JP4728402B2 - 支持体から物質を除去する方法 - Google Patents
支持体から物質を除去する方法 Download PDFInfo
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- JP4728402B2 JP4728402B2 JP2008542435A JP2008542435A JP4728402B2 JP 4728402 B2 JP4728402 B2 JP 4728402B2 JP 2008542435 A JP2008542435 A JP 2008542435A JP 2008542435 A JP2008542435 A JP 2008542435A JP 4728402 B2 JP4728402 B2 JP 4728402B2
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- sulfuric acid
- acid composition
- water vapor
- liquid
- water
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Description
回路の形成は連続した適用、加工、及び支持体からの様々な成分の選択的な除去、によって成される。様々な組成物が半導体ウエハー技術において、支持体からの特定の種類の成分の除去を目的に開発されて来た。例えば、普通SC-1と表示される組成物、それはNH4OH(29重量%)/(H2O2(30重量%)/水の容量比約1:1:5(又はそれより少し高い希釈比)の混合物を含む、は、典型的に、粒子を除去しそして疎水性のシリコン表面を再酸化するために用いられる。同様に、普通SC-2と表示される組成物、それはHCl(37重量%)/H2O2(30重量%)/水の容量比1:1:5(又はそれより少し高い希釈比)の混合物を含む、は、典型的に、金属を除去するために用いられる。更なる組成物、普通ピランハ(Piranha)組成物と呼ばれる、は、H2SO4(98重量%)/H2O2(30重量%)を容量比2:1から20:1で含み、そして典型的に有機汚染物質又はある種の金属層を除去するために用いられる。
本発明の上記の及び他の利点、及びそれらを得るための方法、及び本発明自体は、以下の本発明の実施態様の記載と伴う図を参照することにより、よりよく理解されるであろう。
図1は、20℃の硫酸(98重量%)が20℃の液状の水又は過酸化水素(30重量%)と、急速撹拌ビーカー中で混合されたときの得られた温度を示す。硫酸の容量画分が約100%〜約57%である領域Aにおいて、該硫酸/水混合物の温度は水含有量の増加と共に高くなる。画分が約56%〜約36%である領域Bにおいて、該硫酸/水混合物の温度は水含有量の増加と共に徐々に低下する。画分が約35%〜約10%である領域Cにおいて、混合物の温度は水含有量の増加と共に急速に低下する。過酸化水素と混合された硫酸の温度分布は同一の傾向となるが、最大温度は僅かにより低い。約110度(最終温度130℃)の最大温度上昇が約57容量%の硫酸と約43容量%の水の混合である硫酸/水混合物により得られた。また、最上の軸には、水:硫酸混合物の水対硫酸モル比が示される。領域AとBの境界は約2:1 水:硫酸であり、BとCのそれは約5:1である。
有利に、極めて優れた付着効率と均一性が、側部容器スプレー支柱40(SBSP)を用いて達成できる。しかし、SBSPにより、該室の面に垂直に、該回転台の回転軸の方向真直ぐに投与されたスプレーもまた、該中央スプレー支柱の近くに過剰に液体を付着し易い。該垂直スプレーは、更に該回転台のある配置においてウエハー群の間を通り抜ける液体を無駄にする。極めて優れた付着パターンは、スプレー支柱(そして特に該SBSP)からの液体のスプレーに、該室の主表面から垂直でないように及び/又は該回転台の中心から離れるように、角度をつけることにより観察される。角度をつけたスプレーにより該CSP近くの付着はより少なく集中するが、個々の角度が均一な被覆に十分な訳ではない。本発明の1つの実施態様において、スプレーの角度は一定である。本発明のもう1つの実施態様において、支持体(群)を保持する該回転台は該支持体表面への該液状硫酸組成物の投与中回転しており、そして該液状硫酸組成物は、該液体を該回転台との関係においてスイーピングにより角度を変えてスプレーすることにより投与される。この実施態様の1態様において、スプレーの角度は該液状硫酸組成物の1回の投与中に変化する。この実施態様のもう1つの態様において、処理サイクル中で複数回の液体投与が行われる場合、スプレーの角度は該液状硫酸組成物のある回の投与から次の回の投与において変化する。
A.試料調製
水試料がイオン注入ホトレジスト除去の有効性を評価するため次のように調製された:
直径200mmのシリコンウエハーがShipley UV6248 nm ホトレジストで被覆された。
ウエハーの幾つかにはレジストパターンがつくられ、その他は全面にレジスト層を設けた(夫々、パターンウエハー及びブランケット(blanket)ウエハー)。
パターン及びブランケットウエハーの両方に、40keV、5×1014又は1×1015 原子/cm2(5E14又は1E15)の投与量で砒素を注入した。
レジスト被覆されたウエハーの凡そ2×2cmの断片群が完全パターンウエハー及びブランケットウエハーの群から切り取られ、そして高温エポキシを持つキャリヤーウエハーの中心部近くに取付けられた。5個のレジスト試料が典型的に各々のキャリヤーウエハーに取付けられた:ブランケットレジスト(注入ナシ)、ブランケット5E14、パターン5E14、ブランケット1E15、及びパターン1E15。
加工後、該試料は明視野及び暗視野光学顕微鏡で試験された。表1は、ブランケット及びパターンレジスト試料の評価基準を示す。該パターン試料は様々なリソグラフィーのテストパターンからなる。該パターン試料上の細線配列及びブランケット膜の剥がしは、処理の剥がし効率の尺度を提供した。
該加工室の側壁上に流延された該硫酸/過酸化水素の液状組成物の温度は温度検知器41により測定された。この温度は1秒間隔で記録され該加工を通しての該室の温度の経過を提供した。
ウエハー上の最大温度の測定は、該ウエハー群に取付けた、特定の上昇温度で可逆的に色が変わるラベル(Omega Engineering, Stamford, CTからのTL-10 シリーズ)によりなされた。該ラベルは該剥れる化学品から保護するため高温エポキシを付けた0.7mmのガラス板で覆われた。
上記の方法で調製した該ウエハーは、FSI International, Inc., Chaska, MNから商業的に入手可能なZETA(登録商標)スプレー加工機中で、次の条件で処理された:
1.該試料ウエハーは、27個のウエハー運搬カセット20の溝13中に載せられそして他の溝は裸ウエハーで満たされた。このカセットと第2のバランスカセットは該回転台22上に載せられた。第2の試料ウエハーは必要な場合溝15中に乗せられた。
2.該回転台22は、120rpmで回転し、再循環浴50からの加熱した硫酸(110℃)が、中央36及び側部40スプレー支柱の両方から凡そ5l/分の速度で3分間、該ウエハー上に投与された。50cc/分の過酸化水素が該投与の最後の凡そ1分間、該流れに添加された。この工程は該ウエハーを予熱し且つ完全に濡らすことを提供した。
3.該回転台は120rpmで回転し、該混合多重管90からの新規な硫酸組成物(硫酸及び過酸化水素-SPM)の混合物の900cc/分の流れが、該中央スプレー支柱36から30秒間投与された。該硫酸は、過酸化水素添加前に、ライン内赤外線加熱器により95℃に予熱された。SPM組成物の混合比は、夫々の処理において表2に挙げたように変化した。
4.該加工は、本発明の処理において凡そ8l/分の95℃脱イオン水44が回転台22上に投与され水蒸気を発生した以外は上記3のようにして、6分間継続した。
5.6分間の脱イオン水洗浄の後、該試料は、80℃のSC-1溶液(1:1:15容量比のアンモニア:過酸化水素:水)で75秒処理された。
6.該試料は脱イオン水中で洗浄され窒素ガス中で乾燥された。
実施例1:上記からの処理プロセスEが、SPMの10:1混合物を使用し、水蒸気添加のあり、なし、により2回行なわれた(表2のプロトコール3及び4)。該室の壁に対して流延した(cast off against)該液体の温度は該側部容器温度検出器41により測定された。図4は、2つの処理の温度分布を示す。両方の場合において、硫酸の該5l/分の再循環流れは、最初の3分間の処理において、側部容器検出器を凡そ65℃に加熱した。3〜9分で"SPM"比較例の温度は凡そ7℃低下し58℃近くになった。対照的に、該"SPM+水蒸気"の本発明の実施例は、同じ時間で60℃上昇し125℃になった。該室への水蒸気の添加は、該流延した液体の温度を著しく上昇させた。
該再循環タンクからの硫酸の5l/分の流れが4区分において該中央及び側部スプレー支柱から投与された:20rpmの時計方向回転台回転で45秒間、300rpmの時計方向で45秒間、20rpmの逆時計方向で45秒間、及び300rpm逆時計方向で45秒間。
10:1SPMの1600cc/分の流れ(該再循環タンクからの110℃硫酸の1500cc/分及び新規な20℃の過酸化水素の150cc/分)が2区分において該中央及び側部スプレー支柱から投与された:120rpm時計方向で120秒、120rpm逆時計方向で120秒。8l/分の95℃の水が該回転台上に投与され水蒸気を発生した。増加した化学品暴露時間、上昇した温度、及び回転の方向転換の組合せが該パターン及びブランケット1E15インプラントレジストの完全な除去(全てスコア"5")をもたらした。
Claims (18)
- a)表面に物質を有する半導体支持体を処理室中に置き;
b)硫酸及び/又はその脱水種及び前駆体を含む液状硫酸組成物を、第1の供給ラインから、支持体表面を実質的均一に被覆するのに有効な量で支持体表面に投与し;
c)該支持体表面上の液状硫酸組成物を、第2の供給ラインから投与される水蒸気により、その温度が水蒸気に暴露する前の液状硫酸組成物の温度より高くなるのに有効な量の水蒸気に暴露し;その場合、水蒸気への暴露時における液状硫酸組成物の水/硫酸モル比は5:1未満であり、そして
d)該支持体から物質を除去する、
ことを含む、半導体支持体から物質を除去する方法。 - 該液状硫酸組成物は、その温度が、(i)水蒸気に暴露する前の支持体上の液状硫酸組成物の温度と(ii)水蒸気の温度、の両方よりも高くなるのに有効な量の水蒸気に暴露される、請求項1に記載の方法。
- 水蒸気への暴露時における液状硫酸組成物の水/硫酸モル比は1:2未満である、請求項1に記載の方法。
- 水蒸気が80℃から110℃の温度で供給される、請求項1に記載の方法。
- 物質がホトレジストである、請求項1に記載の方法。
- 支持体が液状硫酸組成物の支持体表面への投与中に回転し、そして液状硫酸組成物は、スイーピングによる支持体の回転中心に対して変化する角度でのスプレーによって投与される、請求項1に記載の方法。
- スプレーの角度が、該液状硫酸組成物の1回の投与の間に変化する、請求項1に記載の方法。
- 該水蒸気が沸騰水から発生され、水蒸気形成装置により該処理槽の内部又は外部のどちらかで水蒸気を形成する、請求項1に記載の方法。
- 該液状硫酸組成物が、複数回の不連続パルスによって支持体表面上に投与される、請求項1に記載の方法。
- a)表面に物質を有する半導体支持体を処理室中に置き;
b)硫酸及び/又はその脱水種及び前駆体を含む液状硫酸組成物を、第1の供給ラインから、支持体表面を実質的均一に被覆するのに有効な量で支持体表面に投与し;
c)該支持体表面上の液状硫酸組成物を、第2の供給ラインから投与される水蒸気により、その温度が水蒸気に暴露する前の液状硫酸組成物の温度より高くなるのに有効な量の水蒸気に暴露し;その場合、水蒸気への暴露時における液状硫酸組成物の水/硫酸モル比は5:1未満であり、そして、該液状硫酸組成物は、該液状硫酸組成物の該水蒸気への暴露の前に、液状の水の添加によって希釈されず;そして
d)該支持体から物質を除去する、
ことを含む、半導体支持体から物質を除去する方法。 - a)表面に物質を有する半導体支持体を処理室中に置き;
b)次のi)及びii)の連続的2工程からなる処理プロセス:i)硫酸及び/又はその脱水種及び前駆体を含む液状硫酸組成物を、第1の供給ラインから、支持体表面を実質的均一に被覆するのに有効な量で支持体表面に投与し;ii)該支持体表面上の液状硫酸組成物を、第2の供給ラインから投与される水蒸気により、その温度が水蒸気に暴露する前の液状硫酸組成物の温度より高くなるのに有効な量の水蒸気に暴露し;そして
c)該支持体から物質を除去し、その場合、水蒸気への暴露時における液状硫酸組成物の水/硫酸モル比は5:1未満である、
ことを含む、半導体支持体から物質を除去する方法。 - 水蒸気への暴露時における液状硫酸組成物の水/硫酸モル比は2:1未満である、請求項1、10及び11の何れか1項に記載の方法。
- 液状硫酸組成物の投与中又は投与後、処理室中に酸化剤が導入される、請求項1に記載の方法。
- 該酸化剤が過酸化水素である、請求項13に記載の方法。
- 該酸化剤がオゾンである、請求項13に記載の方法。
- 液状硫酸組成物の投与中又は投与後、処理室中に酸化剤が導入される、請求項10及び11の何れか1項に記載の方法。
- 水蒸気への暴露の前に、液状硫酸組成物が130℃から200℃の温度で投与される、請求項1、10及び11の何れか1項に記載の方法。
- 水蒸気が処理室の外で発生され、そして水蒸気として処理室中に導入される、請求項1,10及び11の何れか1項に記載の方法。
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KR20190060997A (ko) | 2016-09-30 | 2019-06-04 | 도오꾜오까고오교 가부시끼가이샤 | 세정 조성물, 세정 방법, 및 반도체의 제조 방법 |
US11441101B2 (en) | 2016-09-30 | 2022-09-13 | Tokyo Ohka Kogyo Co., Ltd. | Cleaning composition, cleaning method, and method for manufacturing semiconductor |
Also Published As
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JP2009517865A (ja) | 2009-04-30 |
US8859435B2 (en) | 2014-10-14 |
US20130115782A1 (en) | 2013-05-09 |
TW200731029A (en) | 2007-08-16 |
US7592264B2 (en) | 2009-09-22 |
US20070161248A1 (en) | 2007-07-12 |
CN101900956A (zh) | 2010-12-01 |
JP2012069994A (ja) | 2012-04-05 |
US8394228B2 (en) | 2013-03-12 |
KR20090130197A (ko) | 2009-12-18 |
TWI406110B (zh) | 2013-08-21 |
US20100018951A1 (en) | 2010-01-28 |
JP2010147493A (ja) | 2010-07-01 |
KR20080071988A (ko) | 2008-08-05 |
CN101312794A (zh) | 2008-11-26 |
JP4965673B2 (ja) | 2012-07-04 |
WO2007062111A1 (en) | 2007-05-31 |
JP2010157749A (ja) | 2010-07-15 |
CN101312794B (zh) | 2012-07-04 |
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