CN103210047A - 含n取代的二氮烯*二氧化物和/或n’-羟基-二氮烯*氧化物盐的含水抛光组合物 - Google Patents
含n取代的二氮烯*二氧化物和/或n’-羟基-二氮烯*氧化物盐的含水抛光组合物 Download PDFInfo
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- CN103210047A CN103210047A CN2011800537073A CN201180053707A CN103210047A CN 103210047 A CN103210047 A CN 103210047A CN 2011800537073 A CN2011800537073 A CN 2011800537073A CN 201180053707 A CN201180053707 A CN 201180053707A CN 103210047 A CN103210047 A CN 103210047A
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- acid
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- dioxide
- oxide
- diazene
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Abstract
本发明涉及一种含水抛光组合物,其包含:(A)至少一种水溶性或水分散性化合物,其选自N-取代的二氮烯二氧化物和N′-羟基-二氮烯
Description
技术领域
此外,本发明涉及抛光用于制造电子、机械和光学器件的基底材料的新方法。
引用文献
将在本发明申请中引用的文献作为参考完全引入。
发明背景
化学机械平坦化或抛光(CMP)为实现集成电路(IC)器件局部和整体平坦度的主要方法。该技术通常在一定负载下将含磨料和其它添加剂的CMP组合物或浆料作为活性化学物质施加在旋转的基底表面和抛光垫之间。因此,CMP方法将物理方法如研磨与化学方法如氧化或螯合结合。希望基底材料的去除或抛光不是由纯粹的物理或纯粹的化学作用组成,而是这两者的协同作用,以实现快速均匀的去除。
这样除去基底材料,直至实现所需平坦度或阻挡下层或停蚀层暴露。最终,获得能够通过随后的光刻法、图案化、蚀刻和薄膜处理正确地制造多层IC器件的平坦的无缺陷的表面。
浅沟槽隔离(STI)为通常要求在图案化的晶片基底上相对于氮化硅选择性除去二氧化硅的特定CMP应用。在该情况下,将蚀刻的沟槽过充满介电材料,如二氧化硅,用氮化硅隔离膜作为停蚀层将其抛光。该CMP方法以从隔离膜除去二氧化硅为结束,同时使暴露的氮化硅和沟槽氧化硅的去除最小化。
这要求能够获得高的二氧化硅材料去除量与氮化硅去除量相对比的CMP浆料,在本领域中该比例也被称作氧化物-氮化物选择性。
基于二氧化铈的CMP浆料在STI应用方面已经受到极大关注,这是因为由于二氧化铈与二氧化硅的高的化学亲合性(在本领域中也称作二氧化铈的化学啮合作用),其能够获得较高的氧化物-氮化物选择性。
然而,基于二氧化铈的CMP系列的氧化物-氮化物选择性必须通过“设计”选择性的添加剂改进。
因此,P.W.Carter等人在Electrochemical and Solid-State Letters,8(8)G218-G221(2005),Interfacial Reactivity between Ceria and SiliconDioxide and Silicon Nitride Surfaces,Organic Additive Effects中公开了谷氨酸、吡啶甲酸、4-羟基苯甲酸、咪唑、乙酸、甲酸、3-羟基吡啶甲酸、邻氨基苯甲酸、吡咯甲酸、环己烷甲酸、哌嗪、吡啶、2-苯基乙酸、苯甲酸、3-氨基苯酚、琥珀酸、甜菜碱、甘氨酸、脯氨酸、苯磺酸、吗啉、水杨酸、对苯二甲酸、苹果酸、异丙醇、柠檬酸和草酸对氧化物-氮化物选择性的影响。
Y.N.Prasad等人在Electrochemical and Solid-State Letters,9(12)G337-G339(2006),Role of Amino-Acid Absorption on Silica and SiliconNitride Surfaces during STI CMP中公开了脯氨酸和精氨酸的影响。
Hyun-Goo Kang等人在Journal of Material Research,第22卷,No.3,2007,第777-787页中公开了二氧化铈浆料中磨料粒度和聚(丙烯酸)分子量对在浅沟槽隔离化学机械平坦化中SiO2/Si3N4膜去除选择性的影响。
S.Kim等人在Journal of Colloid and Interface Science,319(2008),第48-52页中公开了对于化学机械抛光(CMP),阴离子聚电解质的吸收行为。
S.V.Babu等人在Electrochemical and Solid-State Letters,7(12)G327-G330(2004),Slurry Additive Effects on the Suppression of SiliconNitride Removal during CMP中研究了精氨酸、赖氨酸、脯氨酸、N-甲基甘氨酸、丙氨酸、甘氨酸、吡啶甲酸、N,N-二甲基甘氨酸、3-氨基丁酸和异烟酸的影响。
Jae-Dong Lee等人在Journal of the Electrochemical Society,149(8)G477-G481,2002,Effects of Nonionic Surfactants on Oxide-To-PolysiliconSelectivity during Chemical Mechanical Polishing中公开了表面活性剂如聚氧化乙烯(PEO)和氧化乙烯-氧化丙烯-氧化乙烯三嵌段共聚物对选择性的影响。然而,未提及氧化物-氮化物选择性。
美国专利US 5,738,800、US 6,042,741、US 6,132,637和US 6,218,305 B公开了含有如下络合剂的基于二氧化铈的CMP浆料:苹果酸,酒石酸,葡糖酸,柠檬酸,邻二羟基苯甲酸和多羟基苯甲酸、邻苯二甲酸、邻苯二酚、连苯三酚(pyrogallol)、五倍子酸、丹宁酸及其盐。此外,基于二氧化铈的CMP浆料含阴离子、阳离子、两性离子或非离子表面活性剂。基于二氧化铈的CMP浆料主张具有高的氧化物-氮化物选择性。
美国专利US 5,759,917、US 6,689,692 B1和US 6,984,588 B2公开了一种含有如下羧酸的基于二氧化铈的CMP浆料:乙酸、己二酸、丁酸、癸酸、己酸、辛酸、柠檬酸、戊二酸、乙醇酸、甲酸、富马酸、乳酸、月桂酸、苹果酸、马来酸、丙二酸、肉豆蔻酸、草酸、棕榈酸、邻苯二甲酸、丙酸、丙酮酸、硬脂酸、琥珀酸、酒石酸、戊酸、2-(2-甲氧基乙氧基)乙酸、2-[2-(2-甲氧基乙氧基)乙氧基]乙酸、聚(乙二醇)二(羧甲基)醚及其衍生物和盐。此外,基于二氧化铈的CMP浆料含水溶性的有机和无机盐,如硝酸盐、磷酸盐和硫酸盐。基于二氧化铈的CMP浆料主张优先于氮化硅层,抛光过充满的氧化硅。
美国专利US 6,299,659 B1公开了一种基于二氧化铈的CMP浆料,其中所述磨料颗粒已用硅烷、钛酸酯、锆酸酯、铝和磷酸酯偶联剂处理,以改进氧化物-氮化物选择性。
美国专利申请US 2002/0034875 A1和美国专利US 6,626,968 B2公开了一种含以下物质的基于二氧化铈的CMP浆料:表面活性剂,pH调节剂,如氢氧化钾、硫酸、硝酸、盐酸或磷酸,以及含亲水性官能团和疏水性官能团的聚合物,如聚乙烯基甲基醚(PVME)、聚甘醇(PEG)、聚氧化乙烯23月桂醚(POLE)、聚丙酸(PPA)、聚丙烯酸(PM)和聚醚二醇二醚(PEGBE)。然而,该基于二氧化铈的CMP浆料增加了氧化物-多晶硅选择性。
美国专利US 6,436,835 B1公开了一种用于浅沟槽隔离方法的基于二氧化铈的CMP浆料,其包含具有羧酸或羧酸盐或磺酸或胺磺酰基的水溶性有机化合物,如聚丙烯酸、聚甲基丙烯酸、萘磺酸-福尔马林缩合物、苹果酸、乳酸、酒石酸、葡糖酸、柠檬酸、琥珀酸、己二酸、富马酸、天冬氨酸、谷氨酸、甘氨酸4-氨基丁酸、6-氨基己酸、12-氨基月桂酸、精氨酸、双甘氨肽、月桂基苯磺酸及其铵盐。基于二氧化铈的CMP浆料主张具有高的氧化物-氮化物选择性。
美国专利US 6,491,843 B1、US 6,544,892 B2和US 6,627,107 B2公开了一种基于二氧化铈的CMP浆料,其含有用于改进氧化物-氮化物选择性的a-氨基酸,如赖氨酸、丙氨酸和脯氨酸。
美国专利US 6,616,514 B1公开了一种基于二氧化铈的CMP浆料,其含具有至少3个在含水介质中不可离解的羟基的有机多元酚;或由至少一种具有至少3个在含水介质中不可离解的羟基的单体,如甘露糖醇、山梨糖醇、甘露糖、木糖醇、山梨糖、蔗糖和糊精形成的聚合物,其用于改进氧化物-氮化物选择性。
日本专利申请JP 2005-336400 A公开了一种基于二氧化铈的CMP浆料,其包含水溶性的缩合磷酸盐,如焦磷酸盐、三聚磷酸盐和六偏磷酸盐以及水溶性的碳酸盐或碳酸氢盐。基于二氧化铈的CMP浆料还可含有水溶性有机溶剂,如甲醇、乙醇、1-丙醇、2-丙醇、1-丁醇、2-丁醇、乙二醇、丙二醇和1,2,3-丙三醇,酮类,如丙酮和甲基乙基酮、四氢呋喃、N,N-二甲基甲酰胺、二甲亚砜和1,4-二烷。
美国专利US 7,071,105 B2和美国专利申请US 2006/0144824 A1公开了一种基于二氧化铈的CMP浆料,其含有包含官能团,pKa为4-9的抛光添加剂。抛光添加剂选自芳基胺、氨基醇、脂族胺、杂环胺、异羟肟酸、氨基羧酸、环状一元羧酸、不饱和一元羧酸、取代苯酚、磺酰胺、硫醇及其盐,尤其是氯化物、溴化物、硫酸盐、磺酸盐、三氟甲基磺酸盐、乙酸盐、三氟乙酸盐、苦味酸盐、全氟丁酸盐以及钠盐、钾盐和铵盐。
特别提及的芳基胺为苯胺、4-氯苯胺、3-甲氧基苯胺、N-甲基苯胺、4-甲氧基苯胺、对甲苯胺、邻氨基苯甲酸、3-氨基-4-羟基苯磺酸、氨基苄基醇、氨基苄基胺、1-(-氨基苯基)吡咯、1-(3-氨基苯基)乙醇、2-氨基苯基醚、2,5-二(4-氨基苯基)-1,3,4-二唑、2-(2-氨基苯基)-1H-1,3,4-三唑、2-氨基苯基、3-氨基苯基、4-氨基苯基、二甲基氨基苯酚、2-氨基硫醇苯酚、3-氨基硫醇苯酚、4-氨基苯基甲基硫化物、2-氨基苯磺酰胺、邻氨基苯磺酸、3-氨基苯硼酸、5-氨基间苯二甲酸、乙酰磺胺、磺胺酸、邻或对氨苯基胂酸,以及(3R)-3-(4-三氟甲基苯基氨基)戊酸。
特别提出的氨基醇为三乙醇胺、苄基二乙醇胺、三(羟基甲基)氨基甲烷、羟基胺和四环素。
特别提出的脂族胺为甲氧基胺、羟基胺、N-甲基羟基胺、N,O-二甲基羟基胺、β-二氟乙胺、乙二胺、三亚乙基二胺、二乙基(丁基氨基)(2-羟基苯基)甲基)膦酸酯、亚氨基乙烷、亚氨基丁烷、三烯丙基胺,氰基胺,如氨基乙腈、二甲基氨基乙腈、2-氨基-2-氰基丙烷、异丙基氨基丙腈、二乙基氨基丙腈、氨基丙腈、二氰基二乙胺,肼,甲基肼、四甲基肼、N,N-二甲基肼、苯基肼、N,N-二乙基肼、三甲基肼、乙基肼及其盐。
特别提及的杂环胺为咪唑、1-甲基咪唑、2-甲基咪唑、2-乙基咪唑、2-羟基甲基咪唑、1-甲基-2-羟基甲基咪唑、苯并咪唑、喹啉、异喹啉、羟基喹啉、三聚氰胺、吡啶、联吡啶、2-甲基吡啶、4-甲基吡啶、2-氨基吡啶、3-氨基吡啶、2,3-吡啶二甲酸、2,5-吡啶二甲酸、2,6-吡啶二甲酸、5-丁基-2-吡啶甲酸、2-吡啶甲酸、3-羟基-2-吡啶甲酸、4-羟基-2-吡啶甲酸、3-苯甲酰基-2-吡啶甲酸、6-甲基-2-吡啶甲酸、3-甲基-2-吡啶甲酸、6-溴-2-吡啶甲酸、6-氯-2-吡啶甲酸、3,6-二氯-2-吡啶甲酸、4-肼基-3,5,6-三氯-2-吡啶甲酸、2-喹啉甲酸、4-甲氧基-2-喹啉甲酸、8-羟基-2-喹啉甲酸、4,8-羟基-2-喹啉甲酸、7-氯-4-羟基-2-喹啉甲酸、5,7-二氯-4-羟基-2-喹啉甲酸、5-硝基-2-喹啉甲酸、1-异喹啉甲酸、3-异喹啉甲酸、吖啶、苯并喹啉、苯并吖啶、氯压定(clonidine)、安纳巴松(anabasine)、降烟碱(nornicotine)、三唑吡啶、吡哆醇、5-羟色胺(serotonin)、组胺、苯并二氮杂草(benzodiazepine)、氮杂环丙烷(aziridine)、吗啉、1,8-二氮杂二环(5,4,0)十一碳烯-7DABCO、六亚甲基四胺、哌嗪、N-苯甲酰基哌嗪、1-甲苯磺酰基哌嗪、N-羧基乙基哌嗪、1,2,3-三唑、1,2,4-三唑、2-氨基噻唑、吡咯、吡咯-2-甲酸、3-吡咯啉-2-甲酸、乙基吡咯啉、环己基吡咯啉、甲苯基吡咯啉、四唑、5-环丙基四唑、5-羟基四唑、5-苯氧基四唑、5-苯基四唑、氟尿嘧啶、甲基硫尿嘧啶、5,5-二苯基乙内酰脲、5,5-二甲基-2,4-唑烷二酮、邻苯二甲酰亚胺、琥珀酰亚胺、3,3-甲基苯基戊二酰亚胺、3,3-二甲基琥珀酰亚胺、咪唑[2,3-b]唑、羟基咪唑[2,3-a]异吲哚、5,5-甲基苯基巴比妥酸、1,5,5-三甲基巴比妥酸、环己烯巴比妥、5,5-二甲基巴比妥酸、1,5-二甲基-5-苯基巴比妥酸及其盐。
特别提及的异羟肟酸为甲异羟肟酸、乙异羟肟酸、苯并异羟肟酸、水杨基异羟肟酸、2-氨基苯并异羟肟酸、2-氯苯并异羟肟酸、2-氟苯并异羟肟酸、2-硝基苯并异羟肟酸、3-硝基苯并异羟肟酸、4-氨基苯并异羟肟酸、4-氯苯并异羟肟酸、4-氟苯并异羟肟酸、4-硝基苯并异羟肟酸及其盐。
特别提及的氨基羧酸为谷氨酸、β-羟基谷氨酸、天冬氨酸、天冬酰胺、重氮丝氨酸、半胱氨酸、组胺酸、3-甲基组胺酸、胞嘧啶、7-氨基头孢菌烷酸和肌肽。
特别提及的环状一元羧酸为萘-2-甲酸、环己烷甲酸、环己基乙酸、2-苯基乳酸、4-羟基苯甲酸、3-羟基苯甲酸、2-吡啶甲酸、顺-和反-环己烷甲酸、苯甲酸及其盐。
特别提及的不饱和一元羧酸为肉桂酸、丙烯酸、3-氯丙-2-烯甲酸、巴豆酸、4-丁-2-烯甲酸、顺-或反-2-戊酸、2-甲基-2-戊酸、2-己烯酸和3-乙基-2-己烯酸及其盐。
特别提及的苯酚为硝基苯酚、2,6-二卤-4-硝基苯酚、2,6-二C1-12烷基-4-硝基苯酚、2,4-二硝基苯酚、3,4-二硝基苯酚、2-C1-12烷基-4,6-二硝基苯酚、2-卤-4,6-二硝基苯酚、二硝基-邻甲苯酚、苦味酸及其盐。
特别提及的磺酰胺为N-氯甲苯基磺酰胺、双氯非那胺(dichlorophenamide)、磺胺苄胺(mafenide)、尼美舒利(nimesulide)、磺胺甲二唑(sulfamethizole)、磺胺培苯(sulfaperin)、乙酰磺胺(sulfacetamide)、磺胺嘧啶(sulfadiazine)、磺胺地托辛(sulfadimethoxine)、磺胺二甲嘧啶(sulfamethazine)、磺胺吡啶(sulfapyridine)、磺胺喹啉(sulfaquinoxaline)及其盐。
特别提及的硫醇为二硫化二氢、半胱胺、半胱氨酰半胱氨酸、甲基半胱氨酸、苯硫酚、对氯苯硫酚、邻氨基苯硫酚、邻巯基苯基乙酸、对硝基苯硫酚、2-巯基乙烷磺酸盐、N-二甲基半胱胺、二丙基半胱胺、二乙基半胱胺、巯基乙基吗啉、巯基乙酸甲酯、巯基乙胺、N-三甲基半胱氨酸、谷胱甘肽、巯基乙基哌啶、二乙基氨基丙硫醇及其盐。
应相信的是,抛光添加剂增加了氧化物-氮化物选择性。
美国专利申请US 2006/0207188 A1公开了一种基于二氧化铈的CMP浆料,其含有聚合物如聚丙烯酸或聚(甲基丙烯酸烷基酯)与单体如丙烯酰胺、甲基丙烯酰胺、乙基-甲基丙烯酰胺、乙烯基吡啶或乙烯基吡咯烷酮的反应产物。应相信的是,反应产物也增加了氧化物-氮化物选择性。
美国专利申请US 2006/0216935 A1公开了一种基于二氧化铈的CMP浆料,其包含蛋白质、赖氨酸和/或精氨酸,以及吡咯烷酮化合物,如聚乙烯基吡咯烷酮(PVP)、N-辛基-2-吡咯烷酮、N-乙基-2-吡咯烷酮、N-羟基乙基-2-吡咯烷酮、N-环己基-2-吡咯烷酮、N-丁基-2-吡咯烷酮、N-己基-2-吡咯烷酮、N-癸基-2-吡咯烷酮、N-十八烷基-2-吡咯烷酮和N-十六烷基-2-吡咯烷酮。基于二氧化铈的CMP浆料还可含分散剂,如聚丙烯酸类、二醇类和聚二醇类。特定实例使用脯氨酸、聚乙烯基吡咯烷酮或N-辛基-2-吡咯烷酮、PPO/PEO嵌段共聚物和戊二醛。应相信的是,基于二氧化铈的CMP浆料未侵略性地除去沟槽二氧化硅,因此允许在终点之外进一步抛光而不显著增加最小梯段高度。
美国专利申请US 2007/0077865 A1公开了一种基于二氧化铈的CMP浆料,其含有优选来自BASF出售的PluronicTM系列的聚氧化乙烯/聚氧化丙烯共聚物。基于二氧化铈的CMP浆料还可含有氨基醇,如2-二甲基氨基-2-甲基-1-丙醇(DMAMP)、2-氨基-2-乙基-1-丙醇(AMP)、2-(2-氨基乙基氨基)乙醇、2-(异丙基氨基)乙醇、2-(甲基氨基)乙醇、2-(二乙基氨基)乙醇、2-(2-二甲基氨基)乙氧基)乙醇、1,1′-[[3-(二甲基氨基)丙基]亚氨基]-二-2-丙醇、2-(2-丁基氨基)乙醇、2-(叔丁基氨基)乙醇、2-(二异丙基氨基)乙醇和N-(3-氨基丙基)吗啉。基于二氧化铈的CMP浆料还可含有季铵化合物,如氢氧化四甲铵,成膜剂,如烷基胺、链烷醇胺、羟基胺、磷酸酯、十二烷基硫酸钠、脂肪酸、聚丙烯酸盐/酯、聚甲基丙烯酸盐/酯、聚乙烯基膦酸盐/酯、聚苹果酸盐/酯、聚苯乙烯磺酸盐/酯、聚乙烯基硫酸盐/酯、苯并三唑、三唑和苯并咪唑,以及络合剂,如乙酰丙酮、乙酸盐/酯、乙醇酸盐/酯、乳酸盐/酯、葡糖酸盐/酯、五倍子酸、草酸盐/酯、邻苯二甲酸盐/酯、柠檬酸盐/酯、琥珀酸盐/酯、酒石酸盐/酯、苹果酸盐/酯、乙二胺四乙酸、乙二醇、焦儿茶酚、连苯三酚、丹宁酸、磷盐和膦酸。应相信的是,基于二氧化铈的CMP浆料提供了氧化硅和/或氮化硅相对于多晶硅的良好选择性。
美国专利申请S 2007/0175104 A1公开了一种包含多晶硅抛光抑制剂的基于二氧化铈的CMP浆料,所述抑制剂选自具有由选自以下的任何成员取代的N-一元取代或N,N-二取代骨架的水溶性聚合物:丙烯酰胺、甲基丙烯酰胺和其α取代的衍生物;聚乙二醇;聚乙烯基吡咯烷酮;烷氧基化的线性脂族醇和基于乙炔的二醇的氧化乙烯加合物。基于二氧化铈的CMP浆料可含有额外的水溶性聚合物,如多糖,如藻酸、果胶酸、羧甲基纤维素、琼脂、可得然胶(curdlan)和普鲁兰多糖(pullulan);聚羧酸,如聚天冬氨酸、聚谷氨酸、聚赖氨酸、聚苹果酸、聚甲基丙烯酸、聚亚氨酸、聚马来酸、聚衣康酸、聚富马酸、聚(对苯乙烯羧酸)、聚丙烯酸、聚丙烯酰胺、氨基聚丙烯酰胺、聚乙醇酸及其盐;以及乙烯基聚合物,如聚乙烯醇和聚丙烯醛。基于二氧化铈的CMP浆料据说具有高的氧化硅对多晶硅选择性。
美国专利申请US 2007/0191244 A1公开了一种基于二氧化铈的CMP浆料,其含有重均分子量为30-500的化合物且含有羟基和羧基或两者均含,如柠檬酸酯、苹果酸酯、葡糖酸酯、酒石酸酯、2-羟基异丁酸酯、己二酸酯、辛酸酯、琥珀酸酯、含EDTA的化合物、戊二酸酯、亚甲基琥珀酸酯、甘露糖、甘油-半乳糖-庚糖、赤-甘露糖-辛糖、阿拉伯糖-半乳糖-壬糖和谷氨酰胺。基于二氧化铈的CMP浆料还可含有线性聚合物酸或具有烷氧基聚链烷二醇侧链的接枝类的聚合物酸。基于二氧化铈的CMP浆料据说获得了抛光晶片的改进的球状平面性。
美国专利申请US 2007/0218811 A1公开了一种基于二氧化铈的CMP浆料,其pH为4-7.5且含有分散剂、聚羧酸以及100-1000ppm其第一可离解酸基的pKa为3.2或更小的强酸。作为实例提及丙烯酸和甲基丙烯酸的聚合物作为阴离子分散剂,聚氧化乙烯衍生物作为非离子分散剂,以及聚乙烯基吡咯烷酮作为阳离子分散剂。特别提及的强酸为硫酸、HCl、硝酸、磷酸、草酸、马来酸、苦味酸、亚硫酸、硫代亚硫酸、氨基硫酸、氯酸、高氯酸、亚氯酸、氢碘酸、高碘酸、碘酸、氢溴酸、过溴酸、铬酸、亚硝酸、二膦酸、三聚磷酸、次膦酸、吡啶甲酸、膦酸、异烟酸、烟酸、三氯乙酸、二氯乙酸、氯乙酸、氰基乙酸、草酰乙酸、硝基乙酸、溴乙酸、氟乙酸、苯氧基乙酸、邻溴苯甲酸、邻硝基苯甲酸、邻氯苯甲酸、对氨基苯甲酸、邻氨基苯甲酸、邻苯二甲酸、富马酸、丙二酸、酒石酸、柠檬酸、邻氯苯胺、2,2′-联吡啶、4,4′-联吡啶、2,6-吡啶二甲酸、丙酮酸、聚苯乙烯磺酸、聚磺酸、谷氨酸、水杨酸、天冬氨酸、2-氨基乙基膦酸、赖氨酸、精氨酸、异白氨酸、肌氨酸、鸟氨酸、鸟嘌呤核苷、瓜氨酸、酪氨酸、缬氨酸、次黄嘌呤、蛋氨酸、赖氨酸和亮氨酸。基于二氧化铈的CMP浆料导致有效的高速操作,较容易的工艺管理以及较小的由于砂路密度差别而导致的膜厚的波动。
电子器件,尤其是半导体集成电路(IC)的制造需要高精度的方法,这尤其涉及高选择性CMP。
尽管现有技术的基于二氧化铈的CMP浆料可具有令人满意的氧化物-氮化物选择性且可产生具有良好的整体和局部平坦度(这通过晶片内不均匀性(WIWNU)和晶片间不均匀性(WTWNU)验证)的抛光晶片,IC结构,尤其是具有LSI(大规模集成)或VLSI(非常大规模集成)的IC的日益减小的尺寸必须使基于二氧化铈的CMP浆料恒定改进,以满足集成电路器件制造商的日益增加的技术和经济要求。
然而,这种恒定改进现有技术的基于二氧化铈的CMP浆料的迫切需要不仅适用于集成电路器件领域,而且在制造以下其它电子器件领域也必须改进抛光和平坦化功效:液晶面板、有机电致发光面板、印刷电路板、微型机、DNA芯片、微型设备、光电池和磁头;以及高精度的机械器件和光学器件,尤其是光学玻璃,如光掩模、透镜和棱镜,无机导电膜,如氧化铟锡(ITO),光学集成电路,光学开关元件,光学波导管,光学单晶,如光学纤维和闪烁器的端面,固体激光器单晶,用于蓝色激光器LED的蓝宝石基底,半导体单晶和用于磁盘的玻璃基底。这种电子和光学器件的制造需要高精度的CMP工艺步骤。
同样,高精度机械器件的制造也需要高精度的CMP工艺步骤。
现有技术的基于二氧化铈的CMP浆料的一个主要缺陷为它们易于受微生物和真菌侵袭。因此,它们在储存时不稳定,这是由于细菌和真菌生长,该生长对磨料二氧化铈颗粒的粒度分布具有有害影响,这又导致二氧化铈颗粒不可逆的聚集和沉降。
人们已经试图通过加入杀菌剂而改进该严重问题。然而,现有技术的杀菌剂也往往以不能预测的方式使磨料的粒度分布不稳定。
N-取代的二氮烯二氧化物和N′-羟基-二氮烯氧化物盐,其制备方法及其作为木材防腐剂以及适用作消毒剂且适用于纺织品、塑料、建筑材料或涂料系统的杀菌剂和杀真菌剂中的用途由德国专利申请DE 38 35 370A1、美国专利US 5,393,874、欧洲专利申请EP 0 588 249 A1和国际专利申请WO 90/01033已知。无论如何未提及N-取代的二氮烯二氧化物和N′-羟基-二氮烯氧化物盐可用于抛光组合物,尤其是用于基于二氧化铈的CMP浆料。
发明目的
因此,本发明目的为提供一种新型含水抛光组合物,尤其是一种新型的化学机械抛光(CMP)组合物,特别是一种新型的基于二氧化铈的CMP浆料,其不再显示现有技术的抛光组合物的缺点和缺陷。
新型含水抛光组合物,尤其是新型的化学机械抛光(CMP)组合物,特别是新型的基于二氧化铈的CMP浆料尤其应显示显著改进的氧化物-氮化物选择性并产生具有优异的整体和局部平坦度(这通过晶片内不均匀性(WIWNU)和晶片间不均匀性(WTWNU)验证)的抛光晶片。因此,它们应极其适用于制造IC结构,尤其是结构尺寸低于50nm的LSI(大规模集成)或VLSI(非常大规模集成)的IC。
此外,新型含水抛光组合物,尤其是新型的化学机械抛光(CMP)组合物,特别是新型的基于二氧化铈的CMP浆料不仅应特别用于集成电路器件的领域,而且还应最有效且有利地用于制造以下其它电子器件的领域:液晶面板、有机电致发光面板、印刷电路板、微型机、DNA芯片、微型设备和磁头;以及高精度的机械器件和光学器件,尤其是光学玻璃,如光掩模、透镜和棱镜,无机导电膜,如氧化铟锡(ITO),光学集成电路,光学开关元件,光学波导管,光学单晶,如光学纤维和闪烁器的端面,固体激光器单晶,用于蓝色激光器LED的蓝宝石基底,半导体单晶和用于磁盘的玻璃基底。
最特别的是,新型的基于二氧化铈的CMP浆料应不再易于受到微生物和真菌侵袭,且因此应在延长储存期间不再显示细菌和真菌生长以及磨料二氧化铈颗粒粒度分布的不稳定。因此,不应产生不可逆的二氧化铈颗粒的聚集和沉降。
本发明的另一目的为提供一种抛光机械、电子和光学器件用基底材料的新方法。
发明内容
因此,已经找到新的含水抛光组合物,其中所述抛光组合物包含:
(B)至少一种类型的磨料颗粒。
下文中,新型含水抛光组合物被称作“本发明组合物”。
此外,已经找到了抛光机械、电子和光学器件用基底材料的新方法,该方法利用了本发明组合物。
下文中,抛光机械、电子和光学器件用基底材料的新方法被称作“本发明方法”。
发明优点
考虑到现有技术,令人惊讶且本领域熟练技术人员可以预期的是,本发明目的可通过本发明组合物、本发明方法和本发明用途解决。
特别令人惊讶的是,本发明组合物显示了显著改进的氧化物-氮化物选择性且产生具有优异的整体和局部平坦度(这通过晶片内不均匀性(WIWNU)和晶片间不均匀性(WTWNU)验证)的抛光晶片。因此,它们极其适用于制造IC结构,尤其是结构尺寸低于50nm的LSI(大规模集成)或VLSI(非常大规模集成)的IC。
此外,本发明组合物不仅特别用于集成电路器件的领域,而且还最有效且有利地用于制造以下其它电子器件的领域:液晶面板、有机电致发光面板、印刷电路板、微型机、DNA芯片、微型设备和磁头;以及高精度的机械器件和光学器件,尤其是光学玻璃,如光掩模、透镜和棱镜,无机导电膜,如氧化铟锡(ITO),光学集成电路,光学开关元件,光学波导管,光学单晶,如光学纤维和闪烁器的端面,固体激光器单晶,用于蓝色激光器LED的蓝宝石基底,半导体单晶和用于磁盘的玻璃基底。
最特别的是,本发明组合物不再易于受到微生物和真菌侵袭,且因此在延长储存期间不再显示细菌和真菌生长以及磨料二氧化铈颗粒粒度分布的不稳定。因此,不产生不可逆的二氧化铈颗粒的聚集和沉降。
因此,最特别的是,本发明组合物用于本发明方法。本发明方法可最有利地用于抛光,尤其是化学机械抛光以下电子器件的基底材料:液晶面板、有机电致发光面板、印刷电路板、微型机、DNA芯片、微型设备和磁头;以及用于高精度的机械器件和光学器件的基底材料,尤其是光学玻璃,如光掩模、透镜和棱镜,无机导电膜,如氧化铟锡(ITO),光学集成电路,光学开关元件,光学波导管,光学单晶,如光学纤维和闪烁器的端面,固体激光器单晶,用于蓝色激光器LED的蓝宝石基底,半导体单晶和用于磁盘的玻璃基底。
发明详述
本发明组合物为含水组合物。这意味着其含有水,尤其是超纯水作为主溶剂和分散剂。然而,本发明组合物可含有至少一种水溶混性有机溶剂,然而,其含量很少,不改变本发明组合物的含水性质。
本发明组合物的水含量优选为60-99.95重量%,更优选70-99.9重量%,甚至更优选80-99.9重量%,最优选90-99.9重量%,其中所述重量百分含数基于本发明组合物的全部重量。
“水溶性”指相关化合物(A)分布在分子水平上的含水介质中,而“水分散性”指它们可细碎分布在含水介质中并形成稳定的悬浮液或乳液,优选稳定的悬浮液。最优选的是,化合物(A)为水溶性的。
R[-N+(-O-)=N-OH]n (I)。
在通式I中,变量R指包含或由至少一种选自以下的残基组成的结构部分:不含或含至少一个杂原子和/或至少一个双官能或三官能链接基团的单体、低聚及聚合,取代及未取代,饱和及未饱和的脂族和脂环族基团,以及不含或含至少一个杂原子的单体、低聚及聚合,取代及未取代的芳族基团。
在通式I中,指数n为1-1000,优选1-500,更优选1-100,甚至更优选1-50,最优选1-10的数字。
当残基R为低聚或聚合的结构部分时,数字n不一定必须为整数,而是也可为分数。这是由于低聚和聚合的结构部分的统计性质。当残基R为单体结构部分时,数字n通常为整数。
给定残基R可包含一种在下文中更详细描述的上述结构部分或这种残基R可含有两种或更多种在下文中更详细描述的上述结构部分,这类基团相互不同且可经由至少一个共价键和/或通过一个或多个在下文中更详细描述的上述链接基团相互链接。
就本发明而言,“单体的”指相关残基R衍生自包含或由单个特征结构单元或两个特征结构单元组成的单体化合物R′。单体化合物R′的分子量优选为40-1000道尔顿。
就本发明而言,“低聚的”指相关残基R衍生自包含或由3至约12个特征重复结构单元组成的低聚化合物R′。低聚化合物R′的重均分子量Mw优选为100-2500道尔顿。
就本发明而言,“聚合的”指相关残基R衍生自包含或由至少12个特征重复结构单元组成的聚合化合物R′。聚合化合物R′的重均分子量Mw优选为500-2,000,000道尔顿,更优选1000-1,000,000道尔顿,最优选5000-500,000道尔顿。
“未取代”指除了下述杂原子之外,相关残基R仅由碳原子和氢原子组成。
“取代”指相关残基R含有至少一个惰性,即在制备、处理、储存和使用本发明组合物中化合物(A)的条件下不反应的取代基。
合适的惰性取代基的实例为卤原子,如氟、氯和溴,羟基,羧酸基,磺酸基,次磷酸基、硝基和腈基,优选氟和氯原子和腈基。
“饱和”指相关残基R不含任何烯属或炔属不饱和基团。因此,“不饱和”指相关残基R含有至少一个烯属和/或炔属不饱和基团。
杂原子优选选自硼、氧、硫、氮、磷和硅,最优选氧和氮。
在上述含义中,双官能团和三官能团链接基团优选为惰性的。
适合的双官能团和三官能团链接基团的实例为碳酸酯、硫代碳酸酯、碳酸盐、硫代碳酸盐、磷酸酯、硫代磷酸酯、次膦酸酯、硫代膦酸酯、亚磷酸盐、硫代膦酸酯、磺酸酯、酰胺、胺、硫代酰胺、磷酸酰胺、硫代磷酸酰胺、膦酸酰胺、硫代膦酸酰胺、磺酸酰胺、亚酰胺、酰肼、氨基甲酸乙酯、脲、硫脲、羰基、硫代羰基、砜和亚砜基,最特别的是碳酸盐、氨基甲酸乙酯、羰基和碳酸酯基,最特别优选碳酸酯基。
饱和的单体脂族结构部分R优选衍生自线性或支化的脂族烃R′,更优选在分子中具有1-20个,甚至更优选1-16个,最优选1-12个,最特别优选1-4个碳原子的线性或支化的脂族烃R′,尤其是甲烷、乙烷、丙烷、丁烷、异丁烷、戊烷、异戊烷、新戊烷、己烷、异己烷、庚烷、辛烷、异辛烷、壬烷、癸烷、十一烷和十二烷,尤其是甲烷、乙烷、丙烷、丁烷和异丁烷。
取代,饱和的单体脂族结构部分R优选衍生自线性或支化的脂族烃R′,更优选在分子中具有1-20个,甚至更优选1-16个,最优选1-12个,最特别优选1-4个碳原子以及至少一个选自氟和氯的卤原子的线性或脂族烃R′。
特别合适的取代,饱和的单体脂族结构部分R的实例衍生自氟代、氯代、二氟代、二氯代、氯氟代、三氟代、三氯代、二氟氯代和氟二氯代甲烷;氟代、氯代、1,1-和1,2-二氟代、1,1-和1,2-二氯代、1-氯代-1-氟代、1-氯代-2-氟代、1-二氟代-2-氟代、2-三氟代、1-二氯代-2-氯代、2-三氯代、1-二氟代-2-氯代、2-二氟代氯代、1-氟代-2-二氯代和2-氟代二氯代乙烷;氟代、氯代、二氟代、二氯代、三氟代、三氯代、四氟代、四氯代、五氟代、五氯代、六氟代、六氯代、六氟代和七氯代丙烷以及混合的氟代氯代丙烷;氟代、氯代、二氟代、二氯代、三氟代、三氯代、四氟代、四氯代、五氟代、五氯代、六氟代、六氯代、七氟代、七氯代、八氟代、八氯代、九氟代和九氯代丁烷和异丁烷以及混合的氟代氯代丁烷和异丁烷。
具有至少一个杂原子的未取代的,饱和的单体脂族结构部分R优选衍生自线性或支化的脂族烃R′,更优选在分子上具有2-20个,甚至更优选2-16个,最优选2-12个,最特别优选2-6个碳原子,以及在2个碳原子之间具有至少1个氮原子和/或氧原子的线性或支化的脂族烃R′。
特别适合的具有至少一个杂原子的未取代的,饱和的单体脂族结构部分R的实例衍生自二甲醚、甲乙醚、二乙醚、2,4-二氧杂戊烷、2,4-氧杂己烷、3,6-二氧杂辛烷、二甲胺、三甲胺、二乙胺、三乙胺、二丙胺和2-氧杂-4-氮杂戊烷。
具有至少一个杂原子的取代的,饱和单体脂族结构部分R衍生自线性或支化的脂族烃R′,更优选在分子上具有2-20个,甚至更优选2-16个,最优选2-12个,最特别优选2-6个碳原子,在2个碳原子之间具有至少一个氮原子和/或氧原子以及具有至少一个氟和/或氯原子的线性或支化的脂族烃R′。
特别合适的具有至少一个杂原子的取代的,饱和单体脂族结构部分R的实例衍生自二甲醚、甲乙醚、二乙醚、2,4-二氧杂戊烷、2,4-氧杂己烷、3,6-二氧杂辛烷、二甲胺、三甲胺、二乙胺、三乙胺、二丙胺和2-氧杂-4-氮杂戊烷,其可优选由至少一个氟原子和/或氯原子和/或腈基取代。
具有至少一个双官能或三官能链接基团的取代或未取代的,饱和单体脂族结构部分R优选衍生自线性或支化的脂族烃R′,更优选在分子上具有2-20,甚至更优选2-16,最优选2-12,最特别优选2-6个碳原子以及至少一个双官能或三官能链接基团的线性或支化的脂族烃R′。相关烃R′也可带有至少一个取代基。
特别合适的取代或未取代的,饱和单体脂族结构部分R的实例衍生自丙酮,甲基乙基酮,二乙酮,甲基丁基酮,乙基丁基酮,乙酰基丙酮,甲酸甲酯、甲酸乙酯、甲酸丙酯、甲酸丁酯和甲酸戊酯,乙酸甲酯、乙酸乙酯、乙酸丙酯和乙酸丁酯,丙酸甲酯、丙酸乙酯和丙酸丙酯,以及丁酸甲酯和丁酸乙酯,其可优选由至少一个氟和/或氯原子取代。
取代或未取代的,饱和的,低聚或聚合的脂族结构部分R优选衍生自乙烯、丙烯、丁烯和异丁烯的线性、支化、超支化、星型、树枝状和梳状均聚物和共聚物。共聚物可含有少量共聚的高级烯烃,如己烯和辛烯。所述均聚物和共聚物可优选由至少一个氟和/或氯原子取代。
含有至少一个杂原子,尤其是至少一个氧原子的取代或未取代的,饱和的,低聚或聚合的脂族结构部分R优选衍生自以下的线性、支化、超支化、星型、树枝状和梳状均聚物和共聚物:烯烃亚胺,尤其是乙烯亚胺,氧化烯烃,尤其是氧化乙烯、氧化丙烯、氧化丁烯和四氢呋喃,以及乙烯基醚和酯,尤其是乙烯基甲基、乙基、丙基和丁基醚和酯。所述均聚物和共聚物也可含有上述双官能或三官能链接基团。
含有至少一个双官能团或三官能团,优选双官能团的链接基团的取代或未取代的,饱和的,低聚或聚合的脂族结构部分R优选衍生自线性、支化、超支化、星型、树枝状和梳状聚碳酸酯、聚氨酯和(甲基)丙烯酸酯(共)聚合物,尤其是聚丙烯酸甲酯和聚甲基丙烯酸甲酯PMMA。所述均聚物和共聚物可优选由至少一个氟和/或氯原子取代。
取代或未取代的,不饱和的,单体和低聚的脂族结构部分R优选衍生自常规和已知的烯属或炔属不饱和单体,如烯烃、炔烃、丙烯酸酯、甲基丙烯酸酯、乙烯基醚、乙烯酯、烯丙基醚、烯丙基酯,以及如 Online2010,Thieme Chemistry,www.roempp.com,″Terpene″,″Sesquiterpene″,″Diterpene″,and″Triterpene″所述的非环状单萜、倍半萜烯、双萜和三萜,这些单体可优选由至少一个氟和/或氯原子和/或腈基取代。
特别合适的取代或未取代的,不饱和的,单体和低聚合的脂族结构部分R的实例为乙烯,丙烯,丁烯,异戊二烯,乙炔,丙炔,丙烯酸甲酯和乙酯,甲基丙烯酸甲酯,乙烯基醚和酯,尤其是乙烯基甲基、乙基、丙基和丁基醚和酯,以及烯丙基甲基、乙基、丙基和丁基醚和酯,罗勒烯,月桂烯,柠檬醛,α-和β-紫罗兰酮和假紫罗兰酮。所述单体可优选由至少一个氟和/或氯原子和/或腈基取代。
取代或未取代的,饱和的,脂环族结构部分R优选衍生自饱和的单环、二环、三环、四环烃,其可优选由至少一个氟和/或氯原子和/或腈基取代。
特别合适的取代或未取代的,饱和的脂环族结构部分R的实例为环丙烷,环丁烷,环戊烷,环己烷,环庚烷,环辛烷,环癸烷,邻-、间-和对孟烷,孟酮,蒈烷,蒎烷,蒈酮,冰片基氯,异冰片基氯,樟脑,莰烷,降冰片烷,8.9.10-三降冰片烷,螺[3.3]庚烷,螺双环己烷,萘烷,氢化茚满,降莰烷,双环[2.2.1]辛烷,金刚烷,异三环癸烷和双金刚烷,其可优选由至少一个氟和/或氯原子和/或腈基取代。
含有至少一个杂原子的取代或未取代的,饱和的脂环族结构部分R优选衍生自含有至少一个杂原子的饱和的单环、二环、三环、四环烃,这类烃可优选由至少一个氟和/或氯原子和/或腈基取代。
特别合适的含有至少一个杂原子,尤其是至少一个氮原子和/或氧原子的取代或未取代的,饱和的脂环族结构部分R的实例衍生自四氢呋喃、1,4-二烷、γ-丁内酯、ε-己内酰胺、吗啉、尿丁啶(uretidine)、异唑烷、吡咯烷、咪唑啉、吡唑烷、哌啶、哌嗪和奎宁环,其可优选由至少一个氟和特定的氯原子和/或腈基取代。
取代或未取代的,不饱和的脂环族结构部分R优选衍生自不饱和的单环、二环、三环、四环烃,其可优选由至少一个氟和/或氯原子和/或腈基取代。
特别合适的取代或未取代的,不饱和的脂环族结构部分R的实例衍生自环丙烯、环丁烯、环戊烯、环戊二烯、环己-1,3-和-1,2-二烯、环庚烯、环辛烯、环癸烯、α-和γ-萜品烯、萜品油烯、α-和β-水芹烯、苎烯、二戊烯、长叶薄荷酮、香芹酮、香芹烯酮、α-和β-蒎烯、红没药烯、杜松烯、β-蛇床烯、樟脑烯和螺[4.5]癸-1,6-二烯,其可优选通过至少一个氟和/或氯原子和/或腈基取代。
含有至少一个杂原子的取代或未取代的,饱和的脂环族结构部分R优选衍生自含有至少一个杂原子的不饱和的单环、二环、三环、四环烃,这类烃可优选由至少一个氟和/或氯原子和/或腈基取代。
特别合适的含有至少一个杂原子,尤其是至少一个氮原子和/或氧原子的取代或未取代的,饱和的脂环族结构部分R的实例衍生自2H-吡喃、2H-吡咯、δ2-吡咯啉、δ2-咪唑啉、δ3-吡唑、吡咯烷(pyrrolenine)和δ4-异唑啉,这类烃可优选由至少一个氟和/或氯原子和/或腈基取代。
取代和未取代的单体芳族结构部分R优选衍生自单环和多环的芳族化合物,尤其是苯、联苯、三联苯、二苯醚、二苯胺、二苯基酮、二苯硫、二苯亚砜、二苯砜、萘、茚满、荧烷、芴酮、蒽和菲,这类烃可优选由至少一个氟和/或氯原子和/或腈基取代。
取代和未取代的,低聚和聚合的芳族结构部分R优选衍生自含有芳族基团的低聚物和聚合物,尤其是聚酯,特别是聚(对苯二甲酸乙二醇酯)PET和聚(对苯二甲酸丁二醇酯)PBT,聚醚,尤其是聚苯醚,如聚(2,6-二甲基苯醚),以及苯乙烯的均聚物和共聚物,这类低聚物和聚合物可优选由至少一个氟和/或氯原子和/或腈基取代。
含有至少一个杂原子的取代和未取代的,单体芳族结构部分R优选衍生自单环和多环杂芳族化合物,尤其是含氧、硫和/或氮的杂芳族化合物,其可优选由至少一个氟和/或氯原子和/或腈基取代。
特别合适的含有至少一个杂原子的取代和未取代的,单体芳族结构部分R的实例衍生自呋喃、噻吩、吡咯、咪唑、吡唑、异噻唑、异唑、三唑、吡啶、吡嗪、嘧啶、哒嗪、苯并噻吩、噻蒽、异苯并呋喃、吩嗪、吲嗪、异吲哚、吲哚、嘌呤、异喹啉、喹啉、酞嗪、1,8-萘啶(naphthyridine)、喹啉、喹唑啉、噌啉、蝶啶、咔唑、吖啶和菲啶,其可优选由至少一个氟和/或氯原子和/或腈基取代。
如上文已说明的,上述结构部分R可以任何方式相互组合,以形成具有通式I的变量R。因此,作为实例,可经由醚基将衍生自苯的结构部分R与衍生自氧化乙烯的共聚物的结构部分R组合,以使N-取代的二氮烯二氧化物(A)更能溶于水。
更优选的是,结构部分R衍生自单体的,饱和的脂族和脂环族以及单体的芳族化合物,甚至更优选未取代的,单体的,饱和的脂族和脂环族以及未取代的,单体的芳族化合物,尤其是甲烷、乙烷、丙烷、丁烷、环戊烷、环己烷和苯。
{R[-N(-O)-N-O]- n}m(Mm+)n (II),
其中变量R具有上述含义且指数n和m均为1-1000,优选1-500,更优选1-100,甚至更优选1-50,最优选1-10的数字。
当残基R为低聚或聚合的结构部分时,数字n和m不一定必须为整数,而是也可为分数。这是由于低聚和聚合的结构部分的统计性质。当残基R为单体结构部分时,数字n和m通常为整数。
变量M指选自有机和无机,单体、低聚和聚合的阳离子的阳离子。
合适的无机阳离子的实例为氨、锂、钠、钾、铷、铯、镁、钙、锶、钡、铝、镓、铟、锗、锡、铅、锑、铋、钪、钇、镧、稀土金属、钛、锆、铪、钒、铌、钽、铬、钼、钨、锰、铼、铁、钌、锇、钴、铑、铱、镍、钯、铂、铜、银、金、锌和镉的阳离子,优选氨、锂、钠和钾的阳离子。
在本发明组合物中N-取代的二氮烯二氧化物(A)和/或N′-羟基-二氮烯氧化物盐(A)的浓度可在宽范围内变化,且因此可最有利地适应本发明的特定组合物、方法和用途。本发明组合物优选基于其全部重量含有0.01-1000ppm,更优选0.05-750ppm,甚至更优选0.075-500ppm,最优选0.1-500ppm化合物(A)。
本发明组合物的第二种基本成分为至少一种类型的磨料颗粒(B)。
原则上,可将常用于抛光,尤其是化学机械抛光或平坦化(CMP)领域中的任何天然或合成的磨料颗粒材料用作成分(B)。磨料颗粒(B)优选选自氧化铝、二氧化硅、氮化硅、碳化硅、二氧化钛、氧化锆、二氧化铈、氧化锌及其混合物。
磨料颗粒(B)的平均粒度可在宽范围内变化,且因此可最有利地适应本发明组合物、方法和用途的特定要求。通过动态光散射法测定的平均粒度优选为1-2000nm,优选1-1000nm,更优选1-750nm,最优选1-500nm。
磨料颗粒(B)最优选包含或由二氧化铈组成。
含有二氧化铈的磨料颗粒(B)可含有少量其它稀土金属氧化物。
含有二氧化铈的磨料颗粒(B)优选为包含核的复合颗粒(B),该核包含或由至少一种与二氧化铈不同的其它磨料颗粒材料,尤其是氧化铝、二氧化硅、二氧化钛、氧化锆、氧化锌及其混合物组成。
这类复合颗粒(B)例如由以下已知:WO 2005/035688 A1,US6,110,396,US 6,238,469 B1,US 6,645,265 B1,K.S.Choi等人,Mat.Res.Soc.Symp.Proc.,第671卷,2001 Materials Research Society,M5.8.1-M5.8.10,S.-H.Lee等人,J.Mater.Res.,第17卷,No.10,(2002),第2744-2749页,A.Jindal等人,Journal of the Electrochemical Society,150(5)G314-G318(2003),Z.Lu,Journal of Materials Research,第18卷,No.10,2003年10月,Materials Research Society,或S.Hedge等人,Electrochemical and Solid-State Letters,7(12)G316-G318(2004)。
最优选的是,复合颗粒(B)为覆盆子类的涂覆颗粒,其包含选自氧化铝、二氧化硅、二氧化钛、氧化锆、氧化锌及其混合物且核尺寸为20-100nm的核,其中所述核涂覆有粒度低于10nm的二氧化铈颗粒。
用于本发明组合物的磨料颗粒(B)的量可在宽范围内变化,且因此可最有利地适应本发明组合物、方法和用途的特定要求。本发明组合物优选含有0.005-10重量%,更优选0.01-8重量%,最优选0.01-6重量%磨料颗粒(B),其中所述重量百分含数基于本发明组合物的全部重量。
本发明组合物可含有至少一种与成分或组分(A)和(B)不同的功能组分(C)。
功能组分(C)优选选自常用于基于二氧化铈的CMP浆料中的化合物。这类化合物(C)的实例在开头描述且例如在以下公开:Y.N.Prasad等人在Electrochemical and Solid-State Letters,9(12)G337-G339(2006)中,Hyun-Goo Kang等人在Journal of Material Research,第22卷,No.3,2007,第777-787页中,S.Kim等人在Journal of Colloid and InterfaceScience,319(2008),第48-52页中,S.V.Babu等人在Electrochemical andSolid-State Letters,7(12)G327-G330(2004)中,Jae-Dong Lee等人在Journal of the Electrochemical Society,149(8)G477-G481,2002中,美国专利US 5,738,800、US 6、042、741、US 6,132,637、US 6,218,305 B、US 5,759,917、US 6,689,692 B1、US 6,984,588 B2、US 6,299,659 B1、US6,626,968 B2、US 6,436,835、B1US 6,491,843 B1、US 6,544,892 B2、US6,627,107 B2、US 6,616,514 B1和US 7,071,105 B2,美国专利申请US2002/0034875 A1、US 2006/0144824 A1、US 2006/0207188 A1、US2006/0216935 A1、US 2007/0077865 A1、US 2007/0175104 A1、US2007/0191244 A1和US 2007/0218811 A1,以及日本专利申请JP2005-336400 A。
此外,功能组分(C)选自与颗粒(B)不同的有机、无机和混合的有机-无机磨料颗粒,具有下限临界溶解温度LCST或上限临界溶解温度UCST的材料,氧化剂、钝化剂、电荷反转剂(charge reversal agent)、具有至少3个在含水介质中不可离解的羟基的有机多元醇,由至少一种具有至少3个在含水介质中不可离解的羟基的单体形成的低聚物和聚合物,配合或螯合剂,摩擦剂(frictive agent),稳定剂,流变剂,表面活性剂,金属阳离子和有机溶剂。
合适的有机磨料颗粒(C)及其有效量例如由美国专利申请US2008/0254628 A1,第4页,第[0054]段或国际申请WO 2005/014753 A1已知,其中公开了包含三聚氰胺和三聚氰胺衍生物,如乙酰胍胺、苯并胍胺和双氰胺的固体颗粒。
合适的无机磨料颗粒(C)及其有效量例如由国际专利申请WO2005/014753 A1,第12页,第1-8行或美国专利US 6,068,787,第6栏,第41行至第7栏,第65行已知。
合适的混合的有机-无机磨料颗粒(C)及其有效量例如由美国专利申请US 2008/0254628 A1,第4页,第[0054]段或US 2009/0013609 A1,第3页,第[0047]段至第6页,第[0087]段已知。
合适的氧化剂(C)及其有效量例如由欧洲专利申请EP 1 036 836 A1,第8页,第[0074]和[0075]段或美国专利US 6,068,787,第4栏,第40行至第7栏,第45行或US 7,300,601 B2,第4栏,第18-34行已知。优选使用有机和无机过氧化物,更优选无机过氧化物。
合适的钝化剂(C)及其有效量例如由美国专利US 7,300,601 B2,第3栏,第59行至第4栏,第9行或美国专利申请US 2008/0254628 A1,跨第4和5页的第[0058]段已知。
合适的配合或螯合剂(C)(也经常称作摩擦剂)(参见美国专利申请US2008/0254628 A1,第5页,第[0061]段)或浸蚀剂或蚀刻剂(参见美国专利申请US 2008/0254628 A1,第4页,第[0054]段)及其有效量例如由美国专利US 7,300,601 B2,第4栏,第35-48行已知。最特别优选使用含至少一个,优选两个,更优选三个伯氨基的氨基酸,尤其是甘氨酸,此外还有双氰胺和三嗪,如三聚氰胺和水溶性的胍胺,特别是三聚氰胺、甲酰缩胍胺(formoguanamine)、乙酰胍胺和2,4-二氨基-6-乙基-1,3,5-三嗪。
合适的稳定剂(C)及其有效量例如由美国专利US 6,068,787,第8栏,第4-56行已知。
合适的流变剂(C)及其有效量例如由美国专利申请US 2008/0254628A1,第5页,第[0065]段至第6页,第[0069]段已知。
合适的表面活性剂(C)及其有效量例如由国际专利申请WO2005/014753 A1,第8页,第23行,至第10页,第17行或美国专利US7,300,601 B2,第5栏,第4行至第6栏,第8行已知。
合适的多价金属离子(C)及其有效量例如由欧洲专利申请EP 1 036 836A1,第8页,第[0076]段至第9页,第[0078]段已知。
合适的有机溶剂(C)及其有效量例如由美国专利US 7,361,603 B2,第7栏,第32-48行或美国专利申请US 2008/0254628 A1,第5页,第[0059]段已知。
显示下限临界溶解温度LCST或上限临界溶解温度UCST的合适材料(C)例如描述在H.Mori、H.Iwaya、A.Nagai和T.Endo的文章,Controlledsynthesis of thermoresponsive polymers derived from L-proline via RAFTpolymerization,在Chemical Communication,2005,4872-4874中;或在D.Schmaljohann的文章,Thermo-and pH-responsive polymers and drugdelivery,Advanced Drug Delivery Reviews,第58(2006)卷,1655-1670中或在美国专利申请US 2002/0198328 A1、US 2004/0209095 A1、US2004/0217009 A1、US 2006/0141254 A1、US 2007/0029198 A1、US2007/0289875 A1、US 2008/0249210 A1、US 2008/0050435 A1 or US2009/0013609 A1,美国专利US 5,057,560、US 5,788,82和US6,682,642B2,国际专利申请WO 01/60926 A1、WO2004/029160 A1、WO2004/0521946 A1、WO 2006/093242 A2或WO 2007/012763 A1中,在欧洲专利申请EP 0 583 814 A1、EP 1 197 587 B1和EP 1 942 179 A1,或德国专利申请DE 26 10 705中;或它们以商标PluronicTM、TetronicTM和BasensolTM由BASF Corporation和BASF SE销售,其证明为BASFCorporation的公司宣传册″PluronicTM&TetronicTM Block CopolymerSurfactants,1996″或美国专利US 2006/0213780 A1。
在第一有利并优选的实施方案中,本发明组合物含至少一种电荷反转剂(C)。
原则上,可使用常用于CMP领域中的任何已知的电荷反转剂(C)。电荷反转剂(C)优选选自含有至少一个选自以下的阴离子基团的单体、低聚和聚合的化合物:羧酸根、亚磺酸根、硫酸根、膦酸根和磷酸根基团。特别合适的电荷反转剂(C)的实例例如描述在美国专利US 7,2065,055 B2,第4栏,第24-45行或日本专利申请JP 2005-336400 A(参见权利要求1-6)中。
本发明组合物中电荷反转剂(C)的浓度可在宽范围内变化,且因此可最有利地适应本发明给定组合物、方法和用途的特定要求。电荷反转剂(C)优选以使得二氧化铈与电荷反转剂(C)的重量比为10-2000,更优选20-1000的量使用。
在第二有利并优选的实施方案中,本发明组合物含有至少一种有机多元醇(C),更优选至少两种具有至少3个在含水介质中不可离解的羟基的有机多元醇(C)和/或由至少一种具有至少3个在含水介质中不可离解的羟基的单体形成的低聚物和聚合物。
有机多元醇(C)更优选选自单糖、二糖、低聚糖、多糖、脱氧糖、氨基糖、醛糖酸、酮糖醛酸(ketoaldonic acid)、糖醛酸、醛糖二酸(aldaric acid)、糖醇和环醇,甚至更优选单糖和环醇,特别优选半乳糖和肌肉-、鲨-、粘质-、手性-、新-、异-、表-和顺-肌醇。最优选将半乳糖和肌肉肌醇用作有机多元醇(C)。
本发明组合物中有机多元醇(C)的浓度可在宽范围内变化,且因此可最有利地适应本发明组合物、方法和用途的特定要求。本发明组合物优选优选以0.001-5重量%,更优选0.005-4重量%,甚至更优选0.01-2重量%,最优选0.01-1重量%的量包含有机多元醇(C),其中重量百分数基于本发明组合物的全部重量。
在第三个最有利且最优选的实施方案中,本发明组合物含有上述电荷反转剂(C)和有机多元醇(C)。
存在的话,功能组分(C)的含量可改变。(C)的总含量基于相应CMP组合物的总重量优选不超过10重量%(“重量%”指“百分重量”),更优选不超过2重量%,最优选不超过0.5重量%,特别是不超过0.1重量%,如不超过0.01重量%。(C)的总含量基于相应组合物的总重量优选为至少0.0001重量%,更优选至少0.001重量%,最优选至少0.008重量%,特别是至少0.05重量%,如至少0.3重量%。
本发明组合物可任选包含至少一种与成分(A)和(B)明显不同的pH调节剂或缓冲剂(D)。
合适的pH调节剂或缓冲剂(D)及其有效量例如由以下已知:欧洲专利申请EP 1 036 836 A1,第8页,第[0080]、[0085]和[0086]段,国际专利中请WO 2005/014753 A1,第12页,第19-24行,美国专利申请US2008/0254628 A1,第6页,第[0073]段或美国专利US 7,300,601 B2,第5栏,第33-63行。pH调节剂或缓冲剂(D)的实例为氢氧化钾、氢氧化铵、四甲基氢氧化铵(TMAH)、硝酸和硫酸。
存在的话,pH调节剂或缓冲剂(D)的含量可改变。(D)的总量基于相应CMP组合物的总重量优选不超过20重量%,更优选不超过7重量%,最优选不超过2重量%,特别是不超过0.5重量%,如不超过0.1重量%。(D)的总量基于相应组合物的总重量优选为至少0.001重量%,更优选至少0.01重量%,最优选至少0.05重量%,特别是至少0.1重量%,如至少0.5重量%。
优选使用上述pH调节剂(D)将本发明组合物的pH优选设置在3-10,更优选4-8,甚至更优选4-7,最优选5-7。
本发明组合物的制备未显示任何特殊性,但可通过将上述成分(A)和(B)以及任选(C)和/或(D)溶解或分散在含水介质,尤其是去离子水中而进行。为此,可使用常规和标准的混合方法和混合装置,如搅拌容器、在线溶解器、高剪切叶轮、超声混合器、均化器喷嘴或逆流混合器。可优选将如此获得的本发明组合物过滤通过具有合适筛孔的过滤器,以除去粗粒颗粒,如固体的细碎分散的磨料颗粒(B)的聚集体或聚集物。
特别的是,电子器件为集成电路器件、液晶面板、有机电致发光面板、印刷电路板、微型机、DNA芯片、微型设备和磁头;机械器件为高精度的机械器件;光学器件为光学玻璃,如光掩模、透镜和棱镜,无机导电膜,如氧化铟锡(ITO),光学集成电路,光学开关元件,光学波导管,光学单晶,如光学纤维和闪烁器的端面,固体激光器单晶,用于蓝色激光器LED的蓝宝石基底,半导体单晶和用于磁盘的玻璃基底。
最优选的是,将N-取代的二氮烯二氧化物和N′-羟基-二氮烯氧化物盐(A)以及其中包含它们的本发明组合物用于集成电路器件的制造,所述集成电路器件尤其含结构尺寸低于50nm的大规模集成或非常大规模集成的集成电路。
最优选的是,本发明组合物极其适于本发明方法。
在本发明方法中,将用于电子、机械和光学器件,尤其是电子器件,最优选集成电路器件的基底材料与本发明组合物至少接触一次并抛光,尤其是化学和机械抛光,直至获得所需平坦度。
本发明方法显示了其在半导体硅晶片的CMP中特定的优点,其中所述硅晶片具有包含低k或超低k材料的隔离层和氮化硅层和/或多晶硅层。
合适的低k或超低k材料以及制备绝缘介电层的合适方法例如描述在美国专利申请US 2005/0176259 A1,第2页,第[0025]-[0027]段,US2005/0014667 A1,第1页,第[0003]段,US 2005/0266683 A1,第1页,第[0003]段和第2页,第[0024]段或US 2008/0280452 A1,第[0024]-[0026]段中或美国专利US 7,250,391 B2,第1栏,第49-54行或欧洲专利申请EP1 306 415 A2,第4页,第[0031]段。
本发明方法特别适合需要在图案化的晶片基底上相对于氮化硅选择性除去二氧化硅的浅沟槽隔离(STI)。在该方法中,使蚀刻的沟槽过充满介电材料,如二氧化硅,用氮化硅隔离膜作为停蚀层将其抛光。在该优选实施方案中,本发明方法以从隔离膜除去二氧化硅为结束,同时使暴露的氮化硅和沟槽氧化硅的去除最小化。
本发明方法未显示特殊性,而是可用常用于具有IC的半导体晶片的制造中CMP的方法和设备进行。
如本领域已知的,用于CMP的典型设备包含覆盖有抛光垫的旋转压板。将晶片安装在其上侧向下面对抛光垫的夹持器或卡盘上。夹持器使晶片固定在水平位置。该抛光和夹持装置的特定排列也作为硬压板设计已知。夹持器可保留位于夹持器保留表面和未被抛光的晶片表面之间的夹持器垫。该垫可用作晶片缓冲垫。
在夹持器下,较大直径的压板通常也是水平定位并展现与待抛光晶片平行的表面。其抛光垫在平坦化方法期间接触晶片表面。在本发明CMP方法期间,将本发明组合物以连续流或以逐滴形式施用至抛光垫上。
夹持器和压板均围绕其各自的从夹持器和压板垂直延伸的轴旋转。旋转的夹持器轴可在相对于旋转压板的位置上保持固定或可相对于压板水平震荡。夹持器的旋转方向通常与压板相同,但这不是必须的。夹持器和压板的旋转速度通常被设置为不同值,但这不是必须的。
通常而言,将压板温度设置在10-70℃的温度下。
其它细节可结合附图1参考国际专利申请WO 2004/063301 A1,尤其是第16页,第[0036]段至第18页,第[0040]段。
经由本发明方法,可获得具有IC的半导体晶片,其包含图案化的低k和超低k材料层,尤其是二氧化硅层且具有优异的平坦度。因此,可获得也具有优异的平坦度以及在最终完成的IC中具有优异的电功能的铜波纹图案。
实施例:
对实施例1-3和对比实验C1和C2而言,组合物1-3和C1和C2通过将成分溶解并分散在超纯净的去离子水中而制备。表1显示了所用成分的量。
表1:用于组合物1-3和C1和C2的制备的成分的量
a)聚磷酸酯;二氧化铈与聚磷酸酯的重量比=200;
实施例4-6和对比实验C3和C4
将实施例1的组合物用于实施例4,实施例2的组合物2用于实施例5,以及将实施例3的组合物3用于实施例6。
将对比实验C1的组合物C1用于对比实验C3,以及将对比实验C2的组合物C2用于对比实验C4。
为测定氧化硅相对于氮化硅的选择性,将含氧化物层或氮化物层的硅晶片用于实施例4-6和对比实验C3和C4。
抛光速率(即材料去除速率MRR)通过重量差测定。在这方面,将1.9kg/L用作热二氧化硅的密度并将3.44kg/L用作氮化硅密度,用于通过Sartorius LA310 S量度仪或Filmmetrics F50反射计计算CMP之前和之后晶片的MRR。抛光实验用具有以下参数的Strasbaugh nSpire(Model6EC),ViPRR浮动的保持环夹持器(floating retaining ring Carrier)进行:
-下压力:3.5psi(240毫巴);
-后侧压力:0.5psi(34.5毫巴);
-保持环压力:2.5psi(172毫巴);
-抛光台/夹持器速率:95/85rpm;
-浆料流动速率:200ml/分钟;
-抛光时间:60s;
-垫修正:原位(9.2-9.0Ibs,41N);
-抛光垫:IC1000 A2叠垫,xy k沟槽式(R&H);
-背衬膜:Strasbaugh,DF200(136孔);
-修整盘:Strasbaugh sasol。
表2总结了所获得的MRR和所计算的氧化硅相对于氮化硅的选择性。
表2:组合物1-3(实施例4-6)和C1和C2(对比实验C3和C4)的材料去除速率和氧化硅相对于氮化硅的选择性
a)材料去除速率[埃/分钟]
b)TEOS(原硅酸四乙酯)的MRR(材料去除速率[埃/分钟])
c)TEOS/Si3N4的选择性
Claims (18)
R[-N+(-O-)=N-OH]n (I),
其中变量R指包含或由至少一种选自以下的残基组成的结构部分:不含或含至少一个杂原子和/或至少一个双官能或三官能链接基团的单体、低聚及聚合,取代及未取代,饱和及未饱和的脂族和脂环族基团,以及不含或含至少一个杂原子的单体、低聚及聚合,取代及未取代的芳族基团;且其中指数n为1-1000的数字;
{R[-N(-O)-N-O]- n}m(Mm+)n (II),
其中变量R具有上述含义,M选自有机和无机,单体、低聚和聚合的阳离子,指数n和m均为1-2000的数字。
3.根据权利要求2的含水抛光组合物,其特征在于n和m均为1-10的整数。
4.根据权利要求3的含水抛光组合物,其特征在于其基于抛光组合物的全部重量含有0.01-1000ppm化合物(A)。
5.根据权利要求1-4中任一项的含水抛光组合物,其特征在于所述磨料颗粒(B)选自氧化铝、二氧化硅、氮化硅、碳化硅、二氧化钛、氧化锆、二氧化铈、氧化锌及其混合物。
6.根据权利要求5的含水抛光组合物,其特征在于所述磨料颗粒(B)包含或由二氧化铈组成。
7.根据权利要求5或6的含水抛光组合物,其特征在于所述磨料颗粒(B)通过动态光散射测量的平均粒径为1-1000nm。
8.根据权利要求1-7中任一项的含水抛光组合物,其特征在于其基于抛光组合物的全部重量含有0.005-10重量%磨料颗粒(B)。
9.根据权利要求1-8中任一项的含水抛光组合物,其特征在于其含有至少一种与组分(A)和(B)不同的功能组分(C)。
10.根据权利要求9的含水抛光组合物,其特征在于所述功能组分(C)选自与颗粒(B)不同的有机、无机和混合的有机-无机磨料颗粒,具有下限临界溶解温度LCST或上限临界溶解温度UCST的材料,氧化剂、钝化剂、电荷反转剂、具有至少3个在含水介质中不可离解的羟基的有机多元醇,由至少一种具有至少3个在含水介质中不可离解的羟基的单体形成的低聚物和聚合物,配合或螯合剂,摩擦剂,稳定剂,流变剂,表面活性剂,金属阳离子和有机溶剂。
11.根据权利要求10的含水抛光组合物,其特征在于所述电荷反转剂(C)选自含有至少一个选自以下的阴离子基团的单体、低聚和聚合的化合物:羧酸根、亚磺酸根、硫酸根、膦酸根和磷酸根基团;以及在于具有至少3个在含水介质中不可离解的羟基的有机多元醇,由至少一种具有至少3个在含水介质中不可离解的羟基的单体形成的低聚物和聚合物选自单糖、二糖、低聚糖、多糖、脱氧糖、氨基糖、醛糖酸、酮糖醛酸、糖醛酸、醛糖二酸、糖醇和环醇。
12.根据权利要求1-8中任一项的含水抛光组合物,其特征在于其含有至少一种与组分(A)和(B)不同的pH调节剂或缓冲剂(D)。
13.根据权利要求1-12中任一项的含水抛光组合物,其特征在于其pH值为3-10。
14.一种抛光电子、机械和光学器件用基底材料的方法,其包括使所述基底材料与含水抛光组合物至少接触一次并抛光所述基底材料直至获得所需平坦度,其特征在于使用根据权利要求1-13中任一项的含水抛光组合物。
15.根据权利要求14的方法,其特征在于所述基底材料包含至少一层包含或由至少一种介电材料组成的层。
17.根据权利要求16的用途,其特征在于所述电子器件为集成电路器件、液晶面板、有机电致发光面板、印刷电路板、微型机、DNA芯片、微型设备和磁头;机械器件为高精度的机械器件;光学器件为光学玻璃,如光掩模、透镜和棱镜,无机导电膜,如氧化铟锡(ITO),光学集成电路,光学开关元件,光学波导管,光学单晶,如光学纤维和闪烁器的端面,固体激光器单晶,用于蓝色激光器LED的蓝宝石基底,半导体单晶和用于磁盘的玻璃基底。
18.根据权利要求17的用途,其特征在于所述集成电路器件含有结构尺寸低于50nm的大规模集成或非常大规模集成的集成电路。
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CN110655868A (zh) * | 2018-06-29 | 2020-01-07 | 弗萨姆材料美国有限责任公司 | 低氧化物沟槽凹陷化学机械抛光 |
CN114634765A (zh) * | 2018-06-29 | 2022-06-17 | 弗萨姆材料美国有限责任公司 | 低氧化物沟槽凹陷化学机械抛光 |
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CN114634765B (zh) * | 2018-06-29 | 2024-04-02 | 弗萨姆材料美国有限责任公司 | 低氧化物沟槽凹陷化学机械抛光 |
Also Published As
Publication number | Publication date |
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IL225084B (en) | 2018-01-31 |
EP2614122A4 (en) | 2014-01-15 |
SG188459A1 (en) | 2013-04-30 |
KR20130133175A (ko) | 2013-12-06 |
US20130200039A1 (en) | 2013-08-08 |
TWI598434B (zh) | 2017-09-11 |
KR101967134B1 (ko) | 2019-04-09 |
RU2013115236A (ru) | 2014-10-20 |
SG10201506215WA (en) | 2015-09-29 |
WO2012032466A1 (en) | 2012-03-15 |
EP2614122A1 (en) | 2013-07-17 |
JP2013540850A (ja) | 2013-11-07 |
TW201217506A (en) | 2012-05-01 |
CN103210047B (zh) | 2018-07-17 |
RU2608890C2 (ru) | 2017-01-26 |
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