JP2019069507A - 多孔質ポリウレタン研磨パッドおよび多孔質ポリウレタン研磨パッドの製造方法 - Google Patents
多孔質ポリウレタン研磨パッドおよび多孔質ポリウレタン研磨パッドの製造方法 Download PDFInfo
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- JP2019069507A JP2019069507A JP2018155575A JP2018155575A JP2019069507A JP 2019069507 A JP2019069507 A JP 2019069507A JP 2018155575 A JP2018155575 A JP 2018155575A JP 2018155575 A JP2018155575 A JP 2018155575A JP 2019069507 A JP2019069507 A JP 2019069507A
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- pore size
- polishing pad
- porous polyurethane
- maximum peak
- pores
- Prior art date
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Images
Classifications
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- B24D3/20—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially organic
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Abstract
Description
多孔質ポリウレタン研磨パッドであって、
ポリウレタン樹脂およびポリウレタン樹脂中で分布した孔を含んで成り、
研磨パッドの断面積に基づく孔の孔サイズ分布において、最大ピークでの孔サイズが平均孔サイズよりも小さく、
最大ピークでの孔サイズが18〜28μmであり、
平均孔サイズが24〜36μmであり、ならびに、
最大ピークでの孔サイズよりも15μm以上大きい孔サイズを有する孔の断面積の合計が、最大ピークでの孔サイズよりも10μm以上15μm未満大きい孔サイズを有する孔の断面積の合計よりも大きい、多孔質ポリウレタン研磨パッドが供される。
多孔質ポリウレタン研磨パッドの製造方法であって、
ウレタン系プレポリマー、硬化剤、固相発泡剤、反応速度制御剤、およびシリコーン系界面活性剤を混合して孔を形成しつつ混合物を成形する際にて、不活性ガスを注入することを含み、
ウレタン系プレポリマー100重量部を基準として1〜3重量部の量の固相発泡剤を用いる、製造方法が供される。
一態様に係る多孔質ポリウレタン研磨パッドは、ポリウレタン樹脂およびポリウレタン樹脂中で分布した孔(又は細孔;pore)を含んで成り、研磨パッドの断面積に基づく孔の孔サイズ分布において、最大ピークでの孔サイズが平均孔サイズよりも小さく、最大ピークでの孔サイズが18〜28μmであり、平均孔サイズが24〜36μmであり、ならびに、最大ピークでの孔サイズよりも15μm以上大きい孔サイズを有する孔の断面積の合計が、最大ピークでの孔サイズよりも10μm以上15μm未満大きい孔サイズを有する孔の断面積の合計よりも大きい。
孔は、ポリウレタン樹脂中に分散するように存在する。具体的には、孔は、固相発泡剤として使用される熱膨張したマイクロカプセルから生じ得る又は不活性ガスから形成され得る。
多孔質ポリウレタン研磨パッドは、第3級アミン系化合物および有機金属化合物からなる群から選択される少なくとも1つの反応速度制御剤;ならびにシリコーン系界面活性剤を更に含んで成ってよい。
シリコーン系界面活性剤は、形成される孔が互いに重なって合体する(又は融合する又は結合する又は癒合する;coalesce)ことを抑制するように作用し得る。界面活性剤の種類は、研磨パッドの製造に一般的に用いられているものであれば特に限定されない。
多孔質ポリウレタン研磨パッドは1〜5mmの厚さを有し得る。具体的には、多孔質ポリウレタン研磨パッドは、1〜3mm、1〜2.5mm、1.5〜5mm、1.5〜3mm、1.5〜2.5mm、1.8〜5mm、1.8〜3mm、又は1.8〜2.5mmであり得る。研磨パッドの厚さが上記範囲内であれば、研磨パッドとしての基本的な物理的特性を十分に示すことが可能である。
一態様では、多孔質ポリウレタン研磨パッドの製造方法であって、ウレタン系プレポリマー、硬化剤、固相発泡剤、反応速度制御剤、およびシリコーン系界面活性剤を混合して孔を形成しつつ混合物を成形する際にて、不活性ガスを注入することを含み、ウレタン系プレポリマー100重量部を基準として1〜3重量部の量の固相発泡剤を用いる、製造方法が供される。
ウレタン系プレポリマーは、上述のようにイソシアネート化合物とポリオールとを反応させることにより作製され得る。研磨パッドにおけるイソシアネート化合物およびポリオールの具体的な種類は上記に例示したとおりである。
硬化剤は、アミン化合物およびアルコール化合物からなる群から選択される少なくとも1つであり得る。具体的には、硬化剤は、芳香族アミン、脂肪族アミン、芳香族アルコール、および脂肪族アルコールからなる群から選択される少なくとも1つを含んで成り得る。
固相発泡剤は、熱膨張(即ちサイズ制御された)マイクロカプセルであり、5〜200μmの平均孔サイズを有するマイクロバルーンの構造であり得る。熱膨張(即ちサイズ制御された)マイクロカプセルは、熱的に膨張可能なマイクロカプセルを熱膨張させることによって得られ得る。
反応速度制御剤は、第3級アミン系化合物および有機金属化合物からなる群から選択される少なくとも1つの反応促進剤であり得る。具体的には、例えば、反応速度制御剤は、トリエチレンジアミン(TEDA)、ジメチルエタノールアミン(DMEA)、テトラメチルブタンジアミン(TMBDA)、2−メチル−トリエチレンジアミン、ジメチルシクロヘキシルアミン(DMCHA)、トリエチルアミン(TEA)、トリイソプロパノールアミン(TIPA)、1,4−ジアザビシクロ(2,2,2)オクタン、ビス(2−メチルアミノエチル)エーテル、トリメチルアミノエチルエタノールアミン、N,N,N,N,N”−ペンタメチルジエチレントリアミン、ジメチルアミノエチルアミン、ジメチルアミノプロピルアミン、ベンジルジメチルアミン、N−エチルモルホリン、N,N−ジメチルアミノエチルモルホリン、N,N−ジメチルシクロヘキシルアミン、2−メチル−2−アザノルボルネン、ジブチル錫ジラウレート、第一錫オクトエート、ジブチル錫ジアセテート、ジオクチル錫ジアセテート、ジブチル錫マレエート、ジブチル錫ジ−2−エチルヘキサノエート、およびジブチル錫ジメルカプチドから成る群から選択される少なくとも1つを含んで成り得る。具体的には、反応速度制御剤は、ベンジルジメチルアミン、N,N−ジメチルシクロヘキシルアミン、およびトリエチルアミンからなる群から選択される少なくとも1つであり得る。
シリコーン系界面活性剤は、形成される孔が互いに重なって合体する(又は融合する又は結合する又は癒合する;coalesce)ことを抑制するように作用し得る。
ウレタン系プレポリマー、硬化剤、固相発泡剤、反応速度制御剤、およびシリコーン系界面活性剤を混合して反応させる際に、不活性ガスを供給し、それによって研磨パッド内に孔を形成する。不活性ガスの種類は、プレポリマーと硬化剤との間における反応に関与しないガスであれば特に限定されない。例えば、不活性ガスとしては、窒素ガス(N2)、アルゴンガス(Ar)およびヘリウム(He)から成る群から選択される少なくとも1つであってよい。具体的には、不活性ガスは、窒素ガス(N2)又はアルゴンガス(Ar)であってよい。
ウレタン系プレポリマーと硬化剤とは、固体状のポリウレタンを形成するためこれらを混合する際に相互に反応する。当該固体状のポリウレタンは次いでシート等に成形される。具体的には、ウレタン系プレポリマー中のイソシアネート末端基は、硬化剤中のアミン基、アルコール基等と反応することが可能である。この場合、ウレタン系プレポリマーと硬化剤との反応に関与することなく、原材料中に不活性ガスおよび固相発泡剤が均一に分散して孔が形成される。
成形については金型を用いて実施する。具体的には、混合ヘッド等で十分に攪拌させた原材料(即ち、ウレタン系プレポリマー、硬化剤、固相発泡剤、反応速度制御剤、シリコーン系界面活性剤および不活性ガスを含んで成る混合物)を金型内に注入して金型内部に充填し得る。ウレタン系プレポリマーと硬化剤との間の反応を金型内で完了させ、それにより金型の形状に適合する固化したケーキ状の成形体が製造される。
以下、下記の実施例により本発明を詳細に説明する。しかしながら、これらの実施例は本発明を例示するために記載しており、本発明の範囲が当該実施例に限定されるものではない。
1−1:デバイスの形態
ウレタン系プレポリマー、硬化剤、不活性ガスおよび反応速度制御剤のための供給ラインを備えた鋳造機にて、未反応のNCOの含有量が9.1重量%であるPUGL−550D(SKC社製)をプレポリマータンクに充填し、硬化剤タンクにビス(4−アミノ−3−クロロフェニル)メタン(石原製)を充填した。不活性ガスとしての窒素(N2)と、反応速度制御剤としての反応促進剤(エアープロダクツ社製のブランド名A1の第3級アミン化合物)を用意した。更に、固相発泡剤(平均孔サイズ20μmを有する、アクゾノーベル社製のブランド名 Expancel461 DET 20 d40)2重量部とシリコーン系界面活性剤1重量部(エボニック社製のブランド名B8462)をウレタン系プレポリマー100重量部に対して予め混合し、次いでプレポリマータンクに充填した。
ウレタン系プレポリマー、硬化剤、反応速度制御剤、および不活性ガスを、各供給ラインを通じて一定速度で混合ヘッドに供給しながら攪拌した。その際、ウレタン系プレポリマー中のNCO基と硬化剤中の反応基とのモル当量比を1:1に調整し、全供給量を10kg/分の速度に維持した。更に、ウレタン系プレポリマー、硬化剤、固相発泡剤、反応速度制御剤、およびシリコーン系界面活性剤の全体積を基準として、25%の体積で不活性ガスを一定供給した。ウレタン系プレポリマー100重量部を基準として1重量部の量で反応速度制御剤を供給した。
実施例1で作製した研磨パッドの特性を下記条件および手順に従い測定した。その結果を下記の表1と図1および図2に示す。
ショアD硬度を測定した。研磨パッドを2cm×2cm(厚さ2mm)のサイズに切断し、次いで温度23℃、30℃、50℃および70℃ならびに湿度50±5%の条件下で16時間置いた。その後、硬度計(D型硬度計)を用いて研磨パッドの硬度を測定した。
研磨パッドを4cm×8.5cmの矩形(厚さ2mm)に切断し、次いで温度23±2℃および湿度50±5%の湿度の条件下で16時間置いた。比重計を用いて研磨パッドの比重を測定した。
研磨パッドを2cm×2cmの正方形(厚さ2mm)に切断し、走査型電子顕微鏡(SEM)を用いて100倍の倍率で観察した。画像解析ソフトウェアを用いて画像を取得し、その画像から全孔のサイズを測定して、全孔のサイズから平均孔サイズ、孔サイズ分布および孔面積比を算出した。このようにして算出された孔サイズ分布を図1に示し、SEM写真を図2に示す。
ユニバーサル試験機(UTM)を用いて50mm/分の速度で研磨パッドを試験する間に破壊直前の極限強度を測定した。
引張強さ測定と同じ方法で試験を実施した。破断直前の最大変形量を測定し、初期長さに対する最大変形量の比を百分率(%)で表した。
引張強度測定と同じ方法で試験を実施した。初期弾性域における歪み−応力曲線の傾きを計算した。
研磨パッドの2.5mm×1.9mmの領域の表面粗さを3Dスコープを用いて測定し、ISO25178−2:2012の粗さ規格に従い表面粗さ(Ra)を計算した。
CVD法により形成したタングステン層を有する300mmのサイズを有するシリコンウェハをCMP研磨装置に設置した。シリコンウェハのタングステン層を下方に向けつつ、プラテン上に設けた研磨パッドにシリコンウェハを設置した。その後、115rpmの速度でプラテンを30秒間回転させつつ2.8psiの研磨荷重でタングステン層を研磨し、研磨パッド上にタングステンスラリーを190ml/分の速度で供給した。研磨完了後、シリコンウェハをキャリアから取り外し、スピンドライヤに取り付け、純水(DIW)で洗浄し、次いでエアで15秒間乾燥させた。(4点プローブ付)接触式シート抵抗測定装置を用いて、研磨前後の乾燥シリコンウェハの層厚を測定した。次いで、下記式1により研磨速度を算出した。
研磨速度=シリコンウェハの研磨厚(Å)/研磨時間(分)
Claims (12)
- 多孔質ポリウレタン研磨パッドであって、
ポリウレタン樹脂およびポリウレタン樹脂中で分布した孔を含んで成り、
研磨パッドの断面積に基づく孔の孔サイズ分布において、最大ピークでの孔サイズが平均孔サイズよりも小さく、
最大ピークでの孔サイズが18〜28μmであり、
平均孔サイズが24〜36μmであり、ならびに、
最大ピークでの孔サイズよりも15μm以上大きい孔サイズを有する孔の断面積の合計が、最大ピークでの孔サイズよりも10μm以上15μm未満大きい孔サイズを有する孔の断面積の合計よりも大きい、多孔質ポリウレタン研磨パッド。 - 孔の断面積の合計が100%である場合に基づく、最大ピークでの孔サイズよりも15μm以上大きい孔サイズを有する孔の断面積の合計と最大ピークでの孔サイズよりも10μm以上15μm未満大きい孔サイズを有する孔の断面積の合計との差が、1〜10%である、請求項1に記載の多孔質ポリウレタン研磨パッド。
- 孔の断面積の合計が100%である場合に基づく、最大ピークでの孔サイズよりも15μm以上大きい孔サイズを有する孔の断面積の合計と最大ピークでの孔サイズよりも10μm以上15μm未満大きい孔サイズを有する孔の断面積の合計との差が、5〜9%である、請求項1に記載の多孔質ポリウレタン研磨パッド。
- 孔が、固相発泡剤により形成された第1孔および気相発泡剤により形成された第2孔を含んで成る、請求項1に記載の多孔質ポリウレタン研磨パッド。
- 第2孔が最大ピークでの孔サイズよりも15μm以上大きい孔サイズを有する孔および最大ピークでの孔サイズよりも小さい孔サイズを有する孔を含んで成る、請求項4に記載の多孔質ポリウレタン研磨パッド。
- 第3級アミン系化合物および有機金属化合物から成る群から選択される少なくとも1つの反応速度制御剤、ならびにシリコーン系界面活性剤を更に含んで成る、請求項1に記載の多孔質ポリウレタン研磨パッド。
- 反応速度制御剤が、トリエチレンジアミン、ジメチルエタノールアミン、テトラメチルブタンジアミン、2−メチル−トリエチレンジアミン、ジメチルシクロヘキシルアミン、トリエチルアミン、トリイソプロパノールアミン、1,4−ジアザビシクロ(2,2,2)オクタン、ビス(2−メチルアミノエチル)エーテル、トリメチルアミノエチルエタノールアミン、N,N,N,N,N”−ペンタメチルジエチレントリアミン、ジメチルアミノエチルアミン、ジメチルアミノプロピルアミン、ベンジルジメチルアミン、N−エチルモルホリン、N,N−ジメチルアミノエチルモルホリン、N,N−ジメチルシクロヘキシルアミン、2−メチル−2−アザノルボルネン、ジブチル錫ジラウレート、第一錫オクトエート、ジブチル錫ジアセテート、ジオクチル錫ジアセテート、ジブチル錫マレエート、ジブチル錫ジ−2−エチルヘキサノエート、およびジブチル錫ジメルカプチドから成る群から選択される少なくとも1つを含んで成る、請求項6に記載の多孔質ポリウレタン研磨パッド。
- 最大ピークでの孔サイズが平均孔サイズよりも1〜10μm小さい、請求項1に記載の多孔質ポリウレタン研磨パッド。
- タングステンの研磨速度が1である場合にて、酸化ケイ素(SiOx)の研磨速度が0.8〜0.99である、請求項1に記載の多孔質ポリウレタン研磨パッド。
- 多孔質ポリウレタン研磨パッドの製造方法であって、
ウレタン系プレポリマー、硬化剤、固相発泡剤、反応速度制御剤、およびシリコーン系界面活性剤を混合して孔を形成しつつ混合物を成形する際にて、不活性ガスを注入することを含み、
ウレタン系プレポリマー100重量部を基準として1〜3重量部の量の固相発泡剤を用いる、製造方法。 - 反応速度制御剤が、第3級アミン系化合物および有機金属化合物から成る群から選択される少なくとも1つの反応促進剤である、請求項10に記載の多孔質ポリウレタン研磨パッドの製造方法。
- 研磨パッドの断面積に基づく孔の孔サイズ分布において、最大ピークでの孔サイズが平均孔サイズよりも小さく、
最大ピークでの孔サイズが18〜28μmであり、
平均孔サイズが24〜36μmであり、ならびに、
最大ピークでの孔サイズよりも15μm以上大きい孔サイズを有する孔の断面積の合計が、最大ピークでの孔サイズよりも10μm以上15μm未満大きい孔サイズを有する孔の断面積の合計よりも大きい、請求項10に記載の多孔質ポリウレタン研磨パッドの製造方法。
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