JP6734046B2 - 膨張調節cmpパッド注型方法 - Google Patents
膨張調節cmpパッド注型方法 Download PDFInfo
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- JP6734046B2 JP6734046B2 JP2015246216A JP2015246216A JP6734046B2 JP 6734046 B2 JP6734046 B2 JP 6734046B2 JP 2015246216 A JP2015246216 A JP 2015246216A JP 2015246216 A JP2015246216 A JP 2015246216A JP 6734046 B2 JP6734046 B2 JP 6734046B2
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Classifications
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/721—Two or more polyisocyanates not provided for in one single group C08G18/73 - C08G18/80
- C08G18/724—Combination of aromatic polyisocyanates with (cyclo)aliphatic polyisocyanates
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- C—CHEMISTRY; METALLURGY
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Description
本発明は、半導体、光学及び磁性基板の少なくとも1つを平坦化するのに適した研磨パッドを提供する。この研磨パッドは、イソシアナート終端プレポリマー及び硬化系の反応生成物を含む、研磨上表面を有する。この研磨上層は更に、プレポリマーの4重量パーセントを超え8重量パーセント未満のレベルでポリマーミクロスフェアを含む。これらの研磨パッドは、除去速度が高く、ウェーハ内均一性が良好で、そしてコンディショニングプロセスに対する感受性が低下している。
[式中、CSは、75%インサイツコンディショニングでのブランケットTEOS除去速度(RR75%インサイツコンディショニング)及び50%インサイツコンディショニングでのブランケットTEOS除去速度(RR50%インサイツコンディショニング)の差、割る50%部分的インサイツコンディショニングでのブランケットTEOS除去速度として定義されるが、コンディショニングには、10.5のpHを持つ濃度12.5重量%(全て蒸留水で1:1比で希釈後)の平均粒径0.1μmを有するフュームドシリカスラリーを、9lbs(又は4.08kg)のコンディショナーダウンフォースで平均粒径150μm、ピッチ400μm及び突起部100μmを持つダイヤモンドコンディショナーと共に用いる]。CS除去速度の値は、定常状態研磨に到達後、又は典型的には少なくともウェーハ約10個後に達成される除去速度を表す。
実施例1
表1は、2つの比較実施例C1及びC2並びに本発明からの2つの実施例1及び2の研磨層の組成をリストしている。使用したイソシアナート終端プレポリマーは、9.1重量%の典型的な未反応イソシアナート(NCO)を含む、Chemtura Corporationから販売されているAdiprene(登録商標)L325とした。硬化系は、4,4’−メチレン−ビス(2−クロロアニリン)(MbOCA)又はMbOCAとVoralux(登録商標)HF 505(6個のヒドロキシル官能基及びMW約11,000の高分子量(MW)多官能ポリオール硬化剤)の組合せのいずれかとした。総活性水素(硬化系中のアミン及びヒドロキシル官能基として)対プレポリマー中のイソシアナート官能基のモル比により算出される反応化学量論は、全ての実施例について0.87とした。流体充填ポリマーミクロスフェアは、予備膨張(DE)及びドライ未膨張(DU)の両方とも、プレポリマーと混合してプレブレンドを形成した。Expancel(登録商標)551DE40d42、Expancel(登録商標)461DE20d70(両方ともDE等級)及びExpancel(登録商標)031DU40(DU等級)は、AkzoNobelから販売されている。総ポリマーミクロスフェアの量は、プレブレンド(プレポリマーとポリミクロスフェアの混合物)中に2.2〜5.25重量パーセントと様々であった。
Adiprene(登録商標)は、Chemtura Corporationのウレタンプレポリマー製品である。
Adiprene L325は、8.95〜9.25重量%の未反応NCOを有する、H12MDI/TDIとポリテトラメチレンエーテルグリコール(PTMEG)とのウレタンプレポリマーである。
*551DE40d42、**461DE20d70、及び***031DE40
551DE40d42、461DE20d70、及び031DE40は、Expancel(登録商標)という商標でAkzoNobelにより製造されている流体充填ポリミクロスフェアである。
研磨条件:
・スラリー:ILD3225(砥粒含量12.5%までDI水で1:1希釈;pH 10.5)
・POUフィルター:Pall 1.5μm
・コンディショナー:Kinik Company製のPDA33A-3;ダイヤモンドサイズ150μm、ダイヤモンドピッチ400μm、ダイヤモンド突起部100±15μm。
・パッド慣らし運転:90/108rpm(プラテン/コンディショニングディスク)、12lbs(5.4kg)で20分間、続いてダウンフォース9lbs(4.1kg)で10分間;高圧上昇(HPR)
・研磨中:コンディショニングダウンフォース9lbs(4.1kg)で完全インサイツコンディショニング
・研磨:93/87rpm(プラテン/ウェーハ)、ダウンフォース4.5psi(31kPa)で60秒間
高空隙率(低SG)ポリマーミクロスフェア充填ポリウレタン研磨パッドをケーキ成形型で注型することには重大な課題が存在していた。この課題は、内蔵窓が試みられたときに一層厳しくなった。これは主として、非常に粘性のプレブレンド及び液体ポリウレタン前駆体の乏しい流動性に起因した。
[式中、μは、充填系の粘度であり、μ0は、未充填材料の粘度であり、μ/μ0は、相対粘度であり、そしてΦは、充填剤の体積分率である]。
予備膨張又は未膨張のいずれかの流体充填ポリマーミクロスフェアは、温度を上昇させると膨張させることができる。膨張の程度は、温度、ポリマー殻のポリマー組成、封入された液体の沸点、及びこのポリマーミクロスフェアが予備膨張であるか未膨張であるかどうかに依存する。熱機械分析(TMA)は、種々の流体充填ポリマーミクロスフェアの膨張を測定するための優れたツールを提供する。TMA法は、TA Instrumentsにより製造されたThermal Mechanical Analyzer Q400で実施した。内径7.54mmのセラミックカップを、TMA Q400の試料台に置いた。外径6.6mmを有するアルミニウム蓋を台上のカップの内側に収めた。直径6.1mmの石英膨張プローブを、ダウンフォース0.06Nの予荷重で蓋を含むカップ中に下ろした。初期試料厚さをこの機器により測定して、得られる厚さを機器によりゼロ設定した。次にこの試料カップ及び蓋を台から取り外し、蓋をカップから取り外した。少量の流体充填ポリマーミクロスフェアをカップに入れ、次に蓋をカップ中に挿入した。このカップ及び蓋をTMA台に戻して、石英プローブを、試料及び蓋を含むカップ中に下ろした。再び厚さを測定して、機器により記録した。次に3℃/分の勾配速度及び0.06Nの予荷重での、30℃から250℃までの温度勾配に関してTMAをプログラムした。
Claims (6)
- 半導体、光学及び磁性基板の少なくとも1つを平坦化するのに適した研磨パッドの製造方法であって:
(i)
イソシアナート終端分子及び硬化剤から形成された液体ポリウレタン材料を得る工程であって、
前記液体ポリウレタン材料は、Tgel温度を有しており、そして流体充填ポリマーミクロスフェアを含有しており、
前記流体充填ポリマーミクロスフェアは、予備膨張及び未膨張の流体充填ポリマーミクロスフェアのブレンドであり、
前記予備膨張及び未膨張の流体充填ポリマーミクロスフェアは、それぞれTstart温度及びTmax温度を有しており、
前記T start 温度は、この温度以上で、予備膨張及び未膨張の流体充填ポリマーミクロスフェアの直径が増大する温度であり、
前記T max 温度は、この温度で、気体が予備膨張及び未膨張の流体充填ポリマーミクロスフェアを通り抜けて逃げることにより、膨張後及び未膨張の流体充填ポリマーミクロスフェアの直径が減少する温度であり、
未膨張の流体充填ポリマーミクロスフェアのTstart温度は、液体ポリウレタン材料のTgel温度よりも少なくとも5℃低い、工程と;
(ii)
予備膨張及び未膨張の流体充填ポリマーミクロスフェアのブレンドを含有する液体ポリウレタン材料を注型することにより、イソシアナート終端分子及び硬化剤を反応させる工程と;
(iii)
液体ポリウレタン材料中の予備膨張及び未膨張の流体充填ポリマーミクロスフェアのブレンドを、少なくとも未膨張の流体充填ポリマーミクロスフェアのTstartの温度まで加熱することによって、未膨張の流体充填ポリマーミクロスフェアの直径を増大させる工程であって、
前記加熱は、気体が予備膨張及び未膨張の流体充填ポリマーミクロスフェアを通り抜けて逃げるTmax温度よりも低い温度までであり、
前記加熱は、液体ポリウレタン材料中に予備膨張及び膨張後の流体充填ポリマーミクロスフェアのブレンドを形成するためである、工程と;
(iv)
液体ポリウレタン材料中の予備膨張及び膨張後の流体充填ポリマーミクロスフェアのブレンドを硬化することにより、液体ポリウレタン材料を、予備膨張及び膨張後の流体充填ポリマーミクロスフェアを含有するポリウレタンマトリックスへと凝固させる工程と;そして
(v)
予備膨張及び膨張後の流体充填ポリマーミクロスフェアを含有する硬化ポリウレタンマトリックスから研磨パッドを仕上げる工程であって、
前記予備膨張及び膨張後の流体充填ポリマーミクロスフェアの最終直径は、空気中でTmax温度から達成された直径より小さく、そして
前記予備膨張及び未膨張の流体充填ポリマーミクロスフェアに含まれる流体の大部分は、予備膨張及び膨張後の流体充填ポリマーミクロスフェア中に残存する工程と、を含み、
前記研磨パッドが、0.5〜0.65g/cm 3 の密度を有する、方法。 - 前記注型が、ケーキ成形型に行われることによって、ポリウレタンケーキ構造を形成し;そしてこのポリウレタンケーキ構造を成形型から外して、このケーキ構造を削って複数のポリウレタンシートにする追加の工程を含み;そして研磨パッドの形成が、このポリウレタンシートから行われる、請求項1記載の方法。
- 前記注型が、液体ポリウレタン材料並びに予備膨張及び膨張後の流体充填ポリマーミクロスフェアのブレンドを透明ブロックの周りに注ぎ入れる工程を含み、そして研磨パッドの形成が、研磨パッド中の透明窓を含む、請求項1記載の方法。
- 前記研磨パッド中に含まれる、ポリマーミクロスフェアの総量が、前記イソシアナート終端分子の4重量%を超え、8重量%未満のレベルである、請求項1〜3のいずれか一項に記載の方法。
- 前記予備膨張及び未膨張のポリマーマトリックスのブレンドの相対粘度が1.1〜7である、請求項1〜3のいずれか一項に記載の方法。
- 前記流体充填ポリマーミクロスフェアのポリマー殻が、無機粒子を取り込んでいる、請求項1〜3のいずれか一項に記載の方法。
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US11697183B2 (en) * | 2018-07-26 | 2023-07-11 | Taiwan Semiconductor Manufacturing Co., Ltd. | Fabrication of a polishing pad for chemical mechanical polishing |
KR102293765B1 (ko) * | 2019-11-21 | 2021-08-26 | 에스케이씨솔믹스 주식회사 | 연마패드, 이의 제조방법, 및 이를 이용한 반도체 소자의 제조방법 |
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US20150038066A1 (en) * | 2013-07-31 | 2015-02-05 | Nexplanar Corporation | Low density polishing pad |
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2014
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CN105710794B (zh) | 2019-02-05 |
CN105710794A (zh) | 2016-06-29 |
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KR102502964B1 (ko) | 2023-02-24 |
KR20160075349A (ko) | 2016-06-29 |
FR3030551A1 (fr) | 2016-06-24 |
JP2016128204A (ja) | 2016-07-14 |
US9586304B2 (en) | 2017-03-07 |
TW201623553A (zh) | 2016-07-01 |
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DE102015016427A1 (de) | 2016-06-23 |
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