JP4881422B2 - 低誘電率を有する水素化オキシ炭化珪素フィルムの製造方法 - Google Patents

低誘電率を有する水素化オキシ炭化珪素フィルムの製造方法 Download PDF

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JP4881422B2
JP4881422B2 JP2009245328A JP2009245328A JP4881422B2 JP 4881422 B2 JP4881422 B2 JP 4881422B2 JP 2009245328 A JP2009245328 A JP 2009245328A JP 2009245328 A JP2009245328 A JP 2009245328A JP 4881422 B2 JP4881422 B2 JP 4881422B2
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oxygen
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ジョン ロボダ マーク
アラン セイファーリイ ジェフリー
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Description

本発明は、基体上に低い誘電率を有する水素化オキシ炭化珪素フィルムを製造する方法に関する。
珪素含有材料から、半導体装置上にＳｉＯ２、ＳｉＮＣ又はＳｉＣ薄膜を形成するために化学蒸着（ＣＶＤ）を用いることは当分野でよく知られている。化学蒸着法は、典型的にはガス状珪素含有材料と反応性ガスとを、半導体基体の入った反応室へ導入することを含む。熱又はプラズマのようなエネルギー源により、珪素含有材料と反応性ガスとの反応を引き起こし、それにより半導体装置上にＳｉＯ２、ＳｉＮＣ又はＳｉＣの薄膜を蒸着する結果を与える。プラズマ促進化学蒸着（ＰＥＣＶＤ）は、低温（＜５００℃）で行われるのが典型的であり、そのためＰＥＣＶＤは半導体装置上に誘電体及び不動態のフィルムを形成するのに適した手段になっている。珪素含有材料には、シラン（ＳｉＨ４）、オルト珪酸テトラエチル（ＴＥＯＳ）、シラシクロブタン及びトリメチルシランのようなアルキルシランが含まれる。
化学蒸着により二酸化珪素（ＳｉＯ２）、無定形ＳｉＮＣ、及び炭化珪素（ＳｉＣ）を形成するためにメチル含有シランを用いることは当分野で知られている。例えば、米国特許第５，４６５，６８０号明細書には、結晶質ＳｉＣフィルムを形成する方法が記載されている。この方法は、基体を６００℃〜１０００℃に加熱し、然る後、標準的化学蒸着法で基体をトリメチルシランに曝すことからなる。ＥＰ出願０７７４５３３には、有機珪素材料と酸素源からなる反応性ガス混合物のＣＶＤによりＳｉＯ２被覆を形成する方法が記載されている。ＥＰ出願０７７１８８６には、有機珪素材料と窒素源からなる反応性ガス混合物のＣＶＤによりＳｉＮＣ被覆を形成する方法が記載されている。
半導体装置の構造が次第に小さくなるに従って、誘電率のみならずフィルムの一体性が重要になってきている。既知のＣＶＤ法により生成するフィルムは、大きな誘電率（即ち、３．８以上）を有する。従って、低い誘電率のフィルムを与える結果になる方法及び材料に対する必要性が存在する。低ｋフローフィル（Low-k Flowfill）（登録商標名）として知られている新しい蒸着法は、３．０未満の誘電率を有するフィルムを生ずる。この方法は、メチルをドープした酸化珪素フィルムを生成させるのにメチルシランと過酸化水素との化学蒸着反応を用いている〔Ｓ．マククラッチー（McClatchie）、Ｋ．ベークマン（Beekmann）、Ａ．キールマッツ（Kiermasz）による「ＣＶＤ法を用いて蒸着した低誘電率酸化物フィルム」（Low Dielectric Constant Oxide Films Deposited Using CVD Techniques）、１９８８年ＤＵＭＩＣ会議予稿集、２／９８，ｐ．３１１−３１８参照〕。しかし、この方法は非標準的ＣＶＤ装置を必要とし、安定性の低い酸素源（過酸化水素）を用い、副生成物として半導体装置には望ましくないことがある水を生じている。
本発明の目的は、化学蒸着により水素化オキシ炭化珪素の低誘電率薄膜を製造する方法を与えることにある。
本発明は、基体、好ましくは半導体装置上に低い誘電率を有する水素化オキシ炭化珪素（Ｈ：ＳｉＯＣ）の薄膜を製造する方法に関する。
本発明は、メチル含有シラン及び酸素付与ガスを含む反応性混合物をプラズマ促進又はオゾン促進化学蒸着することからなる。反応／蒸着工程中に利用される酸素の量を調節することにより、水素、珪素、炭素及び酸素を含むフィルムを形成する。これらのフィルムは、典型的には、３．６以下の誘電率を有し、中間層誘電体として特に適している。
本発明は、基体、好ましくは半導体基体上に水素化オキシ炭化珪素フィルムを形成する方法に関する。このフィルム形成方法は、アルキルシランと酸素付与ガスを含む反応性ガス混合物を、反応中に存在する酸素の量を調節して、化学蒸着反応させることからなる。「半導体基体」とは、焦点面アレー、光電子装置、光電池、光学的装置、トランジスタ型装置、３−Ｄ装置、絶縁体上珪素装置、及び超格子装置を含めた半導体部品の製造で使用することを目的とした珪素を基にした装置及び砒化ガリウムを基にした装置を含めることを意味する。半導体基体には、一つ以上の配線層を有する好ましくはウエーハ段階の集積回路又は金属配線を適用する前の集積回路が含まれる。
ここで製造される水素化オキシ炭化珪素フィルムは、一般式ＳｉｗＯｘＣｙＨｚ（式中、ｗは１０〜３３、好ましくは１８〜２０原子％の値を有し、ｘは１〜６６、好ましくは１８〜２１原子％の値を有し、ｙは１〜６６、好ましくは３１〜３８原子％の値を有し、ｚは０．１〜６０、好ましくは２５〜３２原子％の値を有し、ｗ＋ｘ＋ｙ＋ｚ＝１００原子％である）により表される。
水素化オキシ炭化珪素フィルムは、メチル含有シランと酸素付与ガスを含む反応性ガス混合物から形成する。ここで有用なメチル含有シランには、メチルシラン（ＣＨ３ＳｉＨ３）、ジメチルシラン（（ＣＨ３）２ＳｉＨ２）、トリメチルシラン（（ＣＨ３）３ＳｉＨ）、テトラメチルシラン（（ＣＨ３）４Ｓｉ）が含まれ、好ましくはトリメチルシランである。
蒸着室には制御された量の酸素が存在する。酸素は、用いられる酸素付与ガスの種類、或は使用される酸素付与ガスの量により調節する。もし蒸着室内に余りにも多くの酸素が存在すると、ＳｉＯ２に近い化学量論的組成を有する酸化珪素フィルムが生成し、誘電率は希望のものより高くなる。酸素付与ガスの例は、空気、オゾン、酸素、亜酸化窒素及び酸化窒素であり、好ましくは亜酸化窒素である。酸素付与ガスの量は、典型的には、メチル含有シラン１体積部当たり５体積部未満の酸素付与ガスであり、好ましくはメチル含有シラン１体積部当たり０．１〜４．５体積部の酸素付与ガスである。当業者は、酸素付与ガスの種類及び蒸着条件に基づき、酸素付与ガスの量を容易に決定することができるであろう。
反応性ガス混合物中には他の材料が存在していてもよい。例えば、ヘリウム又はアルゴンのようなキャリヤーガス、ホスフィン又はジボランのようなドーパント、フッ素のようなハロゲン、又はフィルムに付加的な望ましい性質を与える他の材料が存在していてもよい。
反応性ガス混合物は、基体、好ましくは半導体基体の入った蒸着室中に導入し、そこでメチル含有シランと酸素付与ガスとの反応が引き起こされて基体上にフィルムを蒸着する結果になり、そのフィルムは水素、珪素、炭素及び酸素を含み、基体上で３．６以下の誘電率を有する。基体温度を５００℃未満にした化学蒸着（ＣＶＤ）法を用いることができる。５００℃より高い温度は、典型的には、半導体基体、特にアルミニウム配線を有する半導体基体には適さない。プラズマ促進化学蒸着（ＰＥＣＶＤ）が、使用できる温度が低いこと及び工業的に広い用途を有するために好ましい。オゾン促進ＣＶＤを用いることもできる。
ＰＥＣＶＤでは、ガス混合物は、プラズマ領域内にそれを通すことにより反応する。そのような方法で用いられるプラズマは、電気放電、無線周波（radio frequency）又はマイクロ波範囲の電磁場、レーザー又は粒子ビームのような種々の源から誘導されたエネルギーを有する。プラズマ蒸着法で一般に好ましいのは、無線周波（１０ｋＨｚ〜１０２ＭＨｚ）又はマイクロ波（１．０〜１０ＧＨｚ）エネルギーを中間的電力密度（０．１〜５ワット／ｃｍ２）で使用することである。しかし、特定の周波数、電力及び圧力は、一般に装置に適合させる。フィルムは２０〜１０００Ｗの電力、１〜１０，０００ミリトール（０．０１３３〜１１３２．２Ｐａ）の圧力、及び２５〜５００℃の温度でＰＥＣＶＤを用いて形成するのが好ましい。ＣＶＤ成長中、変動する表面トポグラフィーを平坦化するのに役立つ方法として、屡々高密度プラズマと呼ばれている閉込め（confined）低圧（１〜５ミリトール）マイクロ波周波数プラズマを、ＲＦ周波数励起と組合せることができる。この方法は、中間層誘電体の形成に有用である。
ここでは種々の厚さのフィルムを生成させることができる。本発明の方法により０．０１〜１０μｍの厚さを有するフィルムを製造することができる。好ましくはそれらフィルムは０．５〜３．０μｍの厚さを有する。
本発明の方法の一つの利点は、酸素付与ガスとして亜酸化窒素を用いた場合、反応性ガス混合物中の亜酸化窒素の量がかなり変動した場合（１．２：１〜４．５：１体積部のＮ２Ｏ対メチル含有シラン）でも、フィルムの組成及び性質が本質的に同じままになっていることである。
本発明の方法の別の利点は、ＣＶＤ工程中、適当な時間に酸素付与ガスを増大又は排除することにより、例えば、ＳｉＯ２／Ｈ：ＳｉＯＣ／ＳｉＯ２又はＳｉＣ：Ｈ／Ｈ：ＳｉＯＣ／ＳｉＣ：Ｈの多層構造体を生ずるように、順次成長工程を接続させることができることである。反応性ガス流を停止し、酸素付与ガスの量を調節し、然る後、反応性ガス流を再び流して次の層を形成することにより別個の層を生成させることが好ましい。
製造されたフィルムは、誘電率が低いため、ゲート誘電体、プレメタル（premetal）及びインターメタル（intermetal）誘電体、及び不動態被覆のような半導体集積回路を製造する時の中間層誘電体として特に適している。製造されたフィルムは、３．６以下、好ましくは３．２以下、一層好ましくは３．０以下の誘電率を有する。
当業者がここに教示する発明を理解し認識できるように、次の実施例を与える。
実施例１〜９及び比較例１〜２では、誘電体特性を、金属・絶縁体・半導体を用いて測定し（実施例４〜９）、また金属・絶縁体・金属キャパシタを用いて測定した（実施例１〜３、比較例１〜２）。測定は金属ゲート蒸着（頂部電極）直後に行い、３５０〜４００℃の温度範囲でＮ２中で一回以上のアニール工程後に再び行なった。キャパシタの幾何学的形態及びフィルムの厚さから相対的誘電率Ｋを計算した。流量はｓｃｃｍ（標準ｃｍ３／分）単位で表中に示してある。
実施例１〜９
トリメチルシラン（３ＭＳ）及び亜酸化窒素を含む反応性ガス混合物（ガス流量については表１及び２参照）を、基体として０．５μｍのＡｌで被覆した熱酸化（０．１μｍＳｉＯ２）珪素ウエーハ又は裸の珪素ウエーハを用いた容量結合平行板（capacitively coupled parallel plate）ＰＥＣＶＤ装置中へ導入した。ＰＥＣＶＤ装置は、３５０Ｗの電力、２７００ミリトール（３５９．６９Ｐａ）の圧力、及び２５０℃の温度で操作した。キャリヤーガスとしてヘリウムを用いた。実施例１〜９の誘電率、成長速度、及びフィルム応力（圧縮応力）の結果は、表１及び２に示してある。実施例４〜９で製造されたフィルムの組成及び密度を表３に示す。表２から分かるように、亜酸化窒素の量が著しく変化しても、得られるフィルムは本質的に同じ組成及び性質を持っていた。
Figure 0004881422
Figure 0004881422
Figure 0004881422
比較例１〜２
実施例１〜８の場合と同じ手順を用いて、トリメチルシラン及び酸素からなる反応性ガス混合物を、プラズマ促進化学蒸着で用いた。結果を表４に示す。得られたフィルムは、反応性ガス混合物中に用いた多量の酸素のため、本質的にＳｉＯ２フィルムであった。
Figure 0004881422
比較例３
この例は、ＥＰ出願０７７４５３３の実施例３である。６ｓｃｃｍのトリメチルシラン（ＴＭＳ）及び５２３ｓｃｃｍの亜酸化窒素を含む反応性ガス混合物を、基体として珪素ウエーハを用いた容量結合平行板ＰＥＣＶＤ装置中へ導入した。ＰＥＣＶＤ装置は、５０Ｗの電力、１０００ミリトールの圧力、及び３００℃の温度で操作した。ヘリウム（５００ｓｃｃｍ）をキャリヤーガスとして用いた。用いた亜酸化窒素（Ｎ２Ｏ）の量が多いため、得られたフィルムはＳｉＯ２フィルムであった。

Claims (5)

  1. メチル含有シラン及び酸素付与ガスを含む反応性ガス混合物を、基体の入った化学蒸着室へ導入し、前記メチル含有シランと前記酸素付与ガスとの間の反応を２５℃〜５００℃の温度で、前記反応性ガス混合物をプラズマに曝すことにより引き起こし、
    しかも、前記メチル含有シランは、メチルシラン、ジメチルシラン、トリメチルシラン及びテトラメチルシランから選択され、しかも、前記酸素付与ガスは、空気、オゾン、亜酸化窒素及び酸化窒素から成る群から選択され、
    反応中存在する酸素付与ガスの量が、メチル含有シラン１体積部当たり５体積部未満であり、３．６以下の誘電率を有する水素、珪素、炭素及び酸素を含むフィルムを基体上に形成する、
    ことからなる水素化オキシ炭化珪素フィルムの製造方法。
  2. 反応性ガス混合物が、更にキャリヤーガスを含む、請求項１に記載の方法。
  3. 水素化オキシ炭化珪素フィルムが、０．０１〜１０μｍの厚さを有する、請求項１又は２に記載の方法。
  4. メチル含有シランと酸素付与ガスとの反応中、酸素付与ガスの量を増大又は減少して、ＳｉＯ２、Ｈ：ＳｉＯＣ、及びＳｉＣ：Ｈからなる群から選択された連続的層を含むフィルムを形成する、請求項１〜３のいずれか１項に記載の方法。
  5. メチル含有シラン及び酸素付与ガスを含む反応性ガス混合物を、基体の入った化学蒸着室へ導入し、前記メチル含有シランと前記酸素付与ガスとの間の反応を２５℃〜５００℃の温度で、前記反応性ガス混合物をプラズマに曝すことにより引き起こし、
    しかも、前記メチル含有シランは、メチルシラン、ジメチルシラン、トリメチルシラン及びテトラメチルシランから選択され、しかも、前記酸素付与ガスは、空気、オゾン、酸素、亜酸化窒素及び酸化窒素から成る群から選択され、
    反応中存在する酸素付与ガスの量が、メチル含有シラン１体積部当たり５体積部未満であり、３．６以下の誘電率を有する水素、珪素、炭素及び酸素を含むフィルムを基体上に形成する、
    ことからなる水素化オキシ炭化珪素中間層誘電体フィルムの製造方法。
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KR100453612B1 (ko) 2004-10-20
SG72955A1 (en) 2000-05-23
KR19990088593A (ko) 1999-12-27
EP0960958A3 (en) 2000-03-22
JP2010028130A (ja) 2010-02-04
US6159871A (en) 2000-12-12
EP0960958A2 (en) 1999-12-01
US6593655B1 (en) 2003-07-15

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