JP6928040B2 - 銅バリアの化学機械研磨組成物 - Google Patents
銅バリアの化学機械研磨組成物 Download PDFInfo
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- JP6928040B2 JP6928040B2 JP2019148753A JP2019148753A JP6928040B2 JP 6928040 B2 JP6928040 B2 JP 6928040B2 JP 2019148753 A JP2019148753 A JP 2019148753A JP 2019148753 A JP2019148753 A JP 2019148753A JP 6928040 B2 JP6928040 B2 JP 6928040B2
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- Prior art keywords
- colloidal silica
- polishing
- copper
- particles
- abrasive particles
- Prior art date
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
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- C—CHEMISTRY; METALLURGY
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
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- C—CHEMISTRY; METALLURGY
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
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Description
酸化ケイ素(TEOS)、銅(Cu)、black diamond(登録商標)低k誘電体(BD1)、及び窒化タンタル(TaN)の研磨速度を、様々な研磨組成物に対してこの例の中で評価した。アミノプロピルトリアルコキシシラン(アミノシラン)を加水分解した又は部分的に加水分解したコアシェル構造を有するコロイダルシリカ研磨剤粒子を含んだ研磨組成物のそれぞれを、例12において以下で説明するのと同様の手順を使用してシェル中に組み込んだ。例12でのように調製した濃縮した分散体の量を、銅錯化剤及び銅研磨防止剤を含む混合物に加えて、関連する研磨組成物を得た。過酸化水素を各研磨組成物に加えた。9個の研磨組成物を調製して(1A〜1I)、それらのそれぞれは、63nmの平均粒子サイズを有するコロイダルシリカを含んでいた。研磨組成物1A〜1Fは、3.0wt%のコロイダルシリカ及び0.5wt%の過酸化水素を含んでいて、組成物1G〜1Iは、9.0wt%のコロイダルシリカ及び0.2wt%の過酸化水素を含んでいた。各研磨組成物は4.0のpHを有した。表1Aは、研磨組成物1A〜1Iで使用した銅錯化剤及び銅研磨防止剤を示す(表中、ATAは3アミノ1,2,4トリアゾール、BTAはベンゾトリアゾール、CupferronはN−ニトロソ−N−フェニルヒドロキシルアミン、RE−410はエトキシル化ノニルフェノール遊離酸のリン酸エステルである)。
酸化ケイ素(TEOS)、銅(Cu)、black diamond(登録商標)低k誘電体(BD1)、及び窒化タンタル(TaN)の研磨速度を、様々な研磨組成物に対してこの例の中で評価した。アミノプロピルトリアルコキシシラン(アミノシラン)を加水分解した又は部分的に加水分解したコアシェル構造を有するコロイダルシリカ研磨剤粒子を含んだ研磨組成物のそれぞれを、例12において以下で説明するのと同様の手順を使用してシェル中に組み込んだ。例12でのように調製した濃縮した分散体の量を、任意選択の銅錯化剤及び/又は銅研磨防止剤を含む水性混合物に加えて、関連する研磨組成物を得た。8個の研磨組成物を調製して(2A〜2H)、それらのそれぞれは63nmの平均粒子サイズを有する4.5wt%のコロイダルシリカを含んでいた。研磨組成物は、0.5wt%の過酸化水素をさらに含んでいた。表2Aは、銅研磨防止剤(BTA)及び銅錯化剤(Dequest(登録商標)2000)の濃度と、組成物のpHとを示す。
酸化ケイ素(TEOS)、銅(Cu)、black diamond(登録商標)低k誘電体(BD1)、窒化タンタル(TaN)、及び銅パターンの研磨速度を、様々な研磨組成物に対してこの例の中で評価した。アミノプロピルトリアルコキシシラン(アミノシラン)を加水分解した又は部分的に加水分解したコアシェル構造を有するコロイダルシリカ研磨剤粒子を含んだ研磨組成物のそれぞれを、例12において以下で説明するのと同様の手順を使用してシェル中に組み込んだ。例12でのように調製した濃縮した分散体の量を、銅錯化剤含む水性混合物に加えて、関連する研磨組成物を得た。4つの研磨組成物を調製して(3A〜3D)、それらのそれぞれは63nmの平均粒子サイズを有した。研磨組成物3A及び3Bは4.5wt%のコロイダルシリカを含んでいて、組成物3C及び3Dは6.0wt%のコロイダルシリカを含んでいた。各研磨組成物は0.2wt%の過酸化水素を含んでいて、4のpHを有した。研磨組成物は、25ppmのアミノ酸系界面活性剤(ココイルサルコシン酸ナトリウム−Perlastan(登録商標)C30)をさらに含んでいた。研磨組成物3A及び3Cは、150ppmのポリホスホン酸錯化剤(Dequest(登録商標)2000)を含んでいた。研磨組成物3B及び3Dは250ppmのDequest(登録商標)2000を含んでいた。
酸化ケイ素(TEOS)、銅(Cu)、black diamond(登録商標)低k誘電体(BD1)、及び窒化タンタル(TaN)の研磨速度を、様々な研磨組成物に対してこの例の中で評価した。アミノプロピルトリアルコキシシラン(アミノシラン)を加水分解した又は部分的に加水分解したコアシェル構造を有するコロイダルシリカ研磨剤粒子を含んだ研磨組成物のそれぞれを、例12において以下で説明するのと同様の手順を使用してシェル中に組み込んだ。例12でのように調製した濃縮した分散体の量を、銅錯化剤及び銅研磨防止剤を含む混合物に加えて、関連する研磨組成物を得た。4個の研磨組成物を調製して(4A〜4D)、それらのそれぞれは63nmの平均粒子サイズを有する3.0wt%のコロイダルシリカを含んでいた。各研磨組成物は0.5wt%の過酸化水素を含んでいて、4のpHを有した。銅研磨防止剤(2,4−ジヒドロ安息香酸−DHBA)及び銅錯化剤(アミノトリ(メチレンホスホン酸)−Dequest(登録商標)2000)の濃度は以下のようであった。(4A)50ppmのDHBA、100ppmのDequest(登録商標)2000、(4B)50ppmのDHBA、250ppmのDequest(登録商標)2000、(4C)200ppmのDHBA、100ppmのDequest(登録商標)2000、及び(4D)200ppmのDHBA、250ppmのDequest(登録商標)2000。
酸化ケイ素(TEOS)、銅(Cu)、black diamond(登録商標)低k誘電体(BD1)、窒化タンタル(TaN)、及び銅パターンの研磨速度を、様々な研磨組成物に対してこの例の中で評価した。アミノプロピルトリアルコキシシラン(アミノシラン)を加水分解した又は部分的に加水分解したコアシェル構造を有するコロイダルシリカ研磨剤粒子を含んだ研磨組成物のそれぞれを、例12において以下で説明するのと同様の手順を使用してシェル中に組み込んだ。例12でのように調製した濃縮した分散体の量を、銅錯化剤及び銅研磨防止剤を含む混合物に加えて、関連する研磨組成物を得た。4個の研磨組成物を調製して(5A〜5D)、それらのそれぞれは63nmの平均粒子サイズを有する3.0wt%のコロイダルシリカを含んでいた。第5の研磨組成物(対照)は商業的に入手可能なiCue(登録商標)B7002(Cabot Microelectronics,Aurora,Illinoisから入手可能)を含んでいた。対照は、13.3wt%の従来のコロイダルシリカ、0.54wt%の酢酸カリウム、350ppmのβアラニン錯化剤、及び1.0wt%のBTA銅研磨防止剤、並びに殺生物剤及び消泡剤を含んでいた。研磨組成物5A〜5Dは0.2wt%の過酸化水素をさらに含んでいた。対照の組成物は1.0wt%の過酸化水素をさらに含んでいた。表5Aは、コロイダルシリカ(固体)、両性界面活性剤の銅研磨防止剤(ラウリミノジプロピオン酸ナトリウム−Mirataine(登録商標)HC2−HA)、及び銅錯化剤(ピコリン酸)の濃度と、組成物5A〜5D及び対照のpHとを示す。
酸化ケイ素(TEOS)、銅(Cu)、black diamond(登録商標)低k誘電体(BD1)、窒化タンタル(TaN)、及び銅パターンの研磨速度を、様々な研磨組成物に対してこの例の中で評価した。アミノプロピルトリアルコキシシラン(アミノシラン)を加水分解した又は部分的に加水分解したコアシェル構造を有するコロイダルシリカ研磨剤粒子を含んだ研磨組成物のそれぞれを、例12において以下で説明するのと同様の手順を使用してシェル中に組み込んだ。例12でのように調製した濃縮した分散体の量を、銅錯化剤及び銅研磨防止剤を含む混合物に加えて、関連する研磨組成物を得た。4個の研磨組成物を調製して(6A〜6D)、それらのそれぞれは63nmの平均粒子サイズを有する3.0wt%のコロイダルシリカを含んでいた。研磨組成物6A〜6Dは0.2wt%の過酸化水素をさらに含んでいて、4.9のpHを有した。両性界面活性剤の銅研磨防止剤(N−ココイル−L−グルタミン酸モノトリエタノールアミン−Amisoft(登録商標)CT−12)及び銅錯化剤(ピコリン酸)の濃度は以下のようであった。(6A)30ppmの界面活性剤、50ppmのピコリン酸、(6B)30ppmの界面活性剤、250ppmのピコリン酸、(6C)60ppmの界面活性剤、50ppmのピコリン酸、及び(6D)60ppmの界面活性剤、250ppmのピコリン酸。
酸化ケイ素(TEOS)、銅(Cu)、black diamond(登録商標)低k誘電体(BD1)、及び窒化タンタル(TaN)の研磨速度を、様々な研磨組成物に対してこの例の中で評価した。アミノプロピルトリアルコキシシラン(アミノシラン)を加水分解した又は部分的に加水分解したコアシェル構造を有するコロイダルシリカ研磨剤粒子を含んだ研磨組成物のそれぞれを、例12において以下で説明するのと同様の手順を使用してシェル中に組み込んだ。例12でのように調製した濃縮した分散体の量を、銅研磨防止剤及び両性界面活性剤を含む混合物に加えて、関連する研磨組成物を得た。3個の研磨組成物を調製して(7A〜7C)、それらのそれぞれは63nmの平均粒子サイズを有する3.0wt%のコロイダルシリカを含んでいた。各研磨組成物は0.5wt%の過酸化水素を含んでいて、3.9のpHを有した。銅研磨防止剤(3アミノ1,2,4トリアゾール−ATA)及び両性界面活性剤(コカミドプロピルヒドロキシスルタイン−Mirataine(登録商標)CBS)の濃度は以下のようであった。(7A)250ppmのATA、25ppmの界面活性剤、(7B)250ppmのATA、50ppmの界面活性剤、及び(7C)100ppmのATA、50ppmの界面活性剤。
酸化ケイ素(TEOS)、銅(Cu)、black diamond(登録商標)低k誘電体(BD1)、及び窒化タンタル(TaN)の研磨速度を、様々な研磨組成物に対してこの例の中で評価した。アミノプロピルトリアルコキシシラン(アミノシラン)を加水分解した又は部分的に加水分解したコアシェル構造を有するコロイダルシリカ研磨剤粒子を含んだ研磨組成物のそれぞれを、例12において以下で説明するのと同様の手順を使用してシェル中に組み込んだ。例12でのように調製した濃縮した分散体の量を、銅錯化剤及び銅研磨防止剤を含む混合物に加えて、関連する研磨組成物を得た。4個の研磨組成物を調製して(8A〜8D)、それらのそれぞれは63nmの平均粒子サイズを有する9.0wt%のコロイダルシリカを含んでいた。各研磨組成物は0.5wt%の過酸化水素を含んでいて、4のpHを有した。各組成物は、12ppmの銅研磨防止剤(エトキシル化ノニルフェノール遊離酸のリン酸エステル−RE−410)をさらに含んでいた。殺生物剤(ジプロピレングリコール中の1,2−ベンズイソチアゾリン−3−オン及び水−Proxel(登録商標)GXL)及び銅錯化剤(Dequest(登録商標)2000)の濃度は以下のようであった。(8A)50ppmのProxel(登録商標)GXL、125ppmのDequest(登録商標)2000、(8B)50ppmのProxel(登録商標)GXL、250ppmのDequest(登録商標)2000、(8C)350ppmのProxel(登録商標)GXL、125ppmのDequest(登録商標)2000、(8D)350ppmのProxel(登録商標)GXL、250ppmのDequest(登録商標)2000。
濾過の前と後に、コロイダルシリカ試料に対して、ゼータ電位測定及び伝導度測定を行った。200ml容量の各組成物を、(100000ダルトンのMWカットオフと6.3nmの細孔径を有する)再生セルロース限外濾過ディスクMillipore Ultracellを通じて濾過した。残りの分散体(限外濾過ディスクに保持されている分散体)を回収して、硝酸を使用して3の初期pHに調整した脱イオン水を使用して元の200mlに補充した。この手順を合計3回の濾過サイクルで繰り返した(各工程は限外濾過工程と補充工程とを含んでいた)。研磨組成物のゼータ電位及び電気伝導度を、限外濾過手順の前と後に(すなわち、元の研磨組成物と、三重に限界濾過して補充した研磨組成物とに対して)測定した。ゼータ電位を、Model DT1202音響及び電気音響分光計(Dispersion Technologiesから入手可能)を使用して測定した。
酸化ケイ素(TEOS)、銅(Cu)、black diamond(登録商標)低k誘電体(BD1)、及び窒化タンタル(TaN)の研磨速度を、2個の研磨組成物に対してこの例の中で評価した。比較の研磨組成物10Aは、扶桑化学工業株式会社(東京、日本)から入手可能なPL−3Cコロイダルシリカを含んでいた。PL−3Cは、表面処理したコロイダルシリカであり、コロイダルシリカの表面がアミノプロピルトリアルコキシシランで処理される(と結合する)。アミノプロピルトリアルコキシシラン(アミノシラン)を加水分解した又は部分的に加水分解したコアシェル構造を有するコロイダルシリカ研磨剤粒子を含んだ研磨組成物10Bを、例12において以下で説明するのと同様の手順を使用してシェル中に組み込んだ。研磨組成物のそれぞれは、3.0wt%のコロイダルシリカ、0.03wt%のピコリン酸、0.003wt%のN−ココイル−L−グルタミン酸トリエタノール−アンモニウム複合体、0.03wt%のβ−シクロデキストリン、0.5wt%の過酸化水素を、4.0のpHで含んでいた。
2個の濃縮した研磨組成物の貯蔵寿命安定性を、この例の中で評価した。比較の研磨組成物11Aは、扶桑化学工業株式会社(東京、日本)から入手可能なPL−3Cコロイダルシリカを含んでいた。PL−3Cは、表面処理したコロイダルシリカであり、コロイダルシリカの表面がアミノプロピルトリアルコキシシランで処理される(と結合する)。アミノプロピルトリアルコキシシラン(アミノシラン)を加水分解した又は部分的に加水分解したコアシェル構造を有するコロイダルシリカ研磨剤粒子を含んだ研磨組成物11Bを、例12において以下で説明するのと同様の手順を使用してシェル中に組み込んだ。研磨組成物のそれぞれは、9wt%のコロイダルシリカ、0.08wt%のピコリン酸、0.009wt%のN−ココイル−L−グルタミン酸トリエタノール−アンモニウム複合体、0.08wt%のβ−シクロデキストリンを、4.0のpHで含んでいた。表11は、2個の組成物に対する貯蔵寿命安定性を示す。
化学機械研磨組成物を以下のように調製した。2064gの量のBS−1Hコロイダルシリカ分散体(扶桑化学工業株式会社(東京、日本)から入手可能な、約35nmの平均粒子サイズを有する10.5wt%のコロイダルシリカ分散体)を、5882gのDI水に加えた。3−エトキシプロピルアミン(EOPA)をその混合物に加えて、pHを10に調整して、それによって母液を生成した。次いで、母液を80℃まで加熱した。1872.3gのテトラメトキシシランと16.3gの3−アミノプロピルトリメトキシシランとの混合物を、180分間の間、一定速度で(約10.5g/分の速度で)母液に加え、液体温度を80℃で維持した。アミノシラン(又は加水分解した又は部分的に加水分化したアミノシラン)を含有する外部にシリカシェルを有するコロイダルシリカ粒子を含むコロイダルシリカ分散体を得た。このコロイダルシリカ分散体を、通常の圧力で加熱蒸留することによって4600ミリリットルに濃縮した。3000ミリリットルの容量のDI水を分散体に加えて、蒸留の間にメタノールに置き換えた(容積を維持した)。最終的な分散体はおよそ20.1wt%のコロイダルシリカ濃縮物を有した。
2 2つの凝集した一次粒子から構成される粒子
3 3つの凝集した一次粒子から構成される粒子
4 4つの凝集した一次粒子から構成される粒子
5 5つの凝集した一次粒子から構成される粒子
6 6つの凝集した一次粒子から構成される粒子
20 大きな粒子
Claims (22)
- 水系液体キャリアと、
前記液体キャリア中に分散したコロイダルシリカ研磨剤粒子と、
前記コロイダルシリカ研磨剤粒子中に、外表面に対して内側に組み込まれた、窒素含有化合物又はリン含有化合物である化学種であって、テトラエチルアンモニウムを含まない化学種と、
酸化剤と、
銅研磨防止剤及び銅錯化剤の少なくとも1種と
を含み、3〜7の範囲のpHであり、
前記化学種がアミノシラン化合物でない、化学機械研磨組成物。 - 3〜6の範囲のpHを有する、請求項1に記載の組成物。
- 前記コロイダルシリカ研磨剤粒子が13mV以上の永久正電荷を有する、請求項1に記載の組成物。
- 前記コロイダルシリカ研磨剤粒子が、30〜70nmの範囲の平均粒子サイズを有する、請求項1に記載の組成物。
- 1〜10wt%の前記コロイダルシリカ研磨剤粒子を含む、請求項1に記載の組成物。
- 2〜6wt%の前記コロイダルシリカ研磨剤粒子を含む、請求項1に記載の組成物。
- 前記コロイダルシリカ研磨剤粒子の30%以上が3つ以上の凝集一次粒子を含む、請求項1に記載の組成物。
- 前記コロイダルシリカ研磨剤粒子の50%以上が3つ以上の凝集一次粒子を含み、前記コロイダルシリカ研磨剤粒子の20%以上が単量体又は二量体である、請求項1に記載の組成物。
- 前記酸化剤が過酸化水素を含む、請求項1に記載の組成物。
- 銅研磨防止剤及び銅錯化剤の両方を含む、請求項1に記載の組成物。
- 前記銅研磨防止剤がアゾール化合物、6個以上の炭素鎖長を有するアニオン性又は両性の界面活性剤、又はそれらの混合物である、請求項1に記載の組成物。
- 前記銅錯化剤が、ジカルボン酸、ジホスホン酸、ジスルホン酸、アミノ酸、ジアミン、又はそれらの混合物である、請求項1に記載の組成物。
- 1000μS/cm未満の電気伝導度を有する、請求項1に記載の組成物。
- 前記コロイダルシリカ研磨剤粒子が、外部シェルが内部コア上に配置されたコア−シェル構造を有し、前記化学種が前記外部シェルの中に組み込まれる、請求項1に記載の組成物。
- 前記コロイダルシリカが1.90g/cm3超の密度を有する、請求項1に記載の組成物。
- 前記コロイダルシリカ研磨剤粒子の中のシリカに対する前記化学種のモル比が10%未満である、請求項1に記載の組成物。
- 前記コロイダルシリカ研磨剤粒子が13mV以上の永久正電荷を有し、
前記組成物が銅研磨防止剤及び銅錯化剤を含み、
前記銅研磨防止剤がアゾール化合物、6個以上の炭素鎖長を有するアニオン性又は両性の界面活性剤、又はそれらの混合物であり、
前記錯化剤が、ポリカルボン酸、ポリホスホン酸、ジスルホン酸、アミノ酸、ジアミン、又はそれらの混合物であり、
3〜6の範囲のpHを有する、請求項1に記載の組成物。 - 銅層、銅バリア層、及び誘電体層を含む基材を化学機械研磨するための方法であって、
(a)前記基材を、請求項1に記載の化学機械研磨組成物と接触させる工程、
(b)前記基材に対して前記研磨組成物を動かす工程、並びに
(c)前記基材をすり減らして、前記基材から前記銅層、前記銅バリア層、及び前記誘電体層の一部を除去して、それによって、前記基材を研磨する工程を含む方法。 - 前記誘電体層が酸化ケイ素であり、前記誘電体層の研磨速度が、1.5psi以下の下向きの力で1000Å/分超である、請求項18に記載の方法。
- 誘電体:銅の研磨速度選択性が、1.5psi以下の下向きの力で5:1〜2:1の範囲である、請求項18に記載の方法。
- 前記銅バリア層がTaNを含み、前記TaNの研磨速度が、1.5psi以下の下向きの力で400Å/分超である、請求項18に記載の方法。
- 前記銅バリア層がTaNを含み、誘電体:TaNの研磨速度選択性が3:1〜1:1の範囲である、請求項18に記載の方法。
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JP2017525796A (ja) | 2017-09-07 |
SG11201610332PA (en) | 2017-02-27 |
TWI564380B (zh) | 2017-01-01 |
US9556363B2 (en) | 2017-01-31 |
CN106661431A (zh) | 2017-05-10 |
KR102444548B1 (ko) | 2022-09-20 |
US20150376463A1 (en) | 2015-12-31 |
EP3161095A4 (en) | 2018-07-11 |
KR20170026492A (ko) | 2017-03-08 |
JP6612790B2 (ja) | 2019-11-27 |
EP3161095B1 (en) | 2021-05-19 |
EP3161095A1 (en) | 2017-05-03 |
CN106661431B (zh) | 2019-06-28 |
WO2015200684A1 (en) | 2015-12-30 |
TW201614034A (en) | 2016-04-16 |
JP2019206718A (ja) | 2019-12-05 |
EP3161095B8 (en) | 2021-07-07 |
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