JP2019208029A - Cmp用研磨液、cmp用研磨液セット、及び研磨方法 - Google Patents
Cmp用研磨液、cmp用研磨液セット、及び研磨方法 Download PDFInfo
- Publication number
- JP2019208029A JP2019208029A JP2019112966A JP2019112966A JP2019208029A JP 2019208029 A JP2019208029 A JP 2019208029A JP 2019112966 A JP2019112966 A JP 2019112966A JP 2019112966 A JP2019112966 A JP 2019112966A JP 2019208029 A JP2019208029 A JP 2019208029A
- Authority
- JP
- Japan
- Prior art keywords
- polishing
- cerium oxide
- cmp
- oxide particles
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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Abstract
Description
なお、本明細書において、「L」は「リットル」を示す。
なお、本明細書において、水溶性とは、水100gに対して25℃において0.1g以上溶解するものとして定義される。
本発明は、2014年5月30日に出願された特願2014−112855号に記載の主題と関連しており、その開示内容は、参照によりここに援用される。
本発明の実施形態であるCMP用研磨液は、酸化セリウム粒子と、水とを含有する。以下、CMP用研磨液に含まれる各成分について詳細に説明する。
酸化セリウム粒子は、例えば、セリウム化合物を酸化することによって得られる。セリウム化合物としては、炭酸塩、硝酸塩、硫酸塩、しゅう酸塩等のセリウム塩などが挙げられ、中でも炭酸セリウム(セリウムの炭酸塩)が好ましい。
水としては、特に制限されないが、脱イオン水、イオン交換水、超純水等が好ましい。水の含有量は、各含有成分の含有量の残部でよく、CMP用研磨液中に含有されていれば特に限定されない。なお、CMP用研磨液は、必要に応じて水以外の溶媒を更に含有してもよい。水以外の溶媒としては、例えば、エタノール、アセトン等の極性溶媒などが挙げられる。
本発明のCMP用研磨液は、更に添加剤を含有してもよい。添加剤としては、水溶性高分子、有機酸等が挙げられる。
CMP用研磨液には、水溶性高分子を使用できる。水溶性高分子としては、例えば、多糖類、ビニル系ポリマ、アクリル酸系ポリマ等が挙げられる。これにより、研磨終了後の被研磨部(例えば酸化ケイ素部)の平坦性を向上させることができる。より詳細には、凹凸を有する被研磨部を研磨した場合に、一部が過剰に研磨されて皿のように凹む現象、いわゆるディッシングが生じることを抑制できる。この効果は、水溶性高分子と、酸化セリウム粒子とを併用することにより、より効率的に得られる。水溶性高分子は一種類を単独で又は二種類以上を組み合わせて使用できる。前記水溶性高分子の中でも、アクリル酸系ポリマが好ましい。
使用機器(検出器):株式会社日立製作所製、「L−3300型」液体クロマトグラフ用示差屈折率計
ポンプ:株式会社日立製作所製、液体クロマトグラフ用「L−7100」
デガス装置:なし
データ処理:株式会社日立製作所製、GPCインテグレーター「D−2520」
カラム:昭和電工株式会社製、「Shodex Asahipak GF−710HQ」、内径7.6mm×300mm
溶離液:50mM−Na2HPO4水溶液/アセトニトリル=90/10(v/v)
測定温度:25℃
流量:0.6mL/min
測定時間:30min
試料:樹脂分濃度2質量%になるように溶離液と同じ組成の溶液で濃度を調整し、0.45μmのポリテトラフルオロエチレンフィルターでろ過して調製した試料
注入量:0.4μL
標準物質:Polymer Laboratories製、狭分子量ポリアクリル酸ナトリウム
使用機器(検出器):株式会社日立製作所製、RI−モニター「L−3000」
ポンプ:株式会社日立製作所製「L−6000」
デガス装置:昭和電工株式会社製「Shodex DEGAS」(「Shodex」は登録商標)
データ処理:株式会社日立製作所製、GPCインテグレーター「D−2200」
カラム:日立化成株式会社製「GL−R440」、「GL−R430」、「GL−R420」をこの順番で連結して使用
溶離液:テトラヒドロフラン(THF)
測定温度:23℃
流量:1.75mL/min
測定時間:45min
注入量:10μL
標準物質:東ソー株式会社製、標準ポリスチレン(分子量:190000、17900、9100、2980、578、474、370、266)
CMP用研磨液は、水溶性高分子以外に、有機酸を含有してもよい。有機酸は塩であってもよい。以下、本明細書において、有機酸及び有機酸の塩を、単に「有機酸」ともいう。有機酸は、研磨速度を向上させ、且つ研磨終了後の被研磨部(例えば酸化ケイ素部)の平坦性を向上させることができる。より詳細には、凹凸を有する被研磨面を研磨した場合に、研磨時間を短縮できることに加え、一部が過剰に研磨されて皿のように凹む現象、いわゆるディッシングが生じることを抑制できる。この効果は、有機酸と、水溶性高分子と、酸化セリウム粒子とを併用することにより、より効率的に得られる。有機酸は一種類を単独で又は二種類以上を組み合わせて使用できる。
CMP用研磨液には、酸化セリウム粒子を分散させるための分散剤を含有させることができる。分散剤は、酸化セリウム粒子の表面に付着して分散能を発揮する。分散剤としては、水溶性陰イオン性分散剤、水溶性非イオン性分散剤、水溶性陽イオン性分散剤、水溶性両性分散剤等が挙げられる。分散剤は一種類を単独で又は二種類以上を組み合わせて使用できる。中でも水溶性陰イオン性分散剤が好ましく、アクリル酸系ポリマがより好ましい。アクリル酸系ポリマについては前記と同様である。
CMP用研磨液は、例えば、酸化セリウム粒子と水とを混合して酸化セリウム粒子を分散させ、必要に応じて粉砕、分級(ふるいわけ法、遠心分離法、沈降法等)、ろ過等を実施し、更に、任意成分である水溶性高分子、有機酸等を添加することによって得られる。酸化セリウム粒子の主ピーク半値幅は、粉砕、分級、ろ過等により変化しうるが、最終的にCMP用研磨液において0.26〜0.36°の範囲にあればよい。
本発明の実施形態である基板の研磨方法は、絶縁材料が形成された基板を研磨する方法であって、上記CMP用研磨液を用いて、絶縁材料の不要部を除去する方法である。好ましくは研磨対象としての絶縁材料が形成された基板の被研磨面を、研磨定盤の研磨布に押圧した状態で、基板上の被研磨面と研磨布との間に上記CMP用研磨液を供給しながら、基板と研磨定盤とを相対的に動かして絶縁材料を研磨し、絶縁材料の不要部を除去する。
(酸化セリウムの作製)
市販の炭酸セリウム水和物40kgをアルミナ製容器に入れ、800℃で、空気中で2時間焼成することにより黄白色の粉末を20kg得た。この粉末の相同定をX線回折法で行ったところ、酸化セリウムであることを確認した。酸化セリウムの主ピーク半値幅を測定したところ、0.27°であった。
前記で作製した酸化セリウム20kgを、ジェットミルを用いて乾式粉砕(粉砕1)し、酸化セリウム粉末を得た。酸化セリウム粉末の主ピーク半値幅を測定したところ、0.30°であった。乾式粉砕条件は、処理回数2pass、圧力0.6MPaとした。
前記で作製した酸化セリウム粉末100.0gと、脱イオン水897.5gとを混合し、分散剤としてポリアクリル酸アンモニウム水溶液(重量平均分子量:8,000、40質量%)2.5gを添加して、撹拌しながら湿式粉砕(粉砕2)を行い、酸化セリウム粉砕液を得た。酸化セリウム粉砕液に含まれる酸化セリウム粒子の主ピーク半値幅を測定したところ、0.36°であった。湿式粉砕条件は、処理回数25pass、圧力200MPaとした。また、酸化セリウム粒子の主ピーク半値幅の測定用のサンプルは、得られた酸化セリウム粉砕液10gを150℃、1時間で乾燥した乾燥粉を用いた。
前記で作製した酸化セリウム粉砕液を遠心分離し、平均粒径(D50)が150nmになるように上澄み液を取り出した。遠心分離機「himac CF12RX、T3S51」(日立工機株式会社製)を用い、条件を回転数2500min−1、時間5min、温度25℃とした。得られた上澄み液を、酸化セリウム粒子の濃度が4.0質量%となるように脱イオン水で希釈し、酸化セリウムスラリを得た。酸化セリウムスラリに含まれる酸化セリウム粒子の主ピーク半値幅を測定したところ、0.33°であった。測定用のサンプルの調製は、酸化セリウム粉砕液の場合と同様に行った。
有機酸としてp−トルエンスルホン酸一水和物0.084gと、脱イオン水700gとを混合し、水溶性高分子としてポリアクリル酸水溶液(重量平均分子量4,000、40質量%)1.75gを加え、更にアンモニア水(25質量%)を加えてpH4.5に調整した。その後、脱イオン水を加えて、全体量を740.0gとして添加液とした。
得られた添加液に、酸化セリウムスラリ250.0gを添加し、更にアンモニア水(25質量%)を加えて、pH6.0に調整した。その後、脱イオン水を加えて、全体量を1,000gとし、酸化セリウムCMP用研磨液を作製した。酸化セリウムCMP用研磨液は、酸化セリウム粒子を1.0質量%、及び、添加剤としてポリアクリル酸(水溶性高分子)を0.07質量%とp−トルエンスルホン酸(有機酸)を0.0076質量%含む。
粉砕1、粉砕2及び遠心分離の各条件を、表1及び2に示す条件に従って変更し、有機酸の添加量を表3に示す量にした以外は、実施例1と同様の方法により、表3に示す酸化セリウムCMP用研磨液を作製した。遠心分離後に得られた上澄み液の脱イオン水による希釈は、酸化セリウム粒子の濃度を4.0質量%とするために必要な場合に行った。酸化セリウムCMP用研磨液は、酸化セリウム粒子を1.0質量%、及び、添加剤としてポリアクリル酸(水溶性高分子)を0.07質量%とp−トルエンスルホン酸(有機酸)を表3に示す量(0又は0.0076質量%)含む。酸化セリウムCMP用研磨液のpHは6.0であった。
研磨試験用のウエハとして、アドバンテック社製のブランケットウエハ「P−TEOS 1.0μm」(TEOS−CVD法により酸化ケイ素膜が形成されたウエハ、直径300mm)を用いた。
研磨前の絶縁膜の膜厚と研磨後の絶縁膜の膜厚を測定し、研磨前後の膜厚の差及び研磨時間から研磨速度の算出を行った。膜厚の測定には、フィルメトリクス社製の膜厚計「F−80」を使用した。
研磨終了後の研磨試験用のウエハについて、アプライドマテリアルズ社製の検査装置「Complus」を用いて、検出異物サイズを0.2μm以上に設定して異物(凹み及び付着物)を検出した。検出された異物には、傷以外の付着物が含まれるため、アプライドマテリアルズ社製の走査型電子顕微鏡(SEM)「Vision G3」で各異物を観察し、凹みを研磨傷と判断し、研磨傷数をカウントした。
Claims (4)
- 酸化セリウム粒子及び水を含有するCMP用研磨液であって、
前記酸化セリウム粒子の粉末X線回折チャートにおいて、2θ=27.000〜29.980°の範囲に現われる主ピークの半値幅が0.26〜0.36°であり、
前記酸化セリウム粒子の平均粒径が130nm以上175nm未満であり、
1.15μm以上の粒径を有する酸化セリウム粒子の数が5,000×103個/mL以下であるCMP用研磨液。 - 更に水溶性高分子を含有する請求項1に記載のCMP用研磨液。
- 請求項2に記載のCMP用研磨液を得るためのCMP用研磨液セットであって、
酸化セリウム粒子及び水を含有する第一の液と、水溶性高分子及び水を含有する第二の液とを備えたCMP用研磨液セット。 - 絶縁材料が形成された基板を研磨する方法であって、
請求項1又は2に記載のCMP用研磨液、又は、請求項3に記載のCMP用研磨液セットにより得られたCMP用研磨液を用いて、前記絶縁材料の不要部を除去する基板の研磨方法。
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