CN102149783B - 用于抛光含硅基材的方法和组合物 - Google Patents
用于抛光含硅基材的方法和组合物 Download PDFInfo
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- CN102149783B CN102149783B CN200980130098XA CN200980130098A CN102149783B CN 102149783 B CN102149783 B CN 102149783B CN 200980130098X A CN200980130098X A CN 200980130098XA CN 200980130098 A CN200980130098 A CN 200980130098A CN 102149783 B CN102149783 B CN 102149783B
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
- B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces
- B24B37/042—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor
- B24B37/044—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor characterised by the composition of the lapping agent
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3105—After-treatment
- H01L21/31051—Planarisation of the insulating layers
- H01L21/31053—Planarisation of the insulating layers involving a dielectric removal step
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
- H01L21/321—After treatment
- H01L21/32115—Planarisation
- H01L21/3212—Planarisation by chemical mechanical polishing [CMP]
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
本发明提供用于抛光含硅基材的化学机械抛光(CMP)组合物和方法。本发明的方法包括以下步骤:使含硅基材与抛光垫和含水CMP组合物接触,和使该抛光垫与该基材之间发生相对运动,同时保持该CMP组合物的一部分与该基材的该表面接触以磨除该基材的至少一部分。该CMP组合物包含二氧化铈研磨剂、带有具有4~9的pKa的官能团的抛光添加剂、具有亲水部分和亲油部分的非离子型表面活性剂,其中该亲水部分具有500g/mol或更高的数均分子量、和含水载体,其中该组合物的pH为7或更小。该方法减少晶片上的缺陷,尤其是高移除率的局部区域。该方法还可用于以相对于半导体含硅基材的高速率抛光介电含硅基材。
Description
技术领域
本发明涉及用于抛光含硅基材的化学机械抛光组合物和方法。更具体地,本申请涉及含有二氧化铈研磨剂、抛光添加剂和表面活性剂的化学机械抛光组合物及其使用方法。
背景技术
化学机械平坦化或化学机械抛光(CMP)是公知的用于使基材平坦化的技术。CMP利用称为CMP组合物(其也称作CMP浆料)的化学组合物以从基材移除材料。抛光组合物典型地通过使表面与用抛光组合物饱和的抛光垫(例如,抛光布或抛光盘)接触而施加到基材上。基材的抛光典型地进一步借助于抛光组合物的化学活性和/或悬浮于抛光组合物中或并入到抛光垫(例如,固定研磨剂抛光垫)中的研磨剂的机械活性。
常规的CMP组合物和方法在使基材平坦化方面典型地不是完全令人满意的。具体地,当应用于基材时,CMP抛光组合物和方法可导致不太合乎需要的抛光速率和高的表面缺陷率(defectivity)。由于许多基材的性能直接与获得平坦的和无缺陷的表面有关,因此使用导致高的抛光效率、选择性、均匀性和移除速率并且实现具有最少(最小)表面缺陷的高质量抛光的CMP组合物和方法是至关重要的。
期望有提供对硅金属氧化物的高的抛光速率和对多晶硅的低的抛光速率的抛光浆料,其也称为“逆多晶硅(reverse poly)”浆料或“多晶硅上氧化物停止(oxide stop on poly)”浆料。在多种集成方案(包括浮栅电极)的加工中需要这样的浆料。据信,实现高的氧化物-对-多晶硅选择性的困难是由于多晶硅在典型的介电浆料(例如:高pH的基于二氧化硅的浆料)中非常容易被移除。
在含有二氧化铈的常规抛光浆料中,低含量(低于0.5重量%)的二氧化铈的使用可产生过高移除率(removal)的局部区域。这示范于图1中,其中,在晶片(2)上,特征(1)代表高移除率的局部区域的实例并且各等高线代表向该晶片内的10nm形貌变化。这些过高移除率的独立区域有时称为“麻点(pitting)”、“蚀斑(staining)”、“斑点”或“热点(hot spots)”。这些斑点为表面中的面积典型地为约0.001~10mm2且深度典型地为2nm~200nm的凹处。
因此,存在对这样的方法和组合物的需要,其使得实现用于抛光含硅基材的低固体物二氧化铈浆料在逆多晶硅应用中的可靠使用,同时还提供良好的表面均匀性。
发明内容
本发明提供用于抛光含硅基材的化学机械抛光(CMP)方法和组合物,该方法包括以下步骤、基本上由以下步骤组成、或者由以下步骤组成:使含硅基材与抛光垫和CMP组合物接触,和使该抛光垫与该基材之间发生相对运动,同时保持该CMP组合物的一部分与该基材的表面接触以磨除该基材的该表面的至少一部分,由此抛光该基材。该CMP组合物具有7或更小的pH并且包含以下物质、基本上由以下物质组成、或者由以下物质组成:含有二氧化铈研磨剂、带有具有4~9的pKa的官能团的抛光添加剂、和具有亲水部分和亲油部分的非离子型表面活性剂的含水载体。该非离子型表面活性剂的亲水部分具有至少500g/mol的数均分子量。
附图说明
图1为含硅晶片上的高移除率的局部区域的形貌图;
图2为移除速率(/分钟)对跨越具有高移除率的局部区域的直径为200mm的含有二氧化硅的晶片上的对角线的测量点的图,和移除速率(/分钟)对跨越无高移除率的局部区域的直径为200mm的含有二氧化硅的晶片上的对角线的测量点的图;
图3为厚度对跨越经不含表面活性剂的组合物、含有150ppm聚氧乙烯烷基苯基醚非离子型表面活性剂的组合物和含有400ppm聚氧乙烯烷基苯基醚非离子型表面活性剂的组合物抛光的直径为200mm的含有多晶硅的晶片上的对角线的测量点的图;
具体实施方式
本发明提供用于抛光含硅基材的化学机械抛光(CMP)方法,该方法包括以下步骤、基本上由以下步骤组成、或者由以下步骤组成:使含硅基材与抛光垫和CMP组合物接触,和使该抛光垫与该基材之间发生相对运动,同时保持该CMP组合物的一部分与在该垫和该基材之间的表面接触一段足以磨除该基材的该表面的至少一部分的时间。该CMP组合物包含含水载体,该含水载体含有二氧化铈研磨剂、带有具有4~9的pKa的官能团的抛光添加剂、和包含亲水部分和亲油部分的非离子型表面活性剂,其中该亲水部分具有至少500g/mol的数均分子量。该组合物的pH为7或更小。
本发明提供用于抛光含硅基材的方法和组合物,其降低且优选消除该基材上的较高移除率的局部区域(例如,提供低水平的麻点、蚀斑、斑点等)。
本发明特别可用于减少高移除率的局部区域,甚至当CMP浆料中的二氧化铈浓度小于该组合物的0.5重量百分比(重量%)(例如,小于0.2重量%或小于0.1重量%)时也是如此。所用二氧化铈的浓度典型地大于0.005重量%(例如,大于0.01重量%)。优选地,二氧化铈的浓度为0.005重量%~0.5重量%(例如0.01重量%~0.1重量%)。
二氧化铈研磨剂可具有任何合适的初级粒度。该初级粒度合意地通过激光衍射技术测量。典型地,该研磨剂的平均初级粒度为200nm或更小、优选180nm或更小(例如,160nm或更小、140nm或更小、或120nm或更小)。典型地,该研磨剂的平均初级粒度为至少10nm、优选至少20nm(例如,至少40nm、至少60nm、或至少80nm)。典型地,二氧化铈研磨剂的平均初级粒度为约10nm至180nm(例如40nm至120nm)。
CMP组合物优选是抗颗粒团聚的,使得平均团聚体粒度为300nm或更小(例如,250nm或更小、或甚至200nm或更小)。团聚的缺乏也反映在粒度分布的总宽度中,粒度分布的总宽度典型地为平均初级粒度的±35%(例如,±25%、或甚至±15%)。
抛光组合物中包含抛光添加剂以调整正被抛光的含硅介电层的表面性质,以使该表面更易于接受与研磨剂颗粒的相互作用。抛光组合物的pH在决定抛光添加剂与含硅介电层的表面之间的相互作用方面起着重要作用。抛光组合物典型地具有7或更小、优选6.5或更小(例如,5.5或更小)的pH。抛光组合物典型地具有至少2、优选至少3(例如,至少3.5)的pH。为了使抛光添加剂与含硅介电层在该pH范围内进行相互作用,抛光添加剂合乎需要地带有具有4~9、优选4~7(例如,4~6)的pKa(在水中)的官能团。此外,抛光添加剂的总的净电荷大于约-1(例如,净电荷=0、+1、+2等)是合乎需要的。该净电荷被确定为当该具有4~9的pKa的官能团被质子化时该抛光添加剂的电荷。
该抛光添加剂的该官能团可为任何合适的官能团,并且典型地选自下列的基团:胺、羧酸、醇、硫醇、磺酰胺、酰亚胺、异羟肟酸、巴比妥酸、肼、酰胺基喔星(amidoxine)、其盐、及其组合。带有这些官能团并且具有4~9的pKa的抛光添加剂包括选自下列的一种或多种化合物:芳胺、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、经取代的苯酚、磺酰胺、硫醇、及其组合。优选地,抛光添加剂包含选自芳胺、杂环胺、氨基羧酸及其组合的一种或多种化合物。前述抛光添加剂中的任何抛光添加剂可以盐例如选自如下的盐的形式存在:氢氯酸盐、氢溴酸盐、硫酸盐、磺酸盐、三氟甲磺酸盐、乙酸盐、三氟乙酸盐、苦味酸盐、全氟丁酸盐、钠盐、钾盐、铵盐、卤化物盐等。
芳胺可为具有4~9的pKa的任何合适的芳胺。优选地,芳胺为伯芳胺。芳胺可任选地被选自如下的一个或多个取代基取代:C1-12烷基、C1-12烷氧基、C6-12芳基、羧酸基、磺酸基、膦酸基、羟基、硫醇基、磺酰胺基、乙酰胺基、其盐、及其组合。例如,芳胺可为苯胺、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、氨基苄醇、氨基苄胺、1-(2-氨基苯基)吡咯、1-(3-氨基苯基)乙醇、2-氨基苯基醚、2,5-双-(4-氨基苯基)-1,3,4-二唑、2-(2-氨基苯基)-1H-1,3,4-三唑、2-氨基苯酚、3-氨基苯酚、4-氨基苯酚、二甲基氨基苯酚、2-氨基苯硫酚、3-氨基苯硫酚、4-氨基苯硫酚、4-氨基苯基甲基硫醚、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、磺胺醋酰、磺氨酸、邻-氨苯胂酸、对-氨苯胂酸、(3R)-3-(4-三氟甲基苯基氨基)戊酸酰胺、其盐、及其组合。
氨基醇可为具有4~9的pKa的任何合适的氨基醇。例如,氨基醇可选自:三乙醇胺、苄基二乙醇胺、三(羟甲基)氨基甲烷、羟胺、四环素、其盐、及其组合。优选地,氨基醇为叔氨基醇。
脂族胺可为具有4~9的pKa的任何合适的脂族胺。合适的脂族胺包括甲氧基胺、羟胺、N-甲基羟胺、N,O-二甲基羟胺、β-二氟乙基胺、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、氰胺(例如,氨基乙腈、二乙基氨基乙腈、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、二氰基二乙基胺、3-(二甲基氨基)丙腈、其盐、及其组合。脂族胺还可为肼类。优选地,肼类包括选自如下的一种或多种化合物:肼、甲基肼、四甲基肼、N,N-二乙基肼、苯基肼、N,N-二甲基肼、三甲基肼、乙基肼、其盐(例如,氢氯酸盐)、及其组合。
杂环胺可为具有4~9的pKa的任何合适的杂环胺,包括单环、双环和三环胺。典型地,环胺为包含一个或多个氮原子和一个或多个其它原子(例如碳、碳和氧、碳和硫等)的3、4、5或6元环结构。优选地,环胺为5或6元环结构。杂环胺任选地被选自如下的一个或多个取代基取代:H、OH、COOH、SO3H、PO3H、Br、Cl、I、F、NO2、肼基、C1-8烷基(任选地被OH、COOH、Br、Cl、I或NO2取代)、C6-12芳基(任选地被OH、COOH、Br、I或NO2取代)、C(O)H、C(O)R(其中R为C1-8烷基或C6-12芳基)、和C1-8烯基。合乎需要地,杂环胺含有至少一个未取代的杂环氮。例如,杂环胺可为咪唑、1-甲基咪唑、2-甲基咪唑、2-乙基咪唑、2-羟甲基咪唑、1-甲基-2-羟甲基咪唑、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-吡啶二羧酸、2,5-吡啶二羧酸、2,6-吡啶二羧酸、5-丁基-2-吡啶羧酸、4-羟基-2-吡啶羧酸、3-羟基-2-吡啶羧酸、2-吡啶羧酸、3-苯甲酰基-2-吡啶羧酸、6-甲基-2-吡啶羧酸、3-甲基-2-吡啶羧酸、6-溴-2-吡啶羧酸、6-氯-2-吡啶羧酸、3,6-二氯-2-吡啶羧酸、4-肼基-3,5,6-三氯-2-吡啶羧酸、喹啉、异喹啉、2-喹啉羧酸、4-甲氧基-2-喹啉羧酸、8-羟基-2-喹啉羧酸、4,8-二羟基-2-喹啉羧酸、7-氯-4-羟基-2-喹啉羧酸、5,7-二氯-4-羟基-2-喹啉羧酸、5-硝基-2-喹啉羧酸、1-异喹啉羧酸、3-异喹啉羧酸、吖啶、苯并喹啉、苯并吖啶、可乐定、毒藜碱、降烟碱(nomicotine)、三唑并吡啶、吡哆醇、5-羟色胺、组胺、苯并二氮吖丙啶、吗啉、1,8-二氮杂二环[5,4,0]十一碳烯-7(DABCO)、六亚甲基四胺、哌嗪、N-苯甲酰基哌嗪、1-甲苯磺酰基哌嗪、N-乙氧羰基哌嗪、1,2,3-三唑、1,2,4-三唑、2-氨基噻唑、吡咯、吡咯-2-羧酸和其经烷基、卤素或羧酸基取代的衍生物、3-吡咯啉-2-羧酸、乙基吡咯啉、苄基吡咯啉、环己基吡咯啉、甲苯基吡咯啉、四唑、5-环丙基四唑、5-甲基四唑、5-羟基四唑、5-苯氧基四唑、5-苯基四唑、其盐、及其组合。杂环胺还可为酰亚胺、胺啶(aminidine)、或巴比妥酸化合物。例如,合适的酰亚胺包括氟脲嘧啶、甲基硫脲嘧啶、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、其盐、及其组合。合适的胺啶包括咪唑并[2,3-b]硫唑(imidazo[2,3-b]thioxazole)、羟基咪唑并[2,3-a]异吲哚、其盐、及其组合。合适的巴比妥酸包括5,5-甲基苯基巴比妥酸、1,5,5-三甲基巴比妥酸、海索比妥、5,5-二甲基巴比妥酸、1,5-二甲基-5-苯基巴比妥酸、其盐、及其组合。
异羟肟酸可为具有4~9的pKa的任何合适的异羟肟酸。合适的异羟肟酸包括甲酰氧肟酸(formohydroxamic acid)、乙酰氧肟酸、苯基异羟肟酸、水杨基异羟肟酸、2-氨基苯基异羟肟酸、2-氯苯基异羟肟酸、2-氟苯基异羟肟酸、2-硝基苯基异羟肟酸、3-硝基苯基异羟肟酸、4-氨基苯基异羟肟酸、4-氯苯基异羟肟酸、4-氟苯基异羟肟酸、4-硝基苯基异羟肟酸、4-羟基苯基异羟肟酸、其盐、及其组合。
氨基羧酸可为具有4~9的pKa的任何合适的氨基羧酸。一些常见氨基羧酸化合物例如脯氨酸、甘氨酸、苯基甘氨酸等就羧酸部分而言具有2~2.5的pKa和就氨基部分而言具有9~10的pKa,不适于在本发明的范围内使用。相反,诸如谷氨酸、β-羟基谷氨酸、天冬氨酸、天冬酰胺、偶氮丝氨酸、半胱氨酸、组氨酸、3-甲基组氨酸、胞嘧啶、7-氨基头孢烷酸和肌肽(camosine)的氨基羧酸各自含有具有4~9的pKa的官能团。
环状一元羧酸可为具有4~9的pKa的任何合适的环状一元羧酸。先前提出用于抛光含硅介电层的二元羧酸和多元羧酸可具有在所需范围内的pKa,但具有导致无机研磨剂颗粒的不希望有的团聚、粘附和/或快速沉降的总电荷。合乎需要地,环状羧酸化合物包含C4-12环烷基或C6-12芳基。环状羧酸化合物任选地被选自如下的一个或多个取代基取代:H、OH、COOH、Br、Cl、I、F、NO2、肼基、C1-8烷基(任选地被OH、COOH、Br、Cl、I或NO2取代)、C6-12芳基(任选地被OH、COOH、Br、I或NO2取代)、C(O)H、C(O)R(其中R为C1-8烷基或C6-12芳基)、和C1-8烯基。优选地,环状羧酸化合物不为二羟基苯甲酸或多羟基苯甲酸。合适的环状一元羧酸化合物包括苯甲酸、经C1-12-烷基取代的苯甲酸、经C1-12-烷氧基取代的苯甲酸、萘-2-甲酸、环己烷羧酸、环己基乙酸、2-苯基乙酸、4-羟基苯甲酸、3-羟基苯甲酸、2-哌啶羧酸、环丙烷羧酸(例如,顺-2-甲基环丙烷羧酸和反-2-甲基环丙烷羧酸)、其盐、及其组合。尤其优选的抛光添加剂为4-羟基苯甲酸、环己烷羧酸、苯甲酸、其盐、及其组合。
不饱和一元羧酸可为具有4~9的pKa的任何合适的不饱和一元羧酸(例如,烯烃羧酸)。典型地,不饱和一元羧酸为C3-62-链烯酸。优选地,不饱和一元羧酸包括选自如下的一种或多种化合物:肉桂酸、丙烯酸类(例如,丙烯酸、3-氯丙-2-烯羧酸)、丁烯酸类(例如,巴豆酸、3-氯丁-2-烯羧酸、4-氯丁-2-烯羧酸)、戊烯酸类(例如,顺-2-戊烯酸或反-2-戊烯酸、2-甲基-2-戊烯酸)、己烯酸(例如,2-己烯酸、3-乙基-2-己烯酸)、其盐、及其组合。
经取代的苯酚可为具有4~9的pKa的任何合适的经取代的苯酚。优选地,经取代的苯酚含有选自如下的取代基:硝基、氯、溴、氟、氰基、烷氧羰基、烷酰基、酰基、烷基磺酰基、及其组合。合适的硝基苯酚类包括硝基苯酚、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、2,6-二硝基苯酚、3,4-二硝基苯酚、2-C1-12-烷基-4,6-二硝基苯酚、2-卤代-4,6-二硝基苯酚、二硝基-邻-甲酚、三硝基苯酚(例如苦味酸)、其盐、及其组合。
磺酰胺可为具有4~9的pKa的任何合适的磺酰胺。合适的磺酰胺包括N-氯甲苯基磺酰胺、二氯苯磺胺、磺胺米隆、尼美舒利、磺胺甲二唑(sulfamethizole)、磺胺培林(sulfaperin)、磺胺醋酰、磺胺嘧啶、磺胺二甲氧哒嗪、磺胺二甲嘧啶、磺胺吡啶、磺胺喹喔啉、其盐、及其组合。
硫醇可为具有4~9的pKa的任何合适的硫醇。合适的硫醇包括硫化氢、半胱胺、半胱氨酰半胱氨酸、半胱氨酸甲酯、硫酚、对氯硫酚、邻-氨基硫酚、邻-巯基苯乙酸、对-硝基苯硫醇、2-巯基乙磺酸酯、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、巯基乙基胺、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、其盐、及其组合。
当抛光添加剂为芳胺时,抛光添加剂优选包括选自如下的一种或多种化合物:苯胺、邻氨基苯甲酸、氨基苯酚、邻氨基苯磺酸、其盐、及其组合。当抛光添加剂为杂环胺化合物时,抛光添加剂优选包括选自如下的一种或多种化合物:咪唑、喹啉、吡啶、2-甲基吡啶、2-吡啶羧酸、吡啶二羧酸、2-喹啉羧酸、吗啉、哌嗪、三唑、吡咯、吡咯-2-羧酸、四唑、其盐、及其组合。当抛光添加剂为氨基羧酸化合物时,抛光添加剂优选包括选自如下的一种或多种化合物:谷氨酸、天冬氨酸、半胱氨酸、组氨酸、其盐、及其组合。当抛光添加剂为环状一元羧酸化合物时,抛光添加剂优选包含选自如下的一种或多种化合物:苯甲酸、环己烷羧酸、环己基乙酸、2-苯基乙酸、其盐、及其组合。
抛光组合物典型地包含5重量%或更少的抛光添加剂(例如,2重量%或更少的抛光添加剂)。抛光组合物合乎需要地包含0.005重量%或更多(例如,0.01重量%或更多)的抛光添加剂。优选地,抛光组合物包含1重量%或更少(例如,0.5重量%或更少、0.2重量%或更少)的抛光添加剂。优选地,该添加剂包括选自如下的一种或多种化合物:芳胺、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、经取代的苯酚、磺酰胺、硫醇、其盐、及其组合。
表面活性剂的亲水部分包含下列重复单元或基团、基本上由下列重复单元或基团组成、或者由下列重复单元或基团组成:氧基亚乙基(-O-CH2-CH2-)重复单元、乙烯醇[-CH2-CH2(OH)-]重复单元、脱水山梨醇基团、经高度取代的饱和的或部分不饱和的C6-30烷基、或其组合(例如,聚氧乙烯脱水山梨醇)。经高度取代的饱和或部分不饱和的C6-30烷基优选为被一个或多个亲水官能团例如羟基取代的。非离子型表面活性剂的亲水部分的分子量典型地为至少500g/mol(例如,1000g/mol或更大、1500g/mol或更大、或3000g/mol或更大)。对于聚合物或低聚物亲水材料,该分子量优选为数均分子量。具有非常高的数均分子量的化合物可使粘度增加,该粘度增加对浆料贮运(输送,handling)、抛光性能和浆料稳定性是有害的。因此,优选使用包含具有低于1,000,000g/mol(即,低于100,000g/mol、低于50,000g/mol或低于10,000g/mol)的数均分子量的亲水部分的表面活性剂。
表面活性剂的亲油部分可为含有烃部分的不含有机硅的片段((silicone-free fragment),在该烃部分中有6~30个烃单元(例如,10~20个烃单元)。优选地,烃部分为烷基、经烷基取代的芳基、经烷氧基取代的芳基、和经芳基取代的烷基或芳基。
此外,表面活性剂可包括任何这样的炔二醇表面活性剂,该炔二醇表面活性剂包含如下基团、基本上由如下基团组成、或者由如下基团组成:四烷基癸炔头基团和氧基亚乙基尾基团,例如2,4,7,9-四甲基-5-癸炔-4,7-二醇乙氧基化物。表面活性剂还可为两亲性非离子型表面活性剂例如聚氧乙烯烷基醚和聚氧乙烯链烷酸酯,其中其烷基部分为C6-30烷基,该C6-30烷基可为饱和的或部分不饱和的并且任选地支化。例如,两亲性非离子型表面活性剂可包括聚氧乙烯月桂基醚、聚氧乙烯鲸蜡基醚、聚氧乙烯硬脂基醚、聚氧乙烯油酰基醚、聚氧乙烯单月桂酸酯、聚氧乙烯单硬脂酸酯、聚氧乙烯二硬脂酸酯、或聚氧乙烯单油酸酯。类似地,表面活性剂可为聚氧乙烯烷基苯基醚或聚氧乙烯烷基环己基醚,其中其烷基为C6-30烷基,该C6-30烷基可为饱和的或部分不饱和的并且可任选地支化,例如聚氧乙烯辛基苯基醚、聚氧乙烯壬基苯基醚、或聚氧乙烯二壬基苯基醚。
两亲性非离子型表面活性剂还可包括脱水山梨醇链烷酸酯或聚氧乙烯脱水山梨醇链烷酸酯,其中其烷基部分为C6-30烷基,其可为饱和的或部分不饱和的并且可任选地支化。例如,两亲性非离子型表面活性剂可包括脱水山梨醇单月桂酸酯、脱水山梨醇单油酸酯、脱水山梨醇单棕榈酸酯、脱水山梨醇单硬脂酸酯、脱水山梨醇倍半油酸酯(sequioleate)、脱水山梨醇三油酸酯、或脱水山梨醇三硬脂酸酯,以及聚氧乙烯脱水山梨醇单月桂酸酯、聚氧乙烯脱水山梨醇单棕榈酸酯、聚氧乙烯脱水山梨醇单硬脂酸酯、聚氧乙烯脱水山梨醇三硬脂酸酯、聚氧乙烯脱水山梨醇单油酸酯、聚氧乙烯脱水山梨醇三油酸酯、或聚氧乙烯脱水山梨醇四油酸酯。
或者,表面活性剂可包括这样的聚二甲基硅氧烷(polydimethicone)嵌段或接枝共聚物,该聚二甲基硅氧烷嵌段或接枝共聚物包含如下部分、基本上由如下部分组成、或者由如下部分组成:聚二甲基硅氧烷部分和亲水的含氧部分(例如,聚氧乙烯、聚氧乙烯和聚氧丙烯、或者聚氧乙烯和聚乙烯、或烷基缩合葡萄糖、乙氧基化的烷基葡萄糖酯或二酯)。所述嵌段或接枝共聚物可包含上述亲水部分的组合,例如,结合至聚氧乙烯和聚氧丙烯共聚物的聚二甲基硅氧烷部分等。
表面活性剂优选是亲水的,如可通过表面活性剂的亲水亲油平衡(HLB)值确定的。HLB值是表面活性剂在水中的溶解度的指示,且因此与表面活性剂的亲水部分的重量%的量(例如,氧化乙烯的重量%的量)有关。在一些情况下,对于含有氧化乙烯基团的非离子型表面活性剂,表面活性剂HLB值可近似为等于表面活性剂中氧化乙烯基团的重量百分比(重量%)的量乘以20,得到在0与20之间的值。低的HLB值指示亲油性表面活性剂(即,具有少量的亲水基团),高的HLB值指示亲水性表面活性剂(具有大量的亲水基团)。HLB为10或更大的非离子型表面活性剂被归类为“亲水性”非离子型表面活性剂,而HLB小于10的非离子型表面活性剂被归类为“亲油性的”(参见例如,The HLB System,由ICI United States公司出版,1976年)。在优选实施方式中,非离子型表面活性剂为亲水性非离子型表面活性剂且因此具有不小于10(例如,不小于12)的HLB。在优选实施方式中,非离子型表面活性剂为HLB小于19(例如,小于18)的亲水性表面活性剂。
优选的表面活性剂包括聚氧乙烯壬基苯基醚和聚氧乙烯二壬基苯基醚(例如,来自Rhone-Poulenc的表面活性剂、来自BASF的表面活性剂和来自BASF的表面活性剂)、聚氧乙烯-聚氧丙烯共聚物(例如,来自BASF的表面活性剂)和聚二甲基硅氧烷共聚物(例如,来自GE Silicons的表面活性剂)。
典型地,表面活性剂以不小于10ppm、优选不小于20ppm(例如,不小于50ppm、不小于约100ppm、不小于150ppm或不小于200ppm)的浓度存在于抛光组合物中。典型地,表面活性剂以不大于10,000ppm、优选不大于1000ppm(例如,不大于750ppm、或不大于500ppm)的浓度存在。
本文所描述的抛光组合物任选地进一步包含诸如消泡剂和杀生物剂的一种或多种组分。消泡剂和杀生物剂可分别为适合用在CMP浆料中的任何合适的消泡剂和抗微生物剂。
用于抛光组合物中的杀生物剂的浓度典型地为1~50ppm、优选10~20ppm,基于液体载体和溶解或悬浮于其中的任何组分。合适的杀生物剂的实例包括异噻唑啉酮杀生物剂。
存在于抛光组合物中的消泡剂的浓度典型地为5~140ppm,基于液体载体和溶解或悬浮于其中的任何组分。合适的消泡剂包括聚二甲基硅氧烷聚合物(聚二甲基硅氧烷)等。
本文所描述的抛光组合物还任选地包含一种或多种金属络合或螯合剂。例如,这些金属络合或螯合剂可包括单羧酸、二羧酸、三羧酸和多羧酸(例如,EDTA和柠檬酸);单膦酸、二膦酸、三膦酸和多膦酸(例如,膦酸等),以及一元胺、二元胺、三元胺和多元胺。
本发明提供以相对于含硅半导体材料的较高移除速率抛光含硅介电材料的方法和组合物。典型的含硅介电材料包括,例如,二氧化硅、硼硅酸盐、磷硅酸盐、硼磷硅玻璃(BPSG)、未经掺杂的硅酸盐玻璃(USG)、及其组合,以及氮化硅和氮氧化硅。典型的含硅半导体材料包括,例如,多晶硅、单晶硅、p型掺杂硅、和n型掺杂硅。半导体材料还包括例如所谓的III-V族材料(例如,砷化镓和磷化铝)的材料。典型地,本发明提供大于5:1(例如,大于或等于10∶1、大于或等于20∶1、或大于或等于30∶1)的含硅介电材料的移除相对于含硅半导体材料的移除的选择性。在含硅半导体基材上可实现低于/分钟并接近/分钟(例如,低于/分钟、低于/分钟或低于/分钟)的抛光速率。在含硅介电材料上可实现大于/分钟(例如,大于/分钟、大于/分钟或大于/分钟)的抛光速率。
本发明的组合物和方法可用于抛光任何合适的基材。优选地,基材包含至少一个含硅层,该含硅层含有二氧化硅(例如,PETEOS)、单晶硅、多晶硅(polycrystalline silicon)(例如,多晶硅(polysilicon))、经掺杂的硅(例如,氮和磷掺杂的多晶硅)、介电常数为3.5或更小(例如,1~3)的低k介电材料、氮化硅、硼化硅、和硅。本发明的组合物和方法还特别可用于抛光包含锗的基材,但不限于此。
可使用任何测定表面均匀性的质量的方法。为了描述本发明,使用下列测量方法,但不限于此。对角线移除速率分布图(diagonal removal rate profile)是呈对角线跨越晶片测量的移除速率分布图并且通常可通过如图2中所示的5阶和更低阶的多项式方程来描述。例如,可使用椭偏测量术由抛光前的厚度与抛光后的厚度之差计算膜的移除速率。若存在许多高移除率的局部区域的事件,则多项式拟合差,如由低的最小二乘相关性(R2)所明显表明的。较少的高移除率的局部区域的存在改善该相关性。因此,对角线移除分布图的5阶或更低阶的最小二乘拟合的相关系数的平方(R2)可用作评估抛光晶片的表面质量的便利工具。具体而言,0.5(50%)或更大、优选至少0.6(60%)或更大且优选至少0.7(70%)的R2值说明抛光晶片的表面相对不存在过高移除率的局部区域(例如,麻点、斑点、蚀斑等)。
高移除率的局部区域的另一影响是使晶片内不均匀度(within-wafernon-uniformity)增加;然而,该参数可能主要是由于全局现象例如低的整体边缘抛光至中心的抛光速率的差异所致。不均匀度可通过对每个测量点取抛光前晶片与抛光后晶片之间的厚度差的标准偏差来计算。在本文中将该标准偏差相对于总的平均厚度差的量值(以百分比表示)称为晶片表面不均匀度。
高移除率的局部区域还可通过“表面凹陷值(dishing number)”来描述。表面凹陷值是基材上在给定距离(轮廓)范围内的平均高区域与平均较低区域之间的差。典型地,该表面凹陷值用于描述不同材料的两个区域之间(例如氧化硅和铜/氧化硅阵列之间)的凹部(表面凹陷)。本文中所使用的表面凹陷值是指相同材料的高的区域与低的区域之间的差。
当与上述基材一起使用时,本发明的方法和组合物提供优选低于20%(例如,低于15%或低于10%)的晶片内不均匀度值。此外,当使用本发明的方法和组合物时,在1mm~5mm的轮廓上得到小于80nm(例如,小于50nm、小于25nm或小于10nm)的表面凹陷值。
实施例
以下实施例进一步举例说明本发明,但当然不应解释为以任何方式限制其范围。
实施例1
该实施例展示本发明的组合物用于减少PETEOS和多晶硅晶片上的高移除率的局部区域的效力。在本实施例中:
使用常规的CMP装置利用本发明的数种CMP组合物抛光PETEOS(氧化硅)和多晶硅(poly)晶片(200mm直径)。所评估的CMP浆料含有0.1%二氧化铈(100nm直径,平均粒度)、1600ppm的2-吡啶羧酸(抛光添加剂)和用以将pH调节至5的氢氧化铵。各浆料还含有表1或表2中所示量的表面活性剂。出于比较的目的,还使用不含表面活性剂的浆料。用于抛光晶片的抛光参数如下:向下压力在20.2kPa(2.95psi)至21.0kPa(3.05psi)的范围内,压板速度为110rpm,载体速度为101rpm,且流速为200mL/分钟。在用于抛光晶片的抛光工具上使用具有同心沟槽的D100垫(CabotMicroelectronics Corporation,Aurora,IL)并进行原位调节。将晶片各自抛光120秒。在晶片直径上49个等间距点处测量抛光前和抛光后各晶片的厚度,并确定抛光前和抛光后各晶片的总厚度差的标准偏差。然后计算所确定的标准偏差相对于总的厚度差的百分比作为抛光均匀性的量度。因为高移除率的局部区域由于通过氧化硅的光发生折射而呈现为斑点,因此还对PETEOS晶片进行目视检查。相反,在多晶硅上用肉眼更难以观察到高移除率的局部区域。因此,对于多晶硅,使用光学显微镜在5倍放大率下进行目视检查。厚度测定和目视检查的结果总结于表2中。
表1:PETEOS和多晶硅的缺陷(defectivity)数据
表1中的结果表明,包含亲油的经烷氧基取代的芳基和平均分子量大于500g/mol的亲水的聚氧乙烯基团的表面活性剂对于降低高的多晶硅和PETEOS移除率的局部区域是有效的。
图3显示使用含有0ppm、150ppm和400ppm的CO-890的浆料抛光的晶片的损失(抛光前-抛光后厚度)分布图。结果表明,表面活性剂的添加使晶片直径上的分布图变得平滑。平滑度可通过将49个测量点处的厚度(y)对线性位置(x)拟合为二阶多项式表达式来量化。以下方程和最小二乘拟合(即,拟合系数的平方作为百分数表示)由所示表面活性剂水平下的所有晶片的合并数据获得:
a.无表面活性剂:y=0.0238x2+2.5426x+8732.1;R2-=9%,
b.150ppm表面活性剂:y=0.353x2-16.081x+8588.8;R2=71%,
c.400ppm表面活性剂:y=0.4392x2-20.344x+8751.2;R2=95%。
显然,与用不含表面活性剂的常规CMP组合物所获得的拟合相比,本发明的方法和组合物所产生的分布图更接近地拟合多项式方程,如由当应用本发明的方法时的更高的R2值所证实的。该结果表明通过本发明的方法和组合物显著改善了晶片的抛光后表面。
描述高移除率的局部区域的另一方式为通过表面凹陷值描述,该表面凹陷值是通过使用原子力显微镜(AFM)进行5mm轮廓扫描获得的。表2显示在使用0ppm和400ppmCO-890抛光的晶片上的这样的AFM测量结果。在表2中,测量位置“中心”是指晶片中心附近的轮廓,“边缘”是指晶片边缘附近的轮廓,和“中间”是指在该中心测量与边缘测量之间的轮廓。
表2:AFM表面凹陷数据
显然,如通过平均麻点深度的减小所看出的,本发明组合物中表面活性剂的存在降低了局部高移除速率的事件。
实施例2
该实施例展示使用具有非离子型表面活性剂(其中亲水部分具有至少500g/mol的数均分子量)的组合物以低的抛光速率抛光硅晶片的效力。使用常规的CMP装置利用本发明的数种CMP组合物对PETEOS和多晶硅正方形晶片(4cm2)进行抛光。关于pH、二氧化铈浓度和抛光添加剂,所用CMP浆料类似于实施例1所用的浆料。各浆料还含有表3中所示的量的表面活性剂。用于抛光所述晶片的抛光参数与实施例1中的相同,除了流速为100mL/分钟且对多晶硅晶片的抛光时间为30秒之外。在晶片区域上9个等间距点处测量抛光前和抛光后各晶片的厚度。表3显示含有各表面活性剂的组合物对TEOS和多晶硅晶片的抛光速率。亲水物的平均分子量也示于表3中。
表3:抛光速率
表3的数据绘制于图4、5和6中。图4为使用包含具有不同大小的聚氧乙烯部分的聚氧乙烯烷基苯基醚表面活性剂的浆料在多晶硅晶片上的抛光速率的曲线,并且表明当亲水的聚氧乙烯的分子量大于500g/mol时,移除速率降低。图5为使用包含具有不同聚氧乙烯链长度的聚氧乙烯-聚氧丙烯共聚物表面活性剂的浆料在多晶硅晶片上的抛光速率的曲线,并且表明当聚氧乙烯的分子量大于500g/mol时,移除速率降低。最后,图6为使用包含具有不同聚氧乙烯链长度的乙氧基化聚二甲基硅氧烷共聚物表面活性剂的浆料在多晶硅晶片上的抛光速率的曲线,并且表明当聚氧乙烯分子量大于500g/mol时,移除速率降低。
Claims (16)
1.用于抛光含硅基材的化学机械抛光(CMP)方法,该方法包括下列步骤:
(a)使含硅基材的表面与抛光垫和CMP组合物接触,该CMP组合物包含:
(i)含水载体,
(ii)二氧化铈研磨剂,
(iii)带有具有4~9的pKa的官能团的抛光添加剂,和
(iv)包含亲水部分和亲油部分的非离子型表面活性剂,其中该亲水部分具有500g/mol或更高的数均分子量;和其中该CMP组合物具有7或更小的pH;
(b)使该抛光垫与该基材之间发生相对运动,同时保持该CMP组合物的一部分与该基材接触,以磨除该基材的该表面的至少一部分,由此抛光该基材。
2.权利要求1的CMP方法,其中该亲水部分具有1000g/mol或更高的数均分子量。
3.权利要求1的CMP方法,其中该抛光添加剂为杂环胺。
4.权利要求1的CMP方法,其中该抛光添加剂为氨基羧酸。
5.权利要求1的CMP方法,其中该抛光添加剂选自:芳胺、脂族胺、异羟肟酸、环状一元羧酸、不饱和一元羧酸、经取代的苯酚、磺酰胺、硫醇、其盐、及其组合。
6.权利要求1的CMP方法,其中该亲水部分包括聚氧乙烯基团。
7.权利要求1的CMP方法,其中该表面活性剂具有8~20的亲水亲油平衡(HLB)值。
8.权利要求1的CMP方法,其中以下的任意一种或多种适用:
a)该表面活性剂包括聚氧乙烯烷基苯基醚;
b)该表面活性剂包括聚二甲基硅氧烷共聚物;和
c)该表面活性剂包括聚氧乙烯-聚氧丙烯共聚物。
9.权利要求1的CMP方法,其中该pH为2~7。
10.权利要求1的CMP方法,其中该表面活性剂以5ppm~10,000ppm的浓度存在于该CMP组合物中。
11.权利要求1的CMP方法,其中该CMP组合物中的该二氧化铈以0.005重量%~0.5重量%的浓度存在。
12.权利要求1的CMP方法,其中该CMP组合物中的该二氧化铈以0.01重量%~0.1重量%的浓度存在。
13.权利要求1的方法,其中该二氧化铈研磨剂具有10nm~180nm的平均初级粒度。
14.权利要求1的方法,其中该二氧化铈研磨剂具有40nm~120nm的平均初级粒度。
15.CMP组合物,其具有7或更小的pH并且包含含水载体,该含水载体含有二氧化铈研磨剂、带有具有4~9的pKa的官能团的抛光添加剂、以及包含亲水部分和亲油部分的非离子型表面活性剂,其中该亲水部分具有500g/mol或更高的数均分子量。
16.权利要求15的CMP组合物,其中以下的任意一种或多种适用:
a)该表面活性剂包括聚氧乙烯烷基苯基醚;
b)该表面活性剂包括聚二甲基硅氧烷共聚物;和
c)该表面活性剂包括聚氧乙烯-聚氧丙烯共聚物。
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EP2331649A4 (en) | 2013-07-03 |
WO2010014180A3 (en) | 2010-04-22 |
TW201011826A (en) | 2010-03-16 |
US20100029181A1 (en) | 2010-02-04 |
SG189801A1 (en) | 2013-05-31 |
KR101396000B1 (ko) | 2014-05-16 |
IL210029A0 (en) | 2011-02-28 |
JP2011530166A (ja) | 2011-12-15 |
MY149727A (en) | 2013-10-14 |
CN102149783A (zh) | 2011-08-10 |
TWI398917B (zh) | 2013-06-11 |
KR20110053438A (ko) | 2011-05-23 |
US8247327B2 (en) | 2012-08-21 |
US20120280170A1 (en) | 2012-11-08 |
JP5628802B2 (ja) | 2014-11-19 |
IL210029A (en) | 2015-07-30 |
US8597540B2 (en) | 2013-12-03 |
JP2014209662A (ja) | 2014-11-06 |
EP2331649A2 (en) | 2011-06-15 |
WO2010014180A2 (en) | 2010-02-04 |
JP5952352B2 (ja) | 2016-07-13 |
EP2331649B1 (en) | 2018-06-13 |
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