TW202127531A - 化學機械拋光液及其在銅拋光中的應用 - Google Patents
化學機械拋光液及其在銅拋光中的應用 Download PDFInfo
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- 238000005498 polishing Methods 0.000 title claims abstract description 64
- 239000010949 copper Substances 0.000 title claims abstract description 54
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 44
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000000126 substance Substances 0.000 title claims abstract description 34
- 239000002002 slurry Substances 0.000 title abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 16
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- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 125000004106 butoxy group Chemical group [*]OC([H])([H])C([H])([H])C(C([H])([H])[H])([H])[H] 0.000 claims description 14
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 claims description 14
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 235000012239 silicon dioxide Nutrition 0.000 claims description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 125000005233 alkylalcohol group Chemical group 0.000 claims description 6
- 230000001590 oxidative effect Effects 0.000 claims description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 17
- 230000003746 surface roughness Effects 0.000 abstract description 8
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- 229910004298 SiO 2 Inorganic materials 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 5
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 238000007517 polishing process Methods 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000003344 environmental pollutant Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 231100000719 pollutant Toxicity 0.000 description 4
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 239000000356 contaminant Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000009977 dual effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
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- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- HLZKNKRTKFSKGZ-UHFFFAOYSA-N tetradecan-1-ol Chemical compound CCCCCCCCCCCCCCO HLZKNKRTKFSKGZ-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 1
- VWVRASTUFJRTHW-UHFFFAOYSA-N 2-[3-(azetidin-3-yloxy)-4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]pyrazol-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound O=C(CN1C=C(C(OC2CNC2)=N1)C1=CN=C(NC2CC3=C(C2)C=CC=C3)N=C1)N1CCC2=C(C1)N=NN2 VWVRASTUFJRTHW-UHFFFAOYSA-N 0.000 description 1
- LPZOCVVDSHQFST-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-3-ethylpyrazol-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C=1C(=NN(C=1)CC(=O)N1CC2=C(CC1)NN=N2)CC LPZOCVVDSHQFST-UHFFFAOYSA-N 0.000 description 1
- IHCCLXNEEPMSIO-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperidin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 IHCCLXNEEPMSIO-UHFFFAOYSA-N 0.000 description 1
- YJLUBHOZZTYQIP-UHFFFAOYSA-N 2-[5-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-1,3,4-oxadiazol-2-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1=NN=C(O1)CC(=O)N1CC2=C(CC1)NN=N2 YJLUBHOZZTYQIP-UHFFFAOYSA-N 0.000 description 1
- DFGKGUXTPFWHIX-UHFFFAOYSA-N 6-[2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]acetyl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)C1=CC2=C(NC(O2)=O)C=C1 DFGKGUXTPFWHIX-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000001039 wet etching Methods 0.000 description 1
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- C09G—POLISHING COMPOSITIONS; SKI WAXES
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- C09G1/02—Polishing compositions containing abrasives or grinding agents
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Abstract
本發明提供一種化學機械拋光液及其在銅拋光中的應用，所述化學機械拋光液包括非離子表面活性劑、研磨顆粒和氧化劑。本發明旨在提供一種可用於需去除銅基材的多種應用的化學機械拋光液，使用該化學機械拋光液可以在獲得滿足工藝要求的銅的去除速率的同時，降低拋光後銅表面粗糙度和銅表面污染物顆數，保證拋光後的銅表面質量，能夠滿足各種工藝條件下對銅表面的要求。
Description
本發明涉及一種化學機械拋光液及其在銅拋光中的應用。
在積體電路的製造過程中，矽晶圓基片上往往構建了成千上萬的結構單元，這些結構單元通過多層金屬互連進一步形成功能性電路和元器件。隨著金屬互連技術的發展和佈線層數的增加，化學機械拋光(CMP)已經廣泛應用於晶片製造過程中的表面平坦化。這些平坦化的晶片表面有助於多層積體電路的生產，且防止將電介層塗覆在不平表面上引起的畸變。
CMP工藝就是使用一種含磨料的混合物和拋光墊拋光積體電路表面。在典型的化學機械拋光方法中，將襯底直接與旋轉拋光墊接觸，用一載重物在襯底背面施加壓力。在拋光期間，墊片和操作臺旋轉，同時在襯底背面保持向下的力，將磨料和化學活性溶液（通常稱為拋光液或拋光漿料）塗於墊片上，該拋光液與正在拋光的薄膜發生化學反應開始進行拋光過程。
隨著器件特徵尺寸的持續減小，互連性能已成為制約晶片整體性能的關鍵，而制約互連性能的最大挑戰就是尺寸效應造成的電阻電容延遲現象（RC delay），因此降低RC延遲成為積體電路發展中的重要內容。銅具有電阻率低、抗電遷移能率高和RC延遲時間短的優點，已經取代鋁成為積體電路的主要互連金屬。但由於無法對銅材進行有效的等離子蝕刻或濕法蝕刻，因而對於銅作為互連材料的佈線工藝來說，目前普遍採用的技術方案就是雙大馬士革（Dual Damascene）鑲嵌工藝，即：在第一層裡形成溝槽，在溝槽內填充銅阻擋層和銅，形成金屬導線並覆蓋在介電層上。然後通過化學機械拋光（CMP）工藝將介電層上多餘的銅/銅阻擋層除去，在溝槽裡留下單個互連線。CMP技術用於銅互連工藝，使0.13μm後端銅制程變為現實，不同的工藝和制程對銅化學機械拋光液有著不同的技術要求，且隨著積體電路的發展，對銅化學機械拋光工藝的要求也越來越高，不僅需要滿足不同工藝和制程要求的銅的去除速率，還需要保證拋光後的銅的表面質量。銅的質地比較軟，且容易發生氧化，在拋光過程中會形成由CuO、Cu2
O和Cu(OH)2
等構成的多孔氧化物層。所以銅比諸如二氧化矽（TEOS）等的矽材料或諸如鎢的其他材料更脆弱，很容易在拋光過程中造成劃痕等表面損傷。
為解決現有技術在拋光過程中銅表面容易造成損傷，導致表面粗糙度值大和污染物殘留多的問題，本發明提供一種化學機械拋光液，包括非離子表面活性劑、研磨顆粒和氧化劑。
在一些實施例中，所述非離子表面活性劑為(乙氧基)x化(丁氧基)y化烷基醇，其中x為5-20，y為5-20，烷基為碳原子數為11-15的直鏈或支鏈。所述非離子表面活性劑的質量百分比濃度為0.0005-0.5 wt%。優選為0.001-0.1 wt%。
在一些實施例中，所述研磨顆粒為二氧化矽、三氧化二鋁、二氧化鈰、摻雜鋁的二氧化矽中的一種或多種。所述研磨顆粒的質量百分比濃度為0.1-20 wt%，優選為0.1-10 wt%。所述研磨顆粒的粒徑為20-200nm，優選為30-120nm。
在一些實施例中，所述氧化劑為過氧化氫，所述氧化劑的質量百分比濃度為0.05-5 wt%。
在一些實施例中，所述化學機械拋光液的pH值為4-12，優選為5-11。
本發明中的化學機械拋光液中，還可以包含pH調節劑和殺菌劑等其他本領域的添加劑。
本發明的化學機械拋光液可以濃縮製備，在使用前用去離子水稀釋並添加氧化劑至本發明的濃度範圍。
本發明還提供上述化學機械拋光液在銅拋光中的應用。
本申請採用的試劑均市售可得。
應當理解的是，本發明所述wt%均指的是質量百分比濃度。
與現有技術相比較，本發明的優勢在於：
本發明旨在提供一種可用於銅拋光、阻擋層拋光和矽通孔(Through Silicon Via, TSV)拋光等工藝中需去除銅基材的多種應用的化學機械拋光液，使用該化學機械拋光液可以在獲得滿足工藝要求的銅的去除速率的同時，降低和改善拋光後銅表面粗糙度和銅表面污染物顆粒，保證拋光後的銅表面質量能夠滿足各種工藝條件下對銅表面的要求。
下面通過實施例的方式進一步說明本發明，但並不以此將本發明限制在所述的實施例範圍之中。
實施例
製備方法：按照表1中的配方，將除氧化劑以外的其他組分混合均勻，用KOH或HNO3
調節到所需要的pH值。使用前加氧化劑，混合均勻即可。水為餘量。
表1. 對比例1-2和實施例1-11的配方
| 拋光液 | 研磨顆粒 | (乙氧基)x化(丁氧基)y化烷基醇 | 雙氧水 | pH | ||
| 具體物質 | 含量 wt% | 具體物質 | 含量 wt% | 含量 wt% | ||
| 對比1 | SiO2 | 10 | 不加入 | 1 | 10 | |
| (100nm) | ||||||
| 對比2 | SiO2 | 10 | 苯並三氮唑 | 0.05 | 1 | 10 |
| (100nm) | ||||||
| 實施例1 | SiO2 | 10 | (乙氧基)5 (丁氧基)10 C12醇 | 0.05 | 1 | 10 |
| (100nm) | ||||||
| 實施例2 | SiO2 | 10 | (乙氧基)8 (丁氧基)10 C12醇 | 0.1 | 1 | 11 |
| (120nm) | ||||||
| 實施例3 | SiO2 | 5 | (乙氧基)8 (丁氧基)5 C15醇 | 0.02 | 2 | 9 |
| (90nm) | ||||||
| 實施例4 | SiO2 | 0.1 | (乙氧基)9 (丁氧基)7 C13醇 | 0.001 | 5 | 7 |
| (70nm) | ||||||
| 實施例5 | SiO2 | 1 | (乙氧基)10 (丁氧基)14 C12醇 | 0.005 | 0.5 | 6 |
| (30nm) | ||||||
| 實施例6 | SiO2 | 0.5 | (乙氧基)10 (丁氧基)7 C12醇 | 0.01 | 1 | 7 |
| (120nm) | ||||||
| 實施例7 | SiO2 | 8 | (乙氧基)12 (丁氧基)8 C12醇 | 0.1 | 0.2 | 11 |
| (60nm) | ||||||
| 實施例8 | 摻雜鋁的二氧化矽 | 10 | (乙氧基)13 (丁氧基)8 C14醇 | 0.2 | 3 | 8 |
| (45nm) | ||||||
| 實施例9 | 三氧化二鋁 | 0.5 | (乙氧基)16 (丁氧基)6 C13醇 | 0.5 | 0.05 | 5 |
| (150nm) | ||||||
| 實施例10 | 二氧化鈰 | 0.1 | (乙氧基)16 (丁氧基)20 C14醇 | 0.5 | 0.05 | 4 |
| (200nm) | ||||||
| 實施例11 | 二氧化矽 | 20 | (乙氧基)20 (丁氧基)12 C13醇 | 0.0005 | 0.1 | 12 |
| (20nm) |
效果實施例
拋光方法：將按照表1中的配方制得的拋光液按照下述拋光條件對銅晶圓進行拋光，拋光條件：拋光機台為12”Reflexion LK機台，拋光墊為IC1010 pad，下壓力為1.0-3.0psi，轉速為拋光盤/拋光頭=93/87rpm，拋光液流速為300ml/min，拋光時間為1min。用金屬薄膜測厚儀測量拋光前後的銅的電阻率，計算出拋光前後的銅的厚度，獲得銅的去除速率，用原子力顯微鏡AFM測試的拋光後的銅晶圓表面粗糙度，用缺陷掃描器SP2測試的拋光後的銅晶圓表面污染物顆粒數。拋光及測試結果見表2。
表2.對比例1-2和實施例1-11對Cu的去除速率、表面粗糙度、表面污染物顆粒數
| 拋光液 | 下壓力 | Cu | ||
| 去除速率 | 表面粗糙度 (nm) | 表面污染物顆粒數（顆） | ||
| （psi） | （Å/min） | |||
| 對比例1 | 2 | 895 | 5.95 | 2150 |
| 對比例2 | 2 | 324 | 3.46 | 1976 |
| 實施例1 | 2 | 869 | 0.12 | 55 |
| 實施例2 | 2 | 875 | 0.09 | 10 |
| 實施例3 | 1 | 341 | 0.07 | 9 |
| 實施例4 | 3 | 1732 | 0.17 | 31 |
| 實施例5 | 3 | 3029 | 0.21 | 38 |
| 實施例6 | 1 | 1084 | 0.13 | 22 |
| 實施例7 | 1.5 | 687 | 0.08 | 11 |
| 實施例8 | 1.5 | 1543 | 0.15 | 18 |
| 實施例9 | 2 | 2032 | 0.56 | 87 |
| 實施例10 | 2 | 837 | 0.67 | 112 |
| 實施例11 | 2 | 956 | 0.33 | 26 |
如表2所示：相對於對比例1-2，本申請的實施例1-11中加入了乙氧基丁氧基化烷基醇，在不影響Cu去除速率的情況下極大的改善了拋光後Cu的表面粗糙度，並有效的減少了表面污染物的殘留。從實施例4-5可看出即使在高的下壓力3.0psi的拋光條件下，也能獲得較好的Cu的表面質量。因而採用本發明的拋光液在獲得滿足工藝要求的銅去除速率的同時保證拋光後獲得較好的銅表面質量，能夠滿足各種工藝條件下對銅表面的要求。
綜上，本申請的化學機械拋光液可以在獲得滿足工藝要求的銅的去除速率的同時，改善和降低拋光後銅表面粗糙度和銅表面污染物顆粒數，保證拋光後的銅表面質量；且本申請的化學機械拋光液適用壓力範圍大，即使在較高拋光壓力下，本申請的化學機械拋光液在具有高的銅去除速率的同時，也能獲得較好的銅表面質量。克服了現有技術中的技術偏見。
應當注意的是，本發明中的含量，如果沒有特別說明，均為質量百分比含量。
以上對本發明的具體實施例進行了詳細描述，但其只是作為範例，本發明並不限制於以上描述的具體實施例。對於本領域技術人員而言，任何對本發明進行的等同修改和替代也都在本發明的範疇之中。因此，在不脫離本發明的精神和範圍下所作的均等變換和修改，都應涵蓋在本發明的範圍內。
Claims (9)
- 一種化學機械拋光液，其特徵在於，包括非離子表面活性劑、研磨顆粒和氧化劑，其中，所述的非離子表面活性劑為(乙氧基)x化(丁氧基)y化烷基醇，其中x為5-20，y為5-20，烷基為碳原子數為11-15的直鏈或支鏈。
- 如請求項1所述的化學機械拋光液，其中，所述乙氧基化丁氧基化烷基醇的質量濃度為0.0005-0.5 wt%。
- 如請求項2所述的化學機械拋光液，其中，所述乙氧基化丁氧基化烷基醇的質量濃度為0.001-0.1 wt %。
- 如請求項1所述的化學機械拋光液，其中，所述研磨顆粒為二氧化矽、三氧化二鋁、二氧化鈰、摻雜鋁的二氧化矽中的一種或多種。
- 如請求項1所述的化學機械拋光液，其中，所述研磨顆粒的質量濃度為0.1-20 wt%。
- 如請求項1所述的化學機械拋光液，其中，所述氧化劑為過氧化氫。
- 如請求項1所述的化學機械拋光液，其中，所述氧化劑的質量濃度為0.05-5 wt%。
- 如請求項1所述的化學機械拋光液，其中，所述化學機械拋光液的pH值為4-12。
- 一種如請求項1-8任一所述的化學機械拋光液在銅拋光中的應用。
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