JPWO2009131133A1 - 研磨剤及びこの研磨剤を用いた基板の研磨方法 - Google Patents
研磨剤及びこの研磨剤を用いた基板の研磨方法 Download PDFInfo
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- JPWO2009131133A1 JPWO2009131133A1 JP2010509192A JP2010509192A JPWO2009131133A1 JP WO2009131133 A1 JPWO2009131133 A1 JP WO2009131133A1 JP 2010509192 A JP2010509192 A JP 2010509192A JP 2010509192 A JP2010509192 A JP 2010509192A JP WO2009131133 A1 JPWO2009131133 A1 JP WO2009131133A1
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- abrasive
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- weight
- water
- additive
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Abstract
Description
[2]エチレンイミン重合体又はその誘導体
[3]アリルアミン重合体又はその誘導体
[4]ジアリルアミン重合体又はその誘導体
[5]ビニルアミン重合体又はその誘導体
[6]下記一般式(I)〜(IV)の群から選ばれる少なくとも1種類の単量体成分を含む重合体
(3)前記4価の金属水酸化物粒子の平均粒径が、1nm以上400nm以下である前記(1)または(2)に記載の研磨剤。
(1)アミノ糖又はアミノ糖をもつ多糖類、(2)エチレンイミン重合体又はその誘導体、(3)アリルアミン重合体又はその誘導体、(4)ジアリルアミン重合体又はその誘導体、(5)ビニルアミン重合体又はその誘導体、(6)下記一般式(I)〜(IV)の群から選ばれる少なくとも1種類の単量体成分を含む重合体からなる群から、少なくとも一成分が選ばれる。これらは単独で又は二種類以上組み合わせて使用することができる。以下、(1)〜(6)について説明する。
(1)アミノ糖又はアミノ糖をもつ多糖類
本発明において、アミノ糖とは、アミノ基を有する糖類であり、グルコサミン、ガラクトサミンがあげられ、これらの誘導体でもよい。
本発明において、エチレンイミン重合体とは、エチレンイミンを重合したポリマのことであり、直鎖であっても、分岐構造を有していてもよい。また、エチレンイミン重合体は、アミノ基を有するが、このアミノ基は1級、2級、3級、4級アミンのいずれであってもよく、分子内に複数種混在していてもよい。
本発明において、アリルアミン重合体、ジアリルアミン重合体、ビニルアミン重合体(以下、これらの重合体をまとめてアリルアミン系重合体ということがある)とは、アリルアミン、ジアリルアミン、ビニルアミン(以下これらの化合物をアリルアミン系単量体ということがある)を単量体の一つとして重合させた重合体のことであり、これらの誘導体であっても、他の単量体との共重合体であってもよい。また、これらの重合体はアミノ基を有するが、1級、2級、3級、4級のいずれであってもよく、また複数種有していてもよい。
(I)〜(IV)の群から選ばれる少なくとも1種類の単量体成分を含む重合体は、下記(I)〜(IV)の群から選ばれる少なくとも1種類の単量体成分を単量体の一つとして重合させた重合体のことである。
上記一般式(I)〜(IV)において、R1〜R5で表される一価の有機基としては、特に制限はないが、具体的には、例えば、水素原子、炭素数1〜6のアルキル基、フェニル基、ベンジル基、ジフルオロメチル基、トリフルオロメチル基、シアノ基等を挙げることができ、それらの基が置換基を有していてもよい。中でも、入手性や水への溶解性の観点から、水素原子又は炭素数1〜6のアルキル基が好ましく、水素原子又はメチル基がより好ましい。
430gのCe(NH4)2(NO3)6を7300gの純水に溶解し、次いでこの溶液に240gのアンモニア水(25%水溶液)を混合・攪拌して、160gの水酸化セリウム(黄白色)を得た。
キトサン500(和光純薬工業株式会社製、0.5%酢酸水溶液にキトサンを0.5%溶解した場合の粘度500mPa・s)1重量%、酢酸0.3重量%及び水98.7重量%を含有する濃縮添加液を調製した。この濃縮添加液10g、上記で得た濃縮水酸化セリウムスラリ100g並びに水390gを混合し、5重量%のイミダゾール水溶液をpHが5.6になるまで加えて研磨剤を調製した。
キトサン50(和光純薬工業株式会社製、0.5%キトサン、0.5%酢酸水溶液の粘度50mPa・s)1重量%、酢酸0.3重量%及び水98.7重量%を含有する濃縮添加液を調製した。この濃縮添加液10g、上記で得た濃縮水酸化セリウムスラリ100g並びに水390gを混合し、5重量%のイミダゾール水溶液をpHが5.6になるまで加えて研磨剤を調製した。
キトサン5(和光純薬工業株式会社製、0.5%キトサン、0.5%酢酸水溶液の粘度5mPa・s)1重量%、酢酸0.3重量%及び水98.7重量%を含有する濃縮添加液を調製した。この濃縮添加液10g、上記で得た濃縮水酸化セリウムスラリ100g並びに水390gを混合し、5重量%のイミダゾール水溶液をpHが5.6になるまで加えて研磨剤を調製した。
上記濃縮水酸化セリウムスラリ100gと水400gを混合し、5重量%のイミダゾール水溶液を所定のpHになるまで加えて研磨剤を調製した。
酸化セリウム粒子1kg、市販のポリアクリル酸アンモニウム塩水溶液(40重量%)23g及び脱イオン水8977gを混合し、攪拌しながら超音波分散を行った。1ミクロンフィルターでろ過をし、さらに脱イオン水を加えることにより酸化セリウム5重量%の濃縮酸化セリウムスラリを得た。上記の濃縮酸化セリウムスラリ100gと水900gを混合し、pHが4になるまで1N硝酸を加え、研磨剤(固形分:0.5重量%)を調製した。
研磨装置(株式会社荏原製作所製の型番EPO−111)の基板ホルダーに、直径200mmのシリコン(Si)基板上に膜厚1000nmの酸化珪素(SiO2)を全面に形成した評価用ウエハを固定し、一方で直径600mmの研磨定盤に多孔質ウレタン樹脂製の研磨パッドIC−1000(ロデール社製型番、溝形状:パーフォレート)を貼り付けた。
パターンウエハの研磨特性の評価には、市販のCMP特性評価用ウエハ(SEMATECH 864、直径200mm)を用いた。図1は、評価用ウエハの部分拡大断面図であり、図2は、評価用ウエハの上面図であり、図3は、図2の凹凸の領域分布を示す部分拡大図である。この評価用ウエハは、シリコン基板3上へCVD法により厚み150nmの窒化珪素(SiN)膜2を成膜、その後深さ470nm(320nm+150nm)の溝を形成し、さらにHDP−CVD(高密度プラズマ化学気相成長法)により厚み610nmの酸化珪素(SiO2)膜1を形成することで作製されている。
膜厚測定には、光干渉式膜厚装置(ナノメトリクス社製商品名Nanospec AFT−5100)を用いて、センターの、L=500μm、S=500μmパターン(以下、500/500と呼ぶ)、L=100μm、S=100μmパターン(以下、100/100と呼ぶ)、L=25μm、S=25μmパターン(以下、25/25と呼ぶ)、それぞれの凸部と凹部のSiO2残膜厚を測定した。また、凸部は、SiO2が除去された場合、SiN残膜厚を測定した。
上記評価用ウエハに対し、まず荒削り研磨を実施した。研磨装置(株式会社荏原製作所製 型番EPO−111)の基板ホルダーに上記評価用ウエハを固定し、一方で直径600mmの研磨定盤にIC−1000(ロデール社製型番、溝形状:パーフォレート)研磨パッドを貼り付けた。研磨パッド上に絶縁膜4面がパッドと接するように基板ホルダーを押し付け、加工荷重を30kPaに設定した。研磨パッド上に、上記濃縮水酸化セリウムスラリ500gと水500gを混合し、5重量%のイミダゾール水溶液をpHが6.5になるまで加えて調製した研磨剤(水酸化セリウム濃度0.5%)を、200mL/分の速度で滴下しながら、定盤と基板ホルダーとをそれぞれ50rpmで作動させて評価用ウエハを140秒間研磨し、荒削り済みウエハを得た。センターの100/100の凸部SiO2残膜厚は約200nmであった。
研磨剤として、ダイキトサン100D(VL)(大日精化工業株式会社製極低粘度キトサン、脱アセチル化度98%以上。0.5%の酢酸水にキトサンを0.5%溶解した場合の溶液の粘度6mPa・s)2重量%、酢酸1重量%及び水97重量%を含有する濃縮添加液を調製した。この濃縮添加液を48g、上記で得た濃縮水酸化セリウムスラリ320g、水1232gを混合し、10重量%のイミダゾール水溶液をpHが6.5になるまで加えて調製した研磨剤(水酸化セリウム濃度0.2%、ダイキトサン100D(VL)濃度0.06%)を用い、研磨パッドとして、ショアD硬度87のポリウレタン製パッドを用い、前記仕上げ研磨を実施した。
研磨剤として、上記ダイキトサン100D(VL)2重量%、酢酸1重量%、ポリビニルアルコール(和光純薬工業株式会社製、重合度約2000)1重量%、及び水96重量%を含有する濃縮添加液を調製した。この濃縮添加液を48g、上記で得た濃縮水酸化セリウムスラリ320g、水1232gを混合し、10重量%のイミダゾール水溶液をpHが6.5になるまで加えて調製した研磨剤(水酸化セリウム濃度0.2%、ダイキトサン100D(VL)濃度0.06%、ポリビニルアルコール濃度0.03%)を用い、研磨パッドとして、ショアD硬度87のポリウレタン製パッドを用い、前記仕上げ研磨を実施した。
研磨剤として、比較例2の濃縮酸化セリウムスラリ100g、市販のポリアクリル酸アンモニウム塩水溶液(40重量%)5g、水895gを混合し、pHが4.5になるまで1N硝酸を加えて調製した研磨剤(酸化セリウム濃度0.5%、ポリアクリル酸アンモニウム塩濃度0.2%)を用い、前記仕上げ研磨を実施した。
(実施例6)
実施例4で調製した研磨剤(水酸化セリウム濃度0.2%、ダイキトサン100D(VL)濃度0.06%、pH=6.5)の平均粒径の時間変化を追跡した。25℃で100時間放置しても、平均粒径は変化しなかった。
上記で得た濃縮水酸化セリウムスラリ320g、水1232gを混合し、10重量%のイミダゾール水溶液をpHが6.5になるまで加えて研磨剤を調製した(水酸化セリウム濃度0.2%、pH=6.5)。平均粒径の時間変化を追跡したところ、25℃で10時間後に平均粒径は171%に増大し、さらに24時間後には研磨粒子の沈降が認められた。
(実施例7)
上記したダイキトサン100D(VL)0.6重量%、酢酸0.5重量%、イミダゾール0.64重量%、及び水98.26重量%を含有する濃縮添加液100g、上記で得た濃縮水酸化セリウムスラリ200g、水700gを混合し、研磨剤を調製した(水酸化セリウム濃度0.2%、ダイキトサン100D(VL)濃度0.06%)。研磨剤のpHは6.3であった。研磨パッドとして、ショアD硬度81のポリウレタン製パッドを用い、実施例1と同様の方法で研磨を行い、酸化珪素研磨速度、窒化珪素研磨速度、選択比を求めた。
酢酸0.5重量%、イミダゾール0.64重量%、及び水98.86重量%を含有する濃縮添加液100g、上記で得た濃縮水酸化セリウムスラリ200g、水700gを混合し、キトサンを含まない研磨剤を調製した(水酸化セリウム濃度0.2%)。研磨剤のpHは6.3であった。研磨パッドとして、ショアD硬度81のポリウレタン製パッドを用い、実施例1と同様の方法で研磨を行い、酸化珪素研磨速度、窒化珪素研磨速度、選択比を求めた。
比較例2で調製した研磨剤(酸化セリウム濃度0.5重量%)を純水で2.5倍、10倍に希釈し、実施例1と同様の方法で研磨を行い、酸化珪素研磨速度、窒化珪素研磨速度、選択比を求めた。
アリルアミン重合体(日東紡績株式会社製PAA−H−10C)1重量%、酢酸0.3重量%、水98.7重量%を含有する濃縮添加液2.5g、上記濃縮水酸化セリウムスラリ100g及び水395gを混合し、5重量パーセントのイミダゾール水溶液をpHが5.5になるまで加えて研磨剤を調製した。平均粒径は100nm、ゼータ電位は+47mVであった。なお、平均粒径およびゼータ電位は、上記と同様に測定した。
実施例8と同様にして、濃縮添加液の添加量を5.0g、7.5gに変え、研磨剤を調製した。
エチレンイミン重合体(株式会社日本触媒製、商品名エポミン(登録商標)SP−200、数平均分子量10,000)1重量%、酢酸0.3重量%及び水98.7重量%を含有する濃縮添加液15g、上記濃縮水酸化セリウムスラリ100g並びに水385gを混合し、5重量%のイミダゾール水溶液をpHが5.5になるまで加えて研磨剤を調製した。平均粒径は100nm、ゼータ電位は+36mVであった。なお、平均粒径およびゼータ電位は、上記と同様に測定した。
下記の表5記載の各組成になるように、実施例11から濃縮添加液の添加量を25g、50gに変え、研磨剤を調製した。
エチレンイミン重合体(株式会社日本触媒製、商品名エポミンP−1000、30重量%水溶液、数平均分子量70,000)1重量%(ポリマ含有量として)、酢酸0.3重量%及び水98.7重量%を含有する濃縮添加液5g、上記濃縮水酸化セリウムスラリ100g並びに水395gを混合し、5重量%のイミダゾール水溶液をpHが5.5になるまで加えて研磨剤を調製した。
(添加剤の合成)
丸底フラスコにN,N−ジメチルアミノプロピルアクリルアミド(株式会社興人製DMAPAA)15g、水281gを入れ、窒素ガスを導入した。80℃に加熱し、攪拌しながら2,2´−アゾビス(2−メチルプロピオンアミジン)二塩酸塩696mg、水4gからなる水溶液を加えた。80℃で2時間加熱攪拌後、室温(25℃)まで冷却して濃度5重量%の重合体(以下添加剤Xという)溶液を得た。静的光散乱法を用いて分子量を測定したところ、23,000であった。
2 窒化珪素膜
3 シリコン基板
L 凸部の線幅
S 凹部の線幅
Claims (14)
- 水、4価の金属水酸化物粒子及び添加剤を含有する研磨剤であって、該添加剤はカチオン性の重合体および多糖類の少なくとも一方を含む研磨剤。
- 前記4価の金属水酸化物粒子の平均粒径が、1nm以上400nm以下である請求項1または2に記載の研磨剤。
- 研磨剤のpHが3.0以上7.0以下である請求項1〜3のいずれかに記載の研磨剤。
- 前記4価の金属水酸化物粒子の含有量が、研磨剤100重量部に対して0.001重量部以上5重量部以下である請求項1〜4のいずれかに記載の研磨剤。
- 前記4価の金属水酸化物粒子の研磨剤中でのゼータ電位が、+10mV以上である請求項1〜5のいずれかに記載の研磨剤。
- 前記カチオン性の重合体および多糖類の合計の含有量が、研磨剤100重量部に対して0.0001重量部以上である請求項1〜6のいずれかに記載の研磨剤。
- 前記添加剤が、キトサンおよびその誘導体のいずれかである請求項1〜7のいずれかに記載の研磨剤。
- さらにポリビニルアルコールを含有する請求項1〜8のいずれかに記載の研磨剤。
- 少なくとも表面に酸化珪素を含む被研磨面を研磨するために使用される請求項1〜9のいずれかに記載の研磨剤。
- 4価の金属水酸化物が、希土類金属水酸化物及び水酸化ジルコニウムの少なくとも一方である請求項1〜10のいずれかに記載の研磨剤。
- 被研磨膜を形成した基板を研磨定盤の研磨布に押しあて加圧し、請求項1〜11のいずれかに記載の研磨剤を被研磨膜と研磨布との間に供給しながら、基板と研磨定盤とを相対的に動かして被研磨膜を研磨する基板の研磨方法。
- 前記研磨布のショアD硬度が70以上である研磨布を用いる請求項12記載の研磨方法。
- スラリと、添加液とに分けて保存され、研磨直前又は研磨時に混合されて請求項1〜11のいずれかに記載の研磨剤とされる研磨剤セットであって、スラリは4価の金属水酸化物粒子と水を含み、添加液は添加剤と水を含む研磨剤セット。
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