JP2000049157A - 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

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Publication number
JP2000049157A
JP2000049157A JP11150323A JP15032399A JP2000049157A JP 2000049157 A JP2000049157 A JP 2000049157A JP 11150323 A JP11150323 A JP 11150323A JP 15032399 A JP15032399 A JP 15032399A JP 2000049157 A JP2000049157 A JP 2000049157A
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Prior art keywords
oxygen
film
reaction
methyl
dielectric constant
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Inventor
Mark Jon Loboda
ジョン ロボダ マーク
Jeffrey Alan Seifferly
アラン セイファーリイ ジェフリー
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Dow Silicones Corp
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Dow Corning Corp
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Abstract

(57)【要約】 【課題】 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。 【解決手段】 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℃の温度で引き起こし、反応中存
在する酸素の量を調節して、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。

Description

【発明の詳細な説明】
【０００１】
【発明の属する技術分野】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。
【０００２】
【従来の技術】珪素含有材料から、半導体装置上にＳｉ
Ｏ2、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Ｓｉ
Ｃ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。
【０００３】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ＣＶ
Ｄ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。
【０００４】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(McClatchi
e)、Ｋ．ベークマン(Beekmann)、Ａ．キールマッツ(Kie
rmasz)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 D
eposited Using CVD Techniques)、１９８８年ＤＵＭＩ
Ｃ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。
【０００５】
【発明が解決しようとする課題】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。
【０００６】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：Ｓｉ
ＯＣ）の薄膜を製造する方法に関する。
【０００７】
【課題を解決するための手段】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。
【０００８】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。
【０００９】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Ｓｉw Ｏx Ｃy Ｈ z（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。
【００１０】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（ＣＨ3 ＳｉＨ3)、ジメチルシラン（（ＣＨ3)2
ＳｉＨ2)、トリメチルシラン（（ＣＨ3)3 ＳｉＨ）、テ
トラメチルシラン（（ＣＨ3)4 Ｓｉ）が含まれ、好まし
くはトリメチルシランである。
【００１１】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。
【００１２】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。
【００１３】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。
【００１４】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（radi
o 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、１〜１
０，０００ミリトール（０．０１３３〜１１３２．２Ｐ
ａ）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（confin
ed）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。
【００１５】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０．０１〜１０μ
ｍ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。
【００１６】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。
【００１７】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。
【００１８】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。
【００１９】
【実施例】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。
【００２０】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。
【００２１】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 par
allel plate）ＰＥＣＶＤ装置中へ導入した。ＰＥＣＶ
Ｄ装置は、３５０Ｗの電力、２７００ミリトール（３５
９．６９Ｐａ）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。
【００２２】
【表１】
【００２３】
【表２】
【００２４】
【表３】
【００２５】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。
【００２６】
【表４】
【００２７】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５２３ｓ
ｃｃｍ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、１
０００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。
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） // Ｈ０１Ｂ 3/12 ３３６ Ｈ０１Ｂ 3/12 ３３６

Claims (6)

    【特許請求の範囲】
  1. 【請求項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℃の温度で引き起こし、 反応中存在する酸素の量を調節して、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. 【請求項２】 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体積部未満である、請求項１に記載の
    方法。
  3. 【請求項３】 反応性ガス混合物をプラズマに曝すこと
    により反応を引き起こす、請求項１又は２に記載の方
    法。
  4. 【請求項４】 反応性ガス混合物が、更にキャリヤーガ
    スを含む、請求項１〜３のいずれか１項に記載の方法。
  5. 【請求項５】 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１〜４のいずれ
    か１項に記載の方法。
  6. 【請求項６】 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、Ｓｉ
    Ｏ2、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
    〜５のいずれか１項に記載の方法。
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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
JP4881422B2 (ja) 2012-02-22

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