SiC material, and heating the main body container so as to form a temperature gradient within the main body container, thereby forming a SiC-Si equilibrium vapor pressure environment.

9. 7. The method for producing a SiC seed crystal according to claim 1, wherein the basal plane dislocation reduction step comprises: arranging a SiC single crystal body and a SiC material constituting the main body container or another SiC material so as to face each other in a quasi-closed space having an atomic ratio Si / C of 1 or less; and heating the SiC single crystal body so that the SiC material constituting the main body container or the other SiC material is on the low-temperature side and the SiC material constituting the main body container or the other SiC material is on the high-temperature side, thereby forming a SiC-C equilibrium vapor pressure environment.

10. A method for producing a SiC ingot, comprising an ingot growing step of growing single crystal SiC on a SiC seed crystal produced by the production method according to any one of claims 1 to 9.

11. A method for producing a SiC wafer, comprising a slicing step of slicing a SiC wafer from a SiC ingot produced by the method for producing a SiC ingot according to claim 10 so as to expose a film-formed surface.

12. A method for producing a SiC wafer with an epitaxial film, comprising: an epitaxial growth step of forming an epitaxial film on the film formation surface of a SiC wafer produced by the SiC wafer production method according to claim 11.

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