CN103571253B - 高温热退火方法 - Google Patents
高温热退火方法 Download PDFInfo
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- CN103571253B CN103571253B CN201310435005.2A CN201310435005A CN103571253B CN 103571253 B CN103571253 B CN 103571253B CN 201310435005 A CN201310435005 A CN 201310435005A CN 103571253 B CN103571253 B CN 103571253B
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- siloxanes
- vinylbenzene
- film
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Classifications
-
- 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
- H01L21/324—Thermal treatment for modifying the properties of semiconductor bodies, e.g. annealing, sintering
- H01L21/3247—Thermal treatment for modifying the properties of semiconductor bodies, e.g. annealing, sintering for altering the shape, e.g. smoothing the surface
-
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Abstract
高温热退火方法。一种用于加工基材的方法,所述方法包括:提供具有表面的基材;提供共聚物组合物,所述共聚物组合物包括:聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分,其中聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分的数均分子量是5到1,000kg/mol;和,抗氧化剂;施加上述共聚物组合物的薄膜到基材表面;任选地,烘焙上述薄膜;通过在275到350℃和气体气氛下加热薄膜1秒钟到4小时来退火上述薄膜;和,处理上述退火薄膜以从退火薄膜中除去聚(苯乙烯)嵌段和将退火薄膜中的聚(硅氧烷)嵌段转换成SiOx。
Description
技术领域
发明涉及自组装嵌段共聚物领域。特别地,本发明针对用于沉积在基材表面上的聚(苯乙烯)-b-聚(二甲基硅氧烷)嵌段共聚物薄膜组合物的特殊的热退火工艺。
背景技术
某些嵌段共聚物,其由两个或更多不同的均聚物末端相连接而组成,是已知的自组装成具有10纳米至50纳米(nm)特征尺寸的周期性微域。使用这种微域来在表面形成图案的可能性引起越来越多的兴趣,这是由于使用光刻法在纳米级尺寸(尤其是低于45nm)形成图案的昂贵和困难。
然而,在基材上控制嵌段共聚物微域的横向分布仍然是一个挑战。这个问题之前使用光刻预定义地形图和/或基材的化学印刷来解决。先前的研究显示了以薄片形式的自组装嵌段聚合物微域(micro domain)能够随着基材的化学图案取向,在靠近化学预图案的地方产生周期性。其他研究显示,通过控制地形图预图案的底部和侧壁上的嵌段共聚物的表面润湿性能,该薄片(lamellae)能够随着地形图预图案(pre-pattern)取向。该薄片形成比基材预图案更小尺寸的线/空比图案,把地形图预图案细分成更高频率的线型图案;即,具有更小节距的线型图案。对于地形图和/或化学引导预图案,嵌段共聚物图案化的一个限制是在预图形表面的任意处形成图案的倾向。
目前,在给定的基材(例如,场效应晶体管中的门)上各种特征的尺寸缩小的能力受制于用于曝光光刻胶的光的波长(即,193nm)。这些限制在具有<50nm的关键尺寸(CD)的特征的生产中产生了重要的挑战。在自组装过程中,传统嵌段共聚物的使用在取向控制和长范围有序方面存在困难。此外,这种嵌段共聚物在接下来的工艺步骤中经常具有不足的抗蚀能力。
使用直接自组装技术,聚(苯乙烯)和聚(二甲基硅氧烷)的二嵌段共聚物可以应用在纳米级尺寸(尤其是,低于45nm)的图案化中。然而,本领域的传统知识是使用聚(苯乙烯)-b-聚(二甲基硅氧烷)嵌段共聚物在这种操作中不能有效的热退火。因此,本领域技术人员对于聚(苯乙烯)-b-聚(二甲基硅氧烷)嵌段共聚物的加工,发展出了各种代替的技术。
例如,在美国专利公开号2011/0272381;Millward等中,公开了用于加工诸如聚(苯乙烯)-b-聚(二甲基硅氧烷)的二嵌段共聚物的溶剂退火方法。
然而,还存在加工用于直接自组装应用的聚(苯乙烯)-b-聚(硅氧烷)二嵌段共聚物组合物的替代方法的需要。
发明内容
本发明提供一种用于加工基材的方法,包含:提供具有表面的基材;提供共聚物组合物,包含:聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分,其中聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分的数均分子量是5到1,000kg/mol;和,抗氧化剂;施加上述共聚物组合物的薄膜到基材表面;任选地,烘焙上述薄膜;通过在275到350℃和气体气氛下加热薄膜1秒钟到4小时来退火上述薄膜;和,处理上述退火薄膜以从退火薄膜除去聚(苯乙烯)嵌段和将退火薄膜中的聚(硅氧烷)嵌段转换成SiOX。
本发明提供一种用于加工基材的方法,包含:提供具有表面的基材;提供共聚物组合物,包含:聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分,其中聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分的数均分子量是5到1,000kg/mol;和,抗氧化剂,其中抗氧化剂选自下列组成的组:包含至少一个2,6-二-叔-丁基苯酚残基的抗氧化剂;包含至少一个根据下列结构式所示的残基的抗氧化剂
包含至少一个根据下列结构式所示的残基的抗氧化剂
包含至少一个根据下列结构式所示的残基的抗氧化剂
和,
其混合物;施加上述共聚物组合物的薄膜到基材表面;任选地,烘焙上述薄膜;通过在275到350℃和气体气氛下加热薄膜1秒钟到4小时来退火上述薄膜;和,处理上述退火薄膜以从退火薄膜除去聚(苯乙烯)嵌段和将退火薄膜中的聚(硅氧烷)嵌段转换成SiOX。
本发明提供一种用于处理基材的方法,包含:提供具有表面的基材;提供共聚物组合物,包含:聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分,其中聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分的数均分子量是5到1,000kg/mol;和,抗氧化剂,其中抗氧化剂组分选自由下列组成的组;
和,其混合物;施加上述共聚物组合物的薄膜到基材表面;任选地,烘焙上述薄膜;通过在275到350℃和气体气氛下加热薄膜1秒钟到4小时来退火上述薄膜;和,处理上述退火薄膜以从退火薄膜除去聚(苯乙烯)嵌段和将退火薄膜中的聚(硅氧烷)嵌段转换成SiOX。
本发明提供一种根据本发明的方法加工的基材。
本发明提供已经根据本发明的方法加工的基材,其中基材的表面包含亚光刻SiOX特征。
附图说明
图1是根据对比实施例F1制备的产品薄膜的由顶向下扫描电子显微镜(″SEM″)图像的描绘。
图2是根据实施例7制备的产品薄膜的由顶向下扫描电子显微镜(″SEM″)图像的描绘。
图3是根据实施例8制备的产品薄膜的由顶向下扫描电子显微镜(″SEM″)图像的描绘。
具体实施方式
本发明提供一种用于形成光刻有用的线和空间特征的方法,该线和空间特征用于接下来的图案转移加工,该图案转移加工可构造需要微观刻蚀或为微图案化表面的设备(例如,微电子,微传感器和生物芯片)。本发明的方法可形成具有节距尺寸的图案,该节距尺寸可被相对于通过传统光刻法在基材上形成的引导图案的整数因子除。形成这种高分辨的具有更小尺寸(例如,使用传统光刻技术生产的一半或四分之一)图案的能力能够使在例如设计和生产半导体芯片领域形成全新技术。
用于本文和所附的权利要求书中的术语“PSt-b-PSi嵌段共聚物”是聚(苯乙烯)-嵌段-聚(硅氧烷)二嵌段共聚物的缩写。
本文和附加的权利要求中使用的关于本发明的嵌段共聚物的术语“MN”为依据本文实施例使用的方法确定的嵌段共聚物的数均分子量(以g/mol计)。
本文和附加的权利要求中使用的关于本发明的嵌段共聚物组合物中使用的PSt-b-PSi混合物的术语“MN-Blend或混合数均分子量”为PSt-b-PSi混合物中包括的PSt-b-PSi嵌段共聚物的数均分子量的加权平均值。
本文和附加的权利要求中使用的关于本发明的嵌段共聚物的术语“MW”为依据本文实施例使用的方法确定的嵌段共聚物的重均分子量(以g/mol计)。
本文和附加的权利要求中使用的关于本发明的嵌段共聚物组合物中使用的PSt-b-PSi混合物的术语“MW-Blend或混合重均分子量”为PSt-b-PSi混合物中包括的PSt-b-PSi嵌段共聚物的重均分子量的加权平均值。
本文和附加的权利要求中使用的关于本发明的嵌段共聚物的术语“PD”为依据下述等式确定的嵌段共聚物的多分散性:
本文和附加的权利要求中使用的关于单一PSt-b-PSi嵌段共聚物的(a)PSt-b-PSi嵌段共聚物组分的术语“平均分子量”,指的是这种PSt-b-PSi嵌段共聚物的数均分子量;和关于两种或更多不同PSt-b-PSi嵌段共聚物的(b)PSt-b-PSi嵌段共聚物组分的术语“平均分子量”,指的是混合物中两种或更多不同的PSt-b-PSi嵌段共聚物的数均分子量,MN,的加权平均值。
本文和附加的权利要求中使用的关于PSt-b-PSi嵌段共聚物的术语“WfPS”是嵌段共聚物中聚(苯乙烯)嵌段的重量百分比。
本文和附加的权利要求中使用的关于本发明的嵌段共聚物组合物中使用的PSt-b-PSi混合物的术语“WfPS-Blend或混合聚(苯乙烯)重量分数”是PSt-b-PSi混合物中包括的PSt-b-PSi嵌段共聚物中的聚(苯乙烯)嵌段的重量百分比的加权平均值。
本文和附加的权利要求中使用的关于本发明的PSt-b-PSi嵌段共聚物的术语“WfPSi”是嵌段共聚物中聚(硅氧烷)嵌段的重量百分比。
本文和附加的权利要求中使用的关于本发明的嵌段共聚物组合物中使用的PSt-b-PSi混合物的术语“WfPSi-BLEND或混合聚(硅氧烷)重量分数”是PSt-b-PSi混合物中包括的PSt-b-PSi嵌段共聚物中的聚(硅氧烷)嵌段的重量百分比的加权平均值。
嵌段共聚物为两个或更多不同单体合成的聚合物,并且表现出两个或多个化学上不同的聚合物链段,但仍是相互共价键连接。二嵌段共聚物是衍生自两个不同单体(例如,A和B)的嵌段共聚物的特殊种类,其具有包括A残基聚合嵌段和B残基聚合嵌段共价键结合的结构(例如,AAAAA-BBBBB)。
用于本发明方法的共聚物组合物包含聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分和抗氧化剂;其中聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分选自由下列组成的组:(a)单一PSt-b-PSi嵌段共聚物和(b)至少两种不同的PSt-b-PSi嵌段共聚物的混合物。
当用于本发明方法的聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分是单一PSt-b-PSi嵌段共聚物时,使用的PSt-b-PSi嵌段共聚物优选显示出5到1,000kg/mol(优选25到1,000kg/mol;更优选30到1,000kg/mol;更加优选30到100kg/mol;最优选30到60kg/mol)的数均分子量,MN;和1到3(优选1到2;最优选1到1.2)的多分散性,PD。优选,所选的用于本发明方法的聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物显示出0.34到0.64(优选0.47到0.50)的聚(硅氧烷)重量百分数,WfPSi。优选,所选的用于本发明方法的聚(苯乙烯)-B-聚(硅氧烷)嵌段共聚物显示出0.19到0.33(优选0.21到0.28;最优选0.22到0.25)的聚(硅氧烷)重量百分数,WfPSi。根据本文提供的教导,通过选择和控制薄膜沉积条件,例如:(a)基材的表面能(即,通过用接入材料预处理基材的表面),(b)沉积的共聚物组合物的薄膜的厚度,(c)沉积的共聚物组合物的烘烤处理(profile)(即,烘烤温度和烘烤时间)和(d)沉积的共聚物组合物的退火处理(即,退火温度和退火时间),本领域普通技术人员能够使用本发明的方法沉积包含单一PSt-b-PSi嵌段共聚物的这种共聚物组合物,其中在沉积的共聚物组合物中的圆柱形聚(二甲基硅氧烷)域将自组装以使沿着它们平行于基材表面的对称轴取向,或沿着它们垂直于基材表面的对称轴取向或沿着它们平行于和垂直于基材表面对称轴相结合的取向。
当用于本发明方法的聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分是至少两种不同的的PSt-b-PSi嵌段共聚物的混合物时,上述至少两种不同的PSt-b-PSi嵌段共聚物优选选自具有1到1,000kg/mol(优选1到100kg/mol;最优选5到60kg/mol)的数均分子量MN;和1到3(优选1到2;最优选1到1.2)的多分散性PD的PSt-b-PSi嵌段共聚物。所使用的至少两种不同的PSt-b-PSi嵌段共聚物的混合物优选显示出5到1,000kg/mol(优选25到1,000kg/mol、更优选30到1,000kg/mol;更加优选30到100kg/mol;最优选30到60kg/mol)的混合数均分子量,MN-Blend。优选,所使用的至少两种不同的PSt-b-PSi嵌段共聚物的混合物显示出0.34到0.64(优选0.47到0.50)的混合物聚(硅氧烷)重量百分数,WfPSi-Blend。优选,所使用的至少两种不同的PSt-b-PSi嵌段共聚物的混合物显示出0.19到0.33(优选0.21到0.28;最优选0.22到0.25)的混合物聚(硅氧烷)重量百分数,WfPSi-Blend。优选聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分包含至少两种不同的PSt-b-PSi嵌段共聚物的混合物。当在相等分子量(即,MN-single PSt-b-PSi=MN-Blend)和相等聚(二甲基硅氧烷)重量百分数(即,WfPSi-singiepst-b-psi=WfPSi-Blend)的基础上比较,包含PSt-b-PSi嵌段共聚物混合物的共聚物组合物比单一PSt-b-PSi嵌段共聚物组合物提供更有意义的价值,这在于在用于形成周期性纳米结构,例如含硅基材上的线/空间图形的直接自组装领域,上述混合物体系倾向于显示出更快的退火条件和更低的缺陷率(在相等分子量和PSi重量百分数的基础上比较)。根据本文提供的教导,通过选择和控制薄膜沉积条件,例如:(a)基材的表面能(即,通过用接入材料预处理基材的表面),(b)沉积的共聚物组合物的薄膜的厚度,(c)沉积的共聚物组合物的烘烤处理(profile)(即,烘烤温度和烘烤时间)和(d)沉积的共聚物组合物的退火处理(即,退火温度和退火时间),本领域普通技术人员能够使用本发明的方法沉积包含单一PSt-b-PSi嵌段共聚物的这种共聚物组合物,其中在沉积的共聚物组合物中的圆柱形聚(二甲基硅氧烷)域将自组装以使沿着它们平行于基材表面的对称轴取向,或沿着它们垂直于基材表面的对称轴取向或沿着它们平行于和垂直于基材表面对称轴相结合的取向。
优选,用于本发明方法的聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组合物具有聚(苯乙烯)嵌段,其中上述聚(苯乙烯)嵌段包含来自选自苯乙烯、氘代苯乙烯、苯乙烯嵌段改性单体和氘代苯乙烯嵌段改性单体中的至少一种的残基。更优选,其中聚(苯乙烯)嵌段包含0到100wt%(优选,0到15wt%;更优选,0.001到15wt%)的苯乙烯嵌段改性单体衍生单元和氘代苯乙烯嵌段改性单体衍生单元的组合。
优选,上述苯乙烯嵌段单体选自由下列组成的组:羟基苯乙烯(例如,4-羟基苯乙烯;3-羟基苯乙烯;2-羟基苯乙烯;2-甲基-4-羟基苯乙烯;2-叔丁基-4-羟基苯乙烯;3-甲基-4-羟基苯乙烯;2-氟4-羟基苯乙烯;2-氯-4-羟基苯乙烯;3,4-二羟基苯乙烯;3,5-二羟基苯乙烯;3,4,5-三羟基苯乙烯;3,5-二甲基-4-羟基苯乙烯;3,5-叔丁基-4-羟基苯乙烯);甲硅烷氧基(siloxy)苯乙烯(例如,4-三甲基甲硅烷氧基苯乙烯;和3,5-二甲基-4-三甲基甲硅烷氧基苯乙烯);和4-乙酰氧基苯乙烯(例如,3,5-二甲基-4-乙酰氧基苯乙烯;3,5-二溴-4-乙酰氧基苯乙烯;3,5-二氯-4-乙酰氧基苯乙烯);和,其组合物。更优选的苯乙烯嵌段单体选自由下列组成的组:4-羟基苯乙烯;3-羟基苯乙烯;2-羟基苯乙烯;2-甲基-4-羟基苯乙烯;2-叔丁基-4-羟基苯乙烯;3-甲基-4-羟基苯乙烯;2-氟-4-羟基苯乙烯;2-氯-4-羟基苯乙烯;3,4-二羟基苯乙烯;3,5-二羟基苯乙烯;3,4,5-三羟基苯乙烯;3,5-二甲基-4-羟基苯乙烯;3,5-叔丁基-4-羟基苯乙烯;和,其组合物。最优选,上述苯乙烯嵌段改性单体选自由下列组成的组:4-羟基苯乙烯;3-羟基苯乙烯;2-羟基苯乙烯;和,其组合物。
优选,上述氘代苯乙烯嵌段单体选自由下列组成的组:氘代羟基苯乙烯(例如,氘代4-羟基苯乙烯;氘代3-羟基苯乙烯;氘代2-羟基苯乙烯;氘代2-甲基-4-羟基苯乙烯;氘代2-叔丁基-4-羟基苯乙烯;氘代3-甲基-4-羟基苯乙烯;氘代2-氟-4-羟基苯乙烯;氘代2-氯-4-羟基苯乙烯;氘代3,4-二羟基苯乙烯;氘代3,5-二羟基苯乙烯;氘代3,4,5-三羟基苯乙烯;氘代3,5-二甲基-4-羟基苯乙烯;氘代3,5-叔丁基-4-羟基苯乙烯);氘代甲硅烷氧基苯乙烯(例如,氘代4-三甲基甲硅完氧基苯乙烯;和氘代3,5-二甲基-4-三甲基甲硅烷氧基苯乙烯);氘代4-乙酰氧基苯乙烯(例如,氘代3,5-二甲基-4-乙酰氧基苯乙烯;氘代3,5-二溴-4-乙酰氧基苯乙烯;和氘代3,5-二氯-4-乙酰氧基苯乙烯);和,其组合物。更优选,上述氘代苯乙烯嵌段单体选自由下列组成的组:氘代4-羟基苯乙烯;氘代3-羟基苯乙烯;氘代2-羟基苯乙烯;氘代2-甲基4-羟基苯乙烯;氘代2-叔丁基-4-羟基苯乙烯;氘代3-甲基-4-羟基苯乙烯;氘代2-氟-4-羟基苯乙烯;氘代2-氯-4-羟基苯乙烯;氘代3,4-二羟基苯乙烯;氘代3,5-二羟基苯乙烯;氘代3,4,5-三羟基苯乙烯;氘代3,5-二甲基-4-羟基苯乙烯;氘代3,5-叔丁基4-羟基苯乙烯;和,其组合物。最优选,上述氘代苯乙烯嵌段改性单体选自下列组成的组:氘代4-羟基苯乙烯;氘代3-羟基苯乙烯;氘代2-羟基苯乙烯;和,其组合物。
优选,用于本发明方法的聚(硅氧烷)-b-聚(硅氧烷)嵌段共聚物组合物具有聚(硅氧烷)嵌段,其中上述聚(硅氧烷)嵌段包含来自选自硅氧烷单体和氘代硅氧烷单体中的至少一种的残基。更优选,其中聚(硅氧烷)嵌段包含>75wt%(更优选,>90wt%;最优选,>95wt%)的二甲基硅氧烷衍生单元。
优选,上述硅氧烷单体选自下列组成的组:芳基(芳基)硅氧烷(例如,苯基(苯基)硅氧烷);芳基(烷基)硅氧烷(例如,苯基(甲基)硅氧烷);烷基(烷基)硅氧烷(例如,二甲基硅氧烷;甲基(乙基)硅氧烷);卤代烷基(烷基)硅氧烷(例如、三氟丙基(甲基)硅氧烷);烷基硅氧烷;和,其组合物。更优选,上述硅氧烷单体选自下列组成的组:苯基(甲基)硅氧烷,二甲基硅氧烷、甲基(乙基)硅氧烷,三丙基(甲基)硅氧烷和其组合物。最优选,上述硅氧烷单体是二甲基硅氧烷。
优选,上述氘代硅氧烷单体选自下列组成的组:氘代芳基(芳基)硅氧烷(例如,氘代苯基(苯基)硅氧烷);氘代芳基(烷基)硅氧烷(例如,氘代本基(甲基)硅氧烷);氘代烷基(烷基)硅氧烷(例如,氘代二甲基硅氧烷;氘代甲基(乙基)硅氧烷);氘代卤代烷基(烷基)硅氧烷(例如、氘代三氟丙基(甲基)硅氧烷);氘代烷基硅氧烷;和,其组合物。更优选,上述氘代硅氧烷单体选自下列组成的组:氘代苯基(甲基)硅氧烷,氘代二甲基硅氧烷、氘代甲基(乙基)硅氧烷,氘代三丙基(甲基)硅氧烷和其组合物。最优选,上述氘代硅氧烷单体是氘代二甲基硅氧烷。
用于本发明方法的共聚物组合物包含抗氧化剂。优选,用于本发明方法的共聚物组合物包含>2wt%抗氧化剂(基于PSt-b-PSi嵌段共聚物组分的重量)。更优选,上述用于本发明方法的共聚物组合物包含>2到10wt%抗氧化剂(基于PSt-b-PSi嵌段共聚物组分的重量)。最优选,上述用于本发明方法的共聚物组合物包含5到10wt%抗氧化剂(基于PSt-b-PSi嵌段共聚物组分的重量)。
包含于用于本发明方法的共聚物组合物的抗氧化剂可选自主抗氧化剂和助抗氧化剂。优选,上述抗氧化剂选自下列组成的组:包含至少一个(优选至少两个;更优选至少三个;最优选三到四个)2,6-二叔-丁基苯酚部分的抗氧化剂;包含至少一个(优选至少两个;更优选至少三个;最优选三到四个)根据以下结构式的残基的抗氧化剂
和,包含至少一个(优选至少两个;最优选两个)根据以下结构式的残基的抗氧化剂
和,包含至少一个(优选至少两个;最优选两个)根据以下结构式的残基的抗氧化剂
和,其混合物。更优选,上述抗氧化剂选自下列组成的组:
和,其混合物。更加优选,上述抗氧化剂选自下列组成的组:
和
与一种或多种其他抗氧化剂的混合物。最优选,上述抗氧化剂是
优选,包含于用于本发明方法的共聚物组合物的抗氧化剂(或抗氧化剂的混合物)具有≥358g/mol的平均分子量。更优选,包含于用于本发明方法的共聚物组合物的抗氧化剂(或抗氧化剂的混合物)具有≥600g/mol的平均分子量。最优选,包含于用于本发明方法的共聚物组合物的抗氧化剂(或抗氧化剂的混合物)具有≥1,000g/mol的平均分子量。
优选,包含于用于本发明方法的共聚物组合物的抗氧化剂(或抗氧化剂的混合物)具有在760毫米汞柱(101.3kPa)下测量得到的>400℃的平均沸点温度。更优选,包含于用于本发明方法的共聚物组合物的抗氧化剂(或抗氧化剂的混合物)具有在760毫米汞柱(101.3kPa)下测量得到的>500℃的平均沸点温度。更加优选,包含于用于本发明方法的共聚物组合物的抗氧化剂(或抗氧化剂的混合物)具有在760毫米汞柱(101.3kPa)下测量得到的>700℃的平均沸点温度。仍然更加优选,包含于用于本发明方法的共聚物组合物的抗氧化剂(或抗氧化剂的混合物)具有在760毫米汞柱(101.3kPa)下测量得到的>800℃的平均沸点温度。最优选,包含于用于本发明方法的共聚物组合物的抗氧化剂(或抗氧化剂的混合物)具有在760毫米汞柱(101.3kPa)下测量得到的>1,000℃的平均沸点温度。
本发明的方法中使用的共聚物组合物,任选地进一步包含溶剂。适合用于共聚物组合物中的溶剂包括能够将聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分分散成为具有通过动态光散射测量的小于50nm平均流体动力学直径的颗粒或聚集体的液体,所述颗粒或聚集体(aggregate)的平均水力直径小于50nm,由动态光散射法测得。优选,使用的溶剂为选自丙二醇单甲醚醋酸酯(PGMEA),乙氧基乙基丙酸酯,苯甲醚,乳酸乙酯,2-庚酮,环己酮,醋酸戊酯,γ-丁内酯(GBL),N-甲基吡咯烷酮(NMP)和甲苯。更优选,使用的溶剂选自丙二醇单甲醚醋酸酯(PGMEA)和甲苯。最优选,使用的溶剂为甲苯。
本发明的方法中使用的共聚物组合物,任选地进一步包含添加剂。添加剂包括附加的聚合物(包括均聚物和无规共聚物);表面活性剂;光酸产生剂;热酸产生剂;猝灭剂;硬化剂;粘结促进剂;溶解速率改性剂;光固化剂;光敏剂;酸放大剂;增塑剂;取向控制剂;和交联剂。优选的用于嵌段共聚物组合物的添加剂包括表面活性剂。
使用的基材包括具有能涂覆本发明方法中的共聚物组合物的表面的任何基材。优选的基材包括层状基材。优选的基材包括含硅基材(例如,玻璃;二氧化硅;氮化硅;氧氮化硅;含硅半导体基材,诸如硅晶圆,硅晶圆片段,在绝缘基材上的硅,在蓝宝石基材上的硅,在基础半导体基底(base semiconductorfoundation)上的硅的外延层,硅-锗基材);塑料;金属(例如,铜,钌,金,铂,铝,钛和合金);氮化钛;和不含硅的半导体基材(不含硅的晶圆片段,不含硅的晶圆,锗,砷化镓和磷化铟)。最优选的基材为含硅基材。
任选地,在本发明的方法中,涂覆共聚物组合物的基材表面用接入(interposing)材料在应用共聚物组合物之前进行预处理。优选预处理材料以如下的方式起作用:连接层插入基材表面和共聚物组合物之间以增强聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分和基材之间的粘合性。优选,该接入材料形成选自图像层和取向控制层的层。
适合用于本发明方法的图像层包括,例如,能够图案化或选择性激活的任何类型的材料。这种材料包括,例如,聚合物刷和硅烷和硅氧烷化合物的自组装单层。
适合用于本发明方法的取向控制层包括,中性和非中性取向控制层。即,该取向控制层能在基材表面和共聚物组合物之间形成界面,即优选由聚(苯乙烯)或聚(硅氧烷)中的一种润湿——即,非中性取向控制层。中性取向控制层指的是在基材表面和共聚物组合物之间形成界面,即同样的由聚(苯乙烯)嵌段和聚(硅氧烷)嵌段二者润湿。
优选,在沉积共聚物组合物以促进共聚物组合物中的聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分的引导自组装之前用本发明的方法处预理基材。特别地,预处理能够促进用于引导嵌段共聚物膜的自组装的两个传统方法中的一个,即制图外延法和化学外延法。在制图外延法中,基材的表面用地形图案特征预图案化在基材的表面上(例如,沟,洞),其控制引导共聚物组合物的聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分中的聚(苯乙烯)和聚(硅氧烷)嵌段的自组装。
在化学外延法中,基材的表面用表现出组合的图案的薄膜来处理,其中在组合的图案的各部分之间的亲和度对于聚(苯乙烯)嵌段和聚(硅氧烷)嵌段不同。这种化学亲和度的不同对促进该共聚物组合物的聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分的直接自组装起作用。
优选,在本发明的方法中,插入层使用选自旋涂,浸涂,滚涂,喷除和层压(最优选旋涂)的方法形成在基材上。在应用插入层在基材表面上形成材料之后,该材料任选进一步加工除去任何残余溶剂。优选,插入层在高温下(例如,70-340℃)烘烤至少10秒至5分钟以从插入层中除去任何残余的溶剂。优选,烘烤过的插入层用能够从基材的表面除去未键连在插入层材料的任何残余的溶剂冲洗,然后在高温下(例如,70-340℃)再烘烤至少10秒至5分钟以除去任何残余溶剂。
本发明方法中,应用包含聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分和抗氧化剂的共聚物组合物的薄膜至基材表面上优选包含使用选自旋涂,浸涂,滚涂,喷涂和层压(最优选旋涂)的方法沉积共聚物组合物在基材表面上。在应用共聚物组合物的薄膜至基材上之后,该薄膜任选地进一步加工除去任何残余溶剂。优选,该薄膜在高温下(例如,70-340℃)烘烤至少10秒至5分钟以从沉积的共聚物组合物中除去任何残余的溶剂。
在本发明的方法中,共聚物组合物的沉积薄膜然后通过在275到350℃(更优选300到350℃;最优选320到350℃)的温度和气体气氛下加热薄膜热退火1秒钟到4小时(优选2秒钟到1小时;更优选30秒钟到1小时;最优选90秒钟到1小时)来使聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分能够自组装在基材表面上。优选,在选自空气、氮气和氩气的气体气氛下退火沉积薄膜。优选在具有≤150ppm(更优选≤10ppm;更加优选≤7.5ppm;进一步更加优选≤6.5ppm;最优选≤4ppm)的氧气浓度的气体气氛下退火沉积薄膜。更优选在具有≤150ppm(更有选≤10ppm;更加优选≤7.5ppm;进一步更加优选≤6.5ppm;最优选≤4ppm)的氧气浓度的氮气或氩气气氛下退火沉积薄膜。最优选在具有≤100ppm(优选≤7.5ppm;更优选≤6.5ppm;最优选≤4ppm)的氧气浓度的氮气气氛下退火沉积薄膜。
在本发明的方法中,处理退火的薄膜来除去退火的薄膜中的聚(苯乙烯)嵌段和将退火的薄膜中的聚(硅氧烷)嵌段转变成SiOX,提供具有大量空隙(例如,垂直于基材表面的沟;或大量对称轴垂直于基材表面的圆柱状SiOX柱)的薄膜产品。上述处理包含:将薄膜暴露于显示出对薄膜中的聚(苯乙烯)嵌段和薄膜中的聚(硅氧烷)嵌段差别反应性的条件,来促进聚(苯乙烯)域从退火的薄膜中的除去和聚(硅氧烷)域到SiOX的转变。优选,上述处理包含:任选地,将退火的薄膜暴露于含卤素的等离子(例如,CF4)来除去在退火的薄膜表面上形成的任何润湿层;继之以将退火的薄膜暴露于反应性等离子或反应离子刻蚀气氛来除去聚(苯乙烯)域和将聚(硅氧烷)域转变成SiOX。最优选,上述处理包含:将退火的薄膜暴露于含卤素的等离子来除去在退火的薄膜表面上形成的任何润湿层;然后将退火的薄膜暴露于反应性等离子或反应离子刻蚀气氛,其中上述气氛包含由低压离子化氧化气体(优选O2)形成的等离子体;其中除去退火的薄膜中的聚(苯乙烯)域和将退火的薄膜中的聚(硅氧烷)相转变成SiOX。
在下列实施例中将详细描述本发明的一些具体方案。
下列材料在用于本发明实施例之前,都通过装填有活性A-2级氧化铝的柱,也就是四氢呋喃(纯度99.9%,来自Aldrich),苯乙烯(来自Aldrich)和环己烷(HPCL级,来自Fischer)。用于本发明实施例所使用的所有其他材料都是商购材料即使用购得品。
本发明实施例中记录的薄膜的厚度使用NanoSpec/AFT2100薄膜厚度测量工具来测量。薄膜的厚度通过穿过衍射光栅的白光的干涉来确定。所谓“硅上的聚亚酰胺”标准问题用于分析组分波长(380-780nm)以确定薄膜厚度。聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组合物和刷层的厚度作为一个聚合物层一起来测量。该记录的薄膜厚度是嵌段共聚物组合物和刷层结合的厚度。
实施例中记录的数均分子量,MN,和多分散性值,在装配有Agilent1100系列折射率和MiniDAWN光扫描检测器(Wyatt Technology Co.)的Agilent1100系列LC系统中,通过凝胶渗透色谱(GPC)来测量。样品以大约1mg/mL的浓度溶解在HPCL级四氢呋喃(THF)中,并且通过0.20μm针筒式滤器过滤,然后通过两个PLGel300x7.5mm Mixed C柱(5mm,Polymer Laboratories,Inc.)米汪射。保持1mL/min的流动速率和35℃的温度。该柱使用窄分子量标准PS(EasiCalPS-2,Polymer Laboratories,Inc.)来校准。
涉及实施例的质子核磁共振(1H NMR)光谱的结果通过Varian INOVA400MHz NMR光谱完成。使用含氘化的四氢呋喃,THF。使用10秒的延迟时间来确保质子的完全弛豫以定量整合。有关四甲基硅烷的化学变换被记录。
实施例1:羟基-封端的聚苯乙烯刷的制备
在2升玻璃反应器中在氮气气氛下添加环己烷(1500g)。然后通过套管添加苯乙烯(50.34g)至反应器中。然后反应器中的物质被加热至40℃。然后稀释在环己烷中浓度为0.32M的仲丁基锂(19.18g)溶液通过套管被快速的添加至反应器中,导致反应器中的物质变黄。反应器中的物质搅拌30分钟。然后反应器中的物质冷却至30℃。然后环氧乙烷(0.73g)被传送至反应器中。反应器中的物质搅拌15分钟。然后将20mL的HCl在甲醇中的1.4M的溶液添加至反应器中。然后反应器中的聚合物以500mL聚合物溶液/1250mL异丙醇的比率通过沉淀在异丙醇中来分离。然后过滤得到的沉淀且在真空烘箱中在60℃下干燥过夜,得到42g羟基封端的聚苯乙烯刷产品。该羟基封端的聚苯乙烯产品表现出7.4kg/mol的数均分子量,MN和1.07多分散性,PD。
实施例2:PSt-b-PSi二嵌段共聚物的制备
在氩保护气氛下,将环己烷(90mL)和苯乙烯(17.1g)加入到500mL圆底反应器中。然后迅速将0.7mL注料量的1.4M仲-丁基锂环己烷溶液经过套管加入到反应器中,导致反应器中的物料变为黄-橙色。搅拌反应器物料30分钟。然后从反应器中取出一小部分,将其加入到包含无水甲醇的小圆底烧瓶中进行形成的聚苯乙烯嵌段的凝胶渗透色谱分析。接下来将2,2,5,5-四甲基二硅呋喃(472mg)加入到反应器中。橙色慢慢地开始褪色,并且1小时之后,反应器中物料的颜色变为淡黄色。然后将10.5g的新升华的六甲基环三硅氧烷转移到反应器中。反应器中的物料反应1.5小时直到反应器中的物料变为无色。然后把无水四氢呋喃(90mL)加入到反应器中并且继续进行反应3.25小时。然后将三甲基氯硅烷(1mL)加入到反应器中猝灭反应。通过在500mL的甲醇中沉淀分离产品并过滤。用额外的甲醇洗涤后,聚合物重复溶解在150mL的二氯甲烷中,用去离子水洗涤三次然后在500mL甲醇中重新沉淀。然后过滤聚合物并且在70℃的真空干燥炉中干燥过夜,得到20.5g。聚(苯乙烯)-b-聚(二甲基硅氧烷)嵌段共聚物产品显示出24kg/mol的数均分子量,MN;1.01的多分散性,PD和28wt%的聚(硅氧烷)含量(通过1H NMR确定)。
对比实施例S1和实施例3-5共聚物组合物的制备
对比实施例S1和实施例3-5中,通过将根据实施例2制备的PSt-b-PSi嵌段共聚物溶解在丙二醇单甲醚乙酸酯(购自陶氏化学公司的PMA)中制备用于薄膜沉积的具有1.6wt%的固含量的碱性旋涂溶液。将表1中标明的抗氧化剂加入到上述碱性旋涂溶液从而在最终的旋涂溶液中得到标明的浓度。
表1
以商品名称购自BASF
以商品名称购自BASF。
实施例6:基材的制备
通过以3,000rpm的转速在其上旋涂1.5wt%(固体)的根据实施例1制备的羟基-封端聚苯乙烯刷的甲苯溶液1分钟来改性具有原生氧化物层的硅基材表面。然后将基材置于设定在150℃的电炉中1分钟。然后将基材置于设定在250℃的和氮保护气氛下的电炉中20分钟来退火沉积的刷层。然后通过首先将基材浸泡在甲苯1分钟然后在3,000rpm的转速下旋转干燥1分钟,从而用甲苯漂洗基材来洗去任何未粘合的聚合物。然后将基材置于设定在110℃的电炉中烘焙1分钟。
对比实施例F1和实施例7-8:在氮气下的薄膜制备
使用0.2μm的Whatman针筒过滤器手动过滤每一个根据对比实施例S1和实施例3-4制备的旋涂溶液。在对比实施例F1和实施例7-8中,然后在2,500rpm的转速下分别将由对比实施例S1和实施例3-4制备的已过滤旋涂溶液旋涂在根据实施例6制备的独立聚(苯乙烯)刷基材上。然后将基材置于设定在150℃的电炉中1分钟。然后将基材置于设定在340℃的和<10ppm的氧气的氮气气氛下的电炉中一小时来退火沉积薄膜。
在每个气氛薄膜交界面处的退火薄膜上形成PDMS表面润湿层。然后使用两个连续反应性离子刻蚀(RIE)步骤(上述反应性离子刻蚀(RIE)步骤使用PlasmaTherm790i RIE)处理退火薄膜,以露出沉积薄膜的嵌段共聚物形态。首先,利用短时间的CF4等离子体(10mT,50W)RIE处理(8秒钟的后等离子体稳定)来击穿聚(二甲基硅氧烷)的表面润湿层。然后,采用O2等离子体(6mTorr,90W)RIE处理(25秒钟的后等离子体稳定)来除去聚苯乙烯和将PDMS转变为SiOx。
然后使用Zeiss/Leo Gemini982扫描电子显微镜检测等离子体处理的薄膜。使用双面碳带将测试样品固定在SEM载物台上和在分析之前鼓吹氮气。汇总每个测试样品放大50,000倍的图像。在图1-3中分别显示根据对比实施例F1和实施例7-8制备的薄膜产品的由顶向下SEM图像。根据对比实施例F1和实施例7-8中每一个制备的薄膜产品每个都显示出具有间距L0的指纹图案,L0为27nm。
Claims (10)
1.一种用于加工基材的方法,所述方法包括∶
提供具有表面的基材;
提供共聚物组合物,所述共聚物组合物包括:
聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分,其中聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分的数均分子量是5到1,000kg/mol;和,
抗氧化剂;
施加上述共聚物组合物的薄膜到基材表面;
任选地,烘焙上述薄膜;
通过在275到350℃和气体气氛下加热薄膜1秒钟到4小时来退火上述薄膜;和,
处理上述退火薄膜以从退火薄膜中除去聚(苯乙烯)嵌段和将退火薄膜中的聚(硅氧烷)嵌段转换成SiOx。
2.根据权利要求1的方法,其中上述抗氧化剂选自下列组成的组:
包含至少一个2,6-二-叔-丁基苯酚残基的抗氧化剂;
包含至少一个根据下列结构式所示的残基的抗氧化剂
包含至少一个根据下列结构式所示的残基的抗氧化剂
包含至少一个根据下列结构式所示的残基的抗氧化剂
和,其混合物。
3.根据权利要求1的方法,其中上述抗氧化剂选自下组:
和,其混合物。
4.根据权利要求2的方法,其中提供的聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分是单一聚(苯乙烯)-b-聚(硅氧烷)二嵌段共聚物,其具有25到1,000kg/mol的数均分子量,MN;1到3的多分散性,PD;和0.19到0.33的聚(硅氧烷)重量百分数,WfPSi。
5.根据权利要求4的方法,其中上述提供的共聚物组合物进一步包含溶剂;其中上述溶剂选自下列组成的组:丙二醇单甲醚乙酸酯PGMEA、乙氧基乙基丙酸酯、苯甲醚、乳酸乙酯、2-庚酮、环己酮、醋酸戊酯、γ-丁内酯GBL、N-甲基吡咯烷酮NMP和甲苯。
6.根据权利要求2的方法,其中聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物组分是至少两种不同的聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物的混合物;
其中上述至少两种不同的聚(苯乙烯)-b-聚(硅氧烷)嵌段共聚物选自具有1到1,000kg/mol的数均分子量,MN;和,1到3的多分散性,PD的(苯乙烯)-b-聚(硅氧烷)嵌段共聚物;和,其中上述混合物显示出25到1,000kg/mol的混合数均分子量,MN-Blend。
7.根据权利要求6的方法,其中上述混合物显示出0.19到0.33的聚(硅氧烷)在混合重量百分数,WfPSi-Blend。
8.根据权利要求7的方法,其中上述提供的共聚物组合物进一步包含溶剂;其中上述溶剂选自下列组成的组:丙二醇单甲醚乙酸酯PGMEA、乙氧基乙基丙酸酯、苯甲醚、乳酸乙酯、2-庚酮、环己酮、醋酸戊酯、γ-丁内酯GBL、N-甲基吡咯烷酮NMP和甲苯。
9.根据权利要求1的方法,其中上述气体气氛是具有≤100ppm的氧气的氮气气氛。
10.一种根据权利要求1的方法加工的基材。
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