WO2012133561A1 - 研磨用組成物および研磨方法 - Google Patents
研磨用組成物および研磨方法 Download PDFInfo
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- WO2012133561A1 WO2012133561A1 PCT/JP2012/058195 JP2012058195W WO2012133561A1 WO 2012133561 A1 WO2012133561 A1 WO 2012133561A1 JP 2012058195 W JP2012058195 W JP 2012058195W WO 2012133561 A1 WO2012133561 A1 WO 2012133561A1
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- Prior art keywords
- polishing composition
- group
- polishing
- acid
- hydrogen peroxide
- Prior art date
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Classifications
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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
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
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- C—CHEMISTRY; METALLURGY
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- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
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- H01L21/3212—Planarisation by chemical mechanical polishing [CMP]
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- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
Abstract
Description
酸化剤は研磨対象物の表面を酸化する作用を有し、研磨用組成物中に酸化剤を加えた場合には、研磨用組成物による研磨速度が向上する有利がある。
水溶液中において酸化剤との共存下でpHを低下させるpH低下物質は、界面活性剤、水溶性高分子、アミン化合物、金属防食剤および有機溶剤のうち、以下の条件を満たす物質である。すなわち、0.05重量%の界面活性剤または水溶性高分子、あるいは5mmol/Lのアミン化合物、金属防食剤または有機溶剤を含有した水溶液を用意し、水酸化カリウムまたは硫酸をpH調節剤として添加して水溶液のpHを約7.5に調整する。そして、この水溶液100gに対して31重量%過酸化水素水を10.32g、すなわち過酸化水素3.2gを添加した直後の水溶液のpHと、過酸化水素を添加してから常温(23℃~27℃)で8日間静置保管した後の水溶液のpHとを比較する。このときのpHの差が絶対値で0.5以上であるというのがその条件である。
pH緩衝剤は、研磨用組成物100gに対して31重量%過酸化水素水を5.16g、すなわち過酸化水素1.6gを添加した直後の研磨用組成物のpHと、過酸化水素水を添加してから8日後の研磨用組成物のpHとの差を絶対値で0.5以下とするべく研磨用組成物中に配合されている。このpHの差が絶対値で0.5以下であれば、研磨用組成物の研磨性能の経時的な低下を実用的に問題ない程度にまで抑えることができ、安定性に優れた研磨用組成物を提供できる。
研磨用組成物のpHは、3以上であることが好ましく、より好ましくは5以上であり、さらに好ましくは6以上である。pHが大きくなるにつれて、研磨用組成物による研磨対象物表面の過剰なエッチングが起こりにくくなる有利がある。
研磨用組成物は、酸化剤、pH低下物質、およびpH緩衝剤に加えて、それらに分類されない研磨促進剤をさらに含有してもよい。研磨促進剤は、研磨対象物の表面を化学的にエッチングする作用を有し、研磨用組成物による研磨速度を向上させる働きをする。
研磨用組成物は、酸化剤、pH低下物質、およびpH緩衝剤に加えて、それらに分類されない界面活性剤をさらに含有してもよい。研磨用組成物中に界面活性剤を加えた場合には、研磨用組成物を用いた研磨により形成される配線の脇に凹みが生じにくくなるのに加え、研磨用組成物を用いて研磨した後の研磨対象物の表面にディッシングが生じにくくなる有利がある。
研磨用組成物は、酸化剤、pH低下物質、およびpH緩衝剤に加えて、それらに分類されない金属防食剤をさらに含有してもよい。研磨用組成物中に金属防食剤を加えた場合には、界面活性剤を加えた場合と同様、研磨用組成物を用いた研磨により形成される配線の脇に凹みが生じにくくなるのに加え、研磨用組成物を用いて研磨した後の研磨対象物の表面にディッシングが生じにくくなる有利がある。また、金属防食剤は、研磨用組成物中に酸化剤が含まれている場合には、酸化剤による研磨対象物表面の酸化を緩和するとともに、酸化剤による研磨対象物表面の金属の酸化により生じる金属イオンと反応して不溶性の錯体を生成する働きをする。この金属防食剤の働きは、研磨用組成物を用いて研磨した後の研磨対象物の表面の平坦性を向上させる。
研磨用組成物は、酸化剤、pH低下物質、およびpH緩衝剤に加えて、それらに分類されない水溶性高分子をさらに含有してもよい。研磨用組成物中に水溶性高分子を加えた場合には、砥粒の表面または研磨対象物の表面に水溶性高分子が吸着することにより研磨用組成物による研磨速度をコントロールすることが可能であることに加え、研磨中に生じる不溶性の成分を研磨用組成物中で安定化することができる有利がある。
砥粒は研磨対象物を機械的に研磨する作用を有し、研磨用組成物中に砥粒を加えた場合には、研磨用組成物による研磨速度が向上する有利がある。
pH制御剤は、水溶液中において酸化剤との共存下で塩基性物質を発生する化合物として定義される。第2の実施形態の研磨用組成物によれば、pH低下物質とpH制御剤とを含有することにより、研磨用組成物のpHが経時的に変化するのを抑制することができる。そのため、研磨用組成物の研磨性能の経時的な低下を実用的に問題ない程度にまで抑えることができ、安定性に優れた研磨用組成物を提供できる。
酸化剤、pH低下物質、pH緩衝剤、研磨促進剤、界面活性剤および砥粒を水に混合し、実施例1~9の研磨用組成物を調製した。また、酸化剤、pH低下物質、pH緩衝剤に代わる化合物、研磨促進剤、界面活性剤および砥粒を水に混合し、比較例1~5の研磨用組成物を調製した。実施例1~9および比較例1~5の研磨用組成物中のpH緩衝剤またはpH緩衝剤に代わる化合物の詳細は、表3の“pH緩衝剤またはそれに代わる化合物”欄内の“名称”欄と“含有量”欄に示すとおりである。なお、表3には示していないが、実施例1~9および比較例1~5の研磨用組成物はいずれも、酸化剤として51.6g/Lの31重量%過酸化水素水(すなわち16g/Lの過酸化水素)を含有し、pH低下物質としてポリオキシエチレンアルキルエーテルを0.5g/Lおよび1-[N,N-ビス(ヒドロキシエチル)アミノメチル]-5-メチルベンゾトリアゾールと1-[N,N-ビス(ヒドロキシエチル)アミノメチル]-4-メチルベンゾトリアゾールの1:1混合物を0.15g/L含有し、研磨促進剤として10g/Lのグリシンを含有し、界面活性剤として0.3g/Lのラウリルエーテル硫酸アンモニウムを含有し、砥粒としてBET法による平均一次粒子径が30nmのコロイダルシリカを0.1質量%含有している。また、これらの研磨用組成物はいずれも、水酸化カリウムを用いてpHを約7.5に調整している。
実施例1~9および比較例1~5の研磨用組成物を、恒温槽を用いて常温(23℃~27℃)下で8日間静置保管した。調製直後に測定した研磨用組成物のpH値、8日間の静置後に測定した研磨用組成物のpH値、および8日間で生じたpHの変化量をそれぞれ表3の“過酸化水素あり”欄内の“調製直後のpH”欄、“8日後のpH”欄、および“pH変化量”欄に示す。
調製直後または8日間静置後の実施例1~9および比較例1~5の各研磨用組成物を用いて、銅ブランケットウェーハの表面を表4に記載の第1の研磨条件で60秒間研磨した。調製直後の研磨用組成物で得られた研磨速度、8日間の静置後の研磨用組成物で得られた研磨速度、および8日間の静置で生じた研磨速度の変化率をそれぞれ表3の“高圧研磨条件”欄内の“調製直後の研磨速度”欄、“8日後の研磨速度”欄、および“研磨速度変化率”欄に示す。
酸化剤、pH低下物質、pH制御剤、研磨促進剤、界面活性剤および砥粒を水に混合し、実施例11~21の研磨用組成物を調製した。また、酸化剤、pH低下物質、pH制御剤に代わる化合物、研磨促進剤、界面活性剤および砥粒を水に混合し、比較例11~17の研磨用組成物を調製した。実施例11~21および比較例11~17の研磨用組成物中のpH制御剤またはpH制御剤に代わる化合物の詳細は、を表6及び表7の“pH制御剤またはそれに代わる化合物”欄内の“名称”欄と“含有量”欄に示すとおりである。なお、表6及び表7には示していないが、実施例11~21および比較例11~17の研磨用組成物はいずれも、酸化剤として51.6g/Lの31重量%過酸化水素水(すなわち16g/Lの過酸化水素)を含有し、pH低下物質としてポリオキシエチレンアルキルエーテルを0.5g/Lおよび1-[N,N-ビス(ヒドロキシエチル)アミノメチル]-5-メチルベンゾトリアゾールと1-[N,N-ビス(ヒドロキシエチル)アミノメチル]-4-メチルベンゾトリアゾールの1:1混合物を0.15g/L含有し、研磨促進剤として10g/Lのグリシンを含有し、界面活性剤として0.3g/Lのラウリルエーテル硫酸アンモニウムを含有し、砥粒としてBET法による平均一次粒子径が30nmのコロイダルシリカを0.1質量%含有している。また、これらの研磨用組成物はいずれも、水酸化カリウムを用いてpHを約7.5に調整している。
実施例11~21および比較例11~17の研磨用組成物を、恒温槽を用いて常温(23℃~27℃)下で8日間静置保管した。調製直後に測定した研磨用組成物のpH値、8日間の静置後に測定した研磨用組成物のpH値、および8日間で生じたpHの変化量をそれぞれ表6及び表7の“過酸化水素あり”欄内の“調製直後のpH”欄、“8日後のpH”欄、および“pH変化量”欄に示す。
調製直後または8日間静置後の実施例11~21および比較例11~17の各研磨用組成物を用いて、銅ブランケットウェーハの表面を表8に記載の第3の研磨条件で研磨した。調製直後の研磨用組成物で得られた研磨速度、8日間の静置後の研磨用組成物で得られた研磨速度、および8日間の静置で生じた研磨速度の変化率をそれぞれ表6及び表7の“高圧研磨条件”欄内の“調製直後の研磨速度”欄、“8日後の研磨速度”欄、および“研磨速度変化率”欄に示す。
実施例11~21および比較例11~17の各研磨用組成物について、調製直後の研磨用組成物中の塩基性物質の濃度と8日間静置した後の研磨用組成物中の塩基性物質の濃度とを測定した。その濃度の差を表6及び表7の“塩基性物質濃度増加量”欄に示す。なお、各研磨用組成物中の塩基性物質の定量および定性はイオンクロマト分析法で行った。
Claims (16)
- 水溶液中において酸化剤との共存下でpHを低下させる物質、およびpH緩衝剤を含有する研磨用組成物であって、研磨用組成物100gに対して31重量%過酸化水素水を5.16g添加した直後の研磨用組成物のpHと、過酸化水素水を添加してから8日間静置した後の研磨用組成物のpHとの差が絶対値で0.5以下であることを特徴とする研磨用組成物。
- 前記pH緩衝剤がアミド基を有する化合物である、請求項1に記載の研磨用組成物。
- 前記pH緩衝剤がスルホ基およびカルボキシル基の少なくともいずれか一方を有する両性アミノ酸である、請求項1または2に記載の研磨用組成物。
- 前記一般式(1)において、Xはスルホ基またはその塩である、請求項4に記載の研磨用組成物。
- 水溶液中において酸化剤との共存下でpHを低下させる物質、およびpH制御剤を含有する研磨用組成物であって、研磨用組成物100mlに対して31重量%過酸化水素水を5.16g添加した直後の研磨用組成物中の塩基性物質の量に比べて、過酸化水素水を添加してから8日間静置した後の研磨用組成物中の塩基性物質の量が0.1mM以上増加することを特徴とする研磨用組成物。
- 前記研磨用組成物100mlに対して31重量%過酸化水素水を5.16g添加した直後の研磨用組成物のpHと、過酸化水素水を添加してから8日間静置した後の研磨用組成物のpHとの差が絶対値で0.5以下である、請求項6に記載の研磨用組成物。
- 前記塩基性化合物がアンモニアである、請求項6または7に記載の研磨用組成物。
- 前記pH制御剤を5.0mM含んだ100mlの水溶液に31重量%過酸化水素水を10.32g添加した直後の水溶液中の塩基性物質の量に比べて、過酸化水素水を添加してから8日間静置した後の水溶液中の塩基性物質の量が0.2mM以上増加する、請求項6~8のいずれか一項に記載の研磨用組成物。
- 前記pH制御剤がアミド基を有する化合物である、請求項6~9のいずれか一項に記載の研磨用組成物。
- 前記pH制御剤がスルホ基およびカルボキシル基の少なくともいずれか一方を有する両性アミノ酸である、請求項6~10のいずれか一項に記載の研磨用組成物。
- 前記一般式(2)において、Xはスルホ基またはその塩である、請求項12に記載の研磨用組成物。
- 請求項1~13のいずれか一項に記載の研磨用組成物を用いて、金属を研磨する方法。
- 研磨時に研磨用組成物に酸化剤を混合することを特徴とする請求項14に記載の研磨方法。
- 請求項14または15に記載の方法で金属を研磨する工程を有する、金属を含む基板の製造方法。
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KR101628878B1 (ko) * | 2015-09-25 | 2016-06-16 | 영창케미칼 주식회사 | Cmp용 슬러리 조성물 및 이를 이용한 연마방법 |
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CN115160933B (zh) * | 2022-07-27 | 2023-11-28 | 河北工业大学 | 一种用于钴互连集成电路钴cmp的碱性抛光液及其制备方法 |
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Also Published As
Publication number | Publication date |
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EP2693459A4 (en) | 2015-04-22 |
EP2693459A1 (en) | 2014-02-05 |
TW201307540A (zh) | 2013-02-16 |
CN103562337A (zh) | 2014-02-05 |
TWI525182B (zh) | 2016-03-11 |
US20140014872A1 (en) | 2014-01-16 |
KR20140019403A (ko) | 2014-02-14 |
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