CN1158373C - 用于铜/钽基材的化学机械抛光浆料 - Google Patents
用于铜/钽基材的化学机械抛光浆料 Download PDFInfo
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- CN1158373C CN1158373C CNB998095605A CN99809560A CN1158373C CN 1158373 C CN1158373 C CN 1158373C CN B998095605 A CNB998095605 A CN B998095605A CN 99809560 A CN99809560 A CN 99809560A CN 1158373 C CN1158373 C CN 1158373C
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- Prior art keywords
- chemical mechanical
- mechanical polishing
- polishing slurry
- slurry
- weight
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- IIACRCGMVDHOTQ-UHFFFAOYSA-N sulfamic acid Chemical compound NS(O)(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-N 0.000 description 1
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
- BYGOPQKDHGXNCD-UHFFFAOYSA-N tripotassium;iron(3+);hexacyanide Chemical compound [K+].[K+].[K+].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] BYGOPQKDHGXNCD-UHFFFAOYSA-N 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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Abstract
公开了一种包括:磨料、氧化剂、配合剂、成膜剂和有机氨化合物的第一种化学机械抛光浆料;和包括磨料、氧化剂和乙酸且其中氧化剂与乙酸的比例至少为10的第二种抛光浆料,还公开了用第一种和第二种抛光浆料顺序抛光含铜和含钽或氮化钽或钽和氮化钽两种的基材的方法。
Description
发明领域
本发明涉及一种可在抛光包括铜部分和钽部分的基材时使用的化学机械抛光浆料。本发明包括含一种磨料、一种氧化剂、一种配合剂、和至少一种有机氨化合物的第一种化学机械抛光浆料。
现有技术的描述
集成电路由在硅基材上或硅基材内形成的数百万个活化元件构成。这些开始时相互分离的活化元件互连形成功能电路和部件。这些元件通过使用公知的多层互连件互连。互连结构通常具有第一种层金属化的互连层、第二种层金属化层、和某些时候第三层和随后的金属化层。层间界电质如掺杂和不掺杂二氧化硅或低κ电介质氮化钽用于电隔离不同金属化量的硅基材或阱(well)。不同互连层之间的电连接通过使用金属化的通路进行。US 5,741,626描述了制备介电氮化钽层的方法。
在类似方法中,金属接触用于形成在阱中形成的互连层和元件之间的电连接。金属通路和触点可填充各种金属和合金,包括钛(Ti)、氮化钛(TiN)、钽(Ta)、铝-铜(Al-Cu)、硅铝(Al-Si)、铜、钨(W)和其组合。这些金属通路和触点通常使用粘结层如氮化钛(TiN)钛(Ti)、钽(Ta)、氮化钽(TaN)或其组合,由此将金属层与SiO2基材连接。在接触层,粘结层起到扩散阻挡的作用以防止填充的金属与SiO2反应。
在一个半导体制造方法中,金属通路或触点通过均厚金属沉积接着进行化学机械抛光(CMP)进行。在一典型方法中,经层间电介质(ILD)至互连线路或半导体基材蚀刻出通路孔。接着通常在ILD上形成薄粘结层如氮化钽和/或钽,该粘结层直接连接于蚀刻通路孔。然后将金属膜均厚沉积于粘结层上和蚀刻通路孔内。继续进行沉积直至通路孔填充均厚沉积金属为止。最后,通过化学机械抛光(CMP)除去过量的金属形成金属通路。制造和/或CMP通路的方法公开于US 4,671,851、4,910,155和4,944,836中。
在典型的化学机械抛光方法中,将基材直接与旋转抛光垫接触。用一载重物在基材背面施加压力。在抛光期间,垫片和操作台旋转,同时在基材背面上保持向下的力。在抛光期间将磨料和化学活性溶液(通常称为“浆料”)涂于垫片上。该浆料通过与正在抛光的薄膜化学反应开始抛光过程。在硅片/垫片界面涂布浆料下通过垫片相对于基材旋转运动促进抛光过程。按此方式连续抛光直至除去绝缘体上所需的薄膜。浆料组合物在CMP步骤中一种重要的因素。可根据选取的氧化剂、磨料和其它合适的添加剂调节浆料,以按所需的抛光速率提供有效抛光,同时将表面缺陷、磨蚀和磨耗降至最低。此外,抛光浆料可用于提供对目前集成技术中所用的其它薄薄膜材料如钛、氮化钛、钽、氮化钽等的控制抛光选择性。
CMP抛光浆料通常含磨料,如悬浮于含水氧化介质中的二氧化硅或氧化铝。例如,Yu等人的US 5,244,523报道含氧化铝、过氧化氢和氢氧化钾或氢氧化铵的浆料,该浆料可用于以预期速率在很少除去底层绝缘层下除去钨。Yu等人的US 5,209,816公开了可用于抛光铝的包括在水介质中的高氯酸、过氧化氢和固体磨料的浆料。Cadien等的US 5,340,370公开了钨抛光浆料,包括约0.1M铁***、约5重量%的二氧化硅和乙酸钾。加入乙酸使pH缓冲至约3.5。
Beyer等人的US 4,789,648公开了用氧化铝磨料与硫酸、硝酸和乙酸及去离子水的浆料配料。US 5,391,258和5,476,606公开了用于抛光金属与二氧化硅复合物的浆料,该浆料包括含水介质、磨料颗粒和控制二氧化硅除去速率的阴离子。用于CMP的其它抛光浆料描述于Neville等人的US5,527,423、Yu等人的US 5,354,490、Medellin等人的US 5,157,876、Medellin等人的US 5,137,544和Cote等人的US 4,956,313中。
现有技术中公开了许多用浆料抛光金属表面的机理。金属表面可用一种浆料抛光,这种浆料在用机械除去浆料中的金属粒子和其溶解物的处理时不会形成表面膜。在这种机理中,不应降低化学溶解速率来避免湿侵蚀。然而,更优选的机理是通过金属表面和浆料中的一种或多种组分如配合剂和/或成膜剂反应连续形成薄的可磨损层。然后通过机械作用以受控的方式除去该磨损层。当机械抛光处理停止时薄钝化膜留在其表面并控制湿侵蚀处理。当用这种机理的CMP浆料抛光时更容易控制化学机械抛光处理。
目前用化学机械抛光的含铜基材也用Ta和TaN粘合剂层。Ta和TaN十分化学钝化且机械很硬,由此难以抛光除去。使用具有高Cu∶Ta选择性的单一浆料需要对Ta延长的抛光时间,即对铜明显的过抛光时间,这期间明显降低了耐破坏(dishing)和腐蚀性能。
公开文献中讨论了几种相关Cu的化学,但每一种都没有提供成功解决用于包括铜和钽的基材的化学机械抛光浆料所有关键要求的方法。结果,需要一种或多种可成功用于抛光含铜和钽基材的CMP浆料。
发明概述
本发明涉及一种能选择抛光含铜和钽或氮化钽基材的铜部分的第一种化学机械抛光浆料。
本发明还公开了(1)一种能选择抛光含铜和钽和/或氮化钽基材的钽和/或氮化钽部分的第二种化学机械抛光浆料,及(2)用第一种和第二种化学机械抛光浆料连续抛光包括铜部分和钽和/或氮化钽部分的基材的方法。
本发明的另一方面是化学机械抛光浆料前体,该前体无氧化剂并在使用前与氧化剂单独组合来制得可用的CMP浆料。
本发明是第一种化学机械抛光浆料。该第一种化学机械抛光浆料包括至少一种磨料、至少一种氧化剂、至少一种配合剂和至少一种有机氨化合物。第一种抛光浆料的一个优选实施方案是包括氧化铝、至少一种氧化剂、酒石酸、苯并***和至少一种有机氨化合物的组合物。
本发明实施方案的详细描述
本发明涉及第一化学机械抛光浆料及选择性地抛光包含铜和钽、氮化钽及其混合物的基材中的铜的方法。除了组合使用来抛光含铜和钽基材外,第一种化学机械抛光浆料可用来抛光含铜或铜合金的基材。
在详细描述本发明的各种优选实施方案之前,对这里使用的一些术语进行定义。化学机械抛光浆料(“CMP浆料”)为本发明的有用产品,它包括氧化剂、磨料、配合剂、有机氨化合物和其它非必要的成分。该CMP浆料用于抛光多层金属化层,包括但不限于:半导体薄薄膜、集成电路薄薄膜和其中可使用CMP方法的任何其它薄膜和表面。
术语“铜”和“含铜合金”这里可相互交换使用,正如本领域熟练技术人员知道的,该术语包括但不限于含纯铜、铜铝合金、和Ti/TiN/Cu层的基材及Ta/TaN/Cu多层基材。
术语“钽”“含钽合金”本文可相互交换使用,指的是在导电层下如导电铜层下的钽和/或氮化钽层。
第一种化学机械抛光浆料可用于与基材连接的金属、特别是铜和含铜合金金属层的抛光,所述基材选自集成电路、薄薄膜、多层半导体层和硅片。
I.第一种化学机械抛光浆料
第一种CMP浆料可特别有利于高速抛光包括铜部分和钽部分的基材。第一种化学机械抛光浆料可用于抛光除铜以外的其它金属层。
第一种CMP浆料包括至少一种氧化剂。氧化剂有助于将多金属层氧化至其相应的氧化物、氢氧化物或离子。例如在第一种CMP浆料中,氧化剂可用于将金属层氧化至相应的氧化物或氢氧化物,例如钛至氧化钛、钨至氧化钨、铜至氧化铜、和铝至氧化铝。通过对金属进行机械抛光除去相应氧化层的方式,抛光金属和基于金属的组分(包括钛、氮化钛、钽、铜、钨、铝和铝合金如铝/铜合金及其各种混合物和组合物,将本发明的氧化剂加入第一种CMP浆料中是有利的。
用于本发明第一种CMP浆料的氧化剂为一种或多种无机和有机过化合物。由Hawley’s Condensed Chemical Dictionary定义的过化合物是含至少一个过氧基团(-O-O-)的化合物或含一种处于其最高氧化态的元素的化合物。含至少一个过氧基团的化合物的例子包括但不限于过氧化氢和其加合物如过氧化氢脲和过碳酸酯,有机过氧化物如过氧化苯甲酰、过乙酸和过氧化二叔丁基、单过硫酸盐(SO5 =)和二过硫酸盐(S2O8-)和过氧化钠。
含一种处于其最高氧化态的元素的化合物的例子包括但不限于高碘酸、高碘酸盐、高溴酸、高溴酸盐、高氯酸、高氯酸盐、过硼酸、过硼酸盐和高锰酸盐。满足该电化学势要求的非过化合物的例子包括但不限于溴酸盐、氯酸盐、铬酸盐、碘酸盐、碘酸和铈(IV)化合物如硝酸铵铈。
优选的氧化剂为过乙酸、脲-过氧化氢、过氧化氢、单过硫酸、二过硫酸盐、和其盐,和其混合物包括脲和过氧化氢的混合物。最优选的氧化剂为过氧化氢和脲的组合。
氧化剂在第一种化学机械抛光浆料中的存在量可为约0.3至约30.0重量%。优选氧化剂在第一种化学机械抛光浆料中的存在量为约0.3至约17.0重量%,最优选约1.0至约12.0重量%。
一种非必要的氧化剂为过氧化氢脲。由于过氧化氢脲为34.5%过氧化氢和65.5%脲,因此在第一种CMP浆料中必须包括大量的过氧化氢脲,以达到上述设定的所希望的氧化剂加入量。例如,0.5-12.0%重量氧化剂对应于三倍或1.5-36.0重量%的过氧化氢脲的重量。
包括过氧化氢脲的第一种CMP浆料还可通过将过氧化物脲与水混合、和在水溶液中按摩尔比约0.75∶1至约2∶1化合以形成过氧化氢脲氧化剂的方式来配制。
本发明第一种CMP浆料在基材表面上形成钝化层。当形成钝化层时,能妨碍钝化层以使第一种CMP浆料中的磨料组分更易从基材表面除去金属氧化物是很重要的。包括在第一种CMP浆料来妨碍钝化层的一类化合物为配合剂。可用的配合剂包括但不限于:酸如柠檬酸、乳酸、丙二酸、酒石酸、琥珀酸、乙酸、草酸、和其它酸,以及氨基酸和氨基硫酸、磷酸、膦酸和其盐。优选的第一种CMP浆料配合剂为酒石酸。
配合剂在本发明的第一种CMP浆料中的量为约0.2-约5.0重量%、优选为约0.5-约3.0重量%。
本发明的第一种CMP浆料包括至少一种有机氨化合物。有机氮化合物吸附在抛光后的基材上并抑制基材的除去速率。用于第一种CMP浆料的有机氨化合物包括烷基胺、醇胺、氨基酸、脲、脲的衍生物、和其混合物。优选的有机氨化合物是长链烷基胺和醇胺。术语“长链烷基胺”指的是具有7-12或更多碳原子的烷基胺,包括例如壬胺和十二烷胺。可用的醇胺包括但不限于单乙醇胺和三乙醇胺。可用的脲衍生物的例子包括但不限于二脲。优选的有机氨化合物是长链烷基胺、十二烷基胺。优选的醇胺是三乙醇胺。
有机氨在第一种CMP浆料中的量应为约0.005-约10.0%重量。更优选有机氨化合物在第一种CMP浆料中的量为约0.01-约5.0%重量。
本发明的第一种CMP浆料可包括非必要的成膜剂。该成膜剂可是能够有助于在金属层的表面上形成金属氧化物钝化层和溶解抑制层的任何化合物或化合物的混合物。基材表面层的钝化对防止基材表面的湿蚀刻是很重要的。可用的成膜剂是含氮环状化合物如咪唑、苯并***、苯并咪唑、苯并噻唑、和其具有羟基、氨基、亚氨基、羧基、巯基、硝基和烷基取代基的衍生物,以及脲、硫脲等。优选的成膜剂是苯并***(“BTA”)。
非必要的成膜剂在第一种CMP浆料中的量应为约0.01-约1%重量。优选成膜剂在第一种CMP浆料中的量为约0.01-约0.2%重量。
第一种CMP浆料中所含的BTA或其它成膜剂可使浆料中磨料的均匀分散失去稳定。为促进第一种抛光浆料抗沉降、絮凝和分解的稳定性,可使用各种非必要的添加剂如表面活性剂、稳定剂或分散剂。若将表面活性剂加入第一种CMP浆料中,则表面活性剂可为阴离子、阳离子、非离子或两性表面活性剂,或可使用两种或多种表面活性剂的组合物。此外,加入表面活性剂可用于降低硅片的硅片内非均匀性(WIWNU),由此改进硅片的表面和减少硅片表面缺陷。
通常可用于本发明的添加剂如表面活性剂的量应足以获得浆料的有效稳定性,且通常可根据选取的特定表面活性剂和金属氧化物磨料的表面性能而变化。例如,若选取的表面活性剂的用量不足,则对稳定性几乎没有或无效果。另一方面,在CMP浆料中表面活性剂太多会导致浆料中的不合适发泡和/或絮凝。稳定剂如表面活性剂的存在量通常应为约0.001%至0.2重量%。此外,可将添加剂直接加入浆料中或用已知工艺对金属氧化物表面进行处理。在每一情况下,调节添加剂的量以在抛光浆料中达到所需的浓度。优选的表面活性包括十二烷基硫酸钠、月桂基硫酸钠、十二烷基硫酸铵盐和其混合物。可用的表面活性的例子包括Unino Carbide制造的TRITONDF-16、和Air Products and Chemicals制造的SURFYNOL。
理想的是保持本发明第一种CMP浆料的pH为约2.0-约12.0,优选约4.0-约8.0,以有助于控制CMP处理。可用任何已知的酸、碱或胺调节本发明CMP浆料的pH值。然而,优选用不含金属离子的酸或碱,如氢氧化铵和胺、或硝酸、磷酸、硫酸、或有机酸,以避免向本发明CMP浆料引入不希望要的金属组分。
II.第二种化学机械抛光浆料
配制第二种CMP浆料,使得其具有低的对铜的抛光速率,以及典型的对钽或氮化钽的抛光速率。因此,优选第二种CMP浆料的铜与钽的抛光速率低于约2-1,最优选低于约1-5。
第二种CMP浆料包括至少一种氧化剂。氧化剂有助于将多金属层氧化至其相应的氧化物、氢氧化物或离子。例如在第二种CMP浆料中,氧化剂可用于将金属层氧化至相应的氧化物或氢氧化物,例如钽至氧化钽。通过对金属进行机械抛光除去相应氧化层的方式,抛光金属和基于金属的组分(包括钛、氮化钛、钽、铜、钨、铝和铝合金如铝/铜合金及其各种混合物和组合物),将本发明的氧化剂加入第二种CMP浆料中是有利的。
用于本发明第二种CMP浆料的氧化剂使用的氧化剂为一种或多种无机和有机过化合物。由Hawley’s Condensed Chemical Dictionary定义的过化合物是含至少一个过氧基团(-O-O-)的化合物或含一种处于其最高氧化态的元素的化合物。含至少一个过氧基团的化合物的例子包括但不限于过氧化氢和其加合物如过氧化氢脲和过碳酸酯,有机过氧化物如过氧化苯甲酰、过乙酸和过氧化二叔丁基、单过硫酸盐(SO5 =)和二过硫酸盐(S2O8-)和过氧化钠。
含一种处于其最高氧化态的元素的化合物的例子包括但不限于高碘酸、高碘酸盐、高溴酸、高溴酸盐、高氯酸、高氯酸盐、过硼酸、过硼酸盐和高锰酸盐。满足该电化学势要求的非过化合物的例子包括但不限于溴酸盐、氯酸盐、铬酸盐、碘酸盐、碘酸和铈(IV)化合物如硝酸铵铈。
优选的氧化剂的非排他性例子包括但不限于:过乙酸、脲-过氧化氢、过氧化氢、单过硫酸、二过硫酸盐、和其盐,和其包括脲和过氧化氢的混合物的混合物。优选的氧化剂为过氧化氢。
氧化剂在第二种化学机械抛光浆料中的存在量可为约0.3至约30.0重量%。优选氧化剂在第二种CMP浆料中的存在量为约0.3至约17.0重量%,最优选约1.0至约12.0重量%。
包括在第二种CMP浆料中的一类化合物为配合剂。可用的配合剂包括但不限于:酸如柠檬酸、乳酸、酒石酸、琥珀酸、乙酸、草酸和其它酸,以及氨基酸和氨基磺酸、磷酸、膦酸和其盐。优选的配合剂为乙酸。配合剂在本发明的CMP浆料中的量为约0.1-约5.0重量%、优选为约0.1-约3.0重量%。
第二种CMP浆料含有远少于浆料中氧化剂重量的配合剂是很重要的。第二种CMP浆料的氧化剂与配合剂的重量比应大于约10,优选应大于约25。
本发明的第二种CMP浆料可包括非必要的成膜剂。该成膜剂可是能够有助于在金属层的表面上形成金属氧化物钝化层和溶解抑制层的任何化合物或化合物的混合物。基材表面层的钝化对防止基材表面的湿蚀刻是很重要的。可用的成膜剂是含氮环状化合物如咪唑、苯并***、苯并咪唑、苯并噻唑、和其具有羟基、氨基、亚氨基、羧基、巯基、硝基和烷基取代基的衍生物,以及脲、硫脲等。优选的成膜剂是苯并***(“BTA”)。成膜剂在第二种CMP浆料中的量应为约0.01-约1%重量。优选成膜剂在第二种CMP浆料中的量为约0.01-约0.5%重量。
第二种CMP浆料中所含的BTA或其它成膜剂可使浆料中磨料的均匀分散失去稳定。为促进第二种抛光浆料抗沉降、絮凝和分解的稳定性,可使用各种非必要的添加剂如表面活性剂、稳定剂或分散剂。若将表面活性剂加入第二种CMP浆料中,则表面活性剂可为阴离子、阳离子、非离子或两性表面活性剂,或可使用两种或多种表面活性剂的组合物。此外,加入表面活性剂可用于降低硅片的硅片内非均匀性(WIWNU),由此改进硅片的表面和减少硅片表面缺陷。
通常可用于本发明第二种CMP浆料中的添加剂如表面活性剂的量应足以获得浆料的有效稳定性,且通常可根据选取的特定表面活性剂和金属氧化物磨料的表面性能而变化。例如,若选取的表面活性剂的用量不足,则对稳定性几乎没有或无效果。另一方面,在CMP浆料中表面活性剂太多会导致浆料中的不合适发泡和/或絮凝。稳定剂如表面活性剂的存在量通常应为约0.001%至约0.2重量%。此外,可将添加剂直接加入浆料中或用已知工艺对金属氧化物表面进行处理。在每一情况下,调节添加剂的量以在第一种抛光浆料中达到所需的浓度。优选的表面活性包括十二烷基硫酸钠、月桂基硫酸钠、十二烷基硫酸铵盐和其混合物。可用的表面活性的例子包括UninoCarbide制造的TRITONDF-16、和Air Products and Chemicals制造的SURFYNOL。
理想的是保持本发明第二种CMP浆料的pH为约2.0-约12.0,优选约4.0-约8.0,以有助于控制CMP处理。可用任何已知的酸、碱或胺调节本发明CMP浆料的pH值。然而,优选用不含金属离子的酸或碱,如氢氧化铵和胺、或硝酸、磷酸、硫酸、或有机酸,以避免向本发明CMP浆料引入不希望要的金属组分。最优选第二种CMP浆料的pH约为4-约7.5。
III.磨料
本发明的第一种和第二种CMP浆料都包括磨料。该磨料通常为金属氧化物磨料。金属氧化物磨料选自氧化铝、氧化钛、氧化锆、氧化锗、氧化硅、氧化铈及其混合物。本发明的第一种和第二种CMP浆料优选各自包括约0.5至约15.0重量%或更多的磨料。然而,本发明的第一种和第二种CMP浆料更优选各自包括约1.5至约6.0重量%的磨料。
金属氧化物磨料可通过本领域熟练技术人员已知的任何工艺生产。金属氧化物磨料可用任何高温方法如溶胶-凝胶、水热或等离子体方法,或通过制造煅制或沉淀金属氧化物的方法生产。金属氧化物优选为煅烧或沉淀磨料,更优选为煅制磨料如煅制二氧化硅或煅制氧化铝。例如,生产煅制金属氧化物是公知方法,该方法涉及将合适的原料蒸汽(如用于生产氧化铝磨料的氯化铝)在氢气和氧气火焰中水解。在燃烧过程中形成近似球形的熔融颗粒,其直径可通过方法参数变化。这些氧化铝或类似氧化物的熔融球(通常称为初始颗粒)相互通过进行碰撞在其接触点相互稠合形成支化的三维链状聚集体。使聚集体破裂所需的力相当大,且通常认为是不可逆的。在冷却和收集期间,聚集体承受进一步碰撞,可导致一些机械缠结,由此形成附聚物。这些附聚物通过Van derWaals力松散连接并可逆(即可通过在合适介质中的合适分散而去除附聚)。
沉淀磨料可通过常规技术,如通过所需颗粒在高盐浓度、酸或其它凝固剂作用下自水介质中凝固而生产。将这些颗粒通过本领域熟练技术人员已知的常规方法过滤、洗涤、干燥并从其反应产品的残余物中分离。
优选的金属氧化物可具有表面积为约5m2/g至约430m2/g,优选约30m2/g至约170m2/g,所述表面积由S.Brunauer,P.H.Emmet和I.Teller的方法,通常称为BET(美国化学会志,Vol.60,p309(1938))计算。由于在IC工业中严格的纯度要求,优选的金属氧化物应为高纯的。高纯是指来自诸如原料不纯物和痕量加工污染物源的总不纯物含量通常低于1%,优选低于0.01%(即100ppm)。
用于本发明浆料的金属氧化物磨料可包括金属氧化物聚集体或独立单个的球形颗粒。本文所用术语“颗粒”指的是多于一个初级粒子的聚集体和独立单个颗粒两种。
优选金属氧化物磨料包括颗粒尺寸分布低于约1000nm(1μm)(即所有颗粒的直径低于1000nm(1μm))、平均聚集体直径低于约0.4μm,及足以排斥和克服磨料聚集体之间的van der Waals力的金属氧化物聚集体组成。已发现这些金属氧化物磨料在抛光期间对尽可能降低或避免划痕、微细斑点、divot和其它表面缺陷有效。本发明聚集体尺寸分布可通过已知技术如透射电子显微镜(TEM)测定。聚集体平均直径是指用TEM图像分析时的平均等球直径,即基于聚集体横截面的直径。力是指金属氧化物颗粒的表面势或水合力必须足以排斥和克服颗粒之间的van der Waals力。
在另一优选实施方案中,金属氧化物磨料可由具有初始颗粒直径低于0.4μm(400nm)和表面积约10m2/g至约250m2/g的分离的单个金属氧化物颗粒组成。
优选将金属氧化物磨料以金属氧化物的浓水分散体形式加入抛光浆料的水介质中,所述金属氧化物磨料的水分散体通常含有约3%至约45%的固体物,优选10%至20%的固体物。金属氧化物水分散体可用常规工艺生产,例如将金属氧化物磨料慢慢加入合适的介质(如去离子水)中形成胶态分散体。该分散体通常通过对其进行本领域熟练技术人员已知的高剪切混合制得。浆料的pH可调节至远离等电点以获得最大的胶体稳定性。
IV.非必要的添加剂
其它公知的抛光浆料添加剂可加入第一种CMP浆料和/或第二种CMP浆料中。一类非必要的添加剂是可加入第一种/或第二种CMP浆料中以进一步提高或改善硅片屏壁层如钛和钽的抛光速率的无机酸和/或其盐。可用的无机添加剂包括硫酸、磷酸、膦酸、硝酸、HF酸、氯化铵、硫酸、磷酸、膦酸和盐酸的铵盐、钾盐、钠盐或其它阳离子盐。
V.第一种和第二种CMP浆料的制备和使用方法
本发明的第一种和第二种CMP浆料可用本领域熟练技术人员已知的常规工艺生产。通常,将氧化剂和其它非磨料组分按预定浓度在低剪切下混入水介质如去离子水或蒸馏水中,直至这些组分完全溶于介质中。将金属氧化物磨料如煅制氧化铝的浓分散体加入介质中并稀释至磨料在最终CMP浆料中的所需量。
本发明第一种和第二种CMP浆料可以一个包括所有浆料添加剂的包装体系形式提供。但考虑含有氧化剂、特别是过氧化氢的CMP浆料的运输问题,优选本发明的第一种和第二种CMP浆料制备和包装成含有除氧化剂以外的每一种组分的CMP前体,运输到用户处,有使用前在用户的工厂与过氧化氢或其它的氧化剂混合。因此,本发明一方面是包括一种或多种选自干状或水状的催化剂、磨料和稳定剂组分但没有氧化剂的第一种和第二种CMP组合物或和/或浆料前体。在使用前第一种和第二种CMP浆料分别与至少一种氧化剂混合。
已确定,可通过将过氧化氢加入包括脲和任何其它合适浆料组分的浆料前体中得到含过氧化氢脲的CMP浆料的方式,配制本发明包括过氧化氢脲的第一种和第二种CMP浆料。
本发明优选的浆料前体包括脲与至少一种金属氧化物磨料的干燥或含水混合物。另一些组分也可包括于含脲的浆料前体中,用于第一种和第二种CMP浆料。
虽然本发明的CM浆料可用来抛光任何类金属层,但发现本发明的第一种化学机械抛光浆料具有高的铜抛光速率、低的钽和氮化钽抛光速率。另外,第二种化学机械抛光浆料具有所希望的对铜层的低的抛光速率,同时对钽介电绝缘层有所希望的高的抛光速率。
本发明的化学机械抛光浆料的Cu∶Ta抛光选择性比至少为40。
本发明优选的一种用于选择性地抛光含铜及钽、氮化钽或其混合物基材中的铜的化学机械抛光浆料,包括:
0.5-15%重量的氧化铝;
0.5-5%重量的酒石酸;
0.01-0.2%重量的苯并***;
0.005-10.0%重量的选自十二烷基胺、三乙醇胺和其混合物的有机氨化合物;和
包括1-20%重量脲和约1-12.0%重量过氧化氢的混合物的氧化剂,其中该化学机械抛光浆料的pH为约4-8,Cu∶Ta抛光选择性比至少大于10。
第一种和第二种CMP浆料可通过任何适合使用的标准的抛光设备用于所希望的硅片的金属层上。本发明的第一种和第二种CMP浆料最适宜于用于抛光在介电层上包括钽或氮化钽部分和含铜合金部分的基材。
当用来抛光包括钽或氮化钽部分和含铜合金部分的基材时,把第一种化学机械抛光浆料涂于基材上,用抛光机和抛光垫通过常规方法对基材进行抛光。当完成用第一种CMP浆料对基材进行抛光时,可用去离子水或其它溶剂冲洗基材,以从部分抛光的基材上除去第一种CMP浆料。接着,把本发明的第二种CMP浆料涂于基材上,用常规工艺抛光基材,相对于部分抛光基材的铜部分优选抛光钽或氮化钽部分。当完成第二种抛光步骤,用去离子水或其它溶剂冲洗基材,把基材准备用于进一步的加工。
在两个抛光步骤中,在基材抛光期间可以受控的方式把第一种和/或第二种抛光浆料以直接涂于基材上、抛光垫上或这两者上。然而,优选把第一种和第二种CMP浆料涂于垫上,然后把该垫相对于基材放置,然后相对于基材移动该垫,来实现基材的抛光。
第一种和第二种CMP浆料在受控状态以良好的速率抛光铜、钛、氮化钛、钽和氮化钽层。本发明的抛光浆料可在制造半导体集成电路的各个阶段使用,以提供按所需抛光速率进行有效抛光,同时将表面缺陷降至最低。
实施例
我们已发现,第一种CMP浆料能够以高速率抛光铜、以较低的速率抛光钽和氮化钽层,第二种CMP浆料以可接受的速率抛光钽和氮化钽层、以比第一种CMP浆料相对较低的速率抛光铜。
下列实施例说明本发明的优选实施方案以及使用本发明CMP浆料的优选方法。
实施例I
在本实施例中,CMP抛光通过使用两种CMP浆料完成。第一种浆料包括3.0重量%的煅制氧化铝磨料(来自SEMI-SPERSEW-A355分散体,由Microelectronic materials Division of Cabot Corporation,in Aurora,Iilinois出售)、2.5重量%的过氧化氢、3.65%重量脲、1.25%重量酒石酸和50ppm的Triton DF-16表面活性剂的水分散体。第二种浆料包括第一种浆料的所有组分再加上0.015%重量十二烷基胺。将两种所测试的浆料用氢氧化铵调节至pH7.0。
用两种方法测试CMP浆料。用电化学测试每个CMP浆料的Cu和Ta的溶解速率。装置使用具有273恒电位仪和Corrosion Software(由PAR提供)的三电极池中的旋转圆盘电极。用预选的500rpm(或19.94m/秒,最大)电极旋转,转子和电极与磨料垫(40.7kPa(5.9磅/英寸2)向下的力)或向上升高的垫接触,来得到电化学数据。前面的值认为为抛光中化学数据的近似值,后面的值得到所给浆料的中金属的腐蚀速率。具体的,记录电化学数据作为势动能极化曲线,以10mV/秒的速率电势从约-0.25V阴极到开放电路势到一些阳极势变化。测试结果列在表1的3-4列中。
评估使用同种浆料的铜和钽的抛光速率,用IPEC 472抛光机、用20.7kPa(3磅/英寸2)向下的力、操作台速度55rpm和转轴速度60rpm。将该CMP浆料按200ml/分的速率涂于由Rodel制造的IC1000/SUBA IV上。抛光结果列于表1的列5-6中。
表1
浆料 | 金属溶解速率w/磨蚀埃/分 | 磨蚀后的金属腐蚀速率埃/分 | 抛光中的金属除去速率埃/分 | Cu∶Ta选择性比 | |
1 | 3%氧化铝、2.5%H2O2、3.65%脲、1.25%重量酒石酸、50ppmTriton DF-16 | Cu:240Ta:140 | Cu:36Ta:0.4 | Cu:2750Ta:415 | 6.6∶1 |
2 | 同1再加上0.015%重量十二烷基胺 | Cu:240Ta:60 | Cu:4.8Ta:0.12 | Cu:2250Ta:50 | 45∶1 |
向浆料中加入少量十二烷基胺抑制了Ta除去并明显提高Cu∶Ta的选择性比至45∶1。这使得含有机氨化合物的浆料更适宜于用作铜抛光浆料,其对Ta停止抛光。
表1的结果还表明:抛光中的电化学趋势再次表明:十二烷基胺抑制了磨蚀时Ta的溶解,随即其抛光速率明显不同于铜的速率。因此,十二烷基胺是Ta的溶解抑制剂。
实施例2
本实施例研究改变本发明第二种CMP浆料中的氧化剂与配合剂的重量比对Cu和钽抛光速率的影响。本实施例使用具有如下组成的CMP浆料:1.25重量%酒石酸、表2所列量的过氧化氢、3.0重量%氧化铝磨料(W-A355),50ppm Triton DF-16表面活性剂,余量为去离子水。用氢氧化铵调节浆料的pH7.0。
用不同比的酒石酸和过氧化氢氧化剂的浆料的抛光结果列于表2中。除了表2所列的化合物外,每一种浆料还含3.65%重量的脲。由Rodel制造的IC1000/SUBA IV垫、放置于IPEC472工具上的毯式硅片测定抛光速率。用20.7kPa(3磅/英寸2)向下的力、操作台速度55rpm和转轴速度30rpm、浆料流动速率200ml/分抛光硅片。
表2
次数# | 酒石酸% | HPO% | T:HPO | Cu抛光速率埃/分 | Ta抛光速率埃/分 |
1 | 1.25 | 7.5 | 1∶6 | 2,622 | 288 |
2 | 1.25 | 5.0 | 1∶4 | 3,265 | 304 |
3 | 1.25 | 2.5 | 1∶2 | 4,711 | 274 |
抛光结果表明:提高酒石酸/过氧化物的重量比提高了Cu的除去速率,而没有显著影响Ta的速率。
用实施例1所述的电化学法评估使用上述相同基材浆料但改变酒石酸含量(T)和改变过氧化氢含量(HPO)的金属溶解速率,结果列于表3中。
表3
次数# | 酒石酸% | HPO% | T:HPO | 磨蚀时的Cu溶解速率埃/分 | 磨蚀后的Cu腐蚀速率埃/分 |
1 | 0.5 | 6 | 1∶12 | 163 | 16.3 |
2 | 1 | 6 | 1∶6 | 163 | 19.2 |
3 | 0.5 | 2 | 1∶4 | 240 | 19.2 |
4 | 1 | 2 | 1∶2 | 314 | 38.4 |
5 | 3 | 6 | 1∶2 | 360 | 57.6 |
6 | 1 | 1 | 1∶1 | 344 | 504 |
7 | 2 | 2 | 1∶1 | 336 | 62.6 |
8 | 3 | 2 | 1∶1 | 336 | 62.6 |
表2和3的结果表明:铜的抛光速率对应于铜电化学所测的活性,这两者随氧化剂与配合剂的重量比的增加而降低,而钽抛光速率和电化学溶解性实质上不受组成变化的影响。
实施例3
把实施例2的表3中观察到的趋势用作配制抛光钽和氮化钽的第二种化学机械抛光浆料的基础。几种第二种抛光浆料的铜和钽的抛光速率列于下表4。化学抛光浆料中所用的磨料为SEMI-SPERSEW-A355煅制氧化铝分散体,由Cabot Corporation,Aurora,Illinois出售。
表4
浆料 | 铜除去速率埃/分 | Ta除去速率埃/分 | PETEOS除去速率埃/分 | Cu∶Ta选择性 | |
1 | 2%氧化铝、5%H2O2、0.5%酒石酸、pH7.0 | 651 | 337 | 64 | 1.9∶1 |
2 | 5%氧化铝、5%H2O2、0.2%酒石酸、0.2%乙酸、2%脲、0.08%BTA、50ppmTriton DF-16,pH6 | 260 | 244 | 8 | 1∶1 |
3 | 3%氧化铝、5%H2O2、0.2%乙酸、0.08%BTA、50ppmTritonDF-16,pH5.0 | 66 | 135 | 135 | 1∶1.45 |
把氧化剂与配合剂的比提高到大于10的值明显降低了铜的除去速率,如表4所示。另外,表4的数据还表明:为铜的不良配合剂的乙酸显著抑制了铜的除去速率,而钽的除去速率实质上不受影响。
Claims (29)
1.一种用于选择性地抛光含铜及钽、氮化钽或其混合物基材中的铜的化学机械抛光浆料前体,包括:
至少一种磨料;
至少一种选自长链烷基胺、醇胺及其混合物的有机氨化合物;和
至少一种配合剂,其中该浆料具有4.0至8.0的pH;
其中该配合剂选自乙酸、柠檬酸、乳酸、丙二酸、酒石酸、琥珀酸、乙二酸、氨基酸、其盐、和其混合物。
2.权利要求1的化学机械抛光浆料前体,包括成膜剂。
3.权利要求1的化学机械抛光浆料前体,其中该配合剂为酒石酸。
4.权利要求3的化学机械抛光浆料前体,其中酒石酸的量为0.5-5.0%重量。
5.权利要求2至4中任一项的化学机械抛光浆料前体,其中该成膜剂为苯并***。
6.权利要求5的化学机械抛光浆料前体,包括0.01-0.2%重量的苯并***。
7.权利要求1的化学机械抛光浆料前体,包括0.005-10.0%重量的至少一种有机氨化合物。
8.一种用于选择性地抛光含铜及钽、氮化钽或其混合物基材中的铜的化学机械抛光浆料,包括:
至少一种磨料;
至少一种氧化剂;
至少一种选自长链烷基胺、醇胺和其混合物的有机氨化合物;和
至少一种配合剂,其中该浆料具有4.0至8.0的pH;
其中该氧化剂选自含至少一个过氧基团的化合物或含一种处于其最高氧化态的元素的化合物;
该配合剂选自乙酸、柠檬酸、乳酸、丙二酸、酒石酸、琥珀酸、乙二酸、氨基酸、其盐、和其混合物。
9.权利要求8的化学机械抛光浆料,包括成膜剂。
10.权利要求8至9中任一项的化学机械抛光浆料,其中该配合剂为酒石酸。
11.权利要求10的化学机械抛光浆料,其中酒石酸的量为0.5-5.0%重量。
12.权利要求8或9的化学机械抛光浆料,其中该成膜剂为苯并***。
13.权利要求12的化学机械抛光浆料体,包括0.01-0.2%重量的苯并***。
14.权利要求8至13中任一项的化学机械抛光浆料,包括0.005-10.0%重量的至少一种有机氨化合物。
15.权利要求8至14中任一项的化学机械抛光浆料,其中该磨料为至少一种金属氧化物。
16.权利要求15的化学机械抛光浆料,其中其中金属氧化物磨料选自氧化铝、氧化铈、氧化锗、氧化硅、氧化钛、氧化锆及其混合物。
17.权利要求8至14中任一项的化学机械抛光浆料,其中磨料为金属氧化物的水分散体。
18.权利要求17的化学机械抛光浆料,其中金属氧化物磨料由尺寸分布低于1000nm和平均聚集体直径低于400nm的金属氧化物聚集体组成。
19.权利要求15的化学机械抛光浆料,其中金属氧化物磨料由具有初始粒径低于400nm和表面积10m2/g至250m2/g的分离的各金属氧化物球组成。
20.权利要求8至14中任一项的化学机械抛光浆料,其中金属氧化物磨料选自沉淀磨料或煅制磨料。
21.权利要求8至14中任一项的化学机械抛光浆料,其中该磨料为氧化铝的水分散体。
22.权利要求8至21中任一项的化学机械抛光浆料,其中该氧化剂选自过氧化氢、过氧化氢脲、脲和其组合。
23.权利要求8至22中任一项的化学机械抛光浆料,其中该浆料的Cu∶Ta抛光选择性比至少为40。
24.一种用于选择性地抛光含铜及钽、氮化钽或其混合物基材中的铜的化学机械抛光浆料,包括:
氧化铝;
至少一种氧化剂;
酒石酸;
苯并***;和
至少一种选自长链烷基胺、醇胺和其混合物的有机氨化合物;
其中该氧化剂选自含至少一个过氧基团的化合物或含一种处于其最高氧化态的元素的化合物。
25.权利要求24的化学机械抛光浆料,其中该有机氨化合物是十二烷基胺。
26.权利要求24的化学机械抛光浆料,其中该有机氨化合物是三乙醇胺。
27.权利要求24至26中任一项的化学机械抛光浆料,其中该氧化剂选自过氧化氢、过氧化氢脲、脲和其组合。
28.一种用于选择性地抛光含铜及钽、氮化钽或其混合物基材中的铜的化学机械抛光浆料,包括:
0.5-15%重量的氧化铝;
0.5-5%重量的酒石酸;
0.01-0.2%重量的苯并***;
0.005-10.0%重量的选自十二烷基胺、三乙醇胺和其混合物的有机氨化合物;和
包括1-20%重量脲和1-12.0%重量过氧化氢的混合物的氧化剂,其中该化学机械抛光浆料的pH为4-8,Cu∶Ta抛光选择性比至少大于10。
29.权利要求28的化学机械抛光浆料,包括至少一种表面活性剂。
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-
1998
- 1998-06-26 US US09/105,555 patent/US6063306A/en not_active Expired - Lifetime
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1999
- 1999-06-25 KR KR10-2000-7014741A patent/KR100491060B1/ko not_active IP Right Cessation
- 1999-06-25 EP EP99930777A patent/EP1098948B1/en not_active Expired - Lifetime
- 1999-06-25 CN CNB998095605A patent/CN1158373C/zh not_active Expired - Lifetime
- 1999-06-25 WO PCT/US1999/014557 patent/WO2000000567A1/en active IP Right Grant
- 1999-06-25 DE DE69928537T patent/DE69928537T2/de not_active Expired - Lifetime
- 1999-06-25 JP JP2000557321A patent/JP4261058B2/ja not_active Expired - Fee Related
- 1999-06-25 ID IDW20010176A patent/ID28618A/id unknown
- 1999-06-25 CA CA002335033A patent/CA2335033A1/en not_active Abandoned
- 1999-06-25 MY MYPI99002651A patent/MY116324A/en unknown
- 1999-06-25 IL IL14030399A patent/IL140303A0/xx unknown
- 1999-06-25 AU AU47235/99A patent/AU4723599A/en not_active Abandoned
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IL140303A0 (en) | 2002-02-10 |
EP1098948A1 (en) | 2001-05-16 |
CN1312845A (zh) | 2001-09-12 |
DE69928537D1 (de) | 2005-12-29 |
AU4723599A (en) | 2000-01-17 |
US6063306A (en) | 2000-05-16 |
ID28618A (id) | 2001-06-21 |
MY116324A (en) | 2003-12-31 |
KR100491060B1 (ko) | 2005-05-24 |
JP4261058B2 (ja) | 2009-04-30 |
WO2000000567A1 (en) | 2000-01-06 |
KR20010053166A (ko) | 2001-06-25 |
EP1098948B1 (en) | 2005-11-23 |
JP2002519475A (ja) | 2002-07-02 |
DE69928537T2 (de) | 2006-03-30 |
TWI245788B (en) | 2005-12-21 |
CA2335033A1 (en) | 2000-01-06 |
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