JP2000053500A - METHOD AND DEVICE FOR GROWING SINGLE CRYSTAL SiC - Google Patents
METHOD AND DEVICE FOR GROWING SINGLE CRYSTAL SiCInfo
- Publication number
- JP2000053500A JP2000053500A JP10223301A JP22330198A JP2000053500A JP 2000053500 A JP2000053500 A JP 2000053500A JP 10223301 A JP10223301 A JP 10223301A JP 22330198 A JP22330198 A JP 22330198A JP 2000053500 A JP2000053500 A JP 2000053500A
- Authority
- JP
- Japan
- Prior art keywords
- sic
- single crystal
- atoms
- substrate
- pair
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000013078 crystal Substances 0.000 title claims abstract description 118
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000000758 substrate Substances 0.000 claims abstract description 56
- 238000010438 heat treatment Methods 0.000 claims abstract description 34
- 239000002131 composite material Substances 0.000 claims abstract description 18
- 125000004429 atom Chemical group 0.000 claims abstract description 15
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 15
- 230000006698 induction Effects 0.000 claims abstract description 10
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 9
- 239000011261 inert gas Substances 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 238000010030 laminating Methods 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 238000009395 breeding Methods 0.000 claims description 3
- 230000001488 breeding effect Effects 0.000 claims description 2
- 238000007740 vapor deposition Methods 0.000 claims 1
- 229910010271 silicon carbide Inorganic materials 0.000 abstract description 81
- 229910021431 alpha silicon carbide Inorganic materials 0.000 abstract description 16
- 239000012535 impurity Substances 0.000 abstract description 13
- 230000007547 defect Effects 0.000 abstract description 12
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 6
- 238000002230 thermal chemical vapour deposition Methods 0.000 abstract description 6
- 229910052710 silicon Inorganic materials 0.000 abstract description 5
- 230000008707 rearrangement Effects 0.000 abstract description 4
- 238000011109 contamination Methods 0.000 abstract description 3
- 238000000354 decomposition reaction Methods 0.000 abstract description 3
- 238000009792 diffusion process Methods 0.000 abstract description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 61
- 239000000463 material Substances 0.000 description 13
- 239000004065 semiconductor Substances 0.000 description 6
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 5
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000000815 Acheson method Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000000859 sublimation Methods 0.000 description 2
- 230000008022 sublimation Effects 0.000 description 2
- 240000001417 Vigna umbellata Species 0.000 description 1
- 235000011453 Vigna umbellata Nutrition 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000005092 sublimation method Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
- Recrystallisation Techniques (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、単結晶ＳｉＣの育
成方法及びその装置に関するもので、詳しくは、発光ダ
イオードやＸ線光学素子、高温半導体電子素子の基板ウ
エハなどとして用いられる単結晶ＳｉＣの育成方法及び
育成装置に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method and an apparatus for growing single crystal SiC, and more particularly, to a method for growing single crystal SiC used as a substrate wafer for a light emitting diode, an X-ray optical element, a high-temperature semiconductor electronic element, or the like. The present invention relates to a breeding method and a breeding apparatus.
【０００２】[0002]
【従来の技術】ＳｉＣ（炭化珪素）は、耐熱性および機
械的強度に優れているだけでなく、放射線にも強く、さ
らに不純物の添加によって電子や正孔の価電子制御が容
易である上、広い禁制帯幅を持つ（因みに、６Ｈ型のＳ
ｉＣ単結晶で約３．０ｅＶ、４Ｈ型のＳｉＣ単結晶で
３．２６ｅＶ）ために、Ｓｉ（シリコン）やＧａＡｓ
（ガリウムヒ素）などの既存の半導体材料では実現する
ことができない高温、高周波、耐電圧、耐環境性を実現
することが可能で、次世代のパワーデバイス用半導体材
料として注目され、かつ期待されている。2. Description of the Related Art SiC (silicon carbide) is not only excellent in heat resistance and mechanical strength, but also resistant to radiation. In addition, it is easy to control valence electrons and holes by adding impurities. Has a wide forbidden band (By the way, 6H type S
about 3.0 eV for an iC single crystal and 3.26 eV for a 4H type SiC single crystal), such as Si (silicon) or GaAs.
(Gallium arsenide) and other high-temperature, high-frequency, withstand voltage, and environmental resistance that cannot be realized with existing semiconductor materials. I have.
【０００３】この種の単結晶ＳｉＣの育成方法として、
従来、黒鉛るつぼ内の低温側に種結晶を固定配置し、高
温側に原料となるＳｉＣ粉体を挿入配置して黒鉛るつぼ
内を不活性雰囲気中で２１００〜２４００℃まで加熱す
ることによって、上記ＳｉＣ粉体から昇華したＳｉＣガ
スを閉鎖空間内で拡散輸送させて低温に設定されている
種結晶の表面上で再結晶させて単結晶の育成を行なうを
る昇華再結晶法（改良レーリー法）や、アチソン法ある
いは昇華法によって得られたＳｉＣ基板上に、１８５０
℃以上の基板温度で化学気相成長法（ＣＶＤ法）を用い
てエピタキシャル成長させることにより立方晶のＳｉＣ
単結晶（β−ＳｉＣ）を育成させる高温ＣＶＤエピタキ
シャル法等が知られている。As a method for growing this kind of single crystal SiC,
Conventionally, a seed crystal is fixedly arranged on the low-temperature side in a graphite crucible, and SiC powder as a raw material is inserted and arranged on the high-temperature side, and the inside of the graphite crucible is heated to 2100 to 2400 ° C. in an inert atmosphere, whereby Sublimation recrystallization method (improved Rayleigh method) in which SiC gas sublimated from SiC powder is diffused and transported in a closed space and recrystallized on the surface of a seed crystal set at a low temperature to grow a single crystal. Or 1850 on a SiC substrate obtained by the Acheson method or the sublimation method.
Cubic SiC by epitaxial growth using a chemical vapor deposition (CVD) method at a substrate temperature of at least
A high-temperature CVD epitaxial method for growing a single crystal (β-SiC) is known.
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、上記し
た従来の製造方法のうち、昇華再結晶法（改良レーリー
法）にあっては、単結晶の大形化に困難を伴うばかりで
なく、結晶成長の過程で黒鉛るつぼ内の種結晶周辺の環
境が変化するために、不純物等が混入しやすくて高純度
雰囲気及び種結晶側と原料のＳｉＣ粉体側との所定の温
度差を保つことが困難であり、混入した不純物や熱に起
因する歪みの影響で結晶欠陥やマイクロパイプ欠陥等が
発生しやすく、性能的にも品質的にも安定した単結晶が
得られないという問題がある。また、高温ＣＶＤエピタ
キシャル法は、基板温度が高いために再蒸発量も多く、
高純度の還元性雰囲気を作ることも必要で設備的に非常
に困難であり、さらに、エピタキシャル成長のため結晶
成長速度にも自ずと限界があって、単結晶ＳｉＣの生産
性が低く、生産コストが非常に高価なものになるという
問題があり、このことが既述のようにＳｉやＧａＡｓな
どの既存の半導体材料に比べて多くの優れた特徴を有し
ながらも、その実用化を阻止する要因になっている。However, of the above-mentioned conventional production methods, the sublimation recrystallization method (improved Rayleigh method) involves not only difficulty in increasing the size of a single crystal, but also crystal growth. The environment around the seed crystal in the graphite crucible changes during the process, and it is difficult to maintain a high-purity atmosphere and a predetermined temperature difference between the seed crystal side and the raw material SiC powder side because impurities and the like are easily mixed. However, there is a problem that crystal defects, micropipe defects, and the like are likely to occur due to the influence of impurities and heat-induced distortion, and that a single crystal with stable performance and quality cannot be obtained. In the high-temperature CVD epitaxial method, the amount of re-evaporation is large because the substrate temperature is high.
It is also necessary to create a high-purity reducing atmosphere, which makes it extremely difficult in terms of equipment. In addition, the crystal growth rate is naturally limited due to the epitaxial growth, so that the productivity of single-crystal SiC is low and the production cost is extremely low. However, as described above, it has many excellent features as compared with existing semiconductor materials such as Si and GaAs, but is a factor that hinders its practical use. Has become.
【０００５】本発明は上記実情に鑑みてなされたもの
で、成長過程での不純物の混入及び熱歪みの影響による
結晶欠陥やマイクロパイプ欠陥等の発生がなく、非常に
高品質高性能で、かつ、大型の単結晶ＳｉＣを生産性よ
く育成することができ、半導体材料としての実用化を促
進できる単結晶ＳｉＣの育成方法及びその装置を提供す
ることを目的としている。The present invention has been made in view of the above circumstances, and has no crystal defects or micropipe defects due to the contamination of impurities and the influence of thermal distortion during the growth process, and has very high quality and high performance. It is an object of the present invention to provide a single crystal SiC growing method and apparatus capable of growing large single crystal SiC with high productivity and promoting practical use as a semiconductor material.
【０００６】[0006]
【課題を解決するための手段】上記目的を達成するため
に、請求項１に記載の発明に係る単結晶ＳｉＣの育成方
法は、一対の熱盤間に、ＳｉＣ単結晶基板とＳｉ原子及
びＣ原子により構成された多結晶板とを積層してなる複
合体を挟み込み保持させるとともに、不活性ガス雰囲気
中で、かつ、ＳｉＣ飽和蒸気雰囲気下で上記一対の熱盤
の加熱温度を上記多結晶板側が高温、ＳｉＣ単結晶基板
側が低温となるように各別に制御することにより、上記
多結晶板のＳｉ原子及びＣ原子を上記ＳｉＣ単結晶基板
の表面で再配列させてＳｉＣ単結晶基板の結晶方位に倣
った単結晶を一体に育成させることを特徴とするもので
あり、また、請求項４に記載の発明に係る単結晶ＳｉＣ
の育成装置は、ＳｉＣ単結晶基板とＳｉ原子及びＣ原子
により構成された多結晶板とを積層してなる複合体を挟
み込み保持可能な一対の熱盤と、これら一対の熱盤の加
熱温度を各別に制御可能な高周波誘導加熱コイルとを備
え、上記一対の熱盤間に複合体を挟み込み保持させると
ともに、不活性ガス雰囲気中で、かつ、ＳｉＣ飽和蒸気
雰囲気下で、高周波誘導加熱コイルを介して一対の熱盤
の加熱温度を多結晶板側が高温、ＳｉＣ単結晶基板側が
低温となるように制御することによって上記多結晶板の
Ｓｉ原子及びＣ原子を上記ＳｉＣ単結晶基板の表面で再
配列させてＳｉＣ単結晶基板の結晶方位に倣った単結晶
を一体に育成可能に構成したことを特徴とするものであ
る。According to a first aspect of the present invention, there is provided a method for growing a single crystal SiC, comprising the steps of: A composite formed by laminating a polycrystalline plate composed of atoms is sandwiched and held, and the heating temperature of the pair of hot plates is increased in an inert gas atmosphere and in a SiC saturated vapor atmosphere by the polycrystalline plate. By individually controlling the temperature of the SiC single crystal substrate side to be high and the temperature of the SiC single crystal substrate side to be low, the Si atoms and C atoms of the polycrystalline plate are rearranged on the surface of the SiC single crystal substrate, and the crystal orientation of the SiC single crystal substrate is controlled. A single crystal according to the invention according to claim 4, characterized in that a single crystal following the pattern is grown integrally.
Is a pair of hot plates capable of sandwiching and holding a composite formed by laminating a SiC single crystal substrate and a polycrystalline plate composed of Si atoms and C atoms, and a heating temperature of the pair of hot plates. A high-frequency induction heating coil which can be controlled separately. The composite is sandwiched and held between the pair of hot plates, and is passed through the high-frequency induction heating coil in an inert gas atmosphere and in a SiC saturated steam atmosphere. By controlling the heating temperature of the pair of hot plates so that the polycrystalline plate side has a high temperature and the SiC single crystal substrate side has a low temperature, Si atoms and C atoms of the polycrystalline plate are rearranged on the surface of the SiC single crystal substrate. Thus, a single crystal following the crystal orientation of the SiC single crystal substrate can be integrally grown.
【０００７】上記のような構成要件を有する請求項１及
び請求項４に記載の発明によれば、ＳｉＣ単結晶基板と
Ｓｉ原子及びＣ原子により構成された多結晶板とを積層
してなる複合体を挟み込み保持する一対の熱盤の加熱温
度を各別に制御することによって、基板側と多結晶板側
との間で必要な温度差の確保や結晶成長過程で周辺環境
温度が変化したときの温度コントロールなど所定の単結
晶育成にとって最も重要不可欠な要素となる温度条件を
容易に、かつ、微細に調整し保持することが可能であ
り、これによって、周辺環境温度の変化や多結晶板及び
ＳｉＣ単結晶基板の性状のばらつきにかかわらず、両者
の界面をＳｉ原子及びＣ原子の分解拡散並びにそれら原
子のＳｉＣ単結晶基板表面での再配列による単結晶化に
適した温度状態に維持して熱変化に起因する歪みの影響
でマイクロパイプ欠陥が生じることを防止できる。ま
た、ＳｉＣ飽和蒸気雰囲気下での熱処理によって、Ｓｉ
の外部放出によるやせ細り及び周辺雰囲気から界面への
不純物の混入も防止して不純物の混入に起因する結晶欠
陥等の発生もなくすることができ、これによって、高純
度、高品質で、かつ、量的にも大型の単結晶を安定よく
育成させることが可能である。[0007] According to the first and fourth aspects of the present invention having the above constitutional requirements, a composite formed by laminating a SiC single crystal substrate and a polycrystalline plate composed of Si atoms and C atoms. By separately controlling the heating temperature of a pair of hot plates that sandwich and hold the body, it is possible to secure the necessary temperature difference between the substrate side and the polycrystalline plate side, and when the surrounding environmental temperature changes during the crystal growth process. It is possible to easily and finely adjust and maintain temperature conditions, which are the most important elements for growing a given single crystal, such as temperature control, thereby changing the surrounding environmental temperature, polycrystalline plate and SiC. Irrespective of the variation in the properties of the single crystal substrate, the interface between them is maintained at a temperature suitable for the decomposition and diffusion of Si atoms and C atoms and the rearrangement of these atoms on the surface of the SiC single crystal substrate for single crystallization. It is possible to prevent the micropipe defects caused by the effect of the distortion due to thermal changes to. In addition, heat treatment in a SiC saturated steam
Thinning due to external release of the metal and the intrusion of impurities from the surrounding atmosphere into the interface can be prevented, and the occurrence of crystal defects and the like due to the incorporation of impurities can be prevented. Particularly, a large single crystal can be stably grown.
【０００８】上記請求項１に記載の発明に係る単結晶Ｓ
ｉＣの育成方法において、多結晶板としては、請求項２
に記載のように、ＳｉＣ多結晶板、ＳｉＣアモルファス
もしくは高純度ＳｉＣ焼結体のいずれを使用してもよい
が、そのうち特に、請求項３に記載のように、ＳｉＣ単
結晶基板表面への熱化学的蒸着法（以下、熱ＣＶＤ法と
称する）により板状に成膜されたものを使用する場合
は、多結晶板自体が不純物の少ない高純度なものである
ことから、界面に結晶粒界などが形成されず、より高純
度、高品質な単結晶ＳｉＣを得ることができる。[0008] The single crystal S according to the first aspect of the present invention.
In the method of growing iC, the polycrystalline plate may be a polycrystalline plate.
As described in the above, any one of a SiC polycrystalline plate, a SiC amorphous or a high-purity SiC sintered body may be used, and particularly, as described in claim 3, the heat applied to the surface of the SiC single crystal substrate. In the case of using a film formed in a plate shape by a chemical vapor deposition method (hereinafter, referred to as a thermal CVD method), since the polycrystalline plate itself has high purity with few impurities, a crystal grain boundary is formed at an interface. Thus, single crystal SiC of higher purity and higher quality can be obtained.
【０００９】また、上記請求項４に記載の発明に係る単
結晶ＳｉＣの育成装置において、一対の熱盤の構成材料
としては、単結晶化のための加熱温度（２１００〜２３
００℃）に十分に耐える耐熱温度の高い材料、例えば焼
結カーボンやセラミックスなどが考えられるが、特に、
請求項５に記載のように、焼結カーボンから構成する場
合は、材料コストが安い上に製作も容易で、装置全体の
低廉化が図れる。In the apparatus for growing single crystal SiC according to the fourth aspect of the present invention, as a constituent material of the pair of hot plates, a heating temperature (2100-23) for single crystallization is used.
(00 ° C.), a material having a high heat resistance enough to withstand such as sintered carbon and ceramics can be considered.
According to the fifth aspect of the present invention, when made of sintered carbon, the material cost is low, the production is easy, and the entire apparatus can be reduced in cost.
【００１０】[0010]
【発明の実施の形態】以下、本発明の実施の形態を図面
にもとづいて説明する。図１は本発明に係る単結晶Ｓｉ
Ｃの育成に際して使用される複合体３の説明図であり、
この実施の形態では、ＳｉＣ単結晶基板として、アチソ
ン法により作られたα−ＳｉＣ単結晶塊（図示省略）か
ら切り出された平板状の六方晶系（６Ｈ型）のα−Ｓｉ
Ｃ単結晶基板１を使用し、このα−ＳｉＣ単結晶基板１
のＣ軸方向の（０００１）面１ａ上に、熱ＣＶＤ法によ
り約１ｍｍ厚さのβ−ＳｉＣ多結晶板２を成膜し、その
β−ＳｉＣ多結晶板２の表面２ａを表面粗度３Ｓ程度に
平らに研削したものである。Embodiments of the present invention will be described below with reference to the drawings. FIG. 1 shows a single crystal Si according to the present invention.
FIG. 3 is an explanatory diagram of a composite 3 used for growing C;
In this embodiment, a flat hexagonal (6H type) α-Si cut out from an α-SiC single crystal mass (not shown) formed by the Acheson method is used as a SiC single crystal substrate.
Using the C-single-crystal substrate 1, the α-SiC single-crystal substrate 1
A β-SiC polycrystalline plate 2 having a thickness of about 1 mm is formed on the (0001) plane 1a in the C-axis direction by a thermal CVD method, and the surface 2a of the β-SiC polycrystalline plate 2 has a surface roughness of 3S. It has been ground flat to a degree.
【００１１】図２は本発明に係る単結晶ＳｉＣの育成装
置を示す概略構成図であり、この育成装置１０は、上記
図１に示すような複合体３を挟み込み保持可能で、その
挟み込み状態でβ−ＳｉＣ多結晶板２の平らな表面（上
面）２ａ及びα−ＳｉＣ単結晶基板１の裏面（下面）１
ｂに密着可能な平滑面４ａ，５ａ及び外方へ突出する円
柱状部４ｂ，５ｂを有する上下一対の熱盤４，５と、こ
れら一対の熱盤４，５における突出円柱状部４ｂ，５ｂ
の外周面に螺旋状に巻回され高周波電源１１，１２に接
続されて高周波電力の通電量調整によって一対の熱盤
４，５の加熱温度を各別に制御可能とされた高周波誘導
加熱コイル６，７とを備えている。FIG. 2 is a schematic diagram showing a single crystal SiC growing apparatus according to the present invention. The growing apparatus 10 can sandwich and hold the composite 3 as shown in FIG. Flat surface (upper surface) 2a of β-SiC polycrystalline plate 2 and back surface (lower surface) 1 of α-SiC single crystal substrate 1
b, and a pair of upper and lower heating plates 4 and 5 having smooth surfaces 4a and 5a that can be in close contact with b and cylindrical portions 4b and 5b protruding outward, and projecting cylindrical portions 4b and 5b of the pair of heating plates 4 and 5.
The high-frequency induction heating coils 6, which are helically wound around the outer peripheral surfaces of the pair and connected to the high-frequency power supplies 11 and 12 so that the heating temperatures of the pair of heating plates 4 and 5 can be individually controlled by adjusting the amount of high-frequency power supplied. 7 is provided.
【００１２】上記構成の単結晶ＳｉＣ育成装置１０にお
ける一対の熱盤４，５間に、上記複合体３の複数個（図
２では２個の複合体３で示すが、単数であっても、３個
以上であってもよい）を、α−ＳｉＣ単結晶基板１が下
部の熱盤５側に位置するように挟み込み保持させるとと
もに、複合体３の周囲に小豆ぐらいの大きさのＳｉＣ塊
８…を取り囲み配置する。なお、上記一対の熱盤４，５
間の外周部はＳｉＣ等の耐熱性の壁材９で囲繞されてお
り、この壁材９と一対の熱盤４，５とにより単結晶育成
空間Ｓが構成されている。In the single crystal SiC growing apparatus 10 having the above structure, a plurality of the composites 3 (two composites 3 are shown in FIG. Three or more) may be sandwiched and held so that the α-SiC single-crystal substrate 1 is positioned on the lower hot platen 5 side, and the SiC mass 8 about the size of red beans is surrounded around the complex 3. ... is arranged. In addition, the pair of hot plates 4,5
The outer peripheral portion therebetween is surrounded by a heat-resistant wall material 9 such as SiC, and the wall material 9 and a pair of heating plates 4 and 5 form a single crystal growing space S.
【００１３】この状態で、Ａｒなどの不活性ガス気流を
育成空間Ｓ内に注入するとともに、高周波誘導加熱コイ
ル６，７への高周波電力の通電に伴う高周波誘導加熱に
よって上部の熱盤４が２２００℃、下部の熱盤５が２１
５０℃で、α−ＳｉＣ単結晶基板１とβ−ＳｉＣ多結晶
板２との間に約５０℃の温度差がつくように１時間かけ
て平均速度で昇温させ、かつ、その加熱温度で２時間程
度保持させた後、放冷させるといったように、不活性ガ
ス雰囲気中で、かつ、ＳｉＣ飽和蒸気雰囲気下で熱処理
を施すことにより、β−ＳｉＣ多結晶板２からＳｉ原子
及びＣ原子を分解拡散させるとともに、それら拡散した
Ｓｉ原子及びＣ原子を低温側のα−ＳｉＣ単結晶基板１
の表面で該α−ＳｉＣ単結晶基板１の結晶方位に倣って
再配列させて図３に示すように、β−ＳｉＣ多結晶板２
の存在箇所にα−ＳｉＣ単結晶基板１の単結晶部分１´
と一体化されたα−６Ｈ−ＳｉＣ単結晶部分２´を育成
し、所定の単結晶ＳｉＣ（製品）１３を得ることができ
る。In this state, a flow of an inert gas such as Ar is injected into the growth space S, and the upper heating platen 4200 is formed by high-frequency induction heating accompanying the supply of high-frequency power to the high-frequency induction heating coils 6 and 7. ℃, the lower heating plate 5 is 21
At 50 ° C., the temperature is raised at an average rate over one hour so that a temperature difference of about 50 ° C. is obtained between the α-SiC single crystal substrate 1 and the β-SiC polycrystalline plate 2. After holding for about 2 hours, by performing a heat treatment in an inert gas atmosphere and in a SiC saturated vapor atmosphere such as cooling, Si atoms and C atoms are removed from the β-SiC polycrystalline plate 2. While decomposing and diffusing, the diffused Si and C atoms are converted to the low temperature side α-SiC single crystal substrate 1.
On the surface of the substrate, the β-SiC polycrystalline plate 2 is rearranged in accordance with the crystal orientation of the α-SiC single crystal substrate 1 as shown in FIG.
In the single crystal part 1 ′ of the α-SiC single crystal substrate 1
A single crystal SiC (product) 13 can be obtained by growing the α-6H—SiC single crystal portion 2 ′ integrated with the above.
【００１４】上記のように、高周波誘導加熱コイル６，
７への高周波電力の通電量調整に伴い複合体３を挟み込
み保持する一対の熱盤４，５の加熱温度を各別に制御す
ることによって、α−ＳｉＣ単結晶基板１とβ−ＳｉＣ
多結晶板２との間に約５０℃程度の温度差を確保し、か
つ、結晶成長過程で周辺環境温度が変化したときも同様
にそれぞれの加熱温度を各別にコントロールすることに
よって、周辺環境温度の変化やβ−ＳｉＣ多結晶板２及
びα−ＳｉＣ単結晶基板１の性状のばらつきにかかわら
ず、両者の界面をＳｉ原子及びＣ原子の分解拡散並びに
それら原子のα−ＳｉＣ単結晶基板１表面での再配列に
適した温度状態に維持することが可能である。また、複
合体３の周囲に小豆ぐらいの大きさのＳｉＣ塊８…を取
り囲み配置してＳｉＣの飽和蒸気雰囲気下で熱処理する
ことにより、α−ＳｉＣ単結晶基板１及びβ−ＳｉＣ多
結晶板３からのＳｉの放出が抑制されて、α−ＳｉＣ単
結晶基板１及びβ−ＳｉＣ多結晶板３のやせ細りが防止
されると共に、雰囲気から界面への不純物の混入も防止
されるので、結晶成長の途中で、その中に取り込まれる
不純物や熱に起因する歪みによってマイクロパイプ欠陥
や格子欠陥等が発生することもなくなり、高純度、高品
質で、かつ、量的にも安定した大型の単結晶を効率よく
育成することが可能である。As described above, the high-frequency induction heating coils 6
By controlling the heating temperature of the pair of heating plates 4 and 5 for sandwiching and holding the complex 3 in accordance with the adjustment of the amount of high-frequency power supplied to the α-SiC single crystal substrate 1 and the β-SiC
By maintaining a temperature difference of about 50 ° C. between the polycrystalline plate 2 and the surrounding environment temperature during the crystal growth process, similarly controlling each heating temperature separately, Irrespective of the variation of the properties of the β-SiC polycrystalline plate 2 and the α-SiC single crystal substrate 1, the decomposition and diffusion of Si atoms and C atoms and the surface of the α-SiC single crystal substrate 1 It is possible to maintain a temperature state suitable for rearrangement in the above. .. Around the composite 3 and heat-treated in a saturated steam atmosphere of SiC to obtain the α-SiC single crystal substrate 1 and the β-SiC polycrystal plate 3. Release of Si from the substrate and the thinning of the α-SiC single crystal substrate 1 and the β-SiC polycrystalline plate 3 are prevented, and the intrusion of impurities from the atmosphere to the interface is also prevented. In the middle, micropipe defects and lattice defects do not occur due to distortions caused by impurities or heat introduced therein, and high-purity, high-quality, and quantitatively stable large single crystals are produced. It is possible to grow efficiently.
【００１５】特に、上記実施の形態のように、一対の熱
盤４，５間に複数個の複合体３を挟み込み保持させて複
数の単結晶育成を同時に行なうことによって、所定の単
結晶育成による単結晶ＳｉＣ（製品）の生産性向上を図
ることができる。In particular, as in the above embodiment, a plurality of composites 3 are sandwiched and held between a pair of hot plates 4 and 5, and a plurality of single crystals are grown at the same time. The productivity of single crystal SiC (product) can be improved.
【００１６】なお、上記実施の形態では、上記α−Ｓｉ
Ｃ単結晶基板１として６Ｈ型のものを用いたが、４Ｈ型
のものを使用してもよい。In the above embodiment, the α-Si
Although a 6H type substrate is used as the C single crystal substrate 1, a 4H type substrate may be used.
【００１７】また、上記実施の形態では、Ｓｉ原子及び
Ｃ原子により構成される多結晶板として、熱ＣＶＤ法に
より成膜されるβ−ＳｉＣ多結晶板３を用いたもので説
明したが、これに代えて、高純度（１０14atm ／ｃｍ3
以下）のＳｉＣアモルファス板、高純度ＳｉＣ焼結体を
熱ＣＶＤ法による成膜手段でなく、単なる積層手段で使
用しても、上記と同様な高純度、高品質の単結晶ＳｉＣ
を得ることが可能である。In the above-described embodiment, the description has been given of the case where the β-SiC polycrystalline plate 3 formed by the thermal CVD method is used as the polycrystalline plate composed of Si atoms and C atoms. Instead of high purity (10 14 atm / cm 3
The following high purity and high quality single-crystal SiC can be obtained by using the SiC amorphous plate and the high-purity SiC sintered body described above in a simple laminating means instead of a film forming means by a thermal CVD method.
It is possible to obtain
【００１８】[0018]
【発明の効果】以上のように、請求項１及び請求項４に
記載の発明によれば、ＳｉＣ単結晶基板と多結晶板とを
積層してなる複合体を挟み込み保持する一対の熱盤の加
熱温度を各別に制御することにより、基板側と多結晶板
側との間で必要な温度差を確保できるとともに、結晶成
長過程で周辺環境温度が変化したときも自在に温度コン
トロールすることができるといったように、所定の単結
晶育成にとって最も重要不可欠な要素となる温度条件を
容易に、かつ、微細に調整し保持することができる。そ
の上、ＳｉＣ飽和蒸気雰囲気下での熱処理によって、Ｓ
ｉの外部放出によるやせ細り及び周辺雰囲気から界面へ
の不純物の混入も防止することができる。したがって、
周辺環境温度の変化や多結晶板及びＳｉＣ単結晶基板の
性状のばらつきにかかわらず、両者の界面をＳｉ原子及
びＣ原子の分解拡散並びにそれら原子のＳｉＣ単結晶基
板表面での再配列による単結晶化に適した温度状態に維
持して熱変化や不純物の混入に起因する歪みの影響でマ
イクロパイプ欠陥や結晶欠陥等を生じることもなく、高
純度、高品質で、かつ、量的にも大型の単結晶を生産性
よく育成させることができ、これによって、Ｓｉ（シリ
コン）やＧａＡｓ（ガリウムヒ素）などの既存の半導体
材料に比べて高温、高周波、耐電圧、耐環境性に優れパ
ワーデバイス用半導体材料として期待されている単結晶
ＳｉＣの実用化を促進することができるという効果を奏
する。As described above, according to the first and fourth aspects of the present invention, a pair of hot plates for sandwiching and holding a composite formed by laminating a SiC single crystal substrate and a polycrystalline plate are held. By controlling the heating temperature separately, the necessary temperature difference between the substrate side and the polycrystalline plate side can be secured, and the temperature can be freely controlled even when the surrounding environment temperature changes during the crystal growth process. As described above, it is possible to easily and finely adjust and hold the temperature condition which is the most important element for growing a predetermined single crystal. In addition, heat treatment in a SiC saturated steam atmosphere allows
It is also possible to prevent thinning due to external release of i and the entry of impurities from the surrounding atmosphere to the interface. Therefore,
Irrespective of changes in the ambient temperature and variations in the properties of the polycrystalline plate and the SiC single-crystal substrate, the interface between the two is decomposed and diffused by Si and C atoms, and the single crystal is formed by rearrangement of these atoms on the surface of the SiC single-crystal substrate. High temperature, high purity, high quality, and large in terms of quantity without generating micropipe defects or crystal defects due to thermal changes or distortion caused by impurity contamination. Single crystal can be grown with high productivity, and as a result, it is excellent in high temperature, high frequency, withstand voltage and environmental resistance compared to existing semiconductor materials such as Si (silicon) and GaAs (gallium arsenide) for power devices. This has the effect of promoting the practical use of single crystal SiC, which is expected as a semiconductor material.
【００１９】特に、多結晶板として、ＳｉＣ単結晶基板
表面への熱ＣＶＤ法により板状に成膜されたものを使用
する場合は、多結晶板自体が不純物の少ない高純度なも
のであることから、界面に結晶粒界などが形成されず、
単結晶ＳｉＣの純度及び品質を一層向上することができ
る。In particular, when a polycrystalline plate is used which is formed in a plate shape by a thermal CVD method on the surface of a SiC single crystal substrate, the polycrystalline plate itself should be of high purity with few impurities. Therefore, no grain boundaries are formed at the interface,
The purity and quality of single crystal SiC can be further improved.
【００２０】また、単結晶ＳｉＣの育成装置における一
対の熱盤の構成材料として、焼結カーボンを使用する場
合は、材料コストが安い上に熱盤の製作も容易で、装置
全体の低廉化が図ることができる。When sintered carbon is used as a constituent material of the pair of hot plates in the single crystal SiC growing device, the material cost is low, the hot plate can be easily manufactured, and the entire device can be reduced in cost. Can be planned.
【図１】本発明に係る単結晶ＳｉＣの育成方法に使用さ
れる複合体の説明図である。FIG. 1 is an explanatory view of a composite used in a method for growing single-crystal SiC according to the present invention.
【図２】本発明に係る単結晶ＳｉＣの育成装置の概略構
成図である。FIG. 2 is a schematic configuration diagram of a single crystal SiC growing apparatus according to the present invention.
【図３】本発明に係る単結晶ＳｉＣの育成方法によって
育成された単結晶ＳｉＣを示す模式図である。FIG. 3 is a schematic view showing single crystal SiC grown by the method for growing single crystal SiC according to the present invention.
１ α−ＳｉＣ単結晶基板 ２ β−ＳｉＣ多結晶板（Ｓｉ原子とＣ原子により構成
される板材の一例） ３ 複合体 ４，５ 熱盤 ６，７ 高周波誘導加熱コイル １０ 単結晶ＳｉＣの育成装置REFERENCE SIGNS LIST 1 α-SiC single crystal substrate 2 β-SiC polycrystalline plate (an example of a plate material composed of Si atoms and C atoms) 3 composite 4,5 hot platen 6,7 high frequency induction heating coil 10 single crystal SiC growing device
───────────────────────────────────────────────────── フロントページの続き Ｆターム(参考） 4G050 AA03 4G077 AA02 AB02 BE08 DA01 ED06 EG15 5F053 AA50 BB58 DD02 FF04 GG01 HH04 LL02 LL10 RR03 RR05 ──────────────────────────────────────────────────続 き Continued on the front page F term (reference) 4G050 AA03 4G077 AA02 AB02 BE08 DA01 ED06 EG15 5F053 AA50 BB58 DD02 FF04 GG01 HH04 LL02 LL10 RR03 RR05
Claims (5)
ｉ原子及びＣ原子により構成された多結晶板とを積層し
てなる複合体を挟み込み保持させるとともに、不活性ガ
ス雰囲気中で、かつ、ＳｉＣ飽和蒸気雰囲気下で上記一
対の熱盤の加熱温度を上記多結晶板側が高温、ＳｉＣ単
結晶基板側が低温となるように各別に制御することによ
り、上記多結晶板のＳｉ原子及びＣ原子を上記ＳｉＣ単
結晶基板の表面で再配列させてＳｉＣ単結晶基板の結晶
方位に倣った単結晶を一体に育成させることを特徴とす
る単結晶ＳｉＣの育成方法。An SIC single crystal substrate and a S plate are interposed between a pair of hot plates.
While holding a composite formed by laminating a polycrystalline plate composed of i-atoms and C-atoms, the heating temperature of the pair of hot plates is increased in an inert gas atmosphere and in a SiC saturated steam atmosphere. The SiC single crystal is rearranged on the surface of the SiC single crystal substrate by individually controlling the polycrystal plate side to be at a high temperature and the SiC single crystal substrate side at a low temperature. A method for growing single crystal SiC, wherein a single crystal following the crystal orientation of a substrate is grown integrally.
ＳｉＣアモルファスもしくは高純度ＳｉＣ焼結体の中か
ら選択された一種を使用する請求項１に記載の単結晶Ｓ
ｉＣの育成方法。2. The method according to claim 1, wherein the polycrystalline plate is a SiC polycrystalline plate.
The single crystal S according to claim 1, wherein one kind selected from SiC amorphous or high-purity SiC sintered body is used.
How to grow iC.
板表面への熱化学的蒸着法により板状に成膜されたもの
である請求項２に記載の単結晶ＳｉＣの育成方法。3. The method of growing a single-crystal SiC according to claim 2, wherein the SiC polycrystalline plate is formed in a plate shape by a thermochemical vapor deposition method on a surface of a SiC single-crystal substrate.
により構成された多結晶板とを積層してなる複合体を挟
み込み保持可能な一対の熱盤と、 これら一対の熱盤の加熱温度を各別に制御可能な高周波
誘導加熱コイルとを備え、 上記一対の熱盤間に複合体を挟み込み保持させるととも
に、不活性ガス雰囲気中で、かつ、ＳｉＣ飽和蒸気雰囲
気下で、高周波誘導加熱コイルを介して一対の熱盤の加
熱温度を多結晶板側が高温、ＳｉＣ単結晶基板側が低温
となるように制御することによって上記多結晶板のＳｉ
原子及びＣ原子を上記ＳｉＣ単結晶基板の表面で再配列
させてＳｉＣ単結晶基板の結晶方位に倣った単結晶を一
体に育成可能に構成したことを特徴とする単結晶ＳｉＣ
の育成装置。4. A pair of hot plates capable of sandwiching and holding a composite formed by laminating a SiC single crystal substrate and a polycrystalline plate composed of Si atoms and C atoms, and a heating temperature of the pair of hot plates. A high-frequency induction heating coil that can be controlled separately. The composite is sandwiched and held between the pair of hot plates, and is passed through the high-frequency induction heating coil in an inert gas atmosphere and in a SiC saturated steam atmosphere. By controlling the heating temperature of the pair of hot plates so that the temperature of the polycrystalline plate is high and the temperature of the SiC single crystal substrate is low,
A single crystal SiC characterized in that atoms and C atoms are rearranged on the surface of the SiC single crystal substrate so that a single crystal following the crystal orientation of the SiC single crystal substrate can be integrally grown.
Breeding equipment.
成されている請求項４に記載の単結晶ＳｉＣの育成装
置。5. The single crystal SiC growing apparatus according to claim 4, wherein said pair of hot plates are made of sintered carbon.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10223301A JP2936479B1 (en) | 1998-08-06 | 1998-08-06 | Method and apparatus for growing single crystal SiC |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10223301A JP2936479B1 (en) | 1998-08-06 | 1998-08-06 | Method and apparatus for growing single crystal SiC |
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| Publication Number | Publication Date |
|---|---|
| JP2936479B1 JP2936479B1 (en) | 1999-08-23 |
| JP2000053500A true JP2000053500A (en) | 2000-02-22 |
Family
ID=16796011
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10223301A Expired - Fee Related JP2936479B1 (en) | 1998-08-06 | 1998-08-06 | Method and apparatus for growing single crystal SiC |
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| Country | Link |
|---|---|
| JP (1) | JP2936479B1 (en) |
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| JPWO2020195197A1 (en) * | 2019-03-27 | 2021-10-28 | 日本碍子株式会社 | SiC composite substrate and composite substrate for semiconductor devices |
| JP7177248B2 (en) | 2019-03-27 | 2022-11-22 | 日本碍子株式会社 | SiC composite substrate and composite substrate for semiconductor devices |
| JP7372312B2 (en) | 2019-03-27 | 2023-10-31 | 日本碍子株式会社 | SiC composite substrate and composite substrate for semiconductor devices |
| WO2021100564A1 (en) * | 2019-11-20 | 2021-05-27 | 日本碍子株式会社 | Sic substrate and method for manufacturing same |
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