JP6878772B2 - 研磨剤、研磨剤用貯蔵液及び研磨方法 - Google Patents
研磨剤、研磨剤用貯蔵液及び研磨方法 Download PDFInfo
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- JP6878772B2 JP6878772B2 JP2016081282A JP2016081282A JP6878772B2 JP 6878772 B2 JP6878772 B2 JP 6878772B2 JP 2016081282 A JP2016081282 A JP 2016081282A JP 2016081282 A JP2016081282 A JP 2016081282A JP 6878772 B2 JP6878772 B2 JP 6878772B2
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- abrasive
- polishing
- resin
- acid
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Description
本明細書において「工程」との語には、独立した工程だけでなく、他の工程と明確に区別できないもののその工程の所期の作用が達成される工程が含まれる。
本実施形態に係る樹脂研磨用研磨剤(以下、単に「研磨剤」という場合がある)は、研磨時に被研磨面に触れる組成物であり、例えばCMP用研磨剤である。
研磨対象である樹脂としては、ポリベンゾオキサゾール(PBO)、PBOの前駆体、ポリイミド(PI)、フェノール樹脂、エポキシ樹脂、アクリル樹脂、メタクリル樹脂、ノボラック樹脂、不飽和ポリエステル、ポリエステル(不飽和ポリエステルを除く)、ポリアミドイミド、ポリアリルエーテル、複素環含有樹脂(前記で例示した樹脂を除く)などが挙げられる。研磨対象は、これらを主成分とした樹脂であってもよい。前記「複素環含有樹脂」としては、ピロール環含有樹脂、ピリジン環含有樹脂、イミダゾール環含有樹脂等が挙げられる。樹脂の形成方法としては、特に制限はないが、蒸着法、スピーンコート法等が挙げられる。樹脂の形状は、特に制限はないが、例えば膜状(樹脂膜)である。これら樹脂の中で、耐熱性、力学強度、寸法安定性、絶縁特性及び、エッチング耐性に優れる観点から、ポリベンゾオキサゾール、ポリベンゾオキサゾールの前駆体及びポリイミドからなる群より選ばれる少なくとも一種が好ましい。また、本実施形態に係る研磨剤は、配線板又は回路基板の研磨にも用いることができる。
本実施形態に係る研磨剤は、砥粒を含有する。砥粒は、アルミニウム化合物及びアルミニウムイオンからなる群より選ばれる少なくとも一種のアルミニウム成分が付着した粒子を含んでおり、研磨剤中において前記アルミニウム成分が前記粒子に付着している。アルミニウム成分が付着した粒子としては、アルミナからなる粒子を除く。アルミニウム成分は、前記粒子の表面の少なくとも一部に付着していればよい。アルミニウム化合物としては、アルミナ、水酸化アルミニウム等が挙げられる。砥粒は、研磨剤中で正の電荷を有している。研磨剤がこのような砥粒を含有することにより、研磨傷の発生を抑制しつつ樹脂の良好な研磨速度を得ることができる。
本実施形態に係る研磨剤は、水を含有する。水は、他の成分の分散媒、又は、溶媒として用いられる。水としては、他の成分の作用を阻害することを防止するために不純物を可能な限り含有しないものが好ましい。具体的には、水としては、イオン交換樹脂にて不純物イオンを除去した後にフィルタを通して異物を除去した純水、超純水及び蒸留水が好ましい。
本実施形態に係る研磨剤は、砥粒及び水以外の成分として添加剤を含有することができる。添加剤は、研磨剤中の砥粒の分散性の向上、研磨剤の化学的安定性の向上、研磨速度の向上等の目的で用いることができる。添加剤としては、pH調整剤、防食剤、酸化剤、エーテル結合を有する水溶性高分子、有機溶媒、絶縁材料研磨抑制剤、界面活性剤、消泡剤等が挙げられる。研磨剤中の添加剤の含有量は、研磨剤の特性を損なわない範囲で任意に決定できる。
本実施形態に係る研磨剤のpHは、研磨傷の発生を抑制しつつ良好な研磨速度で樹脂を除去する観点から、3.0〜7.0である。研磨剤のpHは、樹脂の研磨速度が更に向上する観点、及び、砥粒の凝集が抑制され、砥粒の良好な分散安定性が得られる観点から、7.0未満が好ましく、6.5以下がより好ましく、6.0以下が更に好ましく、5.0以下が特に好ましい。研磨剤のpHは、充分な機械的研磨力が得られ易く、樹脂の研磨速度が更に向上する観点から、3.5以上が好ましく、4.0以上がより好ましい。これらの観点から、研磨剤のpHは、3.5〜7.0が好ましく、3.5〜6.5がより好ましく、3.5〜5.0が更に好ましく、4.0〜5.0が特に好ましい。研磨剤のpHは、3.0〜5.0であってもよい。pHは液温25℃におけるpHと定義する。
本実施形態に係る研磨剤は、防食剤(防食剤成分、金属防食剤)を含有してもよい。防食剤は、配線金属(銅系金属、コバルト系金属等)に対して保護膜を形成することで配線金属のエッチングを抑制して被研磨面の荒れを低減し易くすることができる。
本実施形態に係る研磨剤は、酸化剤(酸化剤成分、金属酸化剤)を含有してもよい。研磨剤が酸化剤を含有することにより、金属材料(配線金属、バリア金属等。例えば金属層)の研磨速度を向上させることができる。
本実施形態に係る研磨剤は、エーテル結合を有する水溶性高分子を含有してもよい。エーテル結合を有する水溶性高分子を研磨剤が含有することにより、樹脂の更に良好な研磨速度を得ることができる。
本実施形態に係る研磨剤は、有機溶媒を含有してもよい。研磨剤が有機溶媒を含有することにより、樹脂の研磨速度及び研磨剤の濡れ性を更に向上させることができる。有機溶媒としては、特に制限はないが、20℃で液状の溶媒が好ましい。100gの水(20℃)に対する有機溶媒の溶解度は、研磨剤を高濃縮化する観点から、30g以上が好ましく、50g以上がより好ましく、100g以上が更に好ましい。有機溶媒は、一種を単独で、又は、二種以上を組み合わせて使用できる。
本実施形態に係る研磨剤は、絶縁材料の研磨を抑制する成分として、絶縁材料研磨抑制剤(絶縁材料研磨抑制剤成分。例えば無機絶縁膜研磨抑制剤)を含有してもよい。研磨剤が絶縁材料研磨抑制剤を含有することにより、絶縁材料の研磨速度を抑制し、樹脂を絶縁材料に対して選択的に除去できる。
研磨剤は、界面活性剤(界面活性剤成分)を含有していてもよい。研磨剤が界面活性剤を含有することにより、被研磨材料の研磨速度を容易に調整できると共に、研磨傷を容易に低減できる。
研磨剤に含まれる各成分の配合方法及び研磨剤の希釈方法は、特に制限はなく、例えば、翼式攪拌機による攪拌、又は、超音波分散等で各成分を分散又は溶解させることができる。水に対する各成分の混合順序は限定されない。
本実施形態に係る研磨剤用貯蔵液は、前記研磨剤を得るための貯蔵液であり、研磨剤用貯蔵液を水で希釈することにより前記研磨剤が得られる。研磨剤用貯蔵液は、水の量を使用時よりも減じて保管されており、使用前又は使用時に水で希釈されて前記研磨剤として用いられる。研磨剤用貯蔵液は、水の含有量が前記研磨剤よりも少ない点で前記研磨剤と異なっている。希釈倍率は、例えば1.5倍以上である。
本実施形態に係る研磨方法は、研磨剤を用いて樹脂の少なくとも一部を研磨(CMP等)して除去する研磨工程を備えている。前記研磨工程では、樹脂を含む被研磨面を研磨することができる。前記研磨工程では、研磨剤を用いて、樹脂を有する基体を研磨して前記樹脂の少なくとも一部を除去することができる。基体は、例えば、表面に凹部及び凸部を有する基板上に形成された樹脂を有してもよい。基体は、例えば、配線板又は回路基板であってよい。本実施形態に係る研磨方法は、研磨工程の前に、樹脂を有する基体を用意する工程を備えていてもよい。前記樹脂は、ポリベンゾオキサゾール、ポリベンゾオキサゾールの前駆体及びポリイミドからなる群より選ばれる少なくとも一種を含むことが好ましい。
(実施例1)
コロイダルシリカ1(アルミニウム成分(水酸化アルミニウム)が付着した砥粒。平均粒径(D50):30nm)5.00質量部に、超純水をX質量部注いで研磨剤100質量部を得た。コロイダルシリカ1は、コロイダルシリカの全質量に対して分散剤として酢酸を5.0質量%含むコロイダルシリカ分散液を用いて供給した。なお、超純水の配合量(X質量部)は、研磨剤が100質量部になるよう計算して調整した。
砥粒、防食剤、酸化剤及びpH調整剤の種類及び含有量を表1及び表2のとおりに変更した以外は、実施例1と同様の方法で研磨剤を調製した。表1及び表2の各成分の量は、研磨剤の全質量を基準とした含有量(単位:質量%)である。比較例7のコロイダルシリカ2は、アルミニウム成分が付着していないコロイダルシリカ(平均粒径(D50):30nm)である。
表2の砥粒を1.00質量部容器に入れた。次に、超純水をX質量部注いだ後、酢酸でpHを調整して研磨剤100質量部を得た。なお、超純水の配合量(X質量部)は、研磨剤が100質量部になるよう計算して調整した。比較例4のコロイダルシリカ2は、アルミニウム成分が付着していないコロイダルシリカ(平均粒径(D50):30nm)である。比較例5のコロイダルシリカ3は、アミン化合物を付着させたコロイダルシリカ(平均粒径(D50):70nm)である。比較例6のαアルミナは、アルミナからなる粒子である。
研磨剤のpHを下記の条件で測定した。結果を表1及び表2に示す。
測定温度:25±5℃
測定装置:株式会社堀場製作所の商品名:Model(F−51)
測定方法:フタル酸塩pH標準液(pH:4.01)と、中性リン酸塩pH標準液(pH:6.86)と、ホウ酸塩pH標準液(pH:9.18)とをpH標準液として用い、pHメーターを3点校正した後、pHメーターの電極を研磨剤に入れて、2min以上経過して安定した後のpHを前記測定装置により測定した。
研磨剤中における砥粒のゼータ電位を下記のとおり測定した。ゼータ電位測定装置としては、ベックマンコールター社製の商品名:DELSA NANO Cを用いた。ゼータ電位測定装置において測定サンプルの散乱強度が1.0×104〜5.0×104cpsとなるように研磨剤を純水で希釈してサンプルを得た。その後、得られたサンプルをゼータ電位測定用セルに入れてゼータ電位を測定した。全ての実施例において、砥粒の表面は、研磨剤中において正に帯電していた。結果を表1及び表2に示す。
(研磨速度及び研磨傷の評価)
被研磨膜を有する基体として、厚み8000nmのポリベンゾオキサゾール膜(PBO膜)をシリコン基板上に形成して得られた基体と、厚み8000nmのポリイミド膜(PI膜)をシリコン基板上に形成して得られた基体と、厚み1000nmの銅膜(Cu膜)をシリコン基板上に形成して得られた基体とを用いた。前記で調製した研磨剤を用いて、下記研磨条件にて60秒間被研磨膜を化学機械研磨した。なお、銅膜の研磨は、実施例1〜4,7及び比較例7において行った。
研磨装置:片面用研磨機(アプライドマテリアルズ製、商品名:Reflexion LK)
研磨布:スウェード状発泡ポリウレタン樹脂製研磨布
定盤回転数:123回/min
ヘッド回転数:117回/min
研磨圧力:21kPa
研磨剤の供給量:300mL/min
実施例1〜7及び比較例1〜3,7において、銅のエッチング速度(Cuエッチング速度)を評価した。
浸漬後の銅膜の厚み[nm]=1.83×10000/評価用チップ(b)の抵抗値[mΩ] ・・・(1)
銅のエッチング速度(Cuエッチング速度)[nm/min]=(浸漬前の銅膜の厚み[nm]−浸漬後の銅膜の厚み[nm])/1分 ・・・(2)
Claims (11)
- 砥粒、酸化剤及び水を含有する研磨剤であって、
前記砥粒が前記研磨剤中で正の電荷を有し、
前記砥粒のゼータ電位が25mV以上であり、
前記砥粒が、アルミニウム化合物及びアルミニウムイオンからなる群より選ばれる少なくとも一種が付着した粒子(アルミナからなる粒子を除く)を含み、
前記研磨剤のpHが3.0〜7.0である、樹脂研磨用研磨剤。 - 砥粒及び水を含有する樹脂研磨用研磨剤であって、
前記砥粒が前記研磨剤中で正の電荷を有し、
前記砥粒のゼータ電位が25mV以上であり、
前記砥粒が、アルミニウム化合物及びアルミニウムイオンからなる群より選ばれる少なくとも一種が付着した粒子(アルミナからなる粒子を除く)を含み、
前記研磨剤のpHが3.0〜7.0であり、
前記樹脂が、ポリベンゾオキサゾール、ポリベンゾオキサゾールの前駆体及びポリイミドからなる群より選ばれる少なくとも一種を含む、樹脂研磨用研磨剤。 - 前記砥粒がコロイダルシリカを含む、請求項1又は2に記載の研磨剤。
- 前記砥粒の含有量が1.00質量%以下である、請求項1〜3のいずれか一項に記載の研磨剤。
- pHが3.0〜5.0である、請求項1〜4のいずれか一項に記載の研磨剤。
- 防食剤を更に含有する、請求項1〜5のいずれか一項に記載の研磨剤。
- pH調整剤を更に含有する、請求項1〜6のいずれか一項に記載の研磨剤。
- 請求項1〜7のいずれか一項に記載の研磨剤を得るための研磨剤用貯蔵液であって、
水で希釈することにより前記研磨剤が得られる、研磨剤用貯蔵液。 - 請求項1〜7のいずれか一項に記載の研磨剤、又は、請求項8に記載の研磨剤用貯蔵液を水で希釈して得られる研磨剤を用いて、樹脂の少なくとも一部を研磨して除去する工程を備える、研磨方法。
- 前記樹脂が、ポリベンゾオキサゾール、ポリベンゾオキサゾールの前駆体及びポリイミドからなる群より選ばれる少なくとも一種を含む、請求項9に記載の研磨方法。
- 前記樹脂が、ポリベンゾオキサゾール及びポリベンゾオキサゾールの前駆体からなる群より選ばれる少なくとも一種を含む、請求項9に記載の研磨方法。
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