JP6604061B2 - Cmp用研磨液及び研磨方法 - Google Patents
Cmp用研磨液及び研磨方法 Download PDFInfo
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- JP6604061B2 JP6604061B2 JP2015138798A JP2015138798A JP6604061B2 JP 6604061 B2 JP6604061 B2 JP 6604061B2 JP 2015138798 A JP2015138798 A JP 2015138798A JP 2015138798 A JP2015138798 A JP 2015138798A JP 6604061 B2 JP6604061 B2 JP 6604061B2
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- Prior art keywords
- polishing
- cobalt
- cmp
- metal
- polished
- Prior art date
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- 239000002184 metal Substances 0.000 claims description 112
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- 239000010936 titanium Substances 0.000 claims description 31
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 29
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 20
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- 229910052802 copper Inorganic materials 0.000 claims description 18
- 239000010949 copper Substances 0.000 claims description 18
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- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 4
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- 238000005227 gel permeation chromatography Methods 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
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- 229910052715 tantalum Inorganic materials 0.000 description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 3
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
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- WGLQHUKCXBXUDV-UHFFFAOYSA-N 3-aminophthalic acid Chemical class NC1=CC=CC(C(O)=O)=C1C(O)=O WGLQHUKCXBXUDV-UHFFFAOYSA-N 0.000 description 2
- MFKRHJVUCZRDTF-UHFFFAOYSA-N 3-methoxy-3-methylbutan-1-ol Chemical compound COC(C)(C)CCO MFKRHJVUCZRDTF-UHFFFAOYSA-N 0.000 description 2
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- KFIRODWJCYBBHY-UHFFFAOYSA-N 3-nitrophthalic acid Chemical compound OC(=O)C1=CC=CC([N+]([O-])=O)=C1C(O)=O KFIRODWJCYBBHY-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
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- CVSUAFOWIXUYQA-UHFFFAOYSA-M 2,6-Dichlorophenolindophenol sodium salt Chemical compound [Na+].C1=CC([O-])=CC=C1N=C1C=C(Cl)C(=O)C(Cl)=C1 CVSUAFOWIXUYQA-UHFFFAOYSA-M 0.000 description 1
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- DJCYDDALXPHSHR-UHFFFAOYSA-N 2-(2-propoxyethoxy)ethanol Chemical compound CCCOCCOCCO DJCYDDALXPHSHR-UHFFFAOYSA-N 0.000 description 1
- HMOYKDCLYCJGHG-UHFFFAOYSA-N 2-(2h-benzotriazol-4-ylmethyl)butanedioic acid Chemical compound OC(=O)CC(C(O)=O)CC1=CC=CC2=NNN=C12 HMOYKDCLYCJGHG-UHFFFAOYSA-N 0.000 description 1
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- COBPKKZHLDDMTB-UHFFFAOYSA-N 2-[2-(2-butoxyethoxy)ethoxy]ethanol Chemical compound CCCCOCCOCCOCCO COBPKKZHLDDMTB-UHFFFAOYSA-N 0.000 description 1
- WFSMVVDJSNMRAR-UHFFFAOYSA-N 2-[2-(2-ethoxyethoxy)ethoxy]ethanol Chemical compound CCOCCOCCOCCO WFSMVVDJSNMRAR-UHFFFAOYSA-N 0.000 description 1
- FMVOPJLFZGSYOS-UHFFFAOYSA-N 2-[2-(2-ethoxypropoxy)propoxy]propan-1-ol Chemical compound CCOC(C)COC(C)COC(C)CO FMVOPJLFZGSYOS-UHFFFAOYSA-N 0.000 description 1
- LCZVSXRMYJUNFX-UHFFFAOYSA-N 2-[2-(2-hydroxypropoxy)propoxy]propan-1-ol Chemical compound CC(O)COC(C)COC(C)CO LCZVSXRMYJUNFX-UHFFFAOYSA-N 0.000 description 1
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- QCAHUFWKIQLBNB-UHFFFAOYSA-N 3-(3-methoxypropoxy)propan-1-ol Chemical compound COCCCOCCCO QCAHUFWKIQLBNB-UHFFFAOYSA-N 0.000 description 1
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- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
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- 125000003118 aryl group Chemical group 0.000 description 1
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- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
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- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 description 1
- XXJWXESWEXIICW-UHFFFAOYSA-N diethylene glycol monoethyl ether Chemical compound CCOCCOCCO XXJWXESWEXIICW-UHFFFAOYSA-N 0.000 description 1
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- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 description 1
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- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 description 1
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
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- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 1
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Images
Landscapes
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Description
「工程」には、独立した工程だけではなく、他の工程と明確に区別できない場合であっても、当該「工程」において規定される操作が実施される限り、他の工程と明確に区別できない工程も含まれる。
「〜」を用いて示された数値範囲は、「〜」の前後に記載される数値をそれぞれ最小値及び最大値として含む範囲を示す。
CMP用研磨液中の各成分の含有量は、CMP用研磨液中に各成分に該当する物質が複数存在する場合、特に断らない限り、CMP用研磨液中に存在する当該複数の物質の合計量を意味する。
本実施形態に係るCMP用研磨液は、絶縁材料部と、コバルト含有部と、前記絶縁材料部及び前記コバルト含有部を接着するチタン含有部(接着層)と、を有し、かつ、被研磨面に前記コバルト含有部が露出した基板の前記被研磨面を研磨するためのCMP用研磨液である。前記基板の表面は、前記被研磨面を有している。前記基板の前記被研磨面は、主たる成分として銅を含有する銅含有部を有しない態様であってもよく、銅含有部を有する態様であってもよい。
CMP用研磨液は、砥粒を含有する。CMP用研磨液が砥粒を含有することにより、金属含有部(例えば、コバルト含有部の近傍に設けられた金属含有部)の研磨速度が向上する傾向がある。砥粒は、一種を単独で、又は、二種以上を混合して用いることができる。
CMP用研磨液は、トリアゾール骨格を有する化合物(トリアゾール類)を含む金属防食剤を含有する。CMP用研磨液が前記金属防食剤を含有することにより、コバルト含有部の良好な研磨速度を保ちながらコバルト含有部のエッチングを効果的に抑制できる。
CMP用研磨液は、水溶性ポリマを含有する。CMP用研磨液が水溶性ポリマを含有することにより、コバルト含有部のガルバニック腐食の抑制、被研磨面の保護、欠陥(ディフェクト)発生の低減等が可能である。水溶性ポリマは、25℃において水100gに対して0.1g以上溶解するものが好ましい。水溶性ポリマは、一種を単独で、又は、二種以上を混合して用いることができる。
検出器:株式会社日立製作所製、RI−モニター「L−3000」
インテグレーター:株式会社日立製作所製、GPCインテグレーター「D−2200」
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」
カラム:日立化成株式会社製「GL−R440」、「GL−R430」及び「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℃
流速:1.75mL/min
測定時間:45min
注入量:10μL
標準ポリアクリル酸:日立化成テクノサービス株式会社製「PMAA−32」
CMP用研磨液は、有機酸類を更に含有してもよい。有機酸類は、金属含有部(コバルト含有部等の導電性物質部など)の研磨速度を更に向上させる効果を有する。有機酸類には、有機酸、有機酸の塩、有機酸の無水物、及び、有機酸のエステルが含まれる。有機酸類は、一種を単独で、又は、二種以上を混合して用いることができる。
CMP用研磨液は、金属酸化剤を含有してもよい。金属酸化剤としては、特に制限はないが、例えば、過酸化水素、ペルオキソ硫酸塩、硝酸、過ヨウ素酸カリウム、次亜塩素酸、オゾン等が挙げられる。金属酸化剤としては、金属含有部の研磨速度を更に向上させる観点から、過酸化水素が特に好ましい。金属酸化剤は、一種を単独で、又は、二種以上を混合して用いることができる。
CMP用研磨液は、有機溶媒(有機酸類に該当する化合物を除く)を更に含有してもよい。CMP用研磨液が有機溶媒を含有することにより、金属含有部(例えば、コバルト含有部の近傍に設けられた金属含有部)に対するCMP用研磨液の濡れ性を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、水と混合できるものが好ましく、25℃において水100gに対して0.1g以上溶解するものがより好ましい。有機溶媒は、一種を単独で、又は、二種以上を混合して用いることができる。
CMP用研磨液は水を含有する。水は、特に制限されるものではないが、純水を好ましく用いることができる。水は残部として配合されていればよく、含有量に特に制限はない。
CMP用研磨液のpHは、4.0以下であることが好ましい。pHが4.0以下である場合、金属含有部(コバルト含有部等の導電性物質部など)の研磨速度に更に優れる。pHは、好ましくは3.8以下であり、より好ましくは3.6以下であり、更に好ましくは3.5以下である。また、CMP用研磨液のpHは、金属含有部(コバルト含有部等の導電性物質部など)の腐食を更に抑制する観点、また、酸性が強いことによる取扱い難さを解消する観点から、2.0以上が好ましく、2.5以上がより好ましく、2.8以上が更に好ましい。
本実施形態に係る研磨方法は、本実施形態に係るCMP用研磨液を用いて、絶縁材料部と、コバルト含有部と、前記絶縁材料部及び前記コバルト含有部を接着するチタン含有部と、を有し、かつ、被研磨面に前記コバルト含有部が露出した基板の前記被研磨面を研磨して前記コバルト含有部の少なくとも一部を除去する研磨工程を備える。前記被研磨面は、コバルト以外の金属を含有する金属含有部を有してもよい。本実施形態に係る研磨方法は、本実施形態に係るCMP用研磨液を用いて、コバルト含有部と、コバルト以外の金属を含有する金属含有部とを少なくとも有する被研磨面の、コバルト含有部の少なくとも一部を研磨して除去する研磨方法であってもよい。本実施形態に係る研磨方法は、本実施形態に係るCMP用研磨液を用いて、コバルト含有部を有し、かつ、主たる成分として銅を含有する銅含有部を有しない被研磨面の、コバルト含有部の少なくとも一部を研磨して除去する研磨方法であってもよい。
表1及び表2に示す各成分を用いてCMP用研磨液を下記の方法で作製した。
表1及び表2に示す種類の金属防食剤と、有機溶媒として3−メトキシ−3−メチル−1−ブタノールと、水溶性ポリマとしてポリアクリル酸アンモニウム塩(重量平均分子量8,000)と、砥粒(研磨粒子)としてコロイダルシリカ(平均二次粒径60nm)とを容器に入れ、さらに、超純水を注いだ後、酸化剤である過酸化水素水を加え、撹拌により混合して全成分を溶解させ、全体を100質量部としてCMP用研磨液を得た。
CMP用研磨液のpHを下記に従って測定した。
測定温度:25℃
測定器:電気化学計器株式会社製「PHL−40」
測定方法:標準緩衝液(フタル酸塩pH緩衝液 pH:4.01(25℃)、中性リン酸塩pH緩衝液 pH:6.86(25℃)、ホウ酸塩pH緩衝液 pH:9.18(25℃)を用いて3点校正した後、電極をCMP用研磨液に入れて、3min以上経過して安定した後の値を測定した。結果を表1及び表2に示す。
12インチのシリコン基板上に厚み200nmのコバルト層を形成したブランケット基板(a)を用意した。上記ブランケット基板(a)を、20mm角のチップに切り出して評価用チップ(b)を用意した。
浸漬後のコバルト層の厚み[nm]=104.5×(評価用チップ(b)の抵抗値[mΩ]/1000)−0.893 ・・・(1)
コバルト層のエッチング速度(Co−ER)[nm/min]=(浸漬前のコバルト層の厚み[nm]−浸漬後のコバルト層の厚み[nm])/1min ・・・(2)
上記で得られた各研磨液を用いて上記ブランケット基板(a)を下記条件で研磨及び洗浄したときの研磨速度(Co−RR)[nm/min]を求めた。この結果を表1及び表2に示す。
研磨装置:片面金属膜用研磨機(アプライドマテリアルズ社製「Reflexion LK」)
研磨パッド:発泡ポリウレタン樹脂製研磨パッド
定盤回転数:93min−1
研磨ヘッド回転数:87min−1
研磨圧力:10.3kPa(1.5psi)
CMP用研磨液の供給量:300mL/min
研磨時間:0.5min
前記で研磨した被研磨基板の被研磨面にスポンジブラシ(ポリビニルアルコール系樹脂製)を押し付けた後、蒸留水を被研磨基板に供給しながら被研磨基板とスポンジブラシとを回転させ、1min洗浄した。次に、スポンジブラシを取り除いた後、被研磨基板の被研磨面に蒸留水を1分間供給した。最後に、被研磨基板を高速で回転させて蒸留水を弾き飛ばして被研磨基板を乾燥した。
Claims (8)
- 絶縁材料部と、コバルト含有部と、前記絶縁材料部及び前記コバルト含有部を接着するチタン含有部と、を有し、かつ、被研磨面に前記コバルト含有部が露出した基板の前記被研磨面を研磨するためのCMP用研磨液であって、
研磨粒子と、金属防食剤と、水溶性ポリマと、水と、を含有し、
前記研磨粒子の含有量が0.1〜3.5質量%であり、
前記金属防食剤が、トリアゾール骨格を有する化合物を含み、
pHが3.8以下である、CMP用研磨液(但し、フタル酸化合物、イソフタル酸化合物及び下記一般式(I)で表されるアルキルジカルボン酸化合物並びにこれらの塩及び酸無水物からなる群より選択される少なくとも1種からなるカルボン酸誘導体と、金属防食剤と、水とを含有し、pHが4.0以下である、コバルト元素を含む層を研磨するための研磨剤を除く)。
HOOC−R−COOH・・・(I)
(前記一般式(I)中、Rは炭素数が4〜10であるアルキレン基を示す。) - 前記基板の前記被研磨面が、主たる成分として銅を含有する銅含有部を有しない、請求項1に記載のCMP用研磨液。
- pHが2.5〜3.8である、請求項1又は2に記載のCMP用研磨液。
- 前記研磨粒子が、シリカ、アルミナ、セリア、チタニア、ジルコニア、ゲルマニア、及び、これらの変性物からなる群より選ばれる少なくとも一種を含む、請求項1〜3のいずれか一項に記載のCMP用研磨液。
- 前記金属防食剤が5−メチルベンゾトリアゾールを含む、請求項1〜4のいずれか一項に記載のCMP用研磨液。
- 請求項1〜5のいずれか一項に記載のCMP用研磨液を用いて、前記基板の前記被研磨面を研磨して前記コバルト含有部の少なくとも一部を除去する工程を備える、研磨方法。
- 前記被研磨面が、コバルト以外の金属を含有する金属含有部を有する、請求項6に記載の研磨方法。
- 前記絶縁材料部が表面に凹凸を有し、
前記チタン含有部が前記凹凸に沿って前記絶縁材料部を被覆し、
前記コバルト含有部が、前記凹凸の凹部を充填して前記チタン含有部を被覆している、請求項6又は7に記載の研磨方法。
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