JP2018083733A - SiC SINGLE CRYSTAL GROWING METHOD, SiC SINGLE CRYSTAL GROWING APPARATUS, AND SiC SINGLE CRYSTAL INGOT - Google Patents
SiC SINGLE CRYSTAL GROWING METHOD, SiC SINGLE CRYSTAL GROWING APPARATUS, AND SiC SINGLE CRYSTAL INGOT Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 234
- 238000000034 method Methods 0.000 title abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims description 33
- 238000009434 installation Methods 0.000 claims description 30
- 238000002109 crystal growth method Methods 0.000 claims description 22
- 238000005530 etching Methods 0.000 abstract description 22
- 230000007547 defect Effects 0.000 abstract description 18
- 239000000126 substance Substances 0.000 abstract description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 87
- 229910010271 silicon carbide Inorganic materials 0.000 description 84
- 239000007789 gas Substances 0.000 description 18
- 230000002093 peripheral effect Effects 0.000 description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 229910003468 tantalcarbide Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000994 depressogenic effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
Abstract
Description
本発明は、ＳｉＣ単結晶成長方法、ＳｉＣ単結晶成長装置及びＳｉＣ単結晶インゴットに関する。 The present invention relates to a SiC single crystal growth method, a SiC single crystal growth apparatus, and a SiC single crystal ingot.
炭化珪素（ＳｉＣ）は、特徴的な特性を有する。例えば、シリコン（Ｓｉ）と比べて、絶縁破壊電界は１桁大きく、バンドギャップは３倍大きく、熱伝導率は３倍程度高い。そのため炭化珪素（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 characteristic properties. For example, compared to silicon (Si), the breakdown electric field is an order of magnitude larger, the band gap is three times larger, and the thermal conductivity is about three times higher. Therefore, silicon carbide (SiC) is expected to be applied to power devices, high frequency devices, high temperature operation devices, and the like.
近年、ＳｉＣエピタキシャルウェハの高品質化に伴い、ＳｉＣ単結晶インゴットの高品質化が求められている。ＳｉＣ単結晶インゴットは、ＳｉＣ単結晶を結晶成長させて得られる。結晶成長過程で、欠陥が混入しないようにする試みが検討されている。 In recent years, with the improvement in quality of SiC epitaxial wafers, there has been a demand for higher quality of SiC single crystal ingots. The SiC single crystal ingot is obtained by growing a SiC single crystal. Attempts have been made to prevent defects from entering during the crystal growth process.
欠陥は、結晶成長の初期に発生しやすい。炭素や不純物はシリコンより昇華しやすく、結晶成長初期においてガス雰囲気が安定しないためである。例えば、カーボン等が、局所的に析出すると、欠陥の原因となる。 Defects are likely to occur early in crystal growth. This is because carbon and impurities are more easily sublimated than silicon, and the gas atmosphere is not stable in the early stage of crystal growth. For example, when carbon or the like is locally deposited, it causes a defect.
そこで、特許文献１及び特許文献２には、結晶成長面を水素ガスでエッチングし、清浄化することで、高品質な炭化ケイ素単結晶を製造できることが記載されている。 Therefore, Patent Document 1 and Patent Document 2 describe that a high-quality silicon carbide single crystal can be manufactured by etching and cleaning the crystal growth surface with hydrogen gas.
また特許文献３には、坩堝内における種結晶の位置を変化させることで、種結晶の成長面をエッチングする方法が記載されている。 Patent Document 3 describes a method of etching a growth surface of a seed crystal by changing the position of the seed crystal in the crucible.
しかしながら、特許文献１及び２の方法では、坩堝内に水素ガスを導入する必要がある。そのため、水素ガスを導入するための配管を設ける等の必要があり、設備が大掛かりになる。また過剰な水素ガスは、炭素等で構成される坩堝の劣化の原因となりうる。 However, in the methods of Patent Documents 1 and 2, it is necessary to introduce hydrogen gas into the crucible. Therefore, it is necessary to provide piping for introducing hydrogen gas, and the facility becomes large. Excessive hydrogen gas can cause deterioration of a crucible made of carbon or the like.
また特許文献３の方法は、種結晶を大きく移動させる。そのため、坩堝内の原料ガスの流れが乱され、欠陥が混入する原因となりうる。また単結晶を大きく動かす必要や、温度を精密に制御する必要があり、実用的ではない。 Moreover, the method of patent document 3 moves a seed crystal largely. Therefore, the flow of the raw material gas in the crucible is disturbed, which can cause defects to be mixed. In addition, it is not practical because the single crystal needs to be moved greatly and the temperature must be precisely controlled.
本発明は上記問題に鑑みてなされたものであり、欠陥の少ないＳｉＣ単結晶を得ることができるＳｉＣ単結晶成長方法及びＳｉＣ単結晶成長装置を提供することを目的とする。またＳｉＣ単結晶成長装置及びＳｉＣ単結晶成長方法によって得られる特徴あるＳｉＣ単結晶インゴットを提供することを目的とする。 The present invention has been made in view of the above problems, and an object of the present invention is to provide an SiC single crystal growth method and an SiC single crystal growth apparatus capable of obtaining an SiC single crystal with few defects. It is another object of the present invention to provide a characteristic SiC single crystal ingot obtained by a SiC single crystal growth apparatus and a SiC single crystal growth method.
本発明者らは、鋭意検討の結果、加熱時の単結晶の温度を、結晶成長面と反対の裏面側で制御するという新たな方法を見出した。
すなわち、上記課題を解決するため、以下の手段を提供する。
As a result of intensive studies, the present inventors have found a new method in which the temperature of the single crystal during heating is controlled on the back side opposite to the crystal growth surface.
That is, in order to solve the above problems, the following means are provided.
（１）本発明の一態様にかかるＳｉＣ単結晶成長方法は、ＳｉＣ単結晶が結晶成長する成長面に対する裏面における、Ａｒより熱伝達性の高い熱伝達物質の接触状態を、結晶成長の過程において変化させる。 (1) In the SiC single crystal growth method according to one aspect of the present invention, a contact state of a heat transfer material having a higher heat transfer property than Ar on the back surface with respect to a growth surface on which the SiC single crystal grows is obtained in the process of crystal growth. Change.
（２）上記態様にかかるＳｉＣ単結晶成長方法において、前記ＳｉＣ単結晶の裏面と前記熱伝達物質との間に空間を形成し、前記ＳｉＣ単結晶と前記熱伝達物質とを非接触にする工程と、昇温中又は昇温後において、前記ＳｉＣ単結晶と前記熱伝達物質とを接触させる工程と、を有してもよい。 (2) In the SiC single crystal growth method according to the above aspect, a step of forming a space between the back surface of the SiC single crystal and the heat transfer material so that the SiC single crystal and the heat transfer material are not in contact with each other. And a step of bringing the SiC single crystal into contact with the heat transfer substance during or after the temperature rise.
（３）上記態様にかかるＳｉＣ単結晶成長方法において、前記非接触にする工程において、前記熱伝達物質と前記単結晶とを０．５ｍｍ以上離してもよい。 (3) In the SiC single crystal growth method according to the above aspect, in the non-contacting step, the heat transfer substance and the single crystal may be separated by 0.5 mm or more.
（４）本発明の一態様にかかるＳｉＣ単結晶成長装置は、原料を収納できる坩堝と、前記坩堝内において前記原料が設置される原料設置部と対向して配置され、内部に空間を有する単結晶設置部と、前記空間内を摺動できる熱伝達部と、を備え、前記熱伝達部は、前記単結晶設置部に設置される単結晶と接触する接触状態と、前記単結晶と非接触の非接触状態とを、前記空間内を摺動することにより切り替え可能である。 (4) An SiC single crystal growth apparatus according to an aspect of the present invention includes a crucible that can store a raw material, a raw material installation part in which the raw material is installed in the crucible, and a single unit having a space inside. A crystal installation part; and a heat transfer part that can slide in the space, wherein the heat transfer part is in contact with the single crystal installed in the single crystal installation part, and is not in contact with the single crystal. The non-contact state can be switched by sliding in the space.
（５）本発明の一態様にかかるＳｉＣ単結晶インゴットは、ＳｉＣ単結晶と、前記ＳｉＣ単結晶上に結晶成長した結晶成長領域とを有し、前記ＳｉＣ単結晶の中央部が、端部よりも凹んでいる。 (5) An SiC single crystal ingot according to an aspect of the present invention includes an SiC single crystal and a crystal growth region grown on the SiC single crystal, and a center portion of the SiC single crystal is formed from an end portion. Is also recessed.
本実施形態にかかるＳｉＣ単結晶成長装置及びＳｉＣ単結晶成長方法によれば、高品質なＳｉＣ単結晶インゴットを容易にえることができる。 According to the SiC single crystal growth apparatus and the SiC single crystal growth method according to the present embodiment, a high-quality SiC single crystal ingot can be easily obtained.
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、本実施形態の特徴をわかりやすくするために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、本実施形態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, the present embodiment will be described in detail with appropriate reference to the drawings. In the drawings used in the following description, in order to make the features of the present embodiment easier to understand, the features may be enlarged for the sake of convenience, and the dimensional ratios of the components are different from actual ones. There is. The materials, dimensions, and the like exemplified in the following description are merely examples, and the present embodiment is not limited to these, and can be appropriately modified and implemented without changing the gist thereof.
「ＳｉＣ単結晶成長装置」
図１は、本実施形態にかかるＳｉＣ単結晶成長装置の断面模式図である。図１に示すＳｉＣ単結晶成長装置１０は、坩堝１と、単結晶設置部２と、熱伝達部３と、を備える。図１では、理解を容易にするために、単結晶設置部２に単結晶Ｓを設置し、坩堝１内に原料Ｇを収納した状態を図示している。また単結晶設置部２と設置された原料Ｇとの間には、単結晶設置部２から設置された原料Ｇに向かって拡径する公知のテーパーガイド４を有してもよい。
"SiC single crystal growth equipment"
FIG. 1 is a schematic cross-sectional view of the SiC single crystal growth apparatus according to the present embodiment. An SiC single crystal growth apparatus 10 shown in FIG. 1 includes a crucible 1, a single crystal installation unit 2, and a heat transfer unit 3. In FIG. 1, for easy understanding, a state where the single crystal S is installed in the single crystal installation unit 2 and the raw material G is stored in the crucible 1 is illustrated. Further, a known taper guide 4 that increases in diameter toward the raw material G installed from the single crystal installation unit 2 may be provided between the single crystal installation unit 2 and the installed raw material G.
以下、坩堝１内において原料設置部と単結晶設置部２とを結ぶ方向であって、原料Ｇから単結晶Ｓに向かって原料ガスが昇華する方向をｚ方向と言うことがある。 Hereinafter, the direction in which the raw material installation part and the single crystal installation part 2 are connected in the crucible 1 and the raw material gas is sublimated from the raw material G toward the single crystal S may be referred to as the z direction.
坩堝１は、原料Ｇを収納する。原料Ｇを収納できれば、その形状は特に問わない。図１において、坩堝１の底部は原料設置部であり、原料Ｇを収納する。
坩堝１を構成する材料は、ＳｉＣ単結晶を作製する際に使用される公知のものを用いることができる。例えば、耐熱性を有するカーボン、炭化タンタル（ＴａＣ）等を用いる。
The crucible 1 stores the raw material G. The shape is not particularly limited as long as the raw material G can be stored. In FIG. 1, the bottom part of the crucible 1 is a raw material installation part for storing the raw material G.
As the material constituting the crucible 1, a known material used when producing a SiC single crystal can be used. For example, carbon having heat resistance, tantalum carbide (TaC), or the like is used.
単結晶設置部２は、坩堝１内で、設置される原料Ｇと対向する位置に配置される。原料Ｇと対向する位置に単結晶設置部２が設置されていることで、原料Ｇから昇華した原料ガスを効率的に単結晶設置部２に設置される単結晶Ｓへ供給できる。 The single crystal installation part 2 is arrange | positioned in the crucible 1 in the position facing the raw material G installed. Since the single crystal installation unit 2 is installed at a position facing the raw material G, the source gas sublimated from the raw material G can be efficiently supplied to the single crystal S installed in the single crystal installation unit 2.
また単結晶設置部２は、内部に空間を有する。「内部に空間を有する」とは、単結晶設置部２自体の内部に空洞を有していてもよいし、図１に示すように筒状の単結晶設置部２と坩堝１の内壁と、設置される単結晶Ｓとで空間を形成してもよい。 Moreover, the single crystal installation part 2 has a space inside. “Having a space inside” may have a cavity inside the single crystal installation part 2 itself, as shown in FIG. 1, a cylindrical single crystal installation part 2 and the inner wall of the crucible 1, A space may be formed with the single crystal S to be installed.
熱伝達部３は、単結晶設置部２内に形成された空間内を摺動する。摺動方向は、ｚ方向である。熱伝達部３の摺動方法は特に問わない。図１に示すように、熱伝達部３の一部を坩堝１から突出させ、その部分を利用して機械的に摺動させてもよい。
熱伝達部３は、空間内をｚ方向に摺動し、単結晶Ｓに対して熱伝達部３が接触した接触状態と、単結晶Ｓに対して熱伝達部３が非接触の非接触状態と、を切り替える。
The heat transfer unit 3 slides in a space formed in the single crystal installation unit 2. The sliding direction is the z direction. The sliding method of the heat transfer part 3 is not particularly limited. As shown in FIG. 1, a part of the heat transfer part 3 may be protruded from the crucible 1 and mechanically slid using the part.
The heat transfer unit 3 slides in the space in the z direction, and a contact state in which the heat transfer unit 3 is in contact with the single crystal S and a non-contact state in which the heat transfer unit 3 is not in contact with the single crystal S And switch.
熱伝達部３は、アルゴン（Ａｒ）より熱伝達性の高い熱伝達物質を含む。また熱伝達部３は、ＳｉＣ単結晶を製造する際の高温に対して耐熱性を有する必要がある。そのため、熱伝達物質として、例えば、炭化ケイ素（ＳｉＣ）、カーボン、炭化タンタル（ＴａＣ）等を用いることができる。 The heat transfer unit 3 includes a heat transfer material having a higher heat transfer property than argon (Ar). Moreover, the heat transfer part 3 needs to have heat resistance with respect to the high temperature at the time of manufacturing a SiC single crystal. Therefore, for example, silicon carbide (SiC), carbon, tantalum carbide (TaC), or the like can be used as the heat transfer substance.
「ＳｉＣ単結晶成長方法」
本実施形態にかかるＳｉＣ単結晶成長方法は、ＳｉＣ単結晶が結晶成長する成長面に対する裏面における、Ａｒより熱伝達性の高い熱伝達物質の接触状態を、結晶成長の過程において変化させながら行う方法である。
"SiC single crystal growth method"
The SiC single crystal growth method according to the present embodiment is a method in which the contact state of a heat transfer material having a higher heat transfer property than Ar is changed in the course of crystal growth on the back surface with respect to the growth surface on which the SiC single crystal grows. It is.
以下、上述のＳｉＣ単結晶成長装置１０の動作を説明すると共に、本実施形態にかかるＳｉＣ単結晶成長方法について具体的に説明する。 Hereinafter, the operation of the above-described SiC single crystal growth apparatus 10 will be described, and the SiC single crystal growth method according to the present embodiment will be specifically described.
まず、坩堝１内の原料設置部に原料Ｇを設置し、単結晶設置部２に結晶成長の核となる単結晶（種結晶）を設置する。原料Ｇは、焼結したＳｉＣ粉末原料を用いることができ、単結晶はＳｉＣ単結晶である。坩堝内に充填する雰囲気ガスとしては不活性ガスであるＡｒを用いることができる。 First, the raw material G is installed in the raw material installation part in the crucible 1, and the single crystal (seed crystal) serving as the nucleus of crystal growth is installed in the single crystal installation part 2. As the raw material G, a sintered SiC powder raw material can be used, and the single crystal is a SiC single crystal. Ar, which is an inert gas, can be used as the atmosphere gas filled in the crucible.
坩堝１を加熱すると、原料Ｇから原料ガスが昇華する。昇華した原料ガスは、テーパーガイド４に沿って、単結晶Ｓへ供給される。 When the crucible 1 is heated, the source gas is sublimated from the source G. The sublimated source gas is supplied to the single crystal S along the taper guide 4.
単結晶Ｓは、原料ガスが再結晶化することで成長する。結晶成長初期は、欠陥が生じやすい。例えば、ＳｉＣ粉末原料に含まれる不純物は、シリコンより昇華しやすい。結晶成長初期における原料ガスは、カーボンリッチな状態であり、成長表面からシリコンが抜けて、表面が炭化することがある。成長表面のカーボンは、ＳｉＣ単結晶の成長の様相を変え、欠陥を生み出す。そのため、結晶成長初期における欠陥の発生を制御することが求められる。 The single crystal S grows when the source gas is recrystallized. At the initial stage of crystal growth, defects are likely to occur. For example, impurities contained in the SiC powder raw material are more easily sublimated than silicon. The source gas at the initial stage of crystal growth is in a carbon-rich state, and silicon may escape from the growth surface and carbonize the surface. The carbon on the growth surface changes the growth of the SiC single crystal and creates defects. Therefore, it is required to control the generation of defects at the initial stage of crystal growth.
本実施形態では、結晶成長初期に発生する欠陥を単結晶Ｓの結晶成長面と反対側の裏面側から制御する。以下、図２を基に具体的に説明する。 In the present embodiment, defects occurring at the initial stage of crystal growth are controlled from the back side opposite to the crystal growth surface of the single crystal S. Hereinafter, a specific description will be given based on FIG.
図２は、本実施形態にかかるＳｉＣ単結晶成長方法における結晶成長状態を模式的に示した図である。図２（ａ）は、熱伝達物質を含む熱伝達部３と、単結晶Ｓの結晶成長面Ｓａと反対側の裏面Ｓｂと、が接触していない非接触状態であり、図２（ｂ）は、熱伝達物質を含む熱伝達部３と、単結晶Ｓの結晶成長面Ｓａと反対側の裏面Ｓｂと、が接触した接触状態である。図２において、原料ガスｇの流れと、熱の流れｔ１、ｔ２、ｔ３を矢印で図示する。 FIG. 2 is a diagram schematically showing a crystal growth state in the SiC single crystal growth method according to the present embodiment. FIG. 2A shows a non-contact state in which the heat transfer portion 3 containing the heat transfer material and the back surface Sb opposite to the crystal growth surface Sa of the single crystal S are not in contact with each other, and FIG. Is a contact state in which the heat transfer part 3 containing the heat transfer material and the back surface Sb opposite to the crystal growth surface Sa of the single crystal S are in contact with each other. In FIG. 2, the flow of the source gas g and the heat flows t1, t2, and t3 are shown by arrows.
図２（ａ）に示す非接触状態は、熱伝達部３と単結晶Ｓとの間に空間Ｋが形成されている。空間Ｋ内は、原料ガスを含むＡｒが充満しているため、熱伝達部３が接触している場合と比較して熱伝達率が低い。そのため、単結晶Ｓに蓄積された熱を効率的に逃がすことができず、単結晶Ｓは高温になる。単結晶Ｓが高温になると、単結晶Ｓの結晶成長面Ｓａにおいて原料ガスｇが再結晶化することができなくなると共に、その一部が昇華する。 In the non-contact state illustrated in FIG. 2A, a space K is formed between the heat transfer unit 3 and the single crystal S. Since the space K is filled with Ar containing the source gas, the heat transfer coefficient is lower than that in the case where the heat transfer unit 3 is in contact. Therefore, the heat accumulated in the single crystal S cannot be efficiently released, and the single crystal S becomes high temperature. When the single crystal S reaches a high temperature, the source gas g cannot be recrystallized on the crystal growth surface Sa of the single crystal S, and part of the gas sublimates.
これは単結晶Ｓ側の視点から見ると、単結晶Ｓの結晶成長面Ｓａがエッチングされたと換言できる。結晶成長初期の結晶成長面Ｓａをエッチングすると、結晶成長初期に発生する欠陥を除去することができ、得られる単結晶が高品質化する。このことは、例えば、先行文献１及び２等の水素を用いたエッチングにおいても確認されている。 From the viewpoint of the single crystal S side, this can be said that the crystal growth surface Sa of the single crystal S is etched. When the crystal growth surface Sa in the initial stage of crystal growth is etched, defects generated in the initial stage of crystal growth can be removed, and the resulting single crystal is improved in quality. This has also been confirmed, for example, in etching using hydrogen as described in Prior Documents 1 and 2.
非接触状態において、単結晶Ｓの裏面Ｓｂと熱伝達部３との距離は、０．５ｍｍ以上離すことが好ましい。０．５ｍｍ以上離すことで、熱の流れｔ２を十分抑制し、結晶成長面Ｓａをエッチングすることができる。０．１ｍｍ程度の距離の場合、熱の流れｔ２が十分抑制されず、中央付近のエッチングが不十分になる場合がある。単結晶Ｓの裏面Ｓｂと熱伝達部３との距離の上限は装置の構成により決めることができるが、駆動しやすい構造とするために１００ｍｍ以下とすることが好ましい。さらに単結晶Ｓの裏面Ｓｂと熱伝達部３との距離は、摺動距離を短くするために、１０ｍｍ以下とすることがより好ましい。 In the non-contact state, it is preferable that the distance between the back surface Sb of the single crystal S and the heat transfer unit 3 is 0.5 mm or more. By separating by 0.5 mm or more, the heat flow t2 can be sufficiently suppressed and the crystal growth surface Sa can be etched. When the distance is about 0.1 mm, the heat flow t2 may not be sufficiently suppressed, and etching near the center may be insufficient. The upper limit of the distance between the back surface Sb of the single crystal S and the heat transfer unit 3 can be determined by the configuration of the apparatus, but is preferably 100 mm or less in order to make the structure easy to drive. Furthermore, the distance between the back surface Sb of the single crystal S and the heat transfer part 3 is more preferably 10 mm or less in order to shorten the sliding distance.
エッチングされたエッチング面Ｓａ’の形状は、対向する原料Ｇに対して中央部が凹んだ凹面となる。単結晶Ｓは、単結晶設置部２と外周側で接触している。接触面を介して熱が流れるため、単結晶Ｓ内において中央側から外周側に向けた熱の流れｔ１が生まれる。一方で、単結晶Ｓの中央部において熱伝達部３に向けた熱の流れｔ２は抑制されている。その結果、単結晶Ｓ内で比較すると、中央部が高温で外周部が低温になる。つまり、単結晶Ｓの中央部のエッチングが進み、エッチング面Ｓａ’は凹面となる。 The shape of the etched etching surface Sa 'is a concave surface in which the central portion is recessed with respect to the opposite raw material G. The single crystal S is in contact with the single crystal installation part 2 on the outer peripheral side. Since heat flows through the contact surface, in the single crystal S, a heat flow t1 from the central side toward the outer peripheral side is generated. On the other hand, the heat flow t2 toward the heat transfer unit 3 is suppressed at the center of the single crystal S. As a result, when compared in the single crystal S, the central portion is hot and the outer peripheral portion is cold. That is, the etching of the central portion of the single crystal S proceeds and the etching surface Sa ′ becomes a concave surface.
一方で、非接触状態が続くと単結晶Ｓは結晶成長が進まない。そこで、図２（ｂ）に示すように、熱伝達部３を単結晶Ｓに向けて摺動し、単結晶Ｓの裏面Ｓｂと熱伝達部３とを接触させる。 On the other hand, if the non-contact state continues, the crystal growth of the single crystal S does not proceed. Therefore, as shown in FIG. 2B, the heat transfer unit 3 is slid toward the single crystal S, and the back surface Sb of the single crystal S and the heat transfer unit 3 are brought into contact with each other.
単結晶Ｓと熱伝達部３とが接触すると、単結晶Ｓから熱伝達部３へ向けた熱の流れｔ３が生まれる。熱が熱伝達部３に流れることにより、単結晶Ｓは原料ガスｇが再結晶化できる程度に冷却される。そして、単結晶Ｓのエッチング面Ｓａ’に単結晶が結晶成長する。 When the single crystal S and the heat transfer unit 3 come into contact, a heat flow t3 from the single crystal S to the heat transfer unit 3 is generated. When the heat flows to the heat transfer section 3, the single crystal S is cooled to such an extent that the source gas g can be recrystallized. Then, the single crystal grows on the etching surface Sa ′ of the single crystal S.
単結晶Ｓに供給される原料ガスｇの一部は、単結晶Ｓとテーパーガイド４との間を介して、対向する原料Ｇと反対側の後方側に流れる。そのため、単結晶Ｓの結晶成長は、単結晶Ｓの中央部が外周部よりも早くなる。このことは、通常単結晶Ｓを結晶成長させると、原料Ｇに向けて凸な結晶が得られることからも分かる。 Part of the raw material gas g supplied to the single crystal S flows to the rear side opposite to the facing raw material G through the space between the single crystal S and the taper guide 4. Therefore, the crystal growth of the single crystal S is faster at the central portion of the single crystal S than at the outer peripheral portion. This can also be seen from the fact that when the single crystal S is grown normally, a convex crystal toward the raw material G is obtained.
上述のように、非接触状態でエッチングされたエッチング面Ｓａ’は、対向する原料Ｇに対して凹面である。単結晶Ｓの結晶成長は、単結晶Ｓの中央部が外周部よりも早いため、エッチング面Ｓａ’の凹面形状を緩和するように結晶成長が進む。その結果、結晶成長を進めた後に得られる最終的な外周面Ｓｃが過剰に凸になることが抑制される。すなわち、単結晶Ｓ内に生じる歪を緩和し、欠陥等の発生を抑制できる。 As described above, the etching surface Sa ′ etched in the non-contact state is a concave surface with respect to the facing material G. Crystal growth of the single crystal S progresses so as to relax the concave shape of the etching surface Sa ′ because the central portion of the single crystal S is faster than the outer peripheral portion. As a result, the final outer peripheral surface Sc obtained after the crystal growth is prevented from being excessively convex. That is, the strain generated in the single crystal S can be relaxed and the occurrence of defects and the like can be suppressed.
上述のように、本実施形態にかかるＳｉＣ単結晶成長方法によれば、単結晶の結晶成長面をエッチングするか、単結晶の結晶成長面に結晶を成長させるかを自由に制御することができる。また、本実施形態にかかるＳｉＣ単結晶成長方法は、結晶成長の制御をＳｉＣ単結晶の結晶成長面に対する裏面側で制御するという新たな方法である。裏面側で制御するため、ＳｉＣ単結晶の結晶成長への影響も少ない。 As described above, according to the SiC single crystal growth method according to the present embodiment, it is possible to freely control whether the crystal growth surface of the single crystal is etched or the crystal is grown on the crystal growth surface of the single crystal. . The SiC single crystal growth method according to the present embodiment is a new method in which the crystal growth is controlled on the back side with respect to the crystal growth surface of the SiC single crystal. Since the control is performed on the back side, the influence on the crystal growth of the SiC single crystal is small.
また、本実施形態にかかるＳｉＣ単結晶成長装置は、水素等を導入するための配管設備等を整える必要が無い。そのため、本実施形態にかかるＳｉＣ単結晶成長装置によれば、簡便な設備で結晶成長状態を制御することができる。さらに、熱伝達部を摺動させるだけで、エッチング状態と結晶成長状態をスイッチングさせることができ、ＳｉＣ単結晶の結晶成長状態をより精密に制御できる。 In addition, the SiC single crystal growth apparatus according to the present embodiment does not need to prepare piping facilities or the like for introducing hydrogen or the like. Therefore, according to the SiC single crystal growth apparatus concerning this embodiment, a crystal growth state can be controlled with simple equipment. Furthermore, the etching state and the crystal growth state can be switched only by sliding the heat transfer part, and the crystal growth state of the SiC single crystal can be controlled more precisely.
ここまで、図１に示すように、熱伝達部３を単結晶Ｓに対して摺動させることで、単結晶Ｓと熱伝達部３（熱伝達物質）の接触状態を変化させる場合を例に説明した。ＳｉＣ単結晶成長方法は、当該方法に限られず、単結晶Ｓと熱伝達物質との接触、非接触の状態を別の手段で制御してもよい。 Up to this point, as shown in FIG. 1, the case where the contact state between the single crystal S and the heat transfer unit 3 (heat transfer material) is changed by sliding the heat transfer unit 3 with respect to the single crystal S is taken as an example. explained. The SiC single crystal growth method is not limited to this method, and the contact / non-contact state between the single crystal S and the heat transfer material may be controlled by another means.
図３は、本実施形態にかかるＳｉＣ単結晶成長方法における結晶成長状態の別の態様を模式的に示した図である。図３において、図２と同一の構成については、同一の符号を付している。 FIG. 3 is a diagram schematically showing another aspect of the crystal growth state in the SiC single crystal growth method according to the present embodiment. 3, the same components as those in FIG. 2 are denoted by the same reference numerals.
例えば、図３に示すように、単結晶設置部２の一部に開口部２Ａを設け、開口部２Ａを介して原料ガスｇが空間Ｋ内に流入できるようにする（図３（ａ）参照）。開口部２Ａを介して空間Ｋに流入した原料ガスｇは、空間Ｋ内に多結晶Ａを成長させる。その結果、空間Ｋが徐々に埋まっていき、多結晶Ａを介して、熱伝達状態を変化させることができる。 For example, as shown in FIG. 3, an opening 2A is provided in a part of the single crystal installation part 2 so that the source gas g can flow into the space K through the opening 2A (see FIG. 3A). ). The source gas g flowing into the space K through the opening 2 </ b> A causes the polycrystalline A to grow in the space K. As a result, the space K is gradually filled, and the heat transfer state can be changed through the polycrystal A.
なお、図３に示す場合は、接触状態と非接触状態をスイッチングすることは難しく、状態変化は１回のみとなる。しかしながら、状態変化が１回のみであっても、結晶成長初期のエッチングは可能であり、ＳｉＣ単結晶内の高品質化に寄与する。 In the case shown in FIG. 3, it is difficult to switch between a contact state and a non-contact state, and the state change is only once. However, even when the state changes only once, etching at the initial stage of crystal growth is possible, which contributes to high quality in the SiC single crystal.
（ＳｉＣ単結晶インゴット）
図４は、本実施形態にかかるＳｉＣ単結晶インゴットの断面図である。図４に示すＳｉＣインゴットＩは、ＳｉＣ単結晶（単結晶）Ｓと、ＳｉＣ単結晶（単結晶）Ｓ上に結晶成長した結晶成長領域Ｓｇとを有する。
(SiC single crystal ingot)
FIG. 4 is a cross-sectional view of the SiC single crystal ingot according to the present embodiment. The SiC ingot I shown in FIG. 4 has a SiC single crystal (single crystal) S and a crystal growth region Sg grown on the SiC single crystal (single crystal) S.
図４におけるＳｉＣインゴットＩにおいて、ＳｉＣ単結晶Ｓと、結晶成長領域Ｓｇとは窒素濃度が異なり、明確な界面が確認できる。またＳｉＣ単結晶Ｓと結晶成長領域Ｓｇとの窒素濃度等が近似している場合も、ＵＶ照射しながらＳｉＣインゴットの断面を見ることで、わずかな濃度差を強調してＳｉＣ単結晶Ｓの形状を確認できる。 In the SiC ingot I in FIG. 4, the SiC single crystal S and the crystal growth region Sg have different nitrogen concentrations, and a clear interface can be confirmed. In addition, even when the nitrogen concentration of the SiC single crystal S and the crystal growth region Sg is approximate, by looking at the cross section of the SiC ingot while irradiating with UV, a slight concentration difference is emphasized and the shape of the SiC single crystal S Can be confirmed.
図４に示すように、単結晶Ｓの中央部は、端部よりも凹んでいる。これは、本来の単結晶Ｓの結晶成長面Ｓａがエッチングにより後退し、エッチング面Ｓａ’となったためである。 As shown in FIG. 4, the center part of the single crystal S is dented rather than the edge part. This is because the crystal growth surface Sa of the original single crystal S is retreated by etching to become an etching surface Sa ′.
上述のように、中央部が端部よりも凹んだ単結晶Ｓの形状は、上述のＳｉＣ単結晶成長方法におけるエッチングによる独特のものである。 As described above, the shape of the single crystal S in which the central portion is recessed from the end portion is unique by etching in the above-described SiC single crystal growth method.
例えば、水素ガスエッチングの場合、単結晶Ｓに対して水素ガスが均一に供給されるため、結晶成長面Ｓａにおけるエッチング速度はほぼ均一である。すなわち、中央部が窪んだ形状にはならない。またエッチングを行わずに得られた種結晶も、フラット形状か、上述のように中央部が端部より突出した形状となる。さらに、加工により当該形状を得ようとしても、中央部が凹むように加工することは極めて難しい。
そのため、当該特徴を有する単結晶は、上述の単結晶成長装置又は単結晶成長方法によって作製されたものと推定される。
For example, in the case of hydrogen gas etching, since the hydrogen gas is uniformly supplied to the single crystal S, the etching rate on the crystal growth surface Sa is substantially uniform. That is, it does not become a shape in which the central part is depressed. Moreover, the seed crystal obtained without performing etching also has a flat shape or a shape in which the central portion protrudes from the end portion as described above. Furthermore, even if it is going to obtain the said shape by a process, it is very difficult to process so that a center part may be dented.
Therefore, it is presumed that the single crystal having the characteristics is manufactured by the above-described single crystal growth apparatus or single crystal growth method.
本実施形態にかかるＳｉＣインゴットＩは、結晶成長を進めた後に得られる最終的な外周面Ｓｃが過剰に凸になりにくい。すなわち、歪が少なく、高品質なＳｉＣインゴットとなる。また過剰に凸になっていないため、ウェハ上に加工した際の取れ効率が高くすることができる。 In the SiC ingot I according to the present embodiment, the final outer peripheral surface Sc obtained after the crystal growth proceeds is not likely to be excessively convex. That is, it becomes a high quality SiC ingot with little distortion. Moreover, since it is not excessively convex, it is possible to increase the removal efficiency when processed on a wafer.
また、図４では、成長中にドーピング量を調整することにより、結晶成長中の表面形状に対応するコントラストが見えている。結晶成長開始時は、非接触状態でエッチングされたため表面が凹面になっているが、結晶成長開始後は、凹面形状を緩和するように結晶成長が進み、徐々に凸形状に移行しているが、最終的な外周面の形状は過剰に凸になることが抑制されている。 In FIG. 4, the contrast corresponding to the surface shape during crystal growth can be seen by adjusting the doping amount during the growth. At the beginning of crystal growth, the surface is concave because it was etched in a non-contact state, but after crystal growth started, crystal growth progressed to relax the concave shape, and gradually shifted to a convex shape. The final shape of the outer peripheral surface is suppressed from being excessively convex.
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。 The preferred embodiments of the present invention have been described in detail above. However, the present invention is not limited to the specific embodiments, and various modifications can be made within the scope of the gist of the present invention described in the claims. Can be modified or changed.
（実施例１）
オフセット角が４°のＳｉＣ単結晶を坩堝内の単結晶設置部に設置した。この際、単結晶設置部と設置された単結晶との間には、空隙が形成されていた。単結晶設置部と単結晶の間の空隙の幅は、１ｍｍであった。
Example 1
A SiC single crystal having an offset angle of 4 ° was placed in the single crystal placement section in the crucible. At this time, voids were formed between the single crystal installation part and the installed single crystal. The width of the gap between the single crystal installation part and the single crystal was 1 mm.
そして、ＳｉＣ単結晶原料を坩堝内に封入し、坩堝の外周を２３５０℃まで加熱し、ＳｉＣ単結晶原料を昇華させた。そして、１００時間昇華を続け、ＳｉＣ単結晶を２ｃｍ結晶成長させ、ＳｉＣインゴットを作製した。 And the SiC single crystal raw material was enclosed in the crucible, the outer periphery of the crucible was heated to 2350 degreeC, and the SiC single crystal raw material was sublimated. Then, sublimation was continued for 100 hours, and a SiC single crystal was grown by 2 cm to produce a SiC ingot.
得られたＳｉＣインゴットを切断し、その断面を目視で確認した。その結果、単結晶設置部と単結晶の間の空隙が埋まっていることが確認できた。 The obtained SiC ingot was cut and the cross section was visually confirmed. As a result, it was confirmed that the gap between the single crystal installation part and the single crystal was filled.
また、得られたＳｉＣインゴットの貫通欠陥密度（個／ｃｍ２）は、エッチングにより強調された欠陥として顕微鏡を用いて測定した。測定した結果を表１に示す。 Moreover, the penetration defect density (pieces / cm 2 ) of the obtained SiC ingot was measured using a microscope as a defect emphasized by etching. The measured results are shown in Table 1.
（比較例１）
比較例１は、単結晶設置部と単結晶の間に空隙を設けなかった点が実施例１と異なる。その他の条件は、実施例１と同じとした。
そして、ＳｉＣ単結晶を２ｃｍ結晶成長させ、ＳｉＣインゴットを作製した。また、得られたＳｉＣインゴットの貫通欠陥密度（個／ｃｍ２）は、エッチングにより強調された欠陥として顕微鏡を用いて測定した。測定した結果を表１に示す。
(Comparative Example 1)
Comparative Example 1 is different from Example 1 in that no gap was provided between the single crystal installation part and the single crystal. Other conditions were the same as in Example 1.
Then, a SiC single crystal was grown by 2 cm to produce a SiC ingot. Moreover, the penetration defect density (pieces / cm 2 ) of the obtained SiC ingot was measured using a microscope as a defect emphasized by etching. The measured results are shown in Table 1.
表１に示すように、実施例１は、貫通欠陥密度の値が比較例１と比較して大幅に低減された。単結晶設置部と設置された単結晶との間に空隙を設けることにより、結晶成長の初期にＳｉＣ単結晶の結晶成長面がエッチングされ、清浄化されたためと考えられる。 As shown in Table 1, in Example 1, the value of the penetration defect density was significantly reduced as compared with Comparative Example 1. This is probably because the crystal growth surface of the SiC single crystal was etched and cleaned at the initial stage of crystal growth by providing a gap between the single crystal installation part and the installed single crystal.
１０…ＳｉＣ単結晶成長装置、１…坩堝、２…単結晶設置部、２Ａ…開口部、３…熱伝達部、４…テーパーガイド、Ｓ…単結晶、Ｓａ…結晶成長面、Ｓａ’…エッチング面、Ｓｂ…裏面、Ｓｃ…外周面、Ｇ…原料、ｇ…原料ガス、Ｋ…空間、ｔ１，ｔ２，ｔ３…熱の流れ、Ａ…多結晶、Ｉ…ＳｉＣインゴット DESCRIPTION OF SYMBOLS 10 ... SiC single crystal growth apparatus, 1 ... Crucible, 2 ... Single crystal installation part, 2A ... Opening part, 3 ... Heat transfer part, 4 ... Taper guide, S ... Single crystal, Sa ... Crystal growth surface, Sa '... Etching Surface, Sb ... Back surface, Sc ... Outer peripheral surface, G ... Raw material, g ... Raw material gas, K ... Space, t1, t2, t3 ... Heat flow, A ... Polycrystalline, I ... SiC ingot
Claims (5)
昇温中又は昇温後において、前記ＳｉＣ単結晶と前記熱伝達物質とを接触させる工程と、を有する請求項１に記載のＳｉＣ単結晶成長方法。 Forming a space between the back surface of the SiC single crystal and the heat transfer material, and making the SiC single crystal and the heat transfer material non-contact;
The SiC single crystal growth method according to claim 1, further comprising a step of bringing the SiC single crystal into contact with the heat transfer material during or after the temperature increase.
前記坩堝内において前記原料が設置される原料設置部と対向して配置され、内部に空間を有する単結晶設置部と、
前記空間内を摺動できる熱伝達部と、を備え、
前記熱伝達部は、前記単結晶設置部に設置される単結晶と接触する接触状態と、前記単結晶と非接触の非接触状態とを、前記空間内を摺動することにより切り替え可能である、ＳｉＣ単結晶成長装置。 A crucible capable of storing raw materials;
In the crucible, disposed opposite to the raw material installation part where the raw material is installed, a single crystal installation part having a space inside,
A heat transfer part capable of sliding in the space,
The heat transfer unit can switch between a contact state in contact with the single crystal installed in the single crystal installation unit and a non-contact state in non-contact with the single crystal by sliding in the space. SiC single crystal growth equipment.
前記ＳｉＣ単結晶の中央部が、端部よりも凹んでいるＳｉＣ単結晶インゴット。 Having a SiC single crystal and a crystal growth region grown on the SiC single crystal;
A SiC single crystal ingot in which a central portion of the SiC single crystal is recessed from an end portion.
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