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JP7149767B2 - SiC Single Crystal Bonding Method, SiC Ingot Manufacturing Method, and SiC Single Crystal Growth Pedestal - Google Patents

SiC Single Crystal Bonding Method, SiC Ingot Manufacturing Method, and SiC Single Crystal Growth Pedestal Download PDF

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JP7149767B2
JP7149767B2 JP2018152319A JP2018152319A JP7149767B2 JP 7149767 B2 JP7149767 B2 JP 7149767B2 JP 2018152319 A JP2018152319 A JP 2018152319A JP 2018152319 A JP2018152319 A JP 2018152319A JP 7149767 B2 JP7149767 B2 JP 7149767B2
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陽平 藤川
秀隆 鷹羽
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Denso Corp
Resonac Holdings Corp
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    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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    • C30B23/02Epitaxial-layer growth
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    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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Description

本発明は、SiC単結晶の貼合方法、SiCインゴットの製造方法及びSiC単結晶成長用台座に関する。 TECHNICAL FIELD The present invention relates to a SiC single crystal bonding method, a SiC ingot manufacturing method, and a SiC single crystal growth pedestal.

炭化珪素(SiC)は、シリコン(Si)に比べて絶縁破壊電界が1桁大きく、バンドギャップが3倍大きい。また、炭化珪素(SiC)は、シリコン(Si)に比べて熱伝導率が3倍程度高い等の特性を有する。炭化珪素(SiC)は、パワーデバイス、高周波デバイス、高温動作デバイス等への応用が期待されている。 Silicon carbide (SiC) has a dielectric breakdown field one order of magnitude larger and a bandgap three times larger than silicon (Si). In addition, silicon carbide (SiC) has properties such as a thermal conductivity that is about three times as high as that of silicon (Si). Silicon carbide (SiC) is expected to be applied to power devices, high frequency devices, high temperature operation devices and the like.

半導体等のデバイスには、SiCウェハ上にエピタキシャル膜を形成したSiCエピタキシャルウェハが用いられる。SiCウェハ上に化学的気相成長法(Chemical Vapor Deposition:CVD)によって設けられたエピタキシャル膜が、SiC半導体デバイスの活性領域となる。 Devices such as semiconductors use SiC epitaxial wafers obtained by forming an epitaxial film on a SiC wafer. An epitaxial film provided on a SiC wafer by chemical vapor deposition (CVD) serves as an active region of a SiC semiconductor device.

そのため、割れ等の破損が無く、欠陥の少ない、高品質なSiCウェハが求められている。なお、本明細書において、SiCエピタキシャルウェハはエピタキシャル膜を形成後のウェハを意味し、SiCウェハはエピタキシャル膜を形成前のウェハを意味する。 Therefore, there is a demand for a high-quality SiC wafer that is free from damage such as cracks and has few defects. In this specification, the SiC epitaxial wafer means a wafer after forming an epitaxial film, and the SiC wafer means a wafer before forming an epitaxial film.

例えば、特許文献1及び特許文献2には、種結晶として使用されるSiC単結晶の外形の反り及びうねりが、クラックや欠陥の起因になっていることが記載されている。特許文献1には、SiC単結晶と台座の線膨張係数を所定の範囲にすることで、ウェハの反りが低減されることが記載されている。また特許文献2には、種結晶保持部の熱膨張係数を坩堝のその他の部分より小さくすることで、SiC単結晶が成長中に受ける応力を小さくできることが記載されている。 For example, Patent Literature 1 and Patent Literature 2 describe that cracks and defects are caused by external warpage and undulation of SiC single crystals used as seed crystals. Patent Literature 1 describes that by setting the linear expansion coefficients of the SiC single crystal and the pedestal within a predetermined range, the warpage of the wafer is reduced. Further, Patent Document 2 describes that by making the thermal expansion coefficient of the seed crystal holding portion smaller than that of other portions of the crucible, the stress that the SiC single crystal receives during growth can be reduced.

特許第5398492号公報Japanese Patent No. 5398492 特開2009-102187号公報JP 2009-102187 A

SiCウェハのキラー欠陥の一つとして、基底面転位(BPD)がある。SiCウェハのBPDの一部はSiCエピタキシャルウェハにも引き継がれ、デバイスの順方向に電流を流した際の順方向特性の低下の要因となる。BPDは、基底面において生じるすべりが発生の原因の一つであると考えられている欠陥である。 A basal plane dislocation (BPD) is one of the killer defects of SiC wafers. A part of the BPD of the SiC wafer is also inherited by the SiC epitaxial wafer, and causes deterioration of the forward characteristics when current is passed through the device in the forward direction. BPD is a defect that is considered to be caused by one of the causes of slippage that occurs on the basal plane.

特許文献1及び2に記載のように、種結晶として使用されるSiC単結晶の外形の結晶成長時における反りを制御しても、BPDは十分抑制することができない。そのため、BPDの低減が求められている。 As described in Patent Documents 1 and 2, BPD cannot be sufficiently suppressed even by controlling the warpage of the outer shape of the SiC single crystal used as the seed crystal during crystal growth. Therefore, reduction of BPD is demanded.

本発明は上記問題に鑑みてなされたものであり、結晶成長時において原子配列面の湾曲を低減できるSiC単結晶の貼合方法を提供することを目的とする。 SUMMARY OF THE INVENTION It is an object of the present invention to provide a method for bonding SiC single crystals that can reduce the curvature of the plane of atomic arrangement during crystal growth.

本発明者らは、鋭意検討の結果、SiC単結晶の原子配列面(格子面)の湾曲量と、基底面転位(BPD)密度との間に、相関関係があることを見出した。そこで、SiC単結晶を設置する台座の貼付面を所定の形状に加工することで、結晶成長時の原子配列面を平坦化できることを見出した。
すなわち、本発明は、上記課題を解決するために、以下の手段を提供する。
As a result of extensive studies, the present inventors have found that there is a correlation between the amount of curvature of the atomic arrangement plane (lattice plane) of a SiC single crystal and the basal plane dislocation (BPD) density. Therefore, the present inventors have found that the plane of atomic arrangement during crystal growth can be flattened by processing the attachment surface of the pedestal on which the SiC single crystal is placed into a predetermined shape.
That is, the present invention provides the following means in order to solve the above problems.

(1)第1の態様にかかるSiC単結晶の貼合方法は、SiC単結晶の原子配列面の湾曲量及び湾曲方向を少なくとも平面視中央を通る第1の方向と前記第1の方向と直交する第2の方向に沿って測定する測定工程と、前記SiC単結晶の原子配列面と逆方向に湾曲する湾曲面を有する台座を準備する準備工程と、前記原子配列面の湾曲方向と前記湾曲面の湾曲方向とが異なるように前記SiC単結晶と前記台座とを対向させて、貼りつける貼付工程と、を備える。 (1) In the SiC single crystal bonding method according to the first aspect, the bending amount and the bending direction of the atomic arrangement plane of the SiC single crystal are set to a first direction passing through at least the center in a plan view and perpendicular to the first direction. a preparatory step of preparing a pedestal having a curved surface curved in a direction opposite to the atomic arrangement surface of the SiC single crystal; a bending direction of the atomic arrangement surface and the bending and an attaching step of attaching the SiC single crystal and the pedestal so that they are opposed to each other so that the directions of curvature of the surfaces are different from each other.

(2)上記態様にかかるSiC単結晶の貼合方法において、前記原子配列面の湾曲量の絶対値と、前記台座の前記湾曲面の湾曲量の絶対値と、の差が、貼付面のいずれの箇所においても10μm以下であってもよい。 (2) In the SiC single crystal bonding method according to the aspect described above, the difference between the absolute value of the amount of curvature of the atomic arrangement plane and the absolute value of the amount of curvature of the curved surface of the pedestal is It may also be 10 μm or less at the location.

(3)上記態様にかかるSiC単結晶の貼合方法において、前記原子配列面の曲率半径が28m以上であってもよい。 (3) In the method for bonding SiC single crystals according to the aspect described above, the radius of curvature of the atomic arrangement plane may be 28 m or more.

(4)上記態様にかかるSiC単結晶の貼合方法において、前記SiC単結晶の直径が150mm以上である場合に、前記原子配列面の湾曲量の最大値が100μm以下であってもよい。 (4) In the SiC single crystal bonding method according to the aspect described above, when the diameter of the SiC single crystal is 150 mm or more, the maximum amount of curvature of the atomic arrangement plane may be 100 μm or less.

(5)上記態様にかかるSiC単結晶の貼合方法において、前記貼付工程を行う際の前記SiC単結晶の厚みが5mm以下であってもよい。 (5) In the SiC single crystal bonding method according to the aspect described above, the SiC single crystal may have a thickness of 5 mm or less when performing the bonding step.

(6)第2の態様にかかるSiCインゴットの製造方法は、上記態様にかかるSiC単結晶の貼合方法において、前記台座に貼り付けられた前記SiC単結晶を種結晶として結晶成長を行う。 (6) A method for manufacturing a SiC ingot according to a second aspect is the SiC single crystal bonding method according to the above aspect, wherein crystal growth is performed using the SiC single crystal attached to the pedestal as a seed crystal.

(7)上記態様にかかるSiCインゴットの製造方法において、前記台座と前記SiC単結晶との結晶成長温度における熱膨張係数の差が、0.3×10-6/℃以下であってもよい。 (7) In the SiC ingot manufacturing method according to the aspect described above, a difference in thermal expansion coefficient between the pedestal and the SiC single crystal at a crystal growth temperature may be 0.3×10 −6 /° C. or less.

(8)第3の態様にかかるSiC単結晶成長用台座は、貼りつけるSiC単結晶の原子配列面の湾曲方向と反対方向に湾曲する湾曲面を備える。 (8) The SiC single crystal growth pedestal according to the third aspect has a curved surface curved in a direction opposite to the curved direction of the atomic arrangement plane of the SiC single crystal to be attached.

(9)上記態様にかかるSiC単結晶成長用台座は、貼りつけるSiC単結晶の原子配列面の湾曲量の絶対値と、前記湾曲面の湾曲量の絶対値と、の差が、貼付面のいずれの箇所においても10μm以下であってもよい。 (9) In the SiC single crystal growth pedestal according to the above aspect, the difference between the absolute value of the amount of curvature of the atomic arrangement plane of the SiC single crystal to be attached and the absolute value of the amount of curvature of the curved surface is It may be 10 μm or less at any point.

上記態様にかかるSiC単結晶の貼合方法を用いると、結晶成長時の原子配列面を平坦化できる。 By using the SiC single crystal bonding method according to the above aspect, the plane of atomic arrangement during crystal growth can be flattened.

SiC単結晶を平面視中心を通る第1の方向に延在する直線に沿って切断した切断面の模式図である。FIG. 2 is a schematic diagram of a cross section of a SiC single crystal cut along a straight line extending in a first direction and passing through the center in a plan view; SiC単結晶の原子配列面の一例を模式的に示した図である。1 is a diagram schematically showing an example of an atomic arrangement plane of a SiC single crystal; FIG. SiC単結晶の原子配列面の別の例を模式的に示した図である。FIG. 4 is a diagram schematically showing another example of an atomic arrangement plane of a SiC single crystal; 原子配列面の形状の測定方法を具体的に説明するための図である。It is a figure for demonstrating concretely the measuring method of the shape of an atomic arrangement plane. 原子配列面の形状の測定方法を具体的に説明するための図である。It is a figure for demonstrating concretely the measuring method of the shape of an atomic arrangement plane. 原子配列面の形状の測定方法を具体的に説明するための図である。It is a figure for demonstrating concretely the measuring method of the shape of an atomic arrangement plane. 原子配列面の形状の測定方法を具体的に説明するための図である。It is a figure for demonstrating concretely the measuring method of the shape of an atomic arrangement plane. 複数のXRDの測定点から原子配列面の曲率半径を求めた例を示す。An example in which the radius of curvature of an atomic arrangement surface is obtained from a plurality of XRD measurement points is shown. 原子配列面の形状の測定方法の別の例を具体的に説明するための図である。FIG. 5 is a diagram for specifically explaining another example of a method for measuring the shape of an atomic arrangement plane; 原子配列面の形状の測定方法の別の例を具体的に説明するための図である。FIG. 5 is a diagram for specifically explaining another example of a method for measuring the shape of an atomic arrangement plane; SiC単結晶と台座の関係を示す図である。It is a figure which shows the relationship between a SiC single crystal and a base. SiC単結晶を台座に貼りつけた後の状態を模式的に示した図である。It is the figure which showed typically the state after sticking a SiC single crystal on a base. 昇華法に用いられる製造装置の一例の模式図である。It is a schematic diagram of an example of the manufacturing apparatus used for the sublimation method. SiC単結晶の原子配列面の曲率半径と、BPD密度の関係を示すグラフである。4 is a graph showing the relationship between the radius of curvature of the atomic arrangement surface of SiC single crystal and BPD density.

以下、本実施形態について、図を適宜参照しながら詳細に説明する。以下の説明で用いる図面は、便宜上特徴となる部分を拡大して示している場合があり、各構成要素の寸法比率などは実際とは異なっていることがある。以下の説明において例示される材質、寸法等は一例であって、本発明はそれらに限定されるものではなく、その要旨を変更しない範囲で適宜変更して実施することが可能である。 Hereinafter, this embodiment will be described in detail with appropriate reference to the drawings. In the drawings used in the following description, characteristic portions may be enlarged for the sake of convenience, and the dimensional ratio of each component may differ from the actual one. The materials, dimensions, and the like exemplified in the following description are examples, and the present invention is not limited to them, and can be modified as appropriate without changing the gist of the invention.

「SiC単結晶の貼合方法」
本実施形態にかかるSiC単結晶の貼合方法は、測定工程と、準備工程と、貼付工程とを有する。測定工程では、SiC単結晶の原子配列面の形状を、少なくとも平面視中央を通る第1の方向と、第1の方向と直交する第2の方向とに沿って測定する。また準備工程では、SiC単結晶の原子配列面と逆方向に湾曲する湾曲面を有する台座を準備する。さらに貼付工程では、原子配列面の湾曲方向と台座の湾曲面の湾曲方向とが異なるようにSiC単結晶と台座とを対向させて、貼りつける。以下、各工程について具体的に説明する。
"Method for Bonding SiC Single Crystals"
The SiC single crystal bonding method according to the present embodiment includes a measurement process, a preparation process, and a bonding process. In the measuring step, the shape of the atomic arrangement plane of the SiC single crystal is measured along at least a first direction passing through the center in plan view and a second direction orthogonal to the first direction. In the preparation step, a pedestal having a curved surface curved in a direction opposite to the atomic arrangement surface of the SiC single crystal is prepared. Furthermore, in the attaching step, the SiC single crystal and the pedestal are attached so that the curved direction of the atomic arrangement surface and the curved surface of the pedestal are different from each other. Each step will be specifically described below.

<測定工程>
図1は、SiC単結晶1を平面視中心を通る第1の方向に延在する直線に沿って切断した切断面の模式図である。第1の方向は、任意の方向を設定できる。図1では、第1の方向を[1-100]としている。図1において上側は[000-1]方向、すなわち<0001>方向に垂直に切断をした時にカーボン面(C面、(000-1)面)が現れる方向である。以下、第1の方向を[1-100]とした場合を例に説明する。
<Measurement process>
FIG. 1 is a schematic diagram of a cross section obtained by cutting a SiC single crystal 1 along a straight line passing through the center in a plan view and extending in a first direction. Any direction can be set as the first direction. In FIG. 1, the first direction is [1-100]. In FIG. 1, the upper side is the [000-1] direction, that is, the direction in which the carbon plane (C plane, (000-1) plane) appears when cut perpendicular to the <0001> direction. An example in which the first direction is [1-100] will be described below.

ここで結晶方位及び面は、ミラー指数として以下の括弧を用いて表記される。()と{}は面を表す時に用いられる。()は特定の面を表現する際に用いられ、{}は結晶の対称性による等価な面の総称(集合面)を表現する際に用いられる。一方で、<>と[]は方向を表すに用いられる。[]は特定の方向を表現する際に用いられ、<>は結晶の対称性による等価な方向を表現する際に用いられる。 Here, crystal orientations and planes are expressed using the following parentheses as Miller indices. ( ) and { } are used when representing faces. ( ) is used to express a specific plane, and { } is used to express a generic term (aggregate plane) of equivalent planes based on crystal symmetry. On the other hand , <> and [ ] are used to indicate direction. [ ] is used to express a specific direction, and <> is used to express an equivalent direction due to crystal symmetry.

図1に示すように、SiC単結晶1は、複数の原子Aが整列してなる単結晶である。そのため図1に示すように、SiC単結晶の切断面をミクロに見ると、複数の原子Aが配列した原子配列面2が形成されている。切断面における原子配列面2は、切断面に沿って配列する原子Aを繋いで得られる切断方向と略平行な方向に延在する線として表記される。 As shown in FIG. 1, the SiC single crystal 1 is a single crystal in which a plurality of atoms A are aligned. Therefore, as shown in FIG. 1, when microscopically looking at the cut surface of the SiC single crystal, an atomic arrangement plane 2 in which a plurality of atoms A are arranged is formed. The atomic arrangement plane 2 on the cutting plane is expressed as a line extending in a direction substantially parallel to the cutting direction obtained by connecting the atoms A arranged along the cutting plane.

原子配列面2の形状は、SiC単結晶1の最表面の形状によらず、切断面の方向によって異なる場合がある。図2及び図3は、原子配列面2の形状を模式的に示した図である。図2に示す原子配列面2は、中心に向かって凹形状である。そのため、図2に示す原子配列面2は、[1-100]方向と、[1-100]方向に直交する[11-20]方向とで湾曲方向が一致する。これに対し図3に示す原子配列面2は、所定の切断面では凹形状、異なる切断面では凸形状のポテトチップス型(鞍型)の形状である。そのため、図3に示す原子配列面2は、[1-100]方向と、[1-100]方向に直交する[11-20]方向と、で湾曲方向が異なる。 The shape of the atomic arrangement plane 2 does not depend on the shape of the outermost surface of the SiC single crystal 1, but may vary depending on the direction of the cut surface. 2 and 3 are diagrams schematically showing the shape of the atomic arrangement plane 2. FIG. The atomic arrangement plane 2 shown in FIG. 2 is concave toward the center. Therefore, in the atomic arrangement plane 2 shown in FIG. 2, the [1-100] direction and the [11-20] direction perpendicular to the [1-100] direction are curved in the same direction. On the other hand, the atomic array plane 2 shown in FIG. 3 has a potato chip shape (saddle shape), which is concave on a predetermined cross section and convex on a different cross section. Therefore, the atomic arrangement plane 2 shown in FIG. 3 has different bending directions in the [1-100] direction and in the [11-20] direction orthogonal to the [1-100] direction.

つまり、原子配列面2の形状を正確に把握するためには、少なくとも平面視中央を通り互いに直交する2方向(第1の方向及び第2の方向)に沿って、SiC単結晶の原子配列面2の形状を測定する必要がある。またSiC単結晶1の結晶構造は六方晶であり、中心に対して対称な六方向に沿って原子配列面2の形状を測定することが好ましい。中心に対して対称な六方向に沿って原子配列面2の形状を計測すれば、原子配列面2の形状をより精密に求めることができる。 That is, in order to accurately grasp the shape of the atomic arrangement plane 2, the atomic arrangement plane of the SiC single crystal should be measured at least along two directions (first direction and second direction) that pass through the center in plan view and are orthogonal to each other. 2 shapes need to be measured. The crystal structure of the SiC single crystal 1 is hexagonal, and it is preferable to measure the shape of the atomic arrangement plane 2 along six directions symmetrical with respect to the center. By measuring the shape of the atomic arrangement plane 2 along six directions symmetrical with respect to the center, the shape of the atomic arrangement plane 2 can be obtained more precisely.

原子配列面2の形状はX線回折(XRD)により測定できる。測定する面は測定する方向に応じて決定される。測定方向を[hkil]とすると、測定面は(mh mk mi n)の関係を満たす必要がある。ここで、mは0以上の整数であり、nは自然数である。例えば、[11-20]方向に測定する場合は、m=0、n=4として(0004)面、m=2、n=16として(22-416)面等が選択される。一方で、[1-100]方向に測定する場合は、m=0、n=4として(0004)面、m=3、n=16として(3-3016)面等が選択される。すなわち測定面は、測定方向によって異なる面であってもよく、測定される原子配列面2は必ずしも同じ面とはならなくてもよい。上記関係を満たすことで、結晶成長時に及ぼす影響の少ないa面又はm面方向の格子湾曲をc面方向の格子湾曲と誤認することを防ぐことができる。また測定はC面、Si面のいずれの面を選択してもよいが、坩堝の設置面に貼りつける貼付面(第1面)に対して行うことが好ましい。
The shape of the atomic arrangement plane 2 can be measured by X-ray diffraction (XRD). The surface to be measured is determined according to the direction of measurement. Assuming that the measurement direction is [hkil], the measurement surface must satisfy the relationship (mh mk min). Here, m is an integer greater than or equal to 0, and n is a natural number. For example, when measuring in the [11-20] direction, the (0004) plane is selected with m=0 and n=4, and the (22-416) plane with m=2 and n=16. On the other hand, when measuring in the [1-100] direction, the (0004) plane is selected with m=0 and n=4, and the (3-3016) plane with m=3 and n=16. That is, the measurement plane may be a different plane depending on the measurement direction, and the atomic arrangement plane 2 to be measured does not necessarily have to be the same plane. By satisfying the above relationship, it is possible to prevent the lattice curvature in the a-plane or m-plane direction, which has little effect on crystal growth, from being mistaken for the lattice curvature in the c-plane direction. The measurement may be performed on either the C surface or the Si surface, but it is preferable to perform the measurement on the attachment surface (first surface) that is attached to the installation surface of the crucible.

X線回折データは、所定の方向に沿って中心、端部、中心と端部との中点の5点において取得する。原子配列面2が湾曲している場合、X線の反射方向が変わるため、中心とそれ以外の部分とで出力されるX線回折像のピークのω角の位置が変動する。この回折ピークの位置変動から原子配列面2の湾曲方向を求めることができる。また回折ピークの位置変動から原子配列面2の曲率半径も求めることができ、原子配列面2の湾曲量も求めることができる。そして、原子配列面2の湾曲方向及び湾曲量から原子配列面2の形状を求めることができる。 X-ray diffraction data are acquired at five points along a given direction: the center, the edge, and the midpoint between the center and the edge. If the atomic arrangement plane 2 is curved, the X-ray reflection direction changes, so the ω angle position of the peak of the output X-ray diffraction image varies between the center and other portions. The bending direction of the atomic arrangement plane 2 can be determined from the positional variation of the diffraction peak. Also, the radius of curvature of the atomic array surface 2 can be obtained from the positional variation of the diffraction peak, and the amount of curvature of the atomic array surface 2 can also be obtained. Then, the shape of the atomic arrangement plane 2 can be obtained from the bending direction and the amount of bending of the atomic arrangement plane 2 .

(原子配列面の形状の測定方法(方法1)の具体的な説明)
SiC単結晶をスライスした試料(以下、ウェハ20と言う)の外周端部分のXRDの測定値から原子配列面の湾曲方向及び湾曲量を測定する方法について具体的に説明する。一例としてウェハ20を用いて測定方法を説明するが、スライスする前のインゴット状のSiC単結晶においても同様の方法を用いて測定できる。
(Specific explanation of the method for measuring the shape of the atomic arrangement plane (Method 1))
A method for measuring the bending direction and bending amount of the atomic arrangement surface from the XRD measurement value of the outer peripheral end portion of a sample obtained by slicing a SiC single crystal (hereinafter referred to as a wafer 20) will be described in detail. The measurement method will be described using the wafer 20 as an example, but the same method can be used to measure an ingot-shaped SiC single crystal before slicing.

図4に平面視中心を通り原子配列面の測定の方向、例えば[1-100]方向に沿って切断した切断面を模式的に示す。ウェハ20の半径をrとすると、断面の横方向の長さは2rとなる。また図4にウェハ20における原子配列面22の形状も図示している。図4に示すように、ウェハ20自体の形状は平坦であるが、原子配列面22は湾曲している場合がある。図4に示す原子配列面22は左右対称であり、凹型に湾曲している。この対称性は、SiC単結晶(インゴット)の製造条件が通常中心に対して対称性があることに起因する。なお、この対称性とは、完全対称である必要はなく、製造条件の揺らぎ等に起因したブレを容認する近似としての対称性を意味する。 FIG. 4 schematically shows a cross section cut along the direction of measurement of the atomic arrangement plane, eg, the [1-100] direction, passing through the center in plan view. Assuming that the radius of the wafer 20 is r, the lateral length of the cross section is 2r. 4 also shows the shape of the atomic arrangement surface 22 in the wafer 20. As shown in FIG. As shown in FIG. 4, although the shape of the wafer 20 itself is flat, the atomic arrangement surface 22 may be curved. The atomic arrangement plane 22 shown in FIG. 4 is symmetrical and curved concavely. This symmetry results from the fact that manufacturing conditions for SiC single crystals (ingots) are generally symmetrical about the center. Note that this symmetry does not have to be perfect symmetry, but means symmetry as an approximation that allows fluctuations due to fluctuations in manufacturing conditions and the like.

次いで、図5に示すように、XRDをウェハ20の外周端部に対して行い、測定した2点間のX線回折ピーク角度の差Δθを求める。このΔθが測定した2点の原子配列面22の傾きの差になっている。X線回折測定に用いる回折面は、上述のように切断面にあわせて適切な面を選択する。 Next, as shown in FIG. 5, XRD is performed on the outer peripheral edge of the wafer 20 to obtain the difference Δθ between the two measured X-ray diffraction peak angles. This .DELTA..theta. is the difference between the tilts of the atomic arrangement plane 22 at the two points measured. As for the diffraction surface used for the X-ray diffraction measurement, an appropriate surface is selected according to the cut surface as described above.

次に、図6に示すように、得られたΔθから湾曲した原子配列面22の曲率半径を求める。図6には、ウェハ20の原子配列面22の曲面が円の一部であると仮定して、測定した2箇所の原子配列面に接する円Cを示している。図6から幾何学的に、接点を両端とする円弧を含む扇型の中心角φは、測定したX線回折ピーク角度の差Δθと等しくなる。原子配列面22の曲率半径は、当該円弧の半径Rに対応する。円弧の半径Rは以下の関係式で求められる。 Next, as shown in FIG. 6, the radius of curvature of the curved atomic arrangement surface 22 is obtained from the obtained Δθ. FIG. 6 shows a circle C which is in contact with two measured atomic arrangement planes, assuming that the curved surface of the atomic arrangement plane 22 of the wafer 20 is a part of a circle. Geometrically from FIG. 6, the central angle φ of the sector containing the circular arc with both ends at the tangent point is equal to the measured X-ray diffraction peak angle difference Δθ. The radius of curvature of the atomic arrangement plane 22 corresponds to the radius R of the arc. The arc radius R is obtained by the following relational expression.

Figure 0007149767000001
Figure 0007149767000001

そして、この円弧の半径Rとウェハ20の半径rとから、原子配列面22の湾曲量dが求められる。図7に示すように、原子配列面22の湾曲量dは、円弧の半径から、円弧の中心からウェハ20に下した垂線の距離を引いたものに対応する。円弧の中心からウェハ20に下した垂線の距離は、三平方の定理から算出され、以下の式が成り立つ。なお、本明細書では曲率半径が正(凹面)の場合の湾曲量dを正の値とし、負(凸面)の場合の湾曲量dを負の値と定義する。 Then, from the radius R of this arc and the radius r of the wafer 20, the amount of curvature d of the atomic array surface 22 is obtained. As shown in FIG. 7, the amount of curvature d of the atomic array plane 22 corresponds to the radius of the arc minus the distance of the perpendicular from the center of the arc to the wafer 20 . The distance of the perpendicular from the center of the arc to the wafer 20 is calculated from the Pythagorean theorem, and the following equation holds. In this specification, the curvature amount d is defined as a positive value when the curvature radius is positive (concave surface), and the curvature amount d is defined as a negative value when the curvature radius is negative (convex surface).

Figure 0007149767000002
Figure 0007149767000002

上述のように、XRDのウェハ20の外周端部の測定値だけからRを測定することもできる。一方で、この方法を用いると、測定箇所に局所的な歪等が存在した場合において、形状を見誤る可能性もある。その為、複数箇所でX線回折ピーク角度の測定を行って、単位長さ辺りの曲率を以下の式から換算する。 As mentioned above, R can also be measured only from the XRD measurements of the outer edge of the wafer 20 . On the other hand, if this method is used, there is a possibility that the shape may be misunderstood when there is local distortion or the like at the measurement location. Therefore, the X-ray diffraction peak angle is measured at multiple points, and the curvature per unit length is converted from the following formula.

Figure 0007149767000003
Figure 0007149767000003

図8に、複数のXRDの測定点から原子配列面の曲率半径を求めた例を示す。図8の横軸はウェハ中心からの相対位置であり、縦軸はウェハ中心回折ピーク角に対する各測定点の相対的な回折ピーク角度を示す。図8は、ウェハの[1-100]方向を測定し、測定面を(3-3016)とした例である。測定箇所は5カ所で行った。5点はほぼ直線に並んでおり、この傾きから、dθ/dr=8.69×10-4deg/mmが求められる。この結果を上式に適用することで曲率半径R=66mの凹面であることが計算できる。そして、このRとウェハの半径r(75mm)から、原子配列面の湾曲量dが42.6μmと求まる。 FIG. 8 shows an example in which the radius of curvature of the atomic arrangement surface is obtained from a plurality of XRD measurement points. The horizontal axis of FIG. 8 indicates the relative position from the wafer center, and the vertical axis indicates the diffraction peak angle of each measurement point relative to the wafer center diffraction peak angle. FIG. 8 shows an example in which the [1-100] direction of the wafer is measured and the measurement plane is (3-3016). Measurement was performed at five locations. The five points are arranged substantially on a straight line, and dθ/dr=8.69×10 −4 deg/mm can be obtained from this slope. By applying this result to the above formula, it is possible to calculate a concave surface with a curvature radius of R=66 m. Then, from this R and the radius r (75 mm) of the wafer, the amount of curvature d of the atomic array plane is found to be 42.6 μm.

ここまで原子配列面の形状が凹面である例で説明したが、凸面の場合も同様に求められる。凸面の場合は、Rはマイナスとして算出される。 Although the example in which the shape of the atomic arrangement surface is concave has been described so far, the same is required for the convex surface. For convex surfaces, R is calculated as negative.

(原子配列面の形状の別の測定方法(方法2)の説明)
原子配列面の形状は、別の方法で求めてもよい。図9に平面視中心を通り原子配列面の測定の方向、例えば[1-100]方向に沿って切断した切断面を模式的に示す。図9では、原子配列面22の形状が凹状に湾曲している場合を例に説明する。
(Description of another method for measuring the shape of the atomic arrangement plane (Method 2))
The shape of the atomic arrangement plane may be obtained by another method. FIG. 9 schematically shows a cross section cut along the direction of measurement of the atomic arrangement plane, for example, the [1-100] direction, passing through the center in plan view. In FIG. 9, an example in which the shape of the atomic array plane 22 is concavely curved will be described.

図9に示すように、ウェハ20の中心とウェハ20の中心から距離xだけ離れた場所の2箇所で、X線回折の回折ピークを測定する。インゴットの製造条件の対称性からウェハ20の形状は、近似として左右対称とすることができ、原子配列面22はウェハ20の中央部で平坦になると仮定できる。そのため、図10に示すように測定した2点における原子配列面22の傾きの差をΔθとすると、原子配列面22の相対的な位置yは以下の式で表記できる。 As shown in FIG. 9, diffraction peaks of X-ray diffraction are measured at two locations, the center of the wafer 20 and the location separated from the center of the wafer 20 by a distance x. From the symmetry of the ingot manufacturing conditions, the shape of the wafer 20 can be approximately left-right symmetrical, and the atomic arrangement plane 22 can be assumed to be flat at the center of the wafer 20 . Therefore, assuming that the difference in inclination of the atomic arrangement plane 22 at two points measured as shown in FIG.

Figure 0007149767000004
Figure 0007149767000004

中心からの距離xの位置を変えて複数箇所の測定をすることで、それぞれの点でウェハ中心と測定点とにおける原子配列面22の相対的な原子位置を求めることができる。
この方法は、それぞれの測定箇所で原子配列面における原子の相対位置が求められる。そのため、局所的な原子配列面の湾曲量を求めることができる。また、ウェハ20全体における原子配列面22の相対的な原子位置をグラフとして示すことができ、原子配列面22のならびを感覚的に把握するために有益である。
By performing measurements at a plurality of points while changing the position of the distance x from the center, it is possible to obtain the relative atomic positions of the atomic arrangement plane 22 between the wafer center and the measurement point at each point.
This method obtains the relative positions of atoms on the plane of atomic arrangement at each measurement point. Therefore, the curvature amount of the local atomic arrangement plane can be obtained. Moreover, the relative atomic positions of the atomic arrangement plane 22 in the entire wafer 20 can be shown as a graph, which is useful for intuitively grasping the arrangement of the atomic arrangement plane 22 .

ここでは、測定対象をウェハ20の場合を例に説明した。測定対象がSiCインゴットやSiCインゴットから切断された切断体の場合も、同様に原子配列面の湾曲量を求めることができる。 Here, the case where the measurement object is the wafer 20 has been described as an example. When the object to be measured is a SiC ingot or a cut body cut from the SiC ingot, the amount of curvature of the atomic arrangement plane can be obtained in the same manner.

上述の手順で、少なくとも平面視中央を通り互いに直交する2方向(第1の方向及び第2の方向)に沿って、SiC単結晶の原子配列面2の湾曲量を測定する。それぞれの方向の湾曲量及び湾曲方向を求めることで、図2及び図3に示すような原子配列面2の概略形状を求めることができる。 By the above-described procedure, the amount of curvature of the atomic arrangement plane 2 of the SiC single crystal is measured along at least two directions (first direction and second direction) that pass through the center in plan view and are orthogonal to each other. By obtaining the amount of curvature and the direction of curvature in each direction, the schematic shape of the atomic arrangement plane 2 as shown in FIGS. 2 and 3 can be obtained.

<準備工程>
準備工程では、SiC単結晶を貼り付ける台座を準備する。図11は、SiC単結晶1と台座3の関係を示す図である。図11に示すように、台座3は、SiC単結晶1の原子配列面2の湾曲方向と逆方向に湾曲する湾曲面3Aを有する。後述する貼付工程で、SiC単結晶1を台座3に貼り付けることで、原子配列面2の湾曲を解消し、原子配列面2を平坦化することができる。
<Preparation process>
In the preparatory step, a pedestal on which the SiC single crystal is attached is prepared. FIG. 11 is a diagram showing the relationship between the SiC single crystal 1 and the pedestal 3. As shown in FIG. As shown in FIG. 11, pedestal 3 has a curved surface 3A that curves in a direction opposite to the curved direction of atomic arrangement plane 2 of SiC single crystal 1 . By attaching the SiC single crystal 1 to the pedestal 3 in the attachment step described later, the curvature of the atomic arrangement plane 2 can be eliminated and the atomic arrangement plane 2 can be flattened.

貼付工程をおこなった後のSiC単結晶の原子面配列の湾曲量は0であることが望ましい。その為、原子配列面2の湾曲量の絶対値と、台座3の湾曲面3Aの湾曲量の絶対値と、の差は、貼付面のいずれの箇所においても10μm以下であることが好ましく、0であることが最も好ましい。台座3と原子配列面2との湾曲量の絶対値差が小さければ、貼り付け後の原子配列面2をより平坦化できる。また原子配列面2の湾曲量の絶対値と、台座3の湾曲面3Aの湾曲量の絶対値と、の差が0でない場合、変形による応力をSiC単結晶に加えすぎないように、台座3の湾曲面3Aの湾曲量は原子配列面2の湾曲量の絶対値よりも小さいことが好ましい。SiC単結晶を歪ませすぎて、SiC単結晶が割れるリスクを低減させることができる。 It is desirable that the amount of bending of the atomic plane arrangement of the SiC single crystal after the bonding step is zero. Therefore, the difference between the absolute value of the amount of curvature of the atomic arrangement surface 2 and the absolute value of the amount of curvature of the curved surface 3A of the pedestal 3 is preferably 10 μm or less at any point on the attachment surface. is most preferred. If the difference in the absolute value of the amount of curvature between the pedestal 3 and the atomic array surface 2 is small, the atomic array surface 2 can be made flatter after being attached. If the difference between the absolute value of the amount of curvature of the atomic arrangement plane 2 and the absolute value of the amount of curvature of the curved surface 3A of the pedestal 3 is not 0, the pedestal 3 should be adjusted so as not to apply excessive stress due to deformation to the SiC single crystal. It is preferable that the amount of curvature of the curved surface 3A is smaller than the absolute value of the amount of curvature of the atomic arrangement surface 2 . It is possible to reduce the risk of the SiC single crystal cracking due to excessive distortion of the SiC single crystal.

台座3の湾曲面3Aは、SiC単結晶1の原子配列面2の形状を測定してから加工してもよいし、予め事前に湾曲方向及び湾曲量の異なる複数の台座3を準備しておき、それらの中から貼付後に原子配列面2を最も平坦化できるものを選択してもよい。 The curved surface 3A of the pedestal 3 may be processed after measuring the shape of the atomic arrangement surface 2 of the SiC single crystal 1, or a plurality of pedestals 3 with different bending directions and amounts of bending may be prepared in advance. , from which the most planarization of the atomic arrangement surface 2 after application may be selected.

また台座3の熱膨張係数は、SiC単結晶1の熱膨張係数と近いことが好ましい。具体的には、熱膨張係数差が、0.3×10-6/℃以下であることが好ましい。なお、ここで示す熱膨張係数とは、SiC単結晶1を種結晶として結晶成長する温度領域における熱膨張係数を意味し、2000℃近傍の温度を意味する。例えば、黒鉛の熱膨張係数は、加工条件、含有材料等により、4.3×10-6/℃~7.1×10-6/℃の範囲で選択できる。台座3とSiC単結晶1の熱膨張率差が近いことで、結晶成長時の熱膨張率差によってSiC単結晶1が反り、原子配列面2が湾曲することを防ぐことができる。 Moreover, the thermal expansion coefficient of the pedestal 3 is preferably close to the thermal expansion coefficient of the SiC single crystal 1 . Specifically, the thermal expansion coefficient difference is preferably 0.3×10 −6 /° C. or less. The thermal expansion coefficient used here means a thermal expansion coefficient in a temperature range in which crystals grow using the SiC single crystal 1 as a seed crystal, and means a temperature in the vicinity of 2000.degree. For example, the coefficient of thermal expansion of graphite can be selected within the range of 4.3×10 −6 /° C. to 7.1×10 −6 /° C. depending on processing conditions, materials contained, and the like. Since the thermal expansion coefficient difference between the pedestal 3 and the SiC single crystal 1 is close, it is possible to prevent the SiC single crystal 1 from warping and the atomic arrangement surface 2 from being curved due to the thermal expansion coefficient difference during crystal growth.

<貼付工程>
貼付工程では、原子配列面2の湾曲方向と台座3の湾曲面3Aの湾曲方向とが異なるようにSiC単結晶1と台座3とを対向させて、貼りつける。図12は、SiC単結晶1を台座3に貼りつけた後の状態を模式的に示した図である。
<Affixing process>
In the attaching step, the SiC single crystal 1 and the pedestal 3 are opposed to each other so that the curved direction of the atomic arrangement surface 2 and the curved direction of the curved surface 3A of the pedestal 3 are different from each other. FIG. 12 is a diagram schematically showing the state after the SiC single crystal 1 has been attached to the pedestal 3. As shown in FIG.

図11及び図12に示すように、原子配列面2の湾曲方向と台座3の湾曲面3Aの湾曲方向とが反対方向になるようにしてSiC単結晶1を台座3に貼りつけると、SiC単結晶1の原子配列面2が貼付前と比較して平坦化する。 As shown in FIGS. 11 and 12, when the SiC single crystal 1 is attached to the pedestal 3 so that the curved direction of the atomic arrangement surface 2 and the curved direction of the curved surface 3A of the pedestal 3 are opposite to each other, the SiC single crystal The atomic array surface 2 of the crystal 1 is flattened compared to before the attachment.

貼付工程を行う際のSiC単結晶1の厚みは5mm以下であることが好ましい。SiC単結晶10の厚みが厚いと、貼付時にたわみが生じにくい。そのため、台座に対して密着させて貼り付け難くなり、貼付工程後のSiC単結晶の原子配列面(格子面)を平坦に配置し辛くなる。 It is preferable that the thickness of the SiC single crystal 1 is 5 mm or less when performing the attaching step. If the thickness of the SiC single crystal 10 is large, it is difficult for the SiC single crystal 10 to bend during attachment. As a result, it becomes difficult to stick the SiC single crystal in close contact with the pedestal, and it becomes difficult to evenly arrange the atomic arrangement plane (lattice plane) of the SiC single crystal after the sticking process.

また貼付工程において、台座3の湾曲面3Aに対してSiC単結晶1を押し付ける荷重は、原子配列面2の台座3の湾曲面3Aに対する相対的な距離に応じて変えることが好ましい。例えば、SiC単結晶1の原子配列面2が台座3に向って凸に湾曲し、外周に向かうほど原子配列面2と台座3の湾曲面3Aとの距離が離れる場合は、SiC単結晶1の外周側の荷重を内側より強くすることが好ましい。またSiC単結晶1の原子配列面2が台座3に向って凹に湾曲し、内側に向かうほど原子配列面2と台座3の湾曲面3Aとの距離が離れる場合は、SiC単結晶1の内側の荷重を外周側より強くすることが好ましい。 Moreover, in the attaching step, it is preferable to change the load for pressing SiC single crystal 1 against curved surface 3A of pedestal 3 according to the relative distance of atomic arrangement surface 2 from curved surface 3A of pedestal 3 . For example, when the atomic arrangement surface 2 of the SiC single crystal 1 curves convexly toward the pedestal 3 and the distance between the atomic arrangement surface 2 and the curved surface 3A of the pedestal 3 increases toward the outer circumference, the SiC single crystal 1 It is preferable to make the load on the outer peripheral side stronger than that on the inner side. Further, when the atomic arrangement surface 2 of the SiC single crystal 1 curves concavely toward the pedestal 3 and the distance between the atomic arrangement surface 2 and the curved surface 3A of the pedestal 3 increases toward the inside, the inside of the SiC single crystal 1 It is preferable to make the load on the outer peripheral side stronger than that on the outer peripheral side.

また貼付工程は、例えば、接着剤を用いて行う。接着剤は、熱硬化性樹脂等を用いることができる。 Moreover, the sticking process is performed using an adhesive agent, for example. A thermosetting resin or the like can be used as the adhesive.

また貼付工程後に、SiC単結晶1の周囲を減圧する減圧工程をさらに行ってもよい。接着面に気泡等が噛みこんだ場合でも減圧環境にすることで脱泡できる。その結果、塗布時の接着剤の厚みムラをより抑制できる。 Further, after the attaching step, a decompression step of decompressing the surroundings of SiC single crystal 1 may be further performed. Even if air bubbles or the like are caught in the adhesive surface, they can be removed by creating a reduced pressure environment. As a result, thickness unevenness of the adhesive during application can be further suppressed.

また貼付工程に至るSiC単結晶1の原子配列面2の曲率半径は28m以上であることが好ましい。曲率半径が大きいほど、原子配列面2は平坦になる。また、SiC単結晶の直径が150mm以上の場合に、原子配列面の湾曲量の最大値は100μm以下であることが好ましい。原子配列面2の湾曲量が大きいと、原子配列面2を平坦化させるために、SiC単結晶1を原子配列面2の湾曲方向と反対方向に大きく歪ませる必要がある。SiC単結晶1の歪量を所定の範囲内にしておくことで、SiC単結晶1にクラックが生じることや、SiC単結晶1内に応力が蓄積することを抑制できる。 Moreover, the radius of curvature of the atomic array surface 2 of the SiC single crystal 1 leading to the bonding step is preferably 28 m or more. The larger the curvature radius, the flatter the atomic arrangement plane 2 becomes. Further, when the diameter of the SiC single crystal is 150 mm or more, the maximum amount of curvature of the atomic arrangement plane is preferably 100 μm or less. If the amount of curvature of atomic arrangement surface 2 is large, SiC single crystal 1 needs to be largely distorted in the direction opposite to the bending direction of atomic arrangement surface 2 in order to flatten atomic arrangement surface 2 . By keeping the strain amount of SiC single crystal 1 within a predetermined range, cracks in SiC single crystal 1 and accumulation of stress in SiC single crystal 1 can be suppressed.

上述のように、本実施形態にかかるSiC単結晶の貼合方法によれば、原子配列面2の湾曲を小さくすることができる。 As described above, according to the SiC single crystal bonding method according to the present embodiment, the curvature of the atomic arrangement plane 2 can be reduced.

「SiCインゴットの製造方法」
本実施形態にかかるSiCインゴットの製造方法は、上述のSiC単結晶の貼合方法において、台座3に貼り付けられたSiC単結晶1を種結晶として結晶成長を行う。SiCインゴットは、例えば昇華法を用いて製造できる。昇華法は、原料を加熱することによって生じた原料ガスを単結晶(種結晶)上で再結晶化し、大きな単結晶(インゴット)を得る方法である。
"Manufacturing method of SiC ingot"
In the SiC ingot manufacturing method according to the present embodiment, crystal growth is performed using the SiC single crystal 1 attached to the pedestal 3 as a seed crystal in the SiC single crystal bonding method described above. A SiC ingot can be manufactured, for example, using a sublimation method. The sublimation method is a method of recrystallizing a raw material gas generated by heating a raw material on a single crystal (seed crystal) to obtain a large single crystal (ingot).

図13は、昇華法に用いられる製造装置の一例の模式図である。製造装置200は、坩堝100とコイル101とを有する。坩堝100とコイル101との間には、コイル101の誘導加熱により発熱する発熱体(図視略)を有してもよい。 FIG. 13 is a schematic diagram of an example of a manufacturing apparatus used for the sublimation method. Manufacturing apparatus 200 has crucible 100 and coil 101 . Between the crucible 100 and the coil 101, a heating element (not shown) that generates heat by induction heating of the coil 101 may be provided.

坩堝100は、原料Gと対向する位置に設けられた台座3を有する。台座3には、SiC単結晶1が上記の貼合方法に従って貼り付けられている。また坩堝100の内部には、台座3から原料Gに向けて拡径するテーパーガイド102が設けられている。 The crucible 100 has a pedestal 3 provided at a position facing the raw material G. As shown in FIG. SiC single crystal 1 is attached to pedestal 3 according to the above bonding method. Further, inside the crucible 100, a taper guide 102 that expands in diameter from the pedestal 3 toward the raw material G is provided.

コイル101に交流電流を印加すると、坩堝100が加熱され、原料Gから原料ガスが生じる。発生した原料ガスは、テーパーガイド102に沿って台座3に設置されたSiC単結晶1に供給される。SiC単結晶1に原料ガスが供給されることで、SiC単結晶1の主面にSiCインゴットIが結晶成長する。SiC単結晶1の結晶成長面は、カーボン面、又は、カーボン面から10°以下のオフ角を設けた面とすることが好ましい。 When an alternating current is applied to the coil 101, the crucible 100 is heated, and the raw material G is produced as a raw material gas. The generated raw material gas is supplied to SiC single crystal 1 placed on pedestal 3 along taper guide 102 . By supplying the raw material gas to the SiC single crystal 1 , the SiC ingot I is crystal-grown on the main surface of the SiC single crystal 1 . The crystal growth surface of the SiC single crystal 1 is preferably a carbon surface or a surface with an off angle of 10° or less from the carbon surface.

SiCインゴットIは、SiC単結晶1の結晶情報の多くを引き継ぐ。SiC単結晶10の原子配列面2は平坦化されているため、SiCインゴットI内にBPDが発生することを抑制できる。 SiC ingot I inherits most of the crystal information of SiC single crystal 1 . Since the atomic arrangement surface 2 of the SiC single crystal 10 is flattened, the occurrence of BPD in the SiC ingot I can be suppressed.

図14は、SiC単結晶の原子配列面の曲率半径と、BPD密度の関係を示すグラフである。図14に示すように、原子配列面2の曲率半径とSiCインゴットI内のBPD密度とは対応関係を有する。原子配列面2の曲率半径が大きい(原子配列面2の湾曲量が小さい)ほど、BPD密度は少なくなる傾向にある。内部に応力が残留した結晶は、結晶面のすべりを誘起させ、BPDの発生と共に原子配列面2を湾曲させると考えられる。あるいは、逆に、湾曲量が大きい原子配列面2が、ひずみを有し、BPDの原因となることも考えられる。いずれの場合においても、原子配列面の曲率半径が大きい(すなわち、原子配列面の湾曲量が小さい)ほど、BPD密度が小さくなる。 FIG. 14 is a graph showing the relationship between the radius of curvature of the SiC single crystal atomic arrangement surface and the BPD density. As shown in FIG. 14, the radius of curvature of the atomic array surface 2 and the BPD density in the SiC ingot I have a corresponding relationship. The BPD density tends to decrease as the radius of curvature of the atomic arrangement plane 2 increases (the amount of curvature of the atomic arrangement plane 2 decreases). It is thought that a crystal with residual stress inside induces a slip of the crystal plane and bends the atomic arrangement plane 2 along with the occurrence of BPD. Alternatively, conversely, it is conceivable that the atomic arrangement plane 2 having a large amount of curvature has strain and causes BPD. In any case, the larger the radius of curvature of the atomic arrangement plane (that is, the smaller the amount of curvature of the atomic arrangement plane), the smaller the BPD density.

上述のように、本実施形態にかかるSiCインゴットの製造方法は、種結晶として用いられるSiC単結晶1の原子配列面2が平坦化されているため、SiCインゴットI内にBPDが生じることが抑制されている。そのため、BPD密度の少ない良質なSiCインゴットIが得られる。 As described above, in the SiC ingot manufacturing method according to the present embodiment, since the atomic arrangement surface 2 of the SiC single crystal 1 used as the seed crystal is planarized, the occurrence of BPD in the SiC ingot I is suppressed. It is Therefore, a good quality SiC ingot I with a low BPD density is obtained.

最後に得られたSiCインゴットIをスライスしてSiCウェハを作製する。切断する方向は、<0001>に垂直または0~10°のオフ角をつけた方向に切断し、C面に平行、またはC面から0~10°オフ角をつけた面をもつウェハを作製する。ウェハの表面加工は、(0001)面側すなわちSi面側に鏡面加工を施してもよい。Si面は、通常エピタキシャル成長を行う面である。SiCインゴットIはBPDが少ないため、BPDの少ないSiCウェハを得ることができる。キラー欠陥であるBPDが少ないSiCウェハを用いることで、高品質なSiCエピタキシャルウェハを得ることができ、SiCデバイスの歩留りを高めることができる。 Finally, the obtained SiC ingot I is sliced to produce SiC wafers. The cutting direction is perpendicular to <0001> or in a direction with an off angle of 0 to 10° to produce a wafer with a plane parallel to the C plane or at an off angle of 0 to 10° from the C plane. do. The surface of the wafer may be mirror-finished on the (0001) plane side, that is, the Si plane side. The Si face is the face on which epitaxial growth is normally performed. Since the SiC ingot I has less BPD, a SiC wafer with less BPD can be obtained. By using a SiC wafer with less BPD, which is a killer defect, a high-quality SiC epitaxial wafer can be obtained, and the yield of SiC devices can be increased.

また坩堝100を加熱し原料Gを昇華させる際に、周方向の異方性が生じないように、坩堝100を回転させることが好ましい。回転速度は、0.1rpm以上とすることが好ましい。また成長時の成長面における温度変化は少なくすることが好ましい。 Moreover, when the crucible 100 is heated to sublimate the raw material G, it is preferable to rotate the crucible 100 so that anisotropy in the circumferential direction does not occur. The rotation speed is preferably 0.1 rpm or higher. Also, it is preferable to reduce the temperature change on the growth surface during growth.

以上、本発明の好ましい実施の形態について詳述したが、本発明は特定の実施の形態に限定されるものではなく、特許請求の範囲内に記載された本発明の要旨の範囲内において、種々の変形・変更が可能である。 Although the preferred embodiments of the present invention have been described in detail above, the present invention is not limited to specific embodiments, and various can be transformed or changed.

1 SiC単結晶
2,22 原子配列面
20 ウェハ
3 台座
3A 湾曲面
100 坩堝
101 コイル
102 テーパーガイド
200 製造装置
A 原子
I SiCインゴット
G 原料
1 SiC single crystal 2, 22 atomic arrangement surface 20 wafer 3 pedestal 3A curved surface 100 crucible 101 coil 102 taper guide 200 manufacturing apparatus A atom I SiC ingot G raw material

Claims (10)

SiC単結晶の原子配列面の湾曲量及び湾曲方向を少なくとも平面視中央を通る第1の方向と前記第1の方向と直交する第2の方向に沿って測定する測定工程と、
前記SiC単結晶の原子配列面と逆方向に湾曲する湾曲面を有する台座を準備する準備工程と、
前記原子配列面の湾曲方向と前記湾曲面の湾曲方向とが異なるように前記SiC単結晶と前記台座とを対向させて、貼りつける貼付工程と、を備えるSiC単結晶の貼合方法。
a measuring step of measuring the amount of curvature and the direction of curvature of an atomic arrangement plane of a SiC single crystal along at least a first direction passing through the center in plan view and a second direction orthogonal to the first direction;
a preparation step of preparing a pedestal having a curved surface curved in a direction opposite to the atomic arrangement surface of the SiC single crystal;
and a bonding step of bonding the SiC single crystal and the pedestal so that the direction of curvature of the atomic arrangement surface and the direction of curvature of the curved surface are different from each other.
前記原子配列面の湾曲量の絶対値と、前記台座の前記湾曲面の湾曲量の絶対値と、の差が、貼付面のいずれの箇所においても10μm以下である、請求項1に記載のSiC単結晶の貼合方法。 The SiC according to claim 1, wherein a difference between an absolute value of the amount of curvature of the atomic arrangement plane and an absolute value of the amount of curvature of the curved surface of the base is 10 µm or less at any point on the attachment surface. Single crystal lamination method. 前記原子配列面の曲率半径が28m以上である、請求項1又は2に記載のSiC単結晶の貼合方法。 3. The method of bonding SiC single crystals according to claim 1, wherein the radius of curvature of said atomic arrangement plane is 28 m or more. 前記SiC単結晶の直径が150mm以上の場合に、前記原子配列面の湾曲量の最大値が100μm以下である、請求項1~3のいずれか一項に記載のSiC単結晶の貼合方法。 4. The method for bonding SiC single crystals according to claim 1, wherein the maximum amount of curvature of the atomic arrangement plane is 100 μm or less when the SiC single crystal has a diameter of 150 mm or more. 前記貼付工程を行う際の前記SiC単結晶の厚みが5mm以下である、請求項1~4のいずれか一項に記載のSiC単結晶の貼合方法。 The SiC single crystal bonding method according to any one of claims 1 to 4, wherein the SiC single crystal has a thickness of 5 mm or less when performing the bonding step. 請求項1~5のいずれか一項に記載のSiC単結晶の貼合方法において、前記台座に貼り付けられた前記SiC単結晶を種結晶として結晶成長を行う、SiCインゴットの製造方法。 6. The method for manufacturing a SiC ingot according to claim 1, wherein said SiC single crystal bonded to said pedestal is used as a seed crystal for crystal growth. 前記台座と前記SiC単結晶との結晶成長温度における熱膨張係数の差が、0.3×10-6/℃以下である、請求項6に記載のSiCインゴットの製造方法。 7. The method for producing an SiC ingot according to claim 6, wherein a difference in thermal expansion coefficient between said pedestal and said SiC single crystal at a crystal growth temperature is 0.3×10 −6 /° C. or less. 貼りつけるSiC単結晶の貼付け面を下にしたとき、前記SiC単結晶の原子配列面の湾曲方向が凹面状の前記SiC単結晶を貼り付けるための台座であって、前記台座が凸面状に湾曲する湾曲面を備える、SiC単結晶成長用台座。 A pedestal for adhering the SiC single crystal to which the atomic arrangement plane of the SiC single crystal is curved in a concave direction when the adhering surface of the SiC single crystal to be adhered faces downward, the pedestal being curved in a convex shape. A pedestal for SiC single crystal growth, comprising a curved surface that 貼りつけるSiC単結晶の貼付け面を下にしたとき、前記SiC単結晶の原子配列面の湾曲方向が凸面状の前記SiC単結晶を貼り付けるための台座であって、前記台座が凹面状に湾曲する湾曲面を備える、SiC単結晶成長用台座。 A pedestal for adhering the SiC single crystal to which the atomic arrangement plane of the SiC single crystal is curved in a convex direction when the adhering surface of the SiC single crystal to be adhered faces downward, the pedestal being curved concavely. A pedestal for SiC single crystal growth, comprising a curved surface that 貼りつけるSiC単結晶の原子配列面の湾曲量の絶対値と、前記湾曲面の湾曲量の絶対値と、の差が、貼付面のいずれの箇所においても10μm以下である、請求項8又は9に記載のSiC単結晶成長用台座。 10. The difference between the absolute value of the amount of curvature of the atomic arrangement surface of the SiC single crystal to be attached and the absolute value of the amount of curvature of the curved surface is 10 μm or less at any point on the attached surface. The pedestal for SiC single crystal growth according to .
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