JP6915678B2 - 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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- JP6915678B2 JP6915678B2 JP2019505885A JP2019505885A JP6915678B2 JP 6915678 B2 JP6915678 B2 JP 6915678B2 JP 2019505885 A JP2019505885 A JP 2019505885A JP 2019505885 A JP2019505885 A JP 2019505885A JP 6915678 B2 JP6915678 B2 JP 6915678B2
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- abrasive
- silica particles
- polishing
- abrasive grains
- mass
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- C—CHEMISTRY; METALLURGY
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
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- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
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- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Disintegrating Or Milling (AREA)
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。
本実施形態に係る研磨剤は、シリカ粒子を含む砥粒を含有する。シリカ粒子は、シリカを含む粒子である。シリカ粒子におけるシリカの含有量は、シリカ粒子の全量を基準として、50質量%以上であってもよく、70質量%以上であってもよく、90質量%以上であってもよく、95質量%以上であってもよく、98質量%以上であってもよい。シリカ粒子は、シリカからなる粒子(実質的に粒子の100質量%がシリカである粒子)であってもよい。
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、溶媒として用いることができる。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水として、純水、超純水及び蒸留水からなる群より選ばれる少なくとも一種が好ましい。
本実施形態に係る研磨剤のpHは、TEOS膜の更に良好な研磨速度が得られる観点、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、6.0以下がより好ましく、6.0未満が更に好ましく、5.0以下が特に好ましく、5.0未満が極めて好ましく、4.0以下が非常に好ましく、4.0未満がより一層好ましく、3.8以下が更に好ましく、3.5以下が特に好ましく、3.0以下が極めて好ましい。研磨剤のpHは、取り扱いの安全面に優れる観点、及び、充分な機械的研磨力が得られ易く、TEOS膜の研磨速度が更に向上する観点から、2.0以上が好ましく、2.3以上がより好ましく、2.5以上が更に好ましい。これらの観点から、研磨剤のpHは、2.0以上7.0未満が好ましく、2.0〜5.0がより好ましく、2.0〜4.0が更に好ましい。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、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、キレート剤(キレート剤成分)、防食剤、酸化剤、有機溶媒、界面活性剤、消泡剤等が挙げられる。
キレート剤は、上記pH調整剤としての効果以外にも、配線金属及びバリア金属の研磨速度を向上させることができる。キレート剤としては、配線金属及びバリア金属の研磨速度を向上させる観点から、有機酸成分及び無機酸成分からなる群より選ばれる少なくとも一種の酸成分が好ましい。
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、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、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。
グリコール類としては、エチレングリコール、プロピレングリコール、ジエチレングリコール、ジプロピレングリコール、トリエチレングリコール、トリプロピレングリコール等が挙げられる。グリコール類の誘導体としては、グリコールモノエーテル類、グリコールジエーテル類等が挙げられる。グリコールモノエーテル類としては、エチレングリコールモノメチルエーテル、プロピレングリコールモノメチルエーテル、プロピレングリコールモノメチルエーテルアセテート、ジエチレングリコールモノメチルエーテル、ジプロピレングリコールモノメチルエーテル、トリエチレングリコールモノメチルエーテル、トリプロピレングリコールモノメチルエーテル、エチレングリコールモノエチルエーテル、プロピレングリコールモノエチルエーテル、ジエチレングリコールモノエチルエーテル、ジプロピレングリコールモノエチルエーテル、トリエチレングリコールモノエチルエーテル、トリプロピレングリコールモノエチルエーテル、エチレングリコールモノプロピルエーテル、プロピレングリコールモノプロピルエーテル、ジエチレングリコールモノプロピルエーテル、ジプロピレングリコールモノプロピルエーテル、トリエチレングリコールモノプロピルエーテル、トリプロピレングリコールモノプロピルエーテル、エチレングリコールモノブチルエーテル、プロピレングリコールモノブチルエーテル、ジエチレングリコールモノブチルエーテル、ジプロピレングリコールモノブチルエーテル、トリエチレングリコールモノブチルエーテル、トリプロピレングリコールモノブチルエーテル等が挙げられる。グリコールジエーテル類としては、エチレングリコールジメチルエーテル、プロピレングリコールジメチルエーテル、ジエチレングリコールジメチルエーテル、ジプロピレングリコールジメチルエーテル、トリエチレングリコールジメチルエーテル、トリプロピレングリコールジメチルエーテル、エチレングリコールジエチルエーテル、プロピレングリコールジエチルエーテル、ジエチレングリコールジエチルエーテル、ジプロピレングリコールジエチルエーテル、トリエチレングリコールジエチルエーテル、トリプロピレングリコールジエチルエーテル、エチレングリコールジプロピルエーテル、プロピレングリコールジプロピルエーテル、ジエチレングリコールジプロピルエーテル、ジプロピレングリコールジプロピルエーテル、トリエチレングリコールジプロピルエーテル、トリプロピレングリコールジプロピルエーテル、エチレングリコールジブチルエーテル、プロピレングリコールジブチルエーテル、ジエチレングリコールジブチルエーテル、ジプロピレングリコールジブチルエーテル、トリエチレングリコールジブチルエーテル、トリプロピレングリコールジブチルエーテル等が挙げられる。有機溶媒としては、表面張力が低い観点から、グリコール類、及び、グリコール類の誘導体からなる群より選ばれる少なくとも一種が好ましく、表面張力が更に低い観点から、グリコールモノエーテル類がより好ましい。
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ることができる。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、研磨剤を用いて酸化ケイ素膜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、酸化ケイ素膜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、酸化ケイ素膜を有する基体の前記酸化ケイ素膜の少なくとも一部を研磨して除去することができる。酸化ケイ素膜は、TEOS膜及びSiH4膜からなる群より選ばれる少なくとも一種を含んでいてもよい。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膜を有してもよい。基体は、例えば、配線板又は回路基板であってもよい。基体は、基板表面全体に酸化ケイ素膜のみが形成されたものに限らず、基板表面に酸化ケイ素膜の他に窒化ケイ素膜、多結晶シリコン膜等を更に有したものであってもよい。また、当該研磨方法は、所定の配線を有する配線板上に、酸化ケイ素膜;ガラス、窒化ケイ素等の無機絶縁膜;ポリシリコン、Al、Cu、Ti、TiN、W、Ta、TaN等を主として含有する膜などが形成された基体に対しても適用できる。
(実施例1)
砥粒(コロイダルシリカ1)5.00質量部に対し、研磨剤のpHが2.5となるようにマロン酸(pH調整剤)を注いだ後、超純水をX質量部注いで研磨剤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。
砥粒の種類(コロイダルシリカ2〜9)を表1のとおりに変更したこと以外は、実施例1と同様の方法で研磨剤を調製した。
砥粒(コロイダルシリカ1)10.00質量部を容器に入れた。次に、研磨剤のpHが10.0となるようにKOHとマロン酸を注いだ後、超純水をX質量部注いで研磨剤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。
動的光散乱式粒度分布計(COULTER Electronics社製の商品名:COULTER N4SD)を用いて、研磨剤中における砥粒の平均粒径Raveを測定した。結果を表1に示す。
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。ゼータ電位の測定装置としては、ベックマン・コールター株式会社製の商品名:DELSA NANO Cを用いた。ゼータ電位の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。結果を表1に示す。
研磨剤のpHは、下記の条件で測定した。結果を表1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。
被研磨膜を有する基体として、膜厚500nmのTEOS膜をシリコン基板上に有する基体、及び、膜厚200nmのSiH4膜をシリコン基板上に有する基体を用いた。前記基体を20mm角のチップに切り出して評価用チップを用意した。前記で調製した研磨剤を用いて、下記研磨条件にて60秒間評価用チップの被研磨膜を化学機械研磨した。
研磨装置:卓上研磨機(日本エンギス株式会社製、商品名:IMPTECH 10 DVT)
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:120回/min
研磨圧力:33kPa
研磨剤の供給量:10mL/min
Claims (9)
- 砥粒と、水と、を含有する研磨剤であって、
前記砥粒がシリカ粒子を含み、
前記シリカ粒子がコロイダルシリカを含み、
前記砥粒の平均二次粒径Raveが50nm以上であり、
前記砥粒の平均短径Rminに対する前記平均二次粒径Raveの比率Rave/Rminが1.0〜1.3であり、
前記研磨剤中における前記砥粒のゼータ電位が正である、研磨剤(但し、媒体と、前記媒体に分散している砥粒とを含むCMP用研磨液であって、前記砥粒が、シラノール基密度が3.0〜5.0個/nm2でありかつアスペクト比が1.3以下のシリカ粒子Xと、シラノール基密度が1.0〜2.0個/nm2でありかつアスペクト比が1.3を超えるシリカ粒子Yとを含み、前記シリカ粒子X及び前記シリカ粒子Yの全質量に対する前記シリカ粒子Xの質量比が30〜95%である、CMP用研磨液、並びに、媒体と、前記媒体に分散している砥粒とを含むCMP用研磨液であって、前記砥粒が、シラノール基密度が3.0〜5.0個/nm2でありかつアスペクト比が1.3以下のシリカ粒子Xと、シラノール基密度が1.0〜2.0個/nm2でありかつアスペクト比が1.3を超えるシリカ粒子Yとを含み、前記シリカ粒子X及び前記シリカ粒子Yの全質量に対する前記シリカ粒子Xの質量比が20〜80%である、CMP用研磨液を除く)。 - 砥粒と、水と、を含有する研磨剤であって、
前記砥粒がシリカ粒子を含み、
前記シリカ粒子がコロイダルシリカを含み、
前記砥粒の平均二次粒径Raveが50nm以上であり、
前記砥粒の平均短径Rminに対する前記平均二次粒径Raveの比率Rave/Rminが1.71〜2.0であり、
前記研磨剤中における前記砥粒のゼータ電位が正である、研磨剤(但し、媒体と、前記媒体に分散している砥粒とを含むCMP用研磨液であって、前記砥粒が、シラノール基密度が3.0〜5.0個/nm2でありかつアスペクト比が1.3以下のシリカ粒子Xと、シラノール基密度が1.0〜2.0個/nm2でありかつアスペクト比が1.3を超えるシリカ粒子Yとを含み、前記シリカ粒子X及び前記シリカ粒子Yの全質量に対する前記シリカ粒子Xの質量比が30〜95%である、CMP用研磨液、並びに、媒体と、前記媒体に分散している砥粒とを含むCMP用研磨液であって、前記砥粒が、シラノール基密度が3.0〜5.0個/nm2でありかつアスペクト比が1.3以下のシリカ粒子Xと、シラノール基密度が1.0〜2.0個/nm2でありかつアスペクト比が1.3を超えるシリカ粒子Yとを含み、前記シリカ粒子X及び前記シリカ粒子Yの全質量に対する前記シリカ粒子Xの質量比が20〜80%である、CMP用研磨液を除く)。 - 前記平均二次粒径Raveが50〜100nmである、請求項1又は2に記載の研磨剤。
- 前記平均二次粒径Raveが60nmを超える、請求項1〜3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1〜4のいずれか一項に記載の研磨剤。
- pHが2.0〜4.0である、請求項1〜5のいずれか一項に記載の研磨剤。
- 請求項1〜6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1〜6のいずれか一項に記載の研磨剤、又は、請求項7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、酸化ケイ素膜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。
- 前記酸化ケイ素膜が、TEOS膜及びSiH4膜からなる群より選ばれる少なくとも一種を含む、請求項8に記載の研磨方法。
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JP5844135B2 (ja) * | 2010-12-24 | 2016-01-13 | 花王株式会社 | 研磨液組成物の製造方法 |
WO2012102187A1 (ja) * | 2011-01-25 | 2012-08-02 | 日立化成工業株式会社 | Cmp研磨液及びその製造方法、複合粒子の製造方法、並びに基体の研磨方法 |
JP6028432B2 (ja) | 2012-07-17 | 2016-11-16 | 日立化成株式会社 | Cmp用研磨液、cmp用研磨液用貯蔵液及び研磨方法 |
JP2015189898A (ja) * | 2014-03-28 | 2015-11-02 | 株式会社フジミインコーポレーテッド | 研磨用組成物 |
WO2015200668A1 (en) * | 2014-06-25 | 2015-12-30 | Cabot Microelectronics Corporation | Methods for fabricating a chemical-mechanical polishing composition |
CN107533967A (zh) * | 2015-03-30 | 2018-01-02 | 福吉米株式会社 | 研磨用组合物 |
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US20200017718A1 (en) | 2020-01-16 |
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