JP2004217460A - Method of producing hydrogen-doped silicon single crystal - Google Patents

Method of producing hydrogen-doped silicon single crystal Download PDF

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JP2004217460A
JP2004217460A JP2003005935A JP2003005935A JP2004217460A JP 2004217460 A JP2004217460 A JP 2004217460A JP 2003005935 A JP2003005935 A JP 2003005935A JP 2003005935 A JP2003005935 A JP 2003005935A JP 2004217460 A JP2004217460 A JP 2004217460A
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hydrogen
gas
single crystal
silicon single
melt
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JP4341008B2 (en
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Wataru Sugimura
渉 杉村
Masataka Horai
正隆 宝来
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Sumco Corp
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Sumitomo Mitsubishi Silicon Corp
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a method of producing hydrogen-doped silicon single crystals of high quality in which the amount of hydrogen is sufficiently large and correctly controlled even without increasing the concentration of gaseous hydrogen in a gaseous mixture. <P>SOLUTION: At the time when silicon single crystals 21 are grown in a hydrogen-containing inert atmosphere by a CZ (Czochralski) method, a gaseous mixture of gaseous hydrogen and an inert gas is introduced from a gas source 12 into a pull furnace. An annular gas discharge means 15 surrounding the silicon single crystals 21 is provided in the vicinity of the surface of a raw material melt 20, and at least a part of the gaseous mixture is directly fed from the vicinity of the surface of the raw material melt 20 to the part in the vicinity of the interface of solid-liquid on the surface of the melt by the gas discharge means 15. Alternatively, at least a part of the gaseous mixture is fed into the raw material melt 20 by bubbling using a funnel tube. <P>COPYRIGHT: (C)2004,JPO&NCIPI

Description

【0001】
【発明の属する技術分野】
本発明は、水素を含む不活性雰囲気中でCZ法によりシリコン単結晶を育成する水素ドープシリコン単結晶製造方法に関する。
【0002】
【従来の技術】
シリコンウェーハの素材であるシリコン単結晶の製造方法として代表的なものは、CZ法と呼ばれる回転引上げ法である。CZ法によるシリコン単結晶の製造では、周知のとおり、石英ルツボ内に形成したシリコン融液に種結晶を浸漬し、ルツボ及び種結晶を回転させながら種結晶を引上げることにより、種結晶の下方にシリコン単結晶を育成する。
【0003】
このようなCZ引上げにおける炉内雰囲気としては、従来より不活性ガス(主にArガス)が使用されてきた。これは、シリコン融液、炉部材及び結晶との種々の化学反応を抑制し、副生成物として発生する不純物の混入を回避するためである。更に、多量にガス供給を行うことで生じる炉内のガス流れを利用して、金属汚染を回避することもでき、引上げ結晶の高品質化を実現できる。
【0004】
この炉内雰囲気に関し、最近になって、微量の水素ガスを混合することの有効性が報告され始めた(例えば特許文献1〜特許文献4)。この技術によると、結晶中に導入されたGrown−in欠陥、特にCOPに代表される空孔欠陥に水素が作用することにより、シリコン融液への窒素ドープと同様に空孔欠陥の縮小や消滅が可能になるとされている。
【0005】
【特許文献1】
特開昭61−178495号公報
【0006】
【特許文献2】
特開平11−189495号公報
【0007】
【特許文献3】
特開2000−281491号公報
【0008】
【特許文献4】
特開2001−335396号公報
【0009】
【発明が解決しようとする課題】
このようなCZ引上げにおける水素ドープ技術では、水素ガスと不活性ガスの混合ガスが、不活性ガスに代わって引上げ炉内に導入される。導入形態は、通常のCZ引上げにおける不活性ガスの場合と同様に、炉内全体を所定雰囲気に置換することを目的として、プルチャンバの上部から炉内にガス導入を行い、メインチャンバの下部から炉外へガス排出を行うものになっている。つまり引上げ炉の最上部から最下部へ混合ガスが流通される。
【0010】
しかしながら、このような混合ガス導入形態では、混合ガス中の水素ガスが空孔欠陥の発生防止に有効に機能しないことが判明した。その理由は以下のとおりである。
【0011】
水素ガスドープのそもそもの目的は、COPの基となるシリコン中の空孔が凝集する前に空孔を水素と結合させることにより、空孔の凝集を抑制することにある。このため、シリコンが空孔凝集温度(融液固化温度付近)に冷却される前に、そのシリコン中に水素を供給する必要がある。即ち、炉内に導入された素ガスは、引き上げ結晶の外表面からも供給されるが、その水素は結晶品質に及ぼす影響が少ない。これは、引き上げ時間と水素原子のシリコン中の拡散距離を考えた場合、結晶外表面から入った水素は結晶中心部まで到達せず、結晶中心部で生成されるCOPの抑制効果があらわれないためである。したがって、結晶品質の改善に有効に作用させるためには、所定量の水素ガスを坩堝内の融液表面に供給して水素を含有させたシリコン融液から結晶を育成させることが有効であり、固液界面近傍部、あるいはシリコン融液内に直接水素ガスを供給することが有効となる。
【0012】
ところが、シリコン融液を収容するルツボは、混合ガス導入点から遠く離れた引上げ炉下部のメインチャンバ内に配置されている。加えて、混合ガス中の水素ガスは、引上げ炉の内面や炉内の各種部材、特にカーボン部材に捕捉されやすい。その上、この水素ガス量は爆発危険防止等の観点から、最大で3vol%程度と微量に制限されている。これらのために、炉内に導入された水素ガスは僅かしかルツボ内の融液表面に到達せず、COPの発生抑制に有効に作用しない結果になっているのである。
【0013】
本発明の目的は、混合ガス中の水素ガス濃度を上げずとも、CZ法により高品質な水素ドープシリコン単結晶を製造できる水素ドープシリコン単結晶製造方法を提供することにある。
【0014】
【課題を解決するための手段】
上記目的を達成するめに、本発明者らは水素を含む不活性雰囲気中でCZ法によりシリコン単結晶を育成する場合の水素ガス供給法について鋭意検討した。その結果、以下の結論に到達した。
【0015】
前述したように、水素ガスをCOPの発生抑制に有効に作用させるには、相当量の水素ガスをルツボ内の融液表面、なかでも融液表面の固液界面近傍部分に供給する必要がある。これを阻害する最大の理由は、混合ガス中に含まれた微量の水素ガスが、シリコン融液を収容するルツボから最も離れたチャンバ最上部に導入されるために、シリコン融液に到達するまでの経路が長くなり、その経路途中で引上げ炉の内面や炉内の各種部材、特にカーボン部材などに多くが捕捉されてしまう点にある。
【0016】
したがって、混合ガス中に含まれた微量の水素ガスをCOPの発生抑制に有効に作用させるためには、その水素ガスが炉内に吐出されてからシリコン融液に到達するまでの炉内経路長を短くすることが必要となる。
【0017】
本発明はかかる着想を基礎にして完成されたものであり、その第1の水素ドープシリコン単結晶製造方法は、メインチャンバ上にプルチャンバが連結されたCZ引上げ炉により、水素を含む不活性雰囲気中でシリコン単結晶を育成する際に、CZ引上げ炉内に導入すべき水素ガスと不活性ガスの混合ガスの少なくとも一部を、メインチャンバ内のシリコン融液の表面、好ましくはその表面の固液界面近傍部分に直接供給されるようにメインチャンバ内に導入するものである。
【0018】
また、本発明の第2の水素ドープシリコン単結晶製造方法は、水素を含む不活性雰囲気中でCZ法によりシリコン単結晶を育成する際に、引上げ炉内に導入すべき水素ガスと不活性ガスの混合ガスの少なくとも一部をシリコン融液中に直接供給するものである。
【0019】
本発明の水素ドープシリコン単結晶製造方法においては、混合ガスが炉内に導入されてからルツボ内のシリコン融液に到達するまでの経路長が短く、経路途中における炉内部材との衝突が可及的に回避されることにより、水素ガスの捕捉が抑制され、その利用度が上がる。このため、混合ガス中の水素ガス濃度を上げたり混合ガス流量を増大させずとも、シリコン融液を介して結晶中に所望量の水素をドープすることが可能となる。加えて、シリコン融液にガスの供給が行われることにより、空孔の凝集防止に有効な凝固前のシリコンに水素ガスが効率的に導入される点からも、水素ガスの利用度が上がる。
【0020】
前記混合ガスをシリコン融液の表面に直接供給する形態としては、シリコン融液の表面近傍でシリコン単結晶を包囲するようにメインチャンバ内に設けられた環状のガス吐出手段から、前記混合ガスを融液表面、好ましくはその表面の固液界面近傍部分に吹き付けるものが、効率等の点から推奨される。
【0021】
【発明の実施の形態】
以下に本発明の実施形態を図面に基づいて説明する。図1は本発明の水素ドープシリコン単結晶製造方法を実施するのに適したCZ引上げ炉の概略構成図である。
【0022】
CZ引上げ炉は、図1に示すように、炉体として、円筒形状のメインチャンバ1と、メインチャンバ1の下面開口部を塞ぐベースチャンバ2と、メインチャンバ1の上面開口部を塞ぐトップチャンバ3と、トップチャンバ3を介してメインチャンバ1の上に同心状に連結される細長い円筒形状のプルチャンバ4とを備えている。
【0023】
メインチャンバ1内には、ルツボ5が中心部に位置して配置されている。ルツボ5は内側の石英ルツボを外側の黒鉛ルツボで保持した二重構造であり、ベースチャンバ2を貫通してメインチャンバ1内に挿入されたペディスタルと呼ばれる支持軸の上に受け皿を介して支持されている。支持軸は、ルツボ5の昇降及び回転のために、ボトムチャンバ2の下方に配置された駆動機構により、軸方向及び周方向に駆動される。
【0024】
ルツボ5の外側には環状のヒータ6が配置されており、その更に外側には断熱材7がメインチャンバ1の内面に沿って配置されている。
【0025】
メインチャンバ1内には又、ガス吐出手段15がルツボ5の上方に位置して設けられている。ガス吐出手段15は、ルツボ5の上方に同心状に配置されたリング状のヘッダー16と、ヘッダー16をルツボ5の上方の定位置に水平に吊り下げ支持する2本の支持部材17,17とを有している。ヘッダー16は円形に曲成されたチューブであり、その底部には複数のノズル孔が全周にわたって等間隔で形成されている。2本の支持部材17,17は、トップチャンバ3の下面に逆ハ字状に傾斜して取り付けられた管状部材であり、前記ガス吐出管16に後述の混合ガスを供給するガス供給管を兼ねている。
【0026】
メインチャンバ1上のプルチャンバ4内には、引上げ軸としてのワイヤ8が垂らされている。ワイヤ8は、プルチャンバ4の上に設けられた駆動機構9により、巻き上げ及び回転を行う。
【0027】
プルチャンバ4の上部には、炉体内の雰囲気管理のために、ガス導入口11が設けられている。ガス導入口11は、水素ガスと不活性ガスの混合ガスを供給するガス源12に配管13により接続されている。ガス源12は、前述したガス供給管を兼ねる2本の支持部材17,17に、配管13とは別の独立した配管18により接続されている。プルチャンバ4の下部には、メインチャンバ1内に挿入されるドローチューブ14が設けられている。ドローチューブ14は、プルチャンバ4の周壁部と同様のジャケット構造により水冷された円筒体であり、ルツボ5内のシリコン融液から引上げられるシリコン単結晶の冷却を促進すると共に、ガス導入口11からプルチャンバ4内に導入された混合ガスを整流してメインチャンバ1内に導入する整流体筒を兼ねている。一方、ベースチャンバ2にはガス排出口19が設けられている。ガス排出口19は図示されない真空ポンプと接続されている。
【0028】
ドローチュープ14の直径は、大きすぎると単結晶を冷却する効果が薄れ、小さすぎると引き上げ時に結晶の振れ等が発生した場合、育成中の結晶とドローチューブ内壁とが接触して結晶落下の危険性がある。この観点から、ドローチューブ14の直径は育成結晶の直径の1.1〜1.3倍が適当である。そしてリング状のヘッダー16の直径については、小さすぎると結晶に接触する危険性があり、大きすぎると結晶と融液界面に直接吹き付ける作用効果が低減することから、育成結晶の1.1〜1.3倍が適当である。
【0029】
操業では、まず、ルツボ5内にシリコンの原料融液20を形成する。ワイヤ8の下端部に装着した種結晶を原料融液20に漬ける。ルツボ5及びワイヤ8を回転させながら、ワイヤ8を巻き上げることにより、種結晶の下方にシリコンの単結晶21を育成する。育成結晶は、環状のヘッダー16及びドローチューブ14の各内側を通ってプルチャンバ4内に徐々に引き込まれる。
【0030】
このとき、ガス排出口19に接続された真空ポンプを作動させることにより、炉体内を所定の真空度に減圧し、この状態で、ガス源12から配管13及びガス導入口11を介して炉体内に水素ガスと不活性ガス(Arガス)の混合ガスを導入する。ガス導入口11から炉体内に導入された混合ガスは、炉体内を上から下に流通し、ガス排出口19から炉外へ排出される。これにより、炉体内が一応混合ガス雰囲気に管理される。
【0031】
これと同時に、ガス源12から別の配管18を介して2本の支持部材17,17に前記混合ガスを供給する。支持部材17,17に供給された混合ガスは、水平なリング状のヘッダー16に送られ、ヘッダー16の底部に設けられた複数のノズル孔から、プルチャンバ4内を通過することなくメインチャンバ1内へ下向きに吐出される。メインチャンバ1内へ下向きに吐出された混合ガスは、主にルツボ5内の原料融液20の表面、より具体的には、その表面の単結晶21からその外側にかけての範囲に、至近距離からフレッシュ状態で衝突することになる。この結果、複数のノズル孔から吐出される混合ガス中の水素ガスは、単結晶21中の空孔防止に効率的に作用する。
【0032】
なぜなら、ヘッダー16から吐出される混合ガスが至近距離からルツボ5内の融液面に衝突し、水素ガスが炉内の流通経路途中でカーボン部材に捕捉されることなどによる無駄な水素消費が回避されると共に、混合ガスの衝突位置が、主にルツボ5内の融液表面の固液界面近傍部分であることにより、混合ガス中の水素ガスが空孔の凝集抑制に効果的な凝固直前のシリコンに効率よく取り込まれ、単結晶21などへの水素の無駄な取り込みが回避されるからである。
【0033】
こうした効率的な水素取り込みにより、凝固直前の段階でシリコンに所定濃度の水素がドープされ、空孔欠陥の発生が効果的に抑制された高品質な水素ドープシリコン単結晶21が製造されることになる。
【0034】
図2は本発明の水素ドープシリコン単結晶製造方法を実施するのに適した別のCZ引上げ炉の概略構成図である。
【0035】
この引上げ炉は、ガス吐出手段15の構造が、前述した引上げ炉と相違する。他の構造は、前述した引上げ炉と実質同一であり、同一部分に同一番号を付して説明を省略する。
【0036】
ここにおけるガス吐出手段15は、メインチャンバ1内に挿入されるドローチューブ14の外側に設けられた円筒状のヘッダー22を有している。ヘッダー22は、ドローチューブ14とその外側に設けた円筒状の外筒とで構成された2重筒構造であり、そのヘッダー22の底面には複数のノズル孔が全周にわたって等間隔で設けられているそして、このヘッダー22には、ガス源12が、当該ガス源12をプルチャンバ4の上部に接続する配管13とは別の独立した配管18により、接続されている。
【0037】
操業中、ガス源12からプルチャンバ4内に水素ガスと不活性ガスの混合ガスが供給される。同時に、ガス吐出手段15のヘッダー22内にもこの混合ガスが供給される。ヘッダー22内に供給された混合ガスは、当該ヘッダーの底面に設けられた複数のノズル孔からメインチャンバ1内へ下向きに吐出される。メインチャンバ1内へ下向きに吐出された混合ガスは、前述した引上げ炉の場合と同様に、主にルツボ5内の原料融液20の表面、より具体的には、その表面の単結晶21からその外側にかけての範囲に至近距離から衝突する。この結果、複数のノズル孔から吐出される混合ガス中の水素ガスは、単結晶21中の空孔欠陥防止に効率的に作用することになる。
【0038】
図3は本発明の水素ドープシリコン単結晶製造方法を実施するのに適した更に別のCZ引上げ炉の概略構成図である。
【0039】
この引上げ炉は、ルツボ5内の原料融液20に混合ガスを供給する形態が、前述した二つの引上げ炉と相違する。即ち、ルツボ5内の原料融液20に混合ガスを供給する形態は、前述した二つの引上げ炉では、環状のガス吐出手段15から原料融液20の表面、特に融液面の固液界面近傍部分に混合ガスを吹き付けるものであるのに対し、この引上げ炉では、ルツボ5内の原料融液20に浸漬するように、トップチャンバ3を貫通してメインチャンバ1内に差し込まれた石英からなるロート管24を用いて、原料融液20中に混合ガスを吹き込む構成になっている。
【0040】
この形態によっても、炉内に吐出される混合ガスが原料融液20に直接供給され、原料融液20に到達するまでの経路長が実質0に大幅短縮されることにより、混合ガス中の水素ガスが経路途中でカーボン部材に捕捉されることなどによる無駄な水素消費が回避される。また、その水素ガスが空孔の凝集抑制に効果的な凝固直前のシリコンに効率よく取り込まれ、単結晶21などへの水素の無駄な取り込みが回避される。こうした効率的な水素取り込みの結果、凝固直前の段階でシリコンに所定濃度の水素がドープされ、空孔欠陥の発生が効果的に抑制された高品質な水素ドープ単結晶21が製造される。
【0041】
本発明法の実施例として、図1に示す形態により、種々の水素濃度の混合ガスをプルチャンバの上部からとリング状のヘッダーからとに別けて炉内に供給し、混合ガス中の水素濃度と単結晶中の水素濃度との関係を調べた。また、従来例として、混合ガスの全量をプルチャンバの上部から供給し、この場合の混合ガス中の水素濃度と単結晶中の水素濃度との関係を調べた。結果を表1に示す。
【0042】
【表1】

Figure 2004217460
【0043】
結晶径は150mm、本発明法に用いたリング状ヘッダーの管径は10mm、リング径は内径165mm、混合ガスのガス吐出管への分流比は50%とした。また、結晶中の水素濃度の測定には光吸収測定装置(FT−IR)を用いた。結晶中の水素濃度が十分の場合には、光吸収測定装置によってシリコンと水素との複合体としての吸収ピークが観察されるため、この吸収ピークの有無によって水素濃度の適否を判断することができる。表中、○印は十分な大きさの吸収ピークが観察されたものを示し、△印は観察された吸収ピークが小さかったもの、×印は全く吸収ピークが観察されないかったものを示している。
【0044】
表1から明らかなように、本発明例の場合、混合ガス中の水素濃度が3%あたりからシリコンと水素の複合体ピークが確認され、従来法と比較して複合体ピークが確認される水素濃度が低水素濃度側にシフトしていることが分かる。これは、シリコン融液表面に直接供給した水素が効率よく結晶中に取り込まれた結果である。また、本発明例では水素濃度5%の供給で水素が十分に結晶中に取り込まれており、従来法よりもより安全な低水素濃度の操業が可能となる。
【0045】
以上より、本発明法により安全上有利である低水素濃度範囲内で十分に結晶中に水素を導入することが可能になることが分かる。
【0046】
前述した本発明法の各例では、炉内に導入すべき雰囲気ガスの全部を混合ガスとし、その混合ガスの一部をメインチャンバ内の原料融液に至近距離から直接供給し、残りの混合ガスをプルチャンバ上部から炉内に導入したが、混合ガスの全部をメインチャンバ内の原料融液に至近距離から直接供給することもできる。また、炉内に導入すべき雰囲気ガスの一部を混合ガスとしてメインチャンバ内の原料融液に至近距離から直接供給することもできる。この場合、残りの雰囲気ガスは全て不活性ガスであり、例えばプルチャンバの上部から炉内に導入される。
【0047】
【発明の効果】
以上に説明したとおり、本発明の水素ドープシリコン単結晶製造方法は、水素を含む不活性雰囲気中でCZ法によりシリコン単結晶を育成する際に、炉内に導入された水素ガスがルツボ内のシリコン融液に到達するまでの炉内経路長を短く制限することにより、その経路途中における水素ガスの捕捉及びシリコン単結晶への水素ガスの取り込みを回避でき、その水素ガスの効率的な利用を可能にする。これにより、混合ガス中の水素ガス濃度を上げずに、水素量が十分に多くかつ正確に管理された高品質な水素ドープシリコン単結晶を安全に製造できる。
【図面の簡単な説明】
【図1】本発明の水素ドープシリコン単結晶製造方法を実施するのに適したCZ引上げ炉の概略構成図である。
【図2】本発明の水素ドープシリコン単結晶製造方法を実施するのに適した別のCZ引上げ炉の概略構成図である。
【図3】本発明の水素ドープシリコン単結晶製造方法を実施するのに適した更に別のCZ引上げ炉の概略構成図である。
【符号の説明】
1 メインチャンバ
4 プルチャンバ
5 ルツボ
6 ヒータ
8 ワイヤ
11 ガス導入口
12 ガス源
13,18 配管
14 ドローチューブ
15 ガス吐出手段
16,22 ヘッダー
17 支持部材
19 ガス排出口
20 原料融液
21 単結晶
24 ロート管[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a method for producing a hydrogen-doped silicon single crystal in which a silicon single crystal is grown by a CZ method in an inert atmosphere containing hydrogen.
[0002]
[Prior art]
A typical method for producing a silicon single crystal, which is a material of a silicon wafer, is a rotary pulling method called a CZ method. In the production of a silicon single crystal by the CZ method, as is well known, a seed crystal is immersed in a silicon melt formed in a quartz crucible, and the seed crystal is pulled up while rotating the crucible and the seed crystal. A silicon single crystal is grown.
[0003]
An inert gas (mainly Ar gas) has been used as an atmosphere in the furnace in such CZ pulling. This is for suppressing various chemical reactions with the silicon melt, the furnace member, and the crystal, and avoiding contamination of impurities generated as by-products. Furthermore, metal contamination can be avoided by utilizing the gas flow in the furnace generated by supplying a large amount of gas, and high-quality pulled crystals can be realized.
[0004]
With respect to the atmosphere in the furnace, the effectiveness of mixing a small amount of hydrogen gas has recently been reported (for example, Patent Documents 1 to 4). According to this technique, hydrogen acts on the grown-in defects introduced into the crystal, particularly vacancy defects typified by COP, so that the vacancy defects are reduced or eliminated as in the case of nitrogen doping into a silicon melt. It is said that it will be possible.
[0005]
[Patent Document 1]
JP-A-61-178495 [0006]
[Patent Document 2]
JP-A-11-189495
[Patent Document 3]
Japanese Patent Application Laid-Open No. 2000-281491
[Patent Document 4]
JP 2001-335396 A
[Problems to be solved by the invention]
In such a hydrogen doping technique in CZ pulling, a mixed gas of hydrogen gas and an inert gas is introduced into a pulling furnace instead of the inert gas. As with the case of the inert gas in the normal CZ pulling, the gas is introduced into the furnace from the upper part of the pull chamber and the furnace is introduced from the lower part of the main chamber in order to replace the entire inside of the furnace with a predetermined atmosphere. It is designed to discharge gas to the outside. That is, the mixed gas flows from the uppermost part to the lowermost part of the pulling furnace.
[0010]
However, it has been found that in such a mixed gas introduction mode, the hydrogen gas in the mixed gas does not function effectively to prevent the generation of vacancy defects. The reason is as follows.
[0011]
The original purpose of the hydrogen gas doping is to suppress the aggregation of the vacancies by bonding the vacancies to hydrogen before the vacancies in the silicon serving as the COP are agglomerated. For this reason, it is necessary to supply hydrogen into silicon before the silicon is cooled to the vacancy aggregation temperature (near the melt solidification temperature). That is, the raw gas introduced into the furnace is also supplied from the outer surface of the pulled crystal, but the hydrogen has little effect on the crystal quality. This is because, considering the pulling time and the diffusion distance of hydrogen atoms in silicon, hydrogen entering from the outer surface of the crystal does not reach the center of the crystal, and the effect of suppressing COP generated at the center of the crystal does not appear. It is. Therefore, in order to effectively act on the improvement of crystal quality, it is effective to supply a predetermined amount of hydrogen gas to the surface of the melt in the crucible to grow crystals from the silicon melt containing hydrogen, It is effective to supply hydrogen gas directly in the vicinity of the solid-liquid interface or in the silicon melt.
[0012]
However, the crucible containing the silicon melt is disposed in the main chamber at the lower part of the pulling furnace far away from the mixed gas introduction point. In addition, the hydrogen gas in the mixed gas is likely to be captured by the inner surface of the pulling furnace and various members in the furnace, particularly the carbon member. In addition, the amount of hydrogen gas is limited to a very small amount of about 3 vol% at the maximum from the viewpoint of preventing explosion hazard. For these reasons, only a small amount of the hydrogen gas introduced into the furnace reaches the melt surface in the crucible, and as a result, the hydrogen gas does not effectively act to suppress the generation of COP.
[0013]
An object of the present invention is to provide a hydrogen-doped silicon single crystal manufacturing method capable of manufacturing a high-quality hydrogen-doped silicon single crystal by the CZ method without increasing the hydrogen gas concentration in a mixed gas.
[0014]
[Means for Solving the Problems]
In order to achieve the above object, the present inventors have intensively studied a hydrogen gas supply method for growing a silicon single crystal by a CZ method in an inert atmosphere containing hydrogen. As a result, the following conclusion was reached.
[0015]
As described above, in order for hydrogen gas to effectively act to suppress the generation of COP, it is necessary to supply a considerable amount of hydrogen gas to the melt surface in the crucible, especially to the portion near the solid-liquid interface of the melt surface. . The biggest reason for this is that a small amount of hydrogen gas contained in the mixed gas is introduced to the top of the chamber, which is furthest from the crucible that contains the silicon melt, so that it reaches the silicon melt. Is long, and many parts are trapped on the inner surface of the pulling furnace and various members in the furnace, particularly carbon members, in the middle of the path.
[0016]
Therefore, in order to effectively use the trace amount of hydrogen gas contained in the mixed gas to suppress the generation of COP, the path length in the furnace from when the hydrogen gas is discharged into the furnace to when the hydrogen gas reaches the silicon melt is required. Must be shortened.
[0017]
The present invention has been completed on the basis of such an idea, and the first method for producing a hydrogen-doped silicon single crystal is provided in a hydrogen-containing inert atmosphere by a CZ pulling furnace in which a pull chamber is connected to a main chamber. At the time of growing a silicon single crystal by using at least a part of the mixed gas of hydrogen gas and inert gas to be introduced into the CZ pulling furnace, the surface of the silicon melt in the main chamber, preferably the solid-liquid on the surface It is introduced into the main chamber so as to be supplied directly to the portion near the interface.
[0018]
Further, the second method for producing a hydrogen-doped silicon single crystal of the present invention is characterized in that when growing a silicon single crystal by a CZ method in an inert atmosphere containing hydrogen, hydrogen gas and an inert gas to be introduced into a pulling furnace are used. At least a part of the mixed gas is directly supplied into the silicon melt.
[0019]
In the method for producing a hydrogen-doped silicon single crystal of the present invention, the path length from the time when the mixed gas is introduced into the furnace to the time when the mixed gas reaches the silicon melt in the crucible is short. By avoiding as much as possible, trapping of hydrogen gas is suppressed, and the utilization thereof is increased. Therefore, it is possible to dope a desired amount of hydrogen into the crystal via the silicon melt without increasing the concentration of the hydrogen gas in the mixed gas or increasing the flow rate of the mixed gas. In addition, by supplying the gas to the silicon melt, the utilization of the hydrogen gas is increased from the viewpoint that the hydrogen gas is efficiently introduced into the silicon before solidification which is effective in preventing the aggregation of the pores.
[0020]
As a mode of directly supplying the mixed gas to the surface of the silicon melt, the mixed gas is supplied from an annular gas discharge unit provided in the main chamber so as to surround the silicon single crystal near the surface of the silicon melt. A material sprayed on the surface of the melt, preferably on the surface in the vicinity of the solid-liquid interface is recommended from the viewpoint of efficiency and the like.
[0021]
BEST MODE FOR CARRYING OUT THE INVENTION
Hereinafter, embodiments of the present invention will be described with reference to the drawings. FIG. 1 is a schematic configuration diagram of a CZ pulling furnace suitable for carrying out the method for producing a hydrogen-doped silicon single crystal of the present invention.
[0022]
As shown in FIG. 1, the CZ pulling furnace has, as furnace bodies, a cylindrical main chamber 1, a base chamber 2 for closing a lower opening of the main chamber 1, and a top chamber 3 for closing an upper opening of the main chamber 1. And an elongated cylindrical pull chamber 4 concentrically connected to the main chamber 1 via the top chamber 3.
[0023]
In the main chamber 1, a crucible 5 is arranged at a central position. The crucible 5 has a double structure in which an inner quartz crucible is held by an outer graphite crucible, and is supported via a tray on a support shaft called a pedestal inserted into the main chamber 1 through the base chamber 2. ing. The support shaft is driven in the axial direction and the circumferential direction by a drive mechanism disposed below the bottom chamber 2 for raising and lowering and rotating the crucible 5.
[0024]
An annular heater 6 is arranged outside the crucible 5, and a heat insulating material 7 is arranged outside the crucible 5 along the inner surface of the main chamber 1.
[0025]
In the main chamber 1, a gas discharging means 15 is provided above the crucible 5. The gas discharge means 15 includes a ring-shaped header 16 disposed concentrically above the crucible 5, and two support members 17, 17 for suspending and supporting the header 16 horizontally at a fixed position above the crucible 5. have. The header 16 is a tube bent in a circular shape, and a plurality of nozzle holes are formed at the bottom thereof at equal intervals over the entire circumference. The two support members 17 and 17 are tubular members which are attached to the lower surface of the top chamber 3 so as to be inclined in an inverted C-shape, and also serve as a gas supply pipe for supplying a mixed gas described later to the gas discharge pipe 16. ing.
[0026]
In the pull chamber 4 on the main chamber 1, a wire 8 as a pulling shaft is hung. The wire 8 is wound and rotated by a drive mechanism 9 provided on the pull chamber 4.
[0027]
A gas inlet 11 is provided at an upper portion of the pull chamber 4 for managing the atmosphere in the furnace. The gas inlet 11 is connected by a pipe 13 to a gas source 12 for supplying a mixed gas of hydrogen gas and an inert gas. The gas source 12 is connected to the two support members 17, 17 which also serve as gas supply pipes, by a separate pipe 18 separate from the pipe 13. A draw tube 14 inserted into the main chamber 1 is provided below the pull chamber 4. The draw tube 14 is a cylindrical body that is water-cooled by the same jacket structure as the peripheral wall of the pull chamber 4, promotes cooling of the silicon single crystal pulled up from the silicon melt in the crucible 5, and draws the gas from the gas inlet 11 into the pull chamber. 4 also serves as a rectifying body cylinder that rectifies the mixed gas introduced into the main chamber 4 and introduces the mixed gas into the main chamber 1. On the other hand, the base chamber 2 is provided with a gas outlet 19. The gas outlet 19 is connected to a vacuum pump (not shown).
[0028]
If the diameter of the draw tube 14 is too large, the effect of cooling the single crystal is diminished, and if the diameter is too small, the crystal grows and the inner wall of the draw tube come into contact with each other, and when the crystal grows, the danger of crystal falling may occur. There is. From this viewpoint, it is appropriate that the diameter of the draw tube 14 is 1.1 to 1.3 times the diameter of the grown crystal. If the diameter of the ring-shaped header 16 is too small, there is a risk of contact with the crystal. If the diameter is too large, the effect of directly spraying the interface between the crystal and the melt is reduced. .3 times is appropriate.
[0029]
In operation, first, a silicon raw material melt 20 is formed in the crucible 5. The seed crystal attached to the lower end of the wire 8 is immersed in the raw material melt 20. By winding the wire 8 while rotating the crucible 5 and the wire 8, a single crystal 21 of silicon is grown below the seed crystal. The grown crystal is gradually drawn into the pull chamber 4 through each inside of the annular header 16 and the draw tube 14.
[0030]
At this time, the inside of the furnace is depressurized to a predetermined degree of vacuum by operating a vacuum pump connected to the gas outlet 19, and in this state, the furnace body is evacuated from the gas source 12 through the pipe 13 and the gas inlet 11. , A mixed gas of a hydrogen gas and an inert gas (Ar gas) is introduced. The mixed gas introduced into the furnace from the gas inlet 11 flows through the furnace from top to bottom, and is discharged from the gas outlet 19 to the outside of the furnace. Thus, the inside of the furnace is temporarily controlled to a mixed gas atmosphere.
[0031]
At the same time, the mixed gas is supplied from the gas source 12 to the two support members 17, 17 via another pipe 18. The mixed gas supplied to the support members 17, 17 is sent to a horizontal ring-shaped header 16, and passes through a plurality of nozzle holes provided at the bottom of the header 16 without passing through the inside of the pull chamber 4. Is discharged downward. The mixed gas discharged downward into the main chamber 1 mainly reaches the surface of the raw material melt 20 in the crucible 5, more specifically, a range from the single crystal 21 on the surface to the outside thereof, from a short distance. It will collide in a fresh state. As a result, the hydrogen gas in the mixed gas discharged from the plurality of nozzle holes effectively acts to prevent vacancies in the single crystal 21.
[0032]
This is because the mixed gas discharged from the header 16 collides with the melt surface in the crucible 5 from a short distance, and wasteful hydrogen consumption due to the hydrogen gas being captured by the carbon member in the middle of the circulation path in the furnace is avoided. At the same time, the collision position of the mixed gas is mainly in the vicinity of the solid-liquid interface of the melt surface in the crucible 5, so that the hydrogen gas in the mixed gas immediately before solidification is effective in suppressing the aggregation of vacancies. This is because silicon is efficiently incorporated into silicon, and wasteful incorporation of hydrogen into the single crystal 21 or the like is avoided.
[0033]
By such efficient hydrogen uptake, a high-quality hydrogen-doped silicon single crystal 21 is produced in which silicon is doped with a predetermined concentration of hydrogen immediately before solidification, and the generation of vacancy defects is effectively suppressed. Become.
[0034]
FIG. 2 is a schematic configuration diagram of another CZ pulling furnace suitable for carrying out the method for producing a hydrogen-doped silicon single crystal of the present invention.
[0035]
This pulling furnace differs from the above-described pulling furnace in the structure of the gas discharge means 15. Other structures are substantially the same as those of the above-described pulling furnace, and the same portions are denoted by the same reference numerals and description thereof will be omitted.
[0036]
The gas discharge means 15 here has a cylindrical header 22 provided outside the draw tube 14 inserted into the main chamber 1. The header 22 has a double-cylinder structure including the draw tube 14 and a cylindrical outer cylinder provided on the outside thereof. A plurality of nozzle holes are provided on the bottom surface of the header 22 at equal intervals over the entire circumference. The gas source 12 is connected to the header 22 by a separate pipe 18 separate from the pipe 13 connecting the gas source 12 to the upper part of the pull chamber 4.
[0037]
During operation, a mixed gas of hydrogen gas and an inert gas is supplied from the gas source 12 into the pull chamber 4. At the same time, this mixed gas is also supplied into the header 22 of the gas discharge means 15. The mixed gas supplied into the header 22 is discharged downward into the main chamber 1 from a plurality of nozzle holes provided on the bottom surface of the header. The mixed gas discharged downward into the main chamber 1 is mainly discharged from the surface of the raw material melt 20 in the crucible 5, more specifically, from the single crystal 21 on the surface, as in the case of the above-described pulling furnace. It collides from a very close range to the outside. As a result, the hydrogen gas in the mixed gas discharged from the plurality of nozzle holes effectively acts to prevent vacancy defects in the single crystal 21.
[0038]
FIG. 3 is a schematic configuration diagram of still another CZ pulling furnace suitable for carrying out the method for producing a hydrogen-doped silicon single crystal of the present invention.
[0039]
This pulling furnace differs from the above-described two pulling furnaces in the form of supplying the mixed gas to the raw material melt 20 in the crucible 5. That is, the mixed gas is supplied to the raw material melt 20 in the crucible 5 in the above-described two pulling furnaces by using the annular gas discharge means 15 from the surface of the raw material melt 20, particularly near the solid-liquid interface of the melt surface. In contrast to the method in which the mixed gas is blown to the portion, this pulling furnace is made of quartz inserted into the main chamber 1 through the top chamber 3 so as to be immersed in the raw material melt 20 in the crucible 5. The mixed gas is blown into the raw material melt 20 using the funnel tube 24.
[0040]
Also in this mode, the mixed gas discharged into the furnace is directly supplied to the raw material melt 20, and the path length to reach the raw material melt 20 is substantially reduced to substantially zero, so that the hydrogen in the mixed gas is reduced. Useless hydrogen consumption due to the gas being trapped by the carbon member in the middle of the path is avoided. In addition, the hydrogen gas is efficiently taken into silicon immediately before solidification, which is effective in suppressing the aggregation of vacancies, and wasteful incorporation of hydrogen into the single crystal 21 or the like is avoided. As a result of such efficient hydrogen incorporation, a high-quality hydrogen-doped single crystal 21 in which silicon is doped with a predetermined concentration of hydrogen immediately before solidification and generation of vacancy defects is effectively suppressed is produced.
[0041]
As an embodiment of the method of the present invention, according to the embodiment shown in FIG. 1, mixed gas having various hydrogen concentrations is supplied into the furnace separately from the upper portion of the pull chamber and from a ring-shaped header, and the hydrogen concentration in the mixed gas is determined. The relationship with the hydrogen concentration in the single crystal was investigated. Further, as a conventional example, the entire amount of the mixed gas was supplied from the upper part of the pull chamber, and the relationship between the hydrogen concentration in the mixed gas and the hydrogen concentration in the single crystal in this case was examined. Table 1 shows the results.
[0042]
[Table 1]
Figure 2004217460
[0043]
The crystal diameter was 150 mm, the tube diameter of the ring-shaped header used in the method of the present invention was 10 mm, the ring diameter was 165 mm, and the split ratio of the mixed gas to the gas discharge tube was 50%. In addition, a light absorption measurement device (FT-IR) was used for measuring the hydrogen concentration in the crystal. When the concentration of hydrogen in the crystal is sufficient, an absorption peak as a complex of silicon and hydrogen is observed by a light absorption measurement device, and the appropriateness of the hydrogen concentration can be determined based on the presence or absence of the absorption peak. . In the table, ○ indicates that a sufficiently large absorption peak was observed, △ indicates that the observed absorption peak was small, and X indicates that no absorption peak was observed. .
[0044]
As is clear from Table 1, in the case of the present invention, the peak of the composite of silicon and hydrogen is confirmed when the hydrogen concentration in the mixed gas is around 3%, and the peak of the composite is confirmed as compared with the conventional method. It can be seen that the concentration has shifted to the low hydrogen concentration side. This is a result of the fact that hydrogen supplied directly to the surface of the silicon melt was efficiently incorporated into the crystal. In addition, in the example of the present invention, hydrogen is sufficiently taken into the crystal by supplying hydrogen at a concentration of 5%, which enables safer operation at a low hydrogen concentration than the conventional method.
[0045]
From the above, it can be seen that the method of the present invention makes it possible to sufficiently introduce hydrogen into a crystal within a low hydrogen concentration range that is advantageous for safety.
[0046]
In each of the above-described examples of the method of the present invention, all of the atmospheric gases to be introduced into the furnace are mixed gas, a part of the mixed gas is directly supplied to the raw material melt in the main chamber from a short distance, and the remaining mixed gas is supplied. Although the gas was introduced into the furnace from the upper part of the pull chamber, the entire mixed gas may be directly supplied to the raw material melt in the main chamber from a short distance. Also, a part of the atmosphere gas to be introduced into the furnace can be directly supplied as a mixed gas to the raw material melt in the main chamber from a short distance. In this case, the remaining atmospheric gases are all inert gases and are introduced into the furnace, for example, from the upper part of the pull chamber.
[0047]
【The invention's effect】
As described above, in the method for producing a hydrogen-doped silicon single crystal of the present invention, when growing a silicon single crystal by the CZ method in an inert atmosphere containing hydrogen, the hydrogen gas introduced into the furnace contains the hydrogen gas in the crucible. By shortening the path length in the furnace to reach the silicon melt, it is possible to avoid the capture of hydrogen gas in the middle of the path and the incorporation of hydrogen gas into the silicon single crystal, and to use the hydrogen gas efficiently. enable. This makes it possible to safely manufacture a high-quality hydrogen-doped silicon single crystal in which the amount of hydrogen is sufficiently large and accurately controlled without increasing the concentration of hydrogen gas in the mixed gas.
[Brief description of the drawings]
FIG. 1 is a schematic configuration diagram of a CZ pulling furnace suitable for carrying out a method for producing a hydrogen-doped silicon single crystal of the present invention.
FIG. 2 is a schematic configuration diagram of another CZ pulling furnace suitable for carrying out the method for producing a hydrogen-doped silicon single crystal of the present invention.
FIG. 3 is a schematic configuration diagram of still another CZ pulling furnace suitable for carrying out the method for producing a hydrogen-doped silicon single crystal of the present invention.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 Main chamber 4 Pull chamber 5 Crucible 6 Heater 8 Wire 11 Gas inlet 12 Gas source 13, 18 Piping 14 Draw tube 15 Gas discharge means 16, 22 Header 17 Support member 19 Gas outlet 20 Raw material melt 21 Single crystal 24 Funnel

Claims (4)

メインチャンバ上にプルチャンバが連結されたCZ引上げ炉により、水素を含む不活性雰囲気中でシリコン単結晶を育成する際に、CZ引上げ炉内に導入すべき水素ガスと不活性ガスの混合ガスの少なくとも一部を、プルチャンバ内に通すことなくメインチャンバ内のシリコン融液表面に直接供給することを特徴とする水素ドープシリコン単結晶製造方法。When growing a silicon single crystal in an inert atmosphere containing hydrogen by a CZ pulling furnace having a pull chamber connected to a main chamber, at least a mixed gas of hydrogen gas and an inert gas to be introduced into the CZ pulling furnace. A method for producing a hydrogen-doped silicon single crystal, characterized in that a part is directly supplied to a surface of a silicon melt in a main chamber without passing through a pull chamber. 前記混合ガスの少なくとも一部を、前記融液表面の固液界面近傍部分に直接供給することを特徴とする請求項1に記載の水素ドープシリコン単結晶製造方法。The method for producing a hydrogen-doped silicon single crystal according to claim 1, wherein at least a part of the mixed gas is directly supplied to a portion near the solid-liquid interface on the surface of the melt. シリコン融液の表面近傍でシリコン単結晶を包囲するようにメインチャンバ内に設けられた環状のガス吐出手段から、前記混合ガスの少なくとも一部を融液表面に吹き付けることを特徴とする請求項1に記載の水素ドープシリコン単結晶製造方法。2. The method according to claim 1, wherein at least a part of the mixed gas is blown onto the surface of the melt from an annular gas discharge means provided in the main chamber so as to surround the silicon single crystal near the surface of the silicon melt. 3. The method for producing a hydrogen-doped silicon single crystal according to 1. 水素を含む不活性雰囲気中でCZ法によりシリコン単結晶を育成する際に、引上げ炉内に導入すべき水素ガスと不活性ガスの混合ガスの少なくとも一部を、シリコン融液中に直接供給することを特徴とする水素ドープシリコン単結晶製造方法。When growing a silicon single crystal by the CZ method in an inert atmosphere containing hydrogen, at least a part of a mixed gas of a hydrogen gas and an inert gas to be introduced into a pulling furnace is directly supplied into a silicon melt. A method for producing a hydrogen-doped silicon single crystal, comprising:
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US7384480B2 (en) 2005-06-20 2008-06-10 Sumco Corporation Apparatus for manufacturing semiconductor single crystal
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JP4638886B2 (en) * 2006-01-19 2011-02-23 ジルトロニック アクチエンゲゼルシャフト Apparatus and method for producing a single crystal
JP2007191388A (en) * 2006-01-19 2007-08-02 Siltronic Ag Device and method for manufacturing single crystal, single crystal and semiconductor disk
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JP4650345B2 (en) * 2006-05-29 2011-03-16 株式会社Sumco Method for producing silicon single crystal
JP2009184863A (en) * 2008-02-05 2009-08-20 Shin Etsu Handotai Co Ltd Apparatus and method for manufacturing single crystal
WO2017017893A1 (en) * 2015-07-29 2017-02-02 信越半導体株式会社 Silicon single crystal growing device
JP2017030991A (en) * 2015-07-29 2017-02-09 信越半導体株式会社 Growth unit for silicon single crystal

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