CN111566196A - 用于降低磨料颗粒与清洁刷之间的相互作用的组合物和方法 - Google Patents
用于降低磨料颗粒与清洁刷之间的相互作用的组合物和方法 Download PDFInfo
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- CN111566196A CN111566196A CN201880085765.6A CN201880085765A CN111566196A CN 111566196 A CN111566196 A CN 111566196A CN 201880085765 A CN201880085765 A CN 201880085765A CN 111566196 A CN111566196 A CN 111566196A
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C—CHEMISTRY; METALLURGY
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- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C11D3/3765—(Co)polymerised carboxylic acids, -anhydrides, -esters in solid and liquid compositions in liquid compositions
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C11D7/04—Water-soluble compounds
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Abstract
描述从聚合物表面,如从化学机械处理后清洁步骤中所使用的清洁刷的聚合物表面去除磨料颗粒的方法;以及相关的清洁溶液。
Description
技术领域
本发明涉及从聚合物表面,如从化学机械处理后清洁步骤中所使用的清洁刷的聚合物表面去除磨料颗粒的方法。
背景技术
在与微电子装置的生产(制造)有关的技术领域中,所述微电子装置包括集成电路、光学装置、内存装置、磁电组件以及用于电子、内存、光学和类似应用中的其它微装置或微装置组件,微电子装置通过包括从衬底表面精确去除材料的步骤来制备。用于制备某些装置的方法可以包括在衬底表面沉积和选择性地去除不同材料的一系列步骤。在处理期间所应用的材料可为导电材料,如金属、半导体材料,如硅基材料(例如氧化硅)、介电层或聚合物材料等。所述材料可在表面处以在衬底上构建微电子结构层的方式来选择性地涂覆和选择性地去除。可通过选择性化学手段、研磨手段或这些手段的组合来去除材料。
在制备这些装置中,通常使用通过研磨手段来平坦化、平整化或抛光衬底表面的处理步骤。在选择性地在表面处涂覆和去除材料的步骤之间,对表面进行处理,以提供高度精细化(例如平整化、平坦化或抛光)的光洁度。用于所述处理的标准技术为化学机械处理(chemical-mechanical processing,CMP)。在化学机械处理中,使衬底表面与磨料浆液和CMP垫接触,所述垫与表面之间有相对移动。所述浆液含有液体载体(水或有机溶剂)、溶解的化学物质(即有机化学材料)及分散的磨料颗粒。(表面通常将包括粒状副产物,如各种类型的金属氧化物,其从先前的处理步骤中出现。)浆液成分的组合以及垫与衬底表面之间的移动可有效地从衬底表面去除材料,并提供经平坦化或抛光的表面以供进一步处理。
在CMP步骤之后,为浆液的一部分的各种材料,以及已经从衬底表面去除的材料,以化学物质或研磨残余物的形式残留在衬底表面处。化学残余物可为CMP处理后存在于衬底表面处的残余化学成分,并且其为最初存在于CMP浆液中的化学材料或其衍生物(例如反应产物)。磨料颗粒残余物是指最初存在于CMP浆液中并且在CMP步骤结束时残留在衬底表面处的磨料颗粒。其它类型的残余物可为磨料颗粒和化学残余物的组合,如聚结、凝结或沉淀的有机和磨料颗粒材料。
在处理微电子装置期间,例如,在CMP步骤之后或之间,作出了大量努力,以从衬底表面去除残余物。具体地说,必须从衬底表面去除呈残余磨料颗粒形式的残余物,因为残余磨料颗粒会导致表面缺陷如刮痕,以及呈嵌入颗粒形式的装置缺陷,所述缺陷可能对衬底的下游处理或下游产物的质量产生负面影响。去除包括残余磨料颗粒的残余物的方法包括有时被称作“CMP后清洁”技术、方法或步骤的清洁技术。这些方法涉及使用涂覆于包括残余物的衬底表面的清洁溶液,以及通过移动式聚合物刷的接触,以从表面以化学和机械方式去除残余物。
市面上可购得多种CMP后清洁装备和清洁溶液。示例设备包括含有移动刷的清洁室以及在所述清洁室内将清洁溶液分配于衬底表面上并提供衬底与刷之间的运动和接触的***。通常可以加热所述室以便于清洁。在使用中,将清洁溶液涂覆于衬底表面,并使表面与移动刷接触,以去除残余物。尽管这些类型的设备和方法的实例为已知的、为商业适用的并能够对各种衬底进行高效和有效的CMP后清洁,但始终需要对现有技术进行改进,并开发新的甚至更有效的清洁溶液和清洁方法,以从CMP衬底表面去除残余物。
发明内容
本发明涉及适用于从聚合物表面,如从化学机械处理后清洁步骤中所使用的清洁刷的聚合物表面去除磨料颗粒的方法和组合物,以及相关的清洁溶液。本申请人已确定磨料颗粒,尤其是在颗粒的表面具有氢键合基团、在CMP后清洁步骤中所使用的清洁溶液中的正电荷(正ζ电位(ζ电位))或这两者的磨料颗粒,在CMP后清洁步骤期间可被存在于清洁刷的聚合物表面处的氢键合基团所吸引。
在处理微电子期间衬底期间,在CMP后清洁步骤之前,微电子装置衬底在其表面处可能具有残余物,如残余磨料颗粒。在CMP后清洁步骤期间,那些磨料颗粒从衬底表面去除(至少大部分),并变为分散于用于CMP后清洁步骤的清洁溶液中。在清洁溶液中,尤其在低pH(例如低于6或7)的条件下时,分散的磨料颗粒可以呈现正电荷,即正ζ电位。磨料颗粒的表面还可包括氢键合基团,如(-OH)基团,例如在硅石颗粒的情况下的硅烷醇(-SiOH)基团。其上具有氢键合基团的带正电颗粒的表面被静电吸引到CMP后清洁步骤中所使用的聚合物刷的表面处,并且可与存在于所述处的氢键合基团形成氢键。磨料颗粒可被吸引到聚合物刷的表面处并且可在所述处积聚,并且特别是在存在pH较低的清洁溶液的情况下,可通过氢键合维持与表面的吸引力。在CMP后清洁步骤期间,在清洁刷表面处存在及积聚磨料颗粒的一种潜在结果可能为在CMP后清洁步骤之后出现刷痕。
如本文中所用,“氢键合基团”,例如作为颗粒去除剂、刷子的聚合物表面或磨料颗粒的特征,为能够与另一氢键合基团相互作用以形成氢键的极性化合物或极性基团。实例包括基团,其包括与高负电性原子如氮(N)、氧(O)、硫(S)或氟(F)共价键结的氢(H)原子。某些特定的氢键合基团包括:羧酸基、氨基、醇基、膦基、磷酸酯基、膦酸酯基、烷醇胺基、碳酰胺基、脲基、氨基甲酸酯基、酯基、甜菜碱基团、硅烷醇基或含硫基团。
根据目前所描述的清洁溶液和其使用方法,清洁溶液包括溶解的化学成分,称作颗粒去除剂,其有效地在CMP后清洁步骤期间,防止清洁浆液中带正电的磨料颗粒与聚合物刷表面之间形成氢键;在CMP后清洁步骤期间抑制或减少在所述磨料颗粒与聚合物刷表面之间形成氢键;或去除被吸引到聚合物刷的表面并已与所述表面形成氢键的所述磨料颗粒(在CMP后清洁步骤期间,抑或在不存在衬底的情况下,在清洁刷子的单独步骤中)。
在一个方面,本发明涉及一种从化学机械处理后(CMP后)清洁刷中去除磨料颗粒的方法。所述方法包括:提供具有聚合物表面并在所述聚合物表面处具有磨料颗粒残余物的CMP后清洁刷;并提供pH低于7的清洁溶液。清洁溶液含有:清洁剂,和颗粒去除剂。所述方法还包括通过使聚合物表面与清洁溶液接触来从聚合物表面去除磨料颗粒残余物。
在另一方面,本发明涉及一种衬底的化学机械处理后(CMP后)清洁的方法。所述方法包括:提供具有聚合物表面的CMP后清洁刷;并提供清洁溶液,其包括:清洁剂,和颗粒去除剂。所述方法还包括提供包括表面的衬底,其中在衬底表面处具有残余物,所述残余物包括磨料颗粒;并通过将衬底表面和聚合物表面暴露于清洁溶液,同时使衬底表面与聚合物表面接触并且同时使衬底表面相对于聚合物表面移动,从衬底表面去除残余物。
在另一方面,本发明涉及一种适用于在化学机械处理后步骤中清洁衬底的清洁溶液浓缩物。所述清洁溶液浓缩物包括清洁剂,及包括氢键合基团的至少0.1重量%的颗粒去除剂。
附图说明
图1示出用特定发现的方法及材料清洁的晶片的性能数据。
图2示出所提出的刷印形成机制。
图3示出在如所描述的表面处具有硅石的刷子的FTIR谱图数据。
图4示出在不同清洁材料的情况下,在表面处具有硅石的刷子的FTIR谱图数据。
图5及6示出由使用如所描述的各种清洁溶液所导出的数据。
具体实施方式
在不同方面,本说明书涉及:从在CMP后清洁步骤中所使用的清洁刷的表面去除磨料颗粒的方法(所述方法被并入CMP后清洁处理中,或为从刷子中去除磨料颗粒的单独方法或步骤);防止在CMP后清洁处理中在清洁刷的表面上积聚磨料颗粒,以从衬底表面去除残余物的方法;并涉及在这些方法中有效的清洁溶液,其中清洁溶液含有颗粒去除剂。
在化学机械处理,即CMP或“CMP处理”期间,通过控制从表面去除少量材料,对衬底进行处理以使其平坦化或抛光衬底的表面。微电子装置衬底,即简称为“衬底”,可为任何类型的微电子装置或其前体,意指为或含有以下中的任一种的装置或前体:集成电路、光学装置、固态内存装置、硬盘内存装置、磁电组件或另一类型的微装置或微装置组件,其适用于电子、内存、光学或类似应用并且其通过包括以下步骤中的一个或多个的制造过程来制备:对衬底的表面进行化学机械处理,其常常具有多个在衬底表面处沉积及选择性地去除材料组合的步骤。
用于如所描述的方法中的衬底可包括在表面处的为工艺内微电子装置的一部分的任何材料或材料组合,其包括:半导体材料(例如硅)、陶瓷(例如碳化硅、氮化硅)、玻璃材料、导电材料(例如金属和金属合金)、电绝缘(介电质)材料、隔绝材料等。导电材料可为包括铜、钨、银、铝和钴的金属或金属合金,以及其它金属及其合金。电绝缘介电材料可为各种目前已知的或待开发的绝缘、低k或超低k介电材料中的任一种,仅列举几个实例,其包括各种形式的掺杂或多孔二氧化硅、热氧化物、TEOS。可以隔绝层形式存在的衬底材料的实例包括:钽、氮化钽、氮化钛、钴、镍、锰、钌、氮化钌、碳化钌或氮化钌钨。
CMP处理涉及将浆液涂覆于衬底表面,并使浆液及衬底与垫(即“CMP垫”或“CMP抛光垫”)接触,垫与表面之间具有移动。浆液含有经设计以使得从衬底表面摩擦(机械)去除材料的磨料颗粒。浆液通常还将含有溶解于其中的各种化学成分,其可有效地控制(提高或降低)从衬底表面去除某些材料的速率;以提供所需的去除不同材料的选择性;以在CMP步骤期间和之后减少衬底表面处缺陷的存在及残余物的量;或以其它方式促进与CMP处理的效率或在CMP处理结束时衬底的质量相关的改进或期望的结果。
示例浆液(“CMP浆液”)包括液体载体,其大部分为化学材料和磨料颗粒溶解或分散在其中的水(优选为去离子水)。可选择浆液的化学材料,以达到所需去除率、去除的选择性及成品衬底表面的最终表面形貌(例如光滑度、波纹度等)。特定浆液中化学材料的具体类型和量取决于各种因素,如存在于衬底表面处的材料的一种或多种类型、CMP加工条件、CMP步骤中所使用的CMP垫的类型、浆液的磨料颗粒的一种或多种类型等。示例化学成分包括化学材料,如可充当溶剂、表面活性剂、催化剂、稳定剂、氧化剂(oxidizer)、有机抑制剂(以控制去除率)、螯合剂等等的材料。其它可能的化学材料包括pH调节剂(碱、酸)、腐蚀抑制剂及杀生物剂(作为防腐剂)。
磨料颗粒可具有大小和组成特征,以实现从衬底表面高效、任选地选择性并且均匀地去除特定材料。示例磨料颗粒可由氧化铝、铈氧、二氧化铈、锆、氧化锆、硅石(各种形式)、二氧化钛、二氧化锆、金刚石、碳化硅或其它金属、陶瓷或金属氧化物材料制成或含有所述材料。各种大小、大小分布、颗粒形状和其它物理或机械性质的这些类型的磨料颗粒均为可用的,并且可以选择供与各种衬底或CMP处理一起使用。浆液中磨料颗粒的量还可基于与所处理的衬底的类型及CMP处理的特征有关的类似因素来选择。
为了用于处理不同类型的衬底,当颗粒分散于CMP浆液中时,可选择磨料颗粒以呈现可为正电荷或负电荷的静电电荷。分散的磨料颗粒的电荷强度通常被称作颗粒的“ζ电位”(或动电位),其是指围绕颗粒的离子的电荷与浆液的主体液体的电荷(例如液体载体和溶解于其中的任何其它组分)之间的电位差。分散的颗粒的ζ电位通常取决于颗粒分散在其内的液体介质的pH。对于给定的浆液或其它液体介质,带电磨料颗粒的ζ电位在其下为零的pH被称作等电点。当含有分散的磨料颗粒的溶液的pH在远离等电点处增加或减小时,表面电荷(并且因此ζ电位)相应地减少或增加(至更高的负或更高的正ζ电位值)。
在CMP处理步骤期间,浆液中存在各种材料,其包括浆液的溶解和分散(例如悬浮)成分,以及在CMP处理期间,如通过从衬底表面去除所产生的其它溶解或分散的材料。另外存在的材料可为这些材料中任一者的衍生物、反应产物、聚结物、凝结物和沉淀物。在CMP处理步骤期间存在于浆液中的任何所述材料均可能成为在CMP处理步骤结束时残留在衬底表面处的残余物。因此,在CMP步骤之后衬底表面处的残余物可包括:最初存在于CMP浆液中的溶解的化学材料或固体磨料颗粒;在处理期间从衬底表面去除的材料(例如金属离子)或在处理期间通过浆液的化学材料的反应或化学改质(例如氧化或还原)所产生的材料;或这些的组合,包括沉淀物、聚结物及凝结物。
众所周知,在CMP处理步骤之后,各种CMP后清洁步骤适用于去除存在于微电子装置表面上的残余物。这些清洁步骤可以涉及并且通常确实涉及使用专门的CMP后清洁装备,所述装备可以包括清洁设备,其包括其中清洁溶液被输送到衬底表面的清洁室,以及将移动式聚合物刷施加于表面以机械地从衬底表面去除残余物。可以基于如衬底类型、刷子类型、表面处的残余物类型和量、清洁溶液类型等的因素来选择条件和清洁时间(意指衬底表面暴露于移动刷和清洁溶液的时间量)。
涉及使用聚合物刷的各种CMP后清洁工具为已知的并且可市面上购得。这些设备通常包括清洁室,所述清洁室包括可移动的清洁刷(通常为多个清洁刷);清洁溶液源;热源;和***、机构、装置,包括适于在有效地使得从表面机械去除残余物的条件(时间和温度)下将清洁溶液与衬底、清洁溶液及移动刷接触的控制***。出售此类装备的公司尤其包括:英特格公司(Entegris,Inc.);AION;狮柏技术公司(Ceiba Technologies,Inc.);瑞皮公司(Rippey Corp.);应用材料公司(Applied Materials);荏原(Ebarra)。
用于根据本说明书的CMP后清洁设备及方法的聚合物清洁刷包括含有氢键合基团(例如连接于聚合物主链的羟基(-OH))的聚合物表面。包括聚合物表面并且适用于CMP后清洁处理的清洁刷为熟知的。含有羟基连接于聚合物主链的聚合物表面的清洁刷的实例包括由聚合物制成的刷子,所述聚合物至少部分地衍生自乙烯醇,即为乙烯醇的均聚物抑或共聚物的聚合物,此类聚合物(共聚物及均聚物)通常称作聚乙烯醇(也称为“PVOH”或“PVA”)。
在美国专利申请20013/0048018中描述了用于CMP后清洁步骤的清洁刷的实例,所述申请以全文引用的方式并入本文中。如其中所描述,清洁刷可通过使用聚乙烯醇作为起始材料,然后可对其进行处理以形成聚乙烯缩醛弹性材料来制备。可以用醛例如甲醛处理聚乙烯醇起始材料以产生聚乙烯醇刷材料。其它聚合物,代替聚乙烯醇抑或除了聚乙烯醇之外,均适用作刷子的聚合物材料并可包括氢键合基团。所述其它聚合物的实例包括聚合物及共聚物尼龙、聚氨酯及这些的组合,其可形成适合于在商业化CMP后清洁处理中,如本文中所描述从衬底清洁掉残余物的清洁刷。
示例刷子包括圆柱形聚合物(如所描述)泡沫刷,其具有第一端及第二端,及具有多个从刷子的底部表面延伸的结节的外表面。结节沿着刷子的长度位于第一与第二端之间,并通过间隙或开口而彼此分隔。结节可具有任何形状并通常包括圆形顶面及从刷子底部延伸到结节顶面的表面高度。当刷子绕着在第一与第二端之间延伸的轴线旋转时,刷子的外圆柱形表面旋转,表面上的结节也旋转。可以使具有涂覆于其上的清洁溶液的衬底表面与刷子的移动表面及刷子结节接触,以使结节与表面接触,以便于从表面去除残余物。
清洁处理的时间及条件应有效地以高效的方式从衬底表面去除大部分的残留物总量(例如,如通过磨料颗粒残余物所测量)。例如,通过使用典型的CMP后清洁设备及方法,可使清洁溶液与衬底表面接触,并且所述表面将与聚合物刷接触(在衬底表面与刷子之间具有移动)达足以在清洁步骤之前去除存在于表面处的高百分比残余物(例如磨料颗粒残余物)的时间。期望地,适用的CMP后清洁步骤可引起在去除残余物之前去除至少85%存在于衬底表面上的残余物(例如磨料颗粒残余物),更优选为至少90%、甚至更优选为至少95%并且最优选为至少99%。适用于测量残留在衬底表面处的残余物(例如颗粒残余物)的量的方法及装备为熟知的并可市面上购得。
为了达到残余物去除水平,在约20摄氏度至约90摄氏度,优选为约20至约50摄氏度的范围内的温度下,清洁设备对衬底的示例清洁时间可在约1秒至约20分钟,优选约5秒至10分钟的范围内,例如,在约15秒至约5分钟的范围内。在这些时间及温度范围内的处理时间为说明性的,并且如果可有效地从衬底表面至少部分地清洁CMP后残余物,那么可使用任何其它合适的时间及温度条件。
根据本发明,本申请人现在已明确地确认磨料颗粒,尤其是在颗粒的表面处具有氢键合基团、在CMP后清洁步骤中所使用的清洁溶液中的正电荷(正ζ电位)或这两者的磨料颗粒,在CMP后清洁步骤期间可被存在于清洁刷的聚合物表面处的氢键合基团所吸引。
在CMP后清洁步骤之前,微电子装置衬底在其表面处可以具有磨料颗粒残余物。在清洁步骤期间,那些磨料颗粒从衬底表面去除(至少大部分地),并变为分散于用于CMP后清洁步骤的清洁溶液中。在清洁溶液中,尤其在低pH(例如低于6或7)的条件下时,分散的磨料颗粒可以呈现正电荷,即正ζ电位。磨料颗粒的表面还可包括氢键合基团,如(-OH)基团,例如在硅石颗粒的情况下的硅烷醇(-SiOH)基团。其上具有氢键合基团的带正电颗粒的表面被静电吸引到CMP后清洁步骤中所使用的聚合物刷的表面处,并且可与存在于所述处的氢键合基团形成氢键。磨料颗粒可被吸引到聚合物刷的表面处并且可在所述处积聚,并且特别是在存在pH较低的清洁溶液的情况下,可通过氢键合维持与表面的吸引力。
在CMP后清洁步骤期间,在清洁刷表面处存在及积聚磨料颗粒的一种潜在结果可能为在CMP后清洁步骤之后出现刷痕。刷痕(或“刷印”)为CMP后清洁步骤之后存在于衬底表面上的残余磨料颗粒的可见图案。所述图案可包括与用于清洁衬底表面的清洁刷的表面形状或特征,如清洁刷结节的圆形表面相匹配的形状或特征(例如尺寸)。由残余磨料颗粒所形成的刷痕图案的实例包括与结节的形状及大小相匹配的圆形痕迹,以及为由残余磨料颗粒形成的明显线条的线图案,其中线条的长度对应于圆形刷结节的直径。刷痕可由在CMP后清洁步骤之后残留在衬底上的磨料颗粒(即磨料颗粒残余物)的图案构成并由其形成。本说明书的优选CMP后清洁过程可引起在CMP后清洁步骤之后,衬底表面上的刷痕减少或达到最少,或优选为不存在。
根据本发明的示例方法,CMP后清洁步骤涉及包括具有含有氢键合基团的聚合物表面的擦洗刷的设备。另外,清洁步骤中所使用的清洁溶液可具有低pH,如低于约7,例如在约1至约5或6、或约1或2至约3、3.5或4的范围内。这些因素会引起在CMP后清洁步骤期间清洁溶液中存在带正电的磨料颗粒(具有氢键合基团),其中带正电的磨料颗粒会被刷子表面处的氢键合基团吸引,从而引起带正电的磨料颗粒通过氢键合被吸引到聚合物刷表面。
根据申请人的新颖及本发明清洁溶液及其使用方法,清洁溶液包括溶解的化学成分,称作颗粒去除剂,其有效地:在CMP后清洁步骤期间,防止清洁浆液中带正电的磨料颗粒与聚合物刷表面之间形成氢键;在CMP后清洁步骤期间抑制或减少在所述磨料颗粒与聚合物刷表面之间形成氢键;或去除被吸引到聚合物刷的表面并已与所述表面形成氢键的所述磨料颗粒(在CMP后清洁步骤期间,抑或在不存在衬底的情况下,在清洁刷子的单独步骤中)。
因此,本说明书的清洁溶液包括溶液或处于溶液形式,所述溶液包括含有经溶解成分的水性介质(优选为去离子水),所述经溶解成分包括:颗粒去除剂、任选的一种或多种充当清洁剂的成分(例如螯合剂、有机溶剂);以及任选地,少量或微量其它任选的佐剂,如酸、表面活性剂、杀生物剂等。
颗粒去去除剂为化学化合物(包括寡聚物或聚合物),其包括至少一个氢键合基团,并且当存在于如所描述的清洁溶液中,并且在存在带正电的磨料颗粒及清洁刷的聚合物表面时,所述化学化合物可以有效地与:聚合物刷表面的氢键合基团、带正电的磨料颗粒的氢键合基团或这两者结合,其方式及程度使颗粒去除剂将减少存在于清洁刷表面并通过氢键合吸引到清洁刷表面的磨料颗粒的量。
在含有例如在低pH下带正电的分散的磨料颗粒(以残余物形式带到衬底表面上)的清洁溶液中,颗粒去除剂可以抑制或防止带正电的颗粒被存在于聚合物清洁刷表面处的氢键合基团所吸引的方式与带正电的颗粒的氢键合基团结合。另外,在存在包括氢键合基团的清洁刷的情况下,并且在低pH下,颗粒去除剂还可以抑制或防止清洁刷吸引存在于清洁溶液中的带正电的磨料颗粒的方式,与存在于清洁刷表面处的氢键合基团相关联。更一般化地考虑,颗粒去除剂可以防止或破坏包括氢键合基团的带正电磨料颗粒与含有氢键合基团的清洁刷的聚合物表面之间的氢键。颗粒去除剂与清洁刷表面,及颗粒去除剂与均存在于清洁溶液中(例如在CMP后清洁步骤期间)的带正电的磨料颗粒之间的这些效应及相互作用(单独或呈组合形式),有效地减少清洁刷表面的氢键合基团与带正电的磨料颗粒的氢键合基团之间的相互作用量。结果可为,较少的磨料颗粒将存在于清洁刷表面处,并通过氢键合与表面结合。
因此,本发明的清洁溶液包括一定量的颗粒去除剂,当在存在所述磨料颗粒的情况下并且在低pH下清洁溶液暴露于清洁刷时,所述量及类型可有效地减少存在于清洁刷的聚合物表面的带正电的磨料颗粒的量(例如浓度)。
可适用作如所描述的颗粒去除剂的成分的实例包括有机化合物、聚合物、寡聚物等,其含有一个或多个氢键合基团(当存在于清洁溶液中并且在低pH下时),并且其可以包括于清洁溶液中以有效地减少在如所描述的聚合物清洁刷的表面处带正电的磨料颗粒的存在。示例化合物通常包括含氮化合物;氨基酸;含单、二或多羧酸盐的群组;醇(例如多元醇);酸等等。
颗粒去除剂的一些具体实例包括非离性、阴离子、阳离子及两性离子小分子,及在中性pH下可表现为聚电解质的聚合物。阴离子聚合物或阴离子聚电解质可为天然、经改质的天然聚合物或合成聚合物。可包括于如所描述的清洁溶液中的示例性天然及经改质的天然阴离子聚合物包含但不限于:褐藻酸(或盐)、羧甲基纤维素、硫酸葡聚糖、聚(半乳糖醛酸)及其盐。示例性合成阴离子聚电解质包含但不限于:(甲基)丙烯酸(或盐)的均聚物或共聚物、聚(丙烯酸)、顺丁烯二酸(或酸酐)、苯乙烯磺酸(或盐)、乙烯基磺酸(或盐)、烯丙基磺酸(或盐)、丙烯酰氨基丙基磺酸(或盐)等,其中羧酸及磺酸的盐优选经铵或烷基铵阳离子中和。聚电解质阴离子聚合物的优选阳离子为铵阳离子(NH4 +)、胆碱离子(cholinium)+N(CH3)3(CH2CH2OH)及+N(CH3)4。因此,优选的经合并的合成及天然聚电解质阴离子聚合物的实例为(甲基)丙烯酸的均聚物或共聚物、顺丁烯二酸(或酸酐)、苯乙烯磺酸、乙烯基磺酸、烯丙基磺酸、乙烯基膦酸、丙烯酰氨基丙基磺酸、褐藻酸、羧甲基纤维素、硫酸葡聚糖、聚(半乳糖醛酸)及其盐。
阳离子聚合物及阳离子聚电解质可为天然、经改质的天然聚合物或合成聚合物。示例性天然及经改质的天然阳离子聚合物包含但不限于:壳聚糖、阳离子淀粉、聚赖氨酸及其盐。示例性阳离子合成聚电解质包括但不限于:二烯丙基二甲基氯化铵(DADMAC)、二烯丙基二甲基溴化铵、二烯丙基二甲基硫酸铵、二烯丙基二甲基磷酸铵、二甲烯丙基二甲基氯化铵、二乙基丙烯基二甲基氯化铵、二烯丙基二(β-羟乙基)氯化铵、二烯丙基二(β-乙氧基乙基)氯化铵、二甲氨基乙基(甲基)丙烯酸酯酸加成盐及季盐、二乙氨基乙基(甲基)丙烯酸酯酸加成盐及季盐、7-氨基-3,7-二甲基辛基(甲基)丙烯酸酯酸加成盐及季盐、N,N'-二甲氨基丙基丙烯酰胺酸加成盐及季铵化盐的均聚物或共聚物,其中所述季盐包括烷基及苯甲基季铵化盐;烯丙胺;二烯丙胺;乙烯胺(通过乙烯基烷基酰胺聚合物的水解获得);乙烯基吡啶;壳聚糖;阳离子淀粉;聚赖氨酸及其盐。
其它实例包括2-吡咯烷酮、1-(2-羟乙基)-2-吡咯烷酮(HEP)、丙三醇、1,4-丁二醇、亚丁基砜(环丁砜)、二甲砜、乙二醇、丙二醇、二丙二醇、四乙二醇二甲醚、二乙二醇二甲醚、二醇醚(例如二乙二醇单甲醚、三乙二醇单甲醚、二乙二醇单***、三乙二醇单***、乙二醇单丙醚、乙二醇单丁醚、二乙二醇单丁醚(DEGBE)、三乙二醇单丁醚(TEGBE)、乙二醇单己醚(EGHE)、二乙二醇单己醚(DEGHE)、乙二醇苯基醚、丙二醇甲醚、二丙二醇甲醚(DPGME)、三丙二醇甲醚(TPGME)、二丙二醇二甲醚、二丙二醇***、丙二醇正丙醚、二丙二醇正丙醚(DPGPE)、三丙二醇正丙醚、丙二醇正丁醚(DOWANOLPnB)、二丙二醇正丁醚、三丙二醇正丁醚、丙二醇苯基醚(DOWANOL PPh))、正乙基吡咯烷酮、正甲基吡咯烷酮、二甲基甲酰胺、二甲亚砜、乙二醇单己醚、二乙二醇单己醚和其组合。替代地,或另外地,清洁添加剂可包括羟丙基纤维素;羟乙基纤维素;羟乙基甲基纤维素;羟丙基甲基纤维素;羧甲基纤维素;羧甲基纤维素钠(Na CMC);聚乙烯吡咯烷酮(PVP);使用N-乙烯吡咯烷酮单体、聚丙烯酸酯及聚丙烯酸酯的类似物制成的任何聚合物;聚氨基酸(例如聚丙氨酸、聚亮氨酸、聚甘氨酸);聚酰氨基羟基氨基甲酸酯;聚内酯;聚丙烯酰胺;三仙胶;壳聚糖;聚环氧乙烷;聚乙烯醇(PVA);聚乙酸乙烯酯;聚丙烯酸;聚乙亚胺(PEI);糖醇,如山梨糖醇、蔗糖、果糖、乳糖、半乳糖、麦芽糖、赤藻糖醇、麦芽糖醇、苏糖醇、阿糖醇(arabinol)、核糖醇、甘露醇、半乳糖醇、肌醇及木糖醇;去水山梨糖醇的酯;仲醇乙氧基化物,如TERGITOL;多功能醇,其包括季戊四醇、二季戊四醇(dipentaerythitol)、三羟甲基丙烷、二甲基丙酸及木糖酸;核碱基,如尿嘧啶、胞嘧啶、鸟嘌呤、胸嘧啶,及其组合。
再其它实例包括乳酸、顺丁烯二酸、脲、乙醇酸、山梨糖醇、硼砂(即硼酸钠)、脯氨酸、甜菜碱、甘氨酸、组氨酸、三(羟甲基)氨基甲烷(TRIS)、二甲亚砜、环丁砜、丙三醇、SDS(十二烷基硫酸钠)、十二烷基膦酸或其组合。在这些中,某些颗粒去除剂可优选用于微电子装置衬底的CMP后清洁步骤中,例如:顺丁烯二酸、硼砂(即硼酸钠)、二甲亚砜、丙三醇或其组合。
根据某些示例清洁溶液,以清洁溶液的总重量计,使用时(在CMP后清洁处理期间)清洁溶液中一种或多种颗粒去除剂的总量可为至少约0.01重量%,更优选为至少约0.02重量%,如至少0.05重量%。以清洁溶液的总重量计,示例量可为至多约1重量%、更优选为至多约0.3重量%,例如至多约0.2重量%的颗粒去除剂。
根据某些在稀释成使用点组合物之前呈浓缩形式的示例清洁溶液,清洁溶液浓缩物中一种或多种颗粒去除剂的总量以清洁溶液的总重量计可为至少约7%,如至少约10重量%,但以清洁溶液的总重量计不超过20重量%,优选不超过8重量%,例如不超过7重量%的颗粒去除剂。
除了颗粒去除剂之外,如所描述的清洁组合物可优选包括一种或多种其它溶解的化学成分,其例如在CMP后清洁步骤期间充当清洁剂以帮助从衬底表面去除残余物。一种或多种清洁剂可通过各种已知的清洁或隔离机制起作用,如通过溶解为有机材料的残余物、通过分散固体或粒状残余物、或通过其它方式与残余物相互作用或将其分离,所述残余物在CMP步骤之后存在于衬底表面处,或其存在于在CMP后清洁步骤期间用于清洁衬底的清洁溶液中。
已知用于CMP后清洁溶液及方法中的适用的有机溶剂的实例。示例溶剂尤其可为极性有机溶剂、醇、二醇及胺。非限制性实例包括较低分子量醇(如C1至C4烷基醇)、亚烷基二醇、乙醇胺(例如单乙醇胺)、N,N'-二甲基甲酰胺、二甲亚砜、N-甲基吡咯烷酮、N-乙基吡咯烷酮等。
有机胺的说明性实例包括具有通式NR1R2R3的种类,其中R1、R2及R3可彼此相同或不同,并且选自由以下组成的群组:氢、直链或分支链C1-C6烷基(例如甲基、乙基、丙基、丁基、戊基及己基)、直链或分支链C1-C6醇(例如甲醇、乙醇、丙醇、丁醇、戊醇及己醇)及具有式R4-O-R5的直链或分支链醚,其中R4及R5可彼此相同或不同,并且选自由如上所定义的C1-C6烷基组成的群组。当胺包括醚组分时,所述胺可视为烷氧基胺。最优选地,R1、R2及R3中的至少一个为直链或分支链C1-C6醇。实例包括但不限于烷醇胺,如烷醇胺,如氨基乙基乙醇胺、N-甲基氨基乙醇、氨基乙氧基乙醇、二甲基氨基乙氧基乙醇、二乙醇胺、N-甲基二乙醇胺、单乙醇胺、三乙醇胺、1-氨基-2-丙醇、3-氨基-1-丙醇、二异丙胺、异丙胺、2-氨基-1-丁醇、异丁醇胺、二异丙醇胺、三(羟甲基)氨基甲烷(TRIS)、三(羟乙基)氨基甲烷、其它C1-C8烷醇胺及其组合;胺,如三亚乙二胺、乙二胺、己二胺、二亚乙基三胺、三乙胺、三甲胺及其组合;二甘醇胺;吗啉;以及胺与烷醇胺的组合。优选地,有机胺包含单乙醇胺。
一般来说,有机溶剂可以有用的量包括于清洁溶液中,所述量可以本文中所描述的有机溶剂作为清洁剂的方式有效,例如通过溶解有机残余物。包括于给定的清洁溶液中的特定类型及量的有机溶剂可以基于包括以下的因素来选择:被清洁的衬底的类型、存在于衬底表面处的残余物的类型及量、清洁溶液中的其它成分,及CMP后清洁处理中所使用的条件(时间、温度等)。
根据某些示例清洁溶液,使用时(在CMP后清洁处理期间)清洁溶液中一种或多种有机溶剂的总量以清洁溶液的总重量计可低于约1重量%,更优选低于约0.33重量%,最优选不超过0.13重量%,例如,以清洁溶液的总重量计不超过0.067重量%,或不超过0.033重量%。优选地,如果存在,有机溶剂的量以清洁溶液的总重量计可为至少0.0003重量%,更优选为至少0.001重量%,例如,至少0.015或0.025重量%。
根据某些在稀释成使用点组合物之前呈浓缩形式的示例清洁溶液,清洁溶液浓缩物中一种或多种有机溶剂的总量以清洁溶液的总重量计可为不超过20重量%,更优选不超过10重量%,最优选不超过7重量%,例如,不超过2重量%,或不超过1重量%。优选地,如果存在,适用量以清洁溶液的总重量计可为至少0.005重量%,更优选为至少0.01重量%,如至少0.05重量%或至少0.2或0.35重量%。
清洁溶液可任选地含有至少一种螯合剂。一般来说,在CMP后清洁组合物中所使用的螯合剂为化合物,其通常与金属离子,通常为铁离子形成络合物分子,以使清洁溶液内的离子失活并防止通过所述离子的化学反应或活性。已知各种螯合剂用于CMP后清洁组合物中,并且可用于本说明书的清洁组合物及方法中。某些具体实例包括含酸的有机分子,尤其含羧酸的有机分子,如直链或分支链C1-C6羧酸化合物,其包括邻苯二甲酸、丁二酸、柠檬酸、酒石酸、苹果酸、葡糖酸、天冬氨酸或其组合,以及甘氨酸、氨基酸等。柠檬酸可为用于螯合铁离子(例如Fe+2、Fe+3)的优选螯合剂。糖醇如:***糖醇、赤藻糖醇、丙三醇、经氢化的淀粉水解产物(HSH)、异麦芽酮糖醇(isomalt)、乳糖醇、麦芽糖醇、甘露醇、山梨糖醇及木糖醇也为金属离子的优选螯合试剂。
本文中所涵盖的其它金属螯合试剂包括但不限于乙酸、丙酮肟、丙烯酸、己二酸、丙氨酸、精氨酸、天冬酰胺、天冬氨酸、甜菜碱、二甲基乙二肟、甲酸、反丁烯二酸、葡糖酸、谷氨酸、谷氨酰胺、戊二酸、甘油酸、丙三醇、乙醇酸、乙醛酸、组氨酸、亚氨基二乙酸、间苯二甲酸、衣康酸、乳酸、亮氨酸、赖氨酸、顺丁烯二酸、顺丁烯二酸酐、苹果酸、丙二酸、杏仁酸、2,4-戊二酮、苯乙酸、苯丙氨酸、邻苯二甲酸、脯氨酸、丙酸、邻苯二酚、焦蜜石酸(pyromellitic acid)、奎尼酸、丝氨酸、山梨糖醇、丁二酸、酒石酸、对苯二甲酸、偏苯三甲酸、均苯三甲酸(trimesic acid)、酪氨酸、缬氨酸、木糖醇、乙二胺、草酸、鞣酸、吡啶甲酸、1,3-环戊二酮、儿茶酚、五倍子酚、间苯二酚、氢醌、三聚氰酸、巴比妥酸、1,2-二甲基巴比妥酸、丙酮酸、丙硫醇、苯甲羟肟酸、四亚乙基五胺(TEPA)、4-(2-羟乙基)吗啉(HEM)、N-氨基乙基哌(N-AEP)、乙二胺四乙酸(EDTA)、1,2-环己二胺-N,N,N',N'-四乙酸(CDTA)、N-(羟乙基)-乙二胺四乙酸(HEdTA)、亚氨基二乙酸(IDA)、2-(羟乙基)亚氨基二乙酸(HIDA)、氮基三乙酸、氨基三(亚甲基磷酸)、羟基乙叉二膦酸(hydroxyethylidine diphosphonic acid)、乙二氨基四(亚甲基磷酸)、乙二氨基五(亚甲基磷酸)、硫脲、1,1,3,3-四甲基脲、脲、脲衍生物、甘氨酸、半胱氨酸、谷氨酸、异亮氨酸、甲硫氨酸、哌啶、N-(2-氨基乙基)哌啶、吡咯烷、苏氨酸、色氨酸、柳酸、二吡啶甲酸、对甲苯磺酸、5-磺基柳酸及其组合。
适用的螯合剂的其它实例包括衍生自单体的含羧酸基的寡聚物及聚合物,所述单体可以包括以下中的一个或多个:丙烯酸、甲基丙烯酸、顺丁烯二酸、丁二酸、天冬氨酸、2-丙烯酰氨基-2-甲基-1-丙磺酸、丙烯酰胺、膦酸甲基丙烯酰氨基丙基三甲基氯化铵、烯丙基卤化物或其组合。聚丙烯酸可为用于螯合氮化硅(silica nitride)(SiN)的优选螯合剂。再其它实例包括:丙烷-1,2,3-三羧酸、丁烷-1,2,3,4-四羧酸、戊烷-1,2,3,4,5-五羧酸、偏苯三甲酸、均苯三甲酸(trimesinic acid)、焦蜜石酸、苯六甲酸及这些的组合。
一般来说,螯合剂可以有用的量包括于清洁溶液中,所述量可以本文中针对螯合剂所描述的方式有效。包括于给定的清洁溶液中的特定类型及量的螯合剂可以基于包括以下的因素来选择:被清洁的衬底的类型、存在于衬底表面处的残余物的类型、清洁溶液中的其它成分,及CMP后清洁处理的条件。
根据某些示例清洁溶液,使用时(在CMP后清洁处理期间)清洁溶液中一种或多种螯合剂的总量可为至多约5重量%,如至多约2重量%,最优选为至多约1重量%。优选地,如果存在,量以清洁溶液的总重量计可为至少0.0005重量%,更优选为至少0.001重量%,如至少0.007重量%。
根据某些在稀释成使用点组合物之前呈浓缩形式的示例清洁溶液,清洁溶液浓缩物中一种或多种螯合剂的总量以清洁溶液的总重量计可为不超过20重量%,更优选不超过13重量%,最优选不超过10或7重量%,例如,不超过3重量%,或不超过1.5重量%。优选地,量以清洁溶液的总重量计可为至少0.008重量%,更优选为至少0.015重量%,如至少0.1重量%或至少0.3重量%。
清洁溶液可任选地含有其它成分或佐剂,以改进使用清洁溶液的CMP后清洁步骤的清洁效应或效率。任选地,例如,清洁溶液可以包括pH调节剂或缓冲***,以控制清洁溶液浓缩物或使用点组合物的pH。合适的pH调节剂的实例包括可有效降低pH的有机酸及无机酸,如硝酸、硫酸、磷酸、邻苯二甲酸、柠檬酸、己二酸、草酸、甲磺酸、盐酸、丙二酸、顺丁烯二酸等等。其它任选成分包括表面活性剂(任何类型)或杀生物剂。
根据本说明书,相对于以相同方式(使用同样的清洁设备、刷子、清洁溶液量、清洁时间、清洁温度等)、在相同衬底(具有相当的残余物)上进行的相当的清洁方法,除了所述相当的清洁方法的清洁溶液不含如本文中所描述的颗粒去除剂(包括其量),如所描述的并有含有如所描述的颗粒去除剂的清洁溶液的CMP后清洁方法,可适用于在CMP步骤之后清洁衬底,其优选并且有利地以引起CMP后清洁步骤结束时在衬底表面处存在刷痕的发生降低的方式进行。根据本说明书的CMP后衬底清洁方法的实施例,相对于在相同衬底(具有相同或相当的残余物)上进行、使用在其它方面相同但不含颗粒去除剂的清洁溶液的在其它方面相同的CMP后清洁方法,使用如所描述的包括颗粒去除剂(例如以如所描述的量)的清洁溶液,会引起CMP后清洁处理结束时在衬底表面上刷痕(尤其线性刷痕)的存在减少(例如,减少至少50%、75%、90%或95%或99%)。
也根据本说明书,相对于以相同方式(使用同样的清洁设备、刷子、清洁溶液量、清洁时间、清洁温度等)、在相同衬底(具有相当的残余物)上进行的相当的清洁方法,除了所述相当的清洁方法的清洁溶液不含颗粒去除剂(例如以如本文中所描述的量),如所描述的并有如所描述的清洁溶液的CMP后清洁方法,所述清洁溶液含有如所描述的颗粒去除剂(包括如所描述的量),会引起在清洁步骤期间或结束时存在于聚合物清洁刷表面处的磨料颗粒的量减少。根据本说明书的CMP后衬底清洁方法的实施例,相对于在相同衬底上进行、使用在其它方面相同但不含颗粒去除剂的清洁溶液的在其它方面相同的CMP后清洁方法,使用如所描述的清洁溶液,可以减少在CMP后清洁处理期间或结束时如所描述的存在于(例如通过氢键合被吸引)聚合物清洁刷表面的磨料颗粒的存在(例如,减少至少50%、75%、90%或95%或99%)。
示例清洁溶液适用于去除存在于衬底表面处的残余物,或减少清洁刷的聚合物表面处磨料颗粒的存在(即去除)或减少其积聚。在出于这些目的中的任一个来处理衬底或刷子中,清洁溶液并非预期的清洁溶液或用于(如本文中所描述)去除构成衬底表面层的材料。因此,如所描述的清洁溶液不需要并且优选地可不包括任何大量的适用并且具有从衬底表面去除材料的作用的化学材料或研磨材料,这些成分包括通常存在于经设计以用于CMP处理中以从衬底表面去除材料的CMP浆液中的类型的研磨颗粒、氧化剂、表面活性剂、催化剂等。
如所描述的清洁溶液(在用于如本文中所描述的方法之前,呈最初的形式)可不包括可存在于CMP处理步骤中的类型的磨料颗粒。这些为存在于供使用以在CMP处理步骤期间从衬底表面机械地去除材料的CMP浆液中的固体颗粒(例如纳米颗粒)。实例包括硅石颗粒、铈氧颗粒、氧化锆、氧化铝粒子,以及其它以固体(非溶解)形式存在于浆液中的金属及金属氧化物磨料颗粒等。本说明书的清洁溶液(在用于清洁步骤之前,呈最初的形式)可含有以清洁溶液的总重量计不超过1、0.1、0.01、0.001、0.0001重量%的固体磨料颗粒。这些量代表使用时的清洁溶液,及浓缩物组合物。
类似地,如所描述的优选清洁溶液不需要并且可任选地不包括通过与构成CMP衬底的表面层的材料或与浆液的另一种材料进行化学相互作用来起作用的化学材料,以便于从衬底表面有效地去除表面层材料。所述化学材料的实例包括表面活性剂、催化剂(例如金属离子催化剂,尤其铁离子催化剂),及氧化剂等等。以清洁溶液的总重量计,示例清洁溶液可含有不超过1、0.1、0.01、0.001或0.0001重量%的表面活性剂、催化剂或氧化剂中的任一种或其组合。这些量代表使用时的清洁溶液,及浓缩物组合物。
出于从如所描述的清洁溶液中排除催化剂、氧化剂及表面活性剂作为成分的目的,“表面活性剂”为降低两种液体之间或液体与固体之间表面张力(或界面张力)的有机化合物,通常为含有疏水性基团(例如烃(例如烷基)“尾部”)及亲水性基团的有机两亲媒性化合物。表面活性剂可具有任何HLB(亲水性亲脂性平衡(hydrophilic-lipophilicbalance))值,并且可带电、不带电等,许多各种各样的表面活性剂的实例在化学及CMP领域中为熟知的。
“催化剂”为尤其在存在氧化剂的情况下,可有效地向溶液(例如CMP浆液的液体载体)提供金属离子的材料,其能够在CMP衬底的表面层处存在金属材料,尤其在使用所述浆液的CMP处理步骤期间从衬底表面去除的金属材料的情况下可逆氧化及还原,并且其中催化剂的金属离子有助于去除。金属离子型催化剂的实例在CMP领域中为熟知的,并且可以向浆液提供金属离子,如铁、钴、铜、铕、锰、钨、钼、铼或铱的离子。所述铁离子催化剂的实例可溶于液体载体并且可包括铁(铁III)或亚铁(铁II)化合物,如硝酸铁、硫酸铁、卤化铁(包括氟化铁、氯化铁、溴化铁及碘化铁,以及过氯酸铁、过溴酸铁及过碘酸铁),及有机铁化合物,如乙酸铁、乙酰基丙酮酸铁、柠檬酸铁、葡糖酸铁、丙二酸铁、草酸铁、邻苯二甲酸铁及丁二酸铁及其混合物。
氧化剂(也称为氧化剂(oxidizing agent))为即或包括无机或有机过化合物的化合物。过化合物可以被理解为含有至少一个过氧基(-O-O-)的化合物,或含有最高氧化态元素的化合物。含有至少一个过氧基的化合物的实例包括过氧化氢及其加合物,如过氧化脲及过碳酸盐;有机过氧化物,如过氧化苯甲酰、过氧乙酸及二叔丁基过氧化物;单过氧硫酸盐(SO5 =);二过氧硫酸盐(S2O8 =)和过氧化钠。含有最高氧化态元素的化合物的实例包括过碘酸、过碘酸盐、过溴酸、过溴酸盐、过氯酸、过氯酸盐、过硼酸及过硼酸盐及高锰酸盐。用于CMP浆液的通常优选氧化剂为过氧化氢。
在使用时,可稀释如所描述的并且呈浓缩形式的清洁组合物,以形成供CMP后清洁步骤使用的清洁溶液。浓缩物可包括如所描述的化学成分,其量在稀释后将提供具有所需的每一成分浓度的使用点组合物。浓缩物的pH可低于使用组合物的pH,例如,浓缩物的pH可低于2.5或低于2。加入浓缩物中以形成使用组合物的水的量,即稀释率,可以视需要而定。示例浓缩物可以通过10、50、100或200的系数来稀释,例如,通过将一定体积的浓缩物与为所述浓缩物的体积10、50、100或200倍的体积的水合并。
根据用于使用如所描述的清洁溶液的方法的各种实例,微电子装置衬底可以例如使用CMP后清洁设备,在CMP后清洁步骤中进行清洁,以从衬底表面去除残余物,包括磨料颗粒残余物。所述衬底可为微电子装置衬底,一般来说为可以包括基底的平板晶片,其具有已选择性地沉积于所述衬底上并且选择性地从所述衬底去除以产生包括表面层的微电子特征层的材料。表面层可由所述沉积材料制成,所述沉积材料包括一种或多种金属(例如铜、钨、银、钴、镍等)、绝缘或介电材料(例如TEOS、氮化硅)及半导体材料。在构成衬底表面层的沉积材料的表面而非部分处,可能存在如所描述的残余物,包括在CMP步骤中所使用的磨料颗粒。
具有残余物的衬底的具体实例为CMP后微电子装置衬底,其在表面处含有金属特征(例如呈衬垫或互连(例如插塞)结构形式的钨、铜或钴),及一种或多种非金属材料,如介电材料或隔绝层(例如TEOS、氮化硅等等)。衬底在表面处含有残余物,如磨料颗粒。磨料颗粒可为任何适用的类型,例如氧化铝、硅石、铈氧、氧化锆或相关氧化物。磨料颗粒通常将为适用于处理特定类型的晶片及在所述晶片表面处的材料的类型。例如,包括钨特征及在表面处的介电材料的衬底可以通过包括硅石磨料颗粒的CMP步骤预先进行处理。
根据清洁步骤,使在表面处具有残余物的CMP衬底与聚合物清洁刷接触,并将如所描述的清洁溶液分配于清洁刷及衬底表面上。在所需的压力量下,提供刷子与衬底表面之间的相对运动。CMP后清洁步骤可有效减少在CMP步骤后存在于衬底表面处的残余物,包括磨料颗粒的量。
实例
表1中列出说明本文中所描述的本发明的概念的实例,以及比较实例:
表1
PETEOS晶片用基于胶质硅石的CMP浆液在IC 1010垫上进行抛光,并用5种具有不同pH的调配物进行清洁:对照物,pH 6;清洁剂1、2及3(pH=2)及商品dAmmonia,pH 10。抛光在AMAT Reflexion LK抛光工具上进行,并且缺陷检查在≥0.1/0.065/0.060μm缺陷大小的KLAT SP-3工具及KLAT eDR-7100缺陷审查工具(显微镜、SEM、EDX)上进行。
在没有兆频超声波(megasonic)步骤的情况下,清洁用英特格刷(PVP1ARXR1)进行。
图1示出在以pH<6及pH>6清洁的PETEOS晶片上的缺陷度数据,其中仅当使用清洁剂1、2及3时,在pH~2下检测到刷痕。
图2示出在低pH下基于硅石刷氢键合的刷印形成的机制。
负载有硅石的刷子还可使用FTIR光谱法来检测,在此处可以清楚地区分约1100cm-1的硅石Si-O-Si峰与约1016cm-1的刷子特征峰C-O-C(图3)。
表2中呈现具有在这一实验中所使用的H键合硅石刷清洁添加剂的列表:
表2
图4中呈现用含有这些添加剂的pH 2调配物中的一些进行清洁的受硅石污染的刷子的FTIR谱图:
图5及6示出呈样品1-8(表1)(本发明,使用丰富的硅石-H-键合添加剂或刷子-H-键合添加剂)与不具有这些添加剂的比较实例的直接比较形式的PETEOS晶片上的缺陷度。
Claims (20)
1.一种从化学机械处理后(CMP后)清洁刷去除磨料颗粒的方法,所述方法包含:
提供具有聚合物表面并在所述聚合物表面处具有磨料颗粒残余物的CMP后清洁刷,
提供pH低于7的清洁溶液,所述清洁溶液包含:
清洁剂,和
颗粒去除剂,并且
通过使所述聚合物表面与所述清洁溶液接触而从所述聚合物表面去除磨料颗粒残余物。
2.一种衬底的化学机械处理后(CMP后)清洁的方法,所述方法包含:
提供具有聚合物表面的CMP后清洁刷,
提供清洁溶液,其包含:
清洁剂,和
颗粒去除剂,
提供包括表面的衬底,其在所述衬底表面处具有残余物,所述残余物包括磨料颗粒,并且
通过将所述衬底表面和所述聚合物表面暴露于所述清洁溶液,同时使所述衬底表面与所述聚合物表面接触并且同时使所述衬底表面相对于所述聚合物表面移动,从所述衬底表面去除残余物。
3.根据权利要求1所述的方法,其中所述清洁溶液的pH在约1至6范围内。
4.根据权利要求1所述的方法,其中所述聚合物表面包括含有氢键合基团的聚合物。
5.根据权利要求4所述的方法,其中所述聚合物由包含乙烯醇单体的单体制得。
6.根据权利要求1所述的方法,其中所述颗粒去除剂包括一个或多个氢键合基团。
7.根据权利要求6所述的方法,其中所述氢键合基团为:羧酸基、氨基、醇基、膦基、磷酸酯基、膦酸酯基、烷醇胺基、碳酰胺基、脲基、氨基甲酸酯基、酯基、甜菜碱基团、硅烷醇基或含硫基团。
8.根据权利要求6所述的方法,其中所述颗粒去除剂为羧酸化合物、氨基酸化合物、具有至少3个羟基的多元醇、聚环氧烷均聚物或共聚物、含胺均聚物或共聚物。
9.根据权利要求8所述的方法,其中所述颗粒去除剂为:乳酸、顺丁烯二酸、脲、乙醇酸、山梨糖醇、硼砂(即硼酸钠)、脯氨酸、甜菜碱、甘氨酸、组氨酸、TRIS(三(羟甲基)氨基甲烷)、二甲亚砜、环丁砜、丙三醇、山梨糖醇、木糖醇、果糖、甘露糖醇、阿糖醇和葡聚糖或其组合。
10.根据权利要求1所述的方法,其中所述磨料颗粒在所述清洁溶液的pH下展现正电荷。
11.根据权利要求1所述的方法,其中所述磨料颗粒在所述颗粒的表面包括氢键合基团。
12.根据权利要求11所述的方法,其中所述氢键合基团为硅烷醇(SiOH)基团。
13.根据权利要求1所述的方法,其中所述磨料颗粒选自:硅石颗粒、铈土颗粒、二氧化铈颗粒、氧化铝颗粒、二氧化钛、氧化锆、金刚石或碳化硅颗粒或其组合。
14.根据权利要求1所述的方法,其中所述清洁剂包含螯合剂和有机溶剂中的一种或多种。
15.根据权利要求1所述的方法,其中所述清洁剂包含柠檬酸、单乙醇胺、聚丙烯酸或其组合。
16.一种适用于在化学机械处理后步骤中清洁衬底的清洁溶液浓缩物,所述清洁溶液包含:
清洁剂,和
至少0.1重量%的包括氢键合基团的颗粒去除剂。
17.根据权利要求16所述的浓缩物,其包含:
0.1至20重量%的清洁剂,和
0.1至20重量%的所述颗粒去除剂。
18.根据权利要求16所述的浓缩物,其中所述清洁剂包含螯合剂和有机溶剂的一种或多种。
19.根据权利要求16所述的浓缩物,其中所述清洁剂包含柠檬酸、单乙醇胺、聚丙烯酸或其组合。
20.根据权利要求16所述的浓缩物,其中所述清洁溶液的pH小于2.5。
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US20190168265A1 (en) | 2019-06-06 |
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TWI774889B (zh) | 2022-08-21 |
WO2019112751A1 (en) | 2019-06-13 |
JP7108032B2 (ja) | 2022-07-27 |
US20220395865A1 (en) | 2022-12-15 |
TW201925446A (zh) | 2019-07-01 |
US11446708B2 (en) | 2022-09-20 |
KR102447908B1 (ko) | 2022-09-28 |
JP2021505720A (ja) | 2021-02-18 |
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