CN101060095B - 形成受控的空隙的材料和方法 - Google Patents
形成受控的空隙的材料和方法 Download PDFInfo
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- CN101060095B CN101060095B CN2007101035756A CN200710103575A CN101060095B CN 101060095 B CN101060095 B CN 101060095B CN 2007101035756 A CN2007101035756 A CN 2007101035756A CN 200710103575 A CN200710103575 A CN 200710103575A CN 101060095 B CN101060095 B CN 101060095B
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- air gap
- ring
- formation air
- general formula
- layer
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Images
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Abstract
形成受控的空隙的材料和方法,本发明是在基底上形成气隙的方法,该方法包括:提供基底;通过沉积至少一种牺牲材料前体来沉积牺牲层;沉积复合层;除去复合层中的成孔剂以形成多孔层和使层状基底与除去介质接触以基本上除去牺牲材料并且在基底内提供气隙;其中至少一种牺牲材料前体选自有机成孔剂;硅和极性溶剂可溶的金属氧化物和其混合物。
Description
相关申请的交叉参考
本申请要求于2006年4月18日提交的美国临时申请60/792,793的权益。该临时申请的公开内容在这里通过参考进行引用。
发明背景
在微电子和纳米技术工业中均希望能够沉积能作为制备的辅助材料但一旦制备完成能容易除去的材料。在纳米技术领域中一个实例是使用SiO2作为制备的辅助材料以帮助制备硅悬臂结构。一旦制备完成,能通过HF水溶液刻蚀除去SiO2而没有影响硅。然而使用水溶液除去SiO2,由于在水干燥过程中的毛细管效应能引起小结构的坍塌,例如在悬臂制备中。也已经报道能使用XeF2相对于SiO2选择性的刻蚀硅用于该制备,硅覆盖有薄的有机膜,XeF2能通过该有机膜进行扩散。
在微电子工业中使用牺牲材料的一个实例是使用牺牲有机材料以在有机硅酸盐玻璃(OSG)中引入空隙以制备多孔OSG。这些空隙的产生将显著地降低材料的介电常数,因为空气的介电常数是1.0,而OSG材料的介电常数通常>2.7。通过引入有效介电常数为1.0的气隙,获得微电子制备中介电常数的下限。牺牲有机层的使用是实现这一种希望的方法。
能通过各种方式在半导体基底中所述的形成气隙。在器件中所述的形成气隙的一种方法是通过沉积差的保形材料,当在凸起表面间具有间隙的基底顶部沉积时,在这些表面间形成气隙或空隙。在这方面,如图1所示,当间隙部分填充差的保形介电材料时,在一对互连引线间的间隙中所述的形成气隙。该差的保形材料可以通过例如化学气相沉积或其它方式进行沉积。然而,该方法对于目前在铜集成中使用的双层镶嵌方法(例如参见6,057,226)是不适合的。
美国专利申请号2002/0149085和美国专利号6,472,719B1;6,211,057B1;6,297,125B1;6,268,277B1;6,238,987B1和6,228,763B1公开了方法,其中牺牲材料由具有高HF刻蚀率的旋涂玻璃或化学气相沉积的含有氧化物的材料构成,后者被桥层加帽,桥层具有在其中形成的开口。然后使用稀释的HF通过开口除去旋涂的材料。在图2中参见该技术。
美国专利申请号US20040099951A1;美国20040094821A1和2002/1016888和2002/002563和美国专利号6,316,347;6,329,279;和6,498,070;6,713,835B1;6,720,655B1公开了方法,其中牺牲材料是被桥层加帽的有机聚合物,桥层具有一个或多个开口,通过在惰性环境下的热退火或使用氧化剂例如分子氧(O2)烧除以除去聚合物。
发明概述
本发明是在基底中所述的形成气隙的方法。在本发明的一个实施方式中,所述方法包括:提供基底;在基底上沉积具有至少一种有机前体的牺牲层;在基底上沉积具有成孔剂和至少一种含有氧化硅的前体或OSG前体的复合材料层,该成孔剂与牺牲层中的至少一种有机前体相同;对具有牺牲层和复合材料层的基底应用能量以除去牺牲层而提供气隙和除去成孔剂而形成多孔层。
在本发明的另一实施方式中,所述方法包括:提供基底;提供基底;沉积包括硅的牺牲层;沉积具有成孔剂和至少一种含有氧化硅的前体或有机硅酸盐玻璃(OSG)前体的复合层;对具有牺牲层和复合层的基底应用能量以除去成孔剂而形成多孔层;使具有牺牲层和多孔层的基底与能够通过多孔层扩散的含氟试剂在减少的压力下进行接触,以选择性地除去牺牲层而形成气隙。
在本发明的又一实施方式中,所述方法包括:提供基底;沉积具有金属前体的极性溶剂可溶解的金属氧化物牺牲层;沉积具有成孔剂和至少一含硅前体或有机硅酸盐玻璃(OSG)前体的复合层;对具有牺牲层和复合层的基底应用能量以除去成孔剂而形成多孔层;使具有牺牲层和多孔层的基底与极性能够通过多孔层扩散的溶剂接触,以除去牺牲层而形成气隙。
在本发明的另一实施方式中,所述方法包括:提供基底;沉积具有金属前体的极性溶剂可溶的金属氧化物牺牲层;沉积具有成孔剂和至少一种含有氧化硅的前体或有机硅酸盐玻璃(OSG)前体的复合层,该成孔剂与牺牲层中极性溶剂可溶的金属氧化物相同;使具有牺牲层和复合层的基底与极性溶剂接触以除去成孔剂而形成多孔层和除去牺牲层而形成气隙。
附图简述
图1显示通过现有技术的差的步骤覆盖形成的气隙的截面图。
图2显示通过现有技术的桥接层中的空隙除去材料而形成气隙结构的截面图。
图3显示图解说明形成本发明结构的方法递进步骤的截面图,其中使用应用的能量除去空隙空间中的牺牲材料。
图4显示图解说明本发明可替换的方法和实施方式的递进步骤的截面图,其中使用选择性的刻蚀试剂BrF3来除去空隙空间中的硅牺牲材料。
图5显示图解说明本发明另一可替换方法和实施方式的递进步骤的截面图,其中使用极性溶剂例如水来除去空隙空间中的GeO2牺牲材料。
图6显示形成双层镶嵌铜金属互连结构的一种可能途径。
图7显示形成单嵌入式铜金属互连结构的一种可能途径。
图8显示形成双层镶嵌铜金属互连结构的另一可能途径。
图9A、9B和9C是通过本发明制备的具有空隙空间的实际结构的扫描电镜图像。
发明的详细描述
随着电子器件尺寸的持续减少,需要具有非常低介电常数的层间介电(ILD)材料。在过去12年间,介电材料已经从SiO2发展到FSG’s、到OSG’s和现在发展到具有2.0介电常数的多孔OSG’s。为了获得低于2.0的介电常数,必须在OSG薄膜中引入25%或更多的孔隙率。当OSG薄膜中引入的孔隙率量增加时,不仅降低介电常数而且引起机械性能的更大降低。
例如具有介电常数2.9的致密OSG薄膜具有大约3.0GPa的机械硬度。而通过我们PDEMSTM技术(参见例如美国专利6,583,048和美国专利6,846,515,在这里通过参考进行引用),具有大约25%孔隙率的多孔OSG材料具有2.2的介电常数,但仅具有0.8GPa的机械硬度。将该趋势外延到更低的介电常数,具有低于1.9介电常数的材料可能具有低于0.3GPa的机械硬度。我们已经观察到的另一趋势是:当孔隙率百分比增加时,互连路径长度相应增加。通过正电子湮没寿命(PALS)测量的互连路径长度是正电子元素能进行迁移而没有发生碰撞的最长距离的量度,或是连接孔的最长弦。认为互连对于原子层沉积(ALD)考虑和对于与湿处理例如抗蚀剂显影剂、抗蚀剂剥离剂和CMP料浆的相互作用是重要的。因此,认为在k低于大约1.9的一些情况下,ILD提供差的耐机械性或耐阻挡性,在多孔OSG薄膜和气隙间的差异开始消失。
迄今,气隙的制备已经集中在三种主要途径:(i)使用非常不保形的SiO2沉积,导致大的匙孔结构作为气隙,(ii)通过旋涂方法或CVD使用热不稳定的聚合物材料进行沉积,(iii)通过使用O2等离子体的活性离子刻蚀下层薄膜或通过使用HF湿刻蚀进行气隙的各向同性刻蚀。
本发明描述了制备气隙或空隙空间的三种可替代的方法。所有这三种途径利用液体或气体通过多孔OSG或SiO2层进行扩散的能力。该层的孔隙率能在0.1-99体积%孔隙率,更优选10-50体积%孔隙率的范围。第一种方法利用有机牺牲材料产生气隙。这是使用例如用于多孔OSG薄膜制备的授予专利PDEMSTM产品的多孔介电层的推广。在该方法中,使用相同的有机前体,在复合层方法中,牺牲层和成孔剂与OSG共沉积。以这种方式,能利用一种有机材料用于牺牲层和用于制备多孔OSG。第二种方法与第一种方法相似,在由硅构成的牺牲材料上使用多孔加帽层。在该方法中,在图案化前或后、并在除去成孔剂以产生多孔SiO2或OSG层后,给牺牲层覆盖复合层,然后将制备的片子暴露于气体中,相对于SiO2或OSG,选择性地刻蚀硅,例如XeF2或BrF3能通过多孔SiO2或OSG层进行扩散以除去下面的硅结构并剩下空隙。第三种方法使用在极性溶剂中可溶的(即,水)牺牲无机材料例如GeO2或B2O3。在该方法中,在图案化前或后、并在除去成孔剂以产生多孔SiO2或OSG层后,给牺牲层覆盖复合层,然后将制备的片暴露于水或其它极性溶剂,水或其它极性溶剂能通过多孔SiO2或OSG层进行扩散以除去可溶性无机材料(即GeO2或B2O3)并剩下空隙。在水或极性溶剂中添加表面活性剂以提高通过多孔层的扩散是有利的,特别是如果多孔层是疏水的OSG材料。
下面是适用于本发明的氧化硅基前体的非限制性的实施例。在下面的化学式以及整个申请文件中的所有化学式中,术语“独立地”应理解为:主题R基团不仅相对于带有不同上标的其它R基团独立地进行选择,而且相对于任何其它类型相同的R基团独立地进行选择。例如在化学式R1 n(OR2)4-nSi中,当n=2或3时,两个或三个R1无需彼此相同或与R2相同。
-R1 n(OR2)3-nSi,其中R1能独立地为H、或C1-C4直链或支链的、饱和的、单或多不饱和的、环状的、部分或完全氟化的;R2独立地为H、或C1-C6直链或支链的、饱和的、单或多不饱和的、环状的、芳香族的、部分或完全氟化的,n是1-3。
-例如:二乙氧基甲基硅烷、二甲基二甲氧基硅烷
-R1 n(OR2)3-nSi-O-R3 m(OR4)3-m,其中R1和R3能独立地为H、或C1-C4直链或支链的、饱和的、单或多不饱和的、环状的、部分或完全氟化的;R2和R4能独立地为H、或C1-C6直链或支链的、饱和的、单或多不饱和的、环状的、芳香族的、部分或完全氟化的,n是1-3并且m是1-3。
-例如1,3二甲基-1,3-二乙氧基二硅氧烷
-R1 n(OR2)3-nSi-SiR3 m(OR4)3-m,其中R1和R3能独立地为H、或C1-C4直链或支链的、饱和的、单或多不饱和的、环状的、部分或完全氟化的;R2和R4能独立地为H、或C1-C6直链或支链的、饱和的、单或多不饱和的、环状的、芳香族的、部分或完全氟化的,n是1-3并且m是1-3。
-实例:1,2-二甲基-1,1,2,2-四乙氧基二硅氧烷
-R1 n(O(O)CR2)4-nSi,其中R1能独立地为H、或C1-C4直链或支链的、饱和的、单或多不饱和的、环状的、部分或完全氟化的;R2能独立地为H、或C1-C6直链或支链的、饱和的、单或多不饱和的、环状的、芳香族的、部分或完全氟化的,n是1-3。
-实例:二甲基二乙酰氧基硅烷
-R1 n(O(O)CR2)3-nSi-O-SiR3 m(O(O)CR4)3-m,其中R1和R3能独立地为H、或C1-C4直链或支链的、饱和的、单或多不饱和的、环状的、部分或完全氟化的;R2和R4能独立地为H、或C1-C6直链或支链的、饱和的、单或多不饱和的、环状的、芳香族的、部分或完全氟化的,n是1-3并且m是1-3。
-实例:1,3-二甲基-1,3-二乙酰氧基二硅氧烷
-R1 n(O(O)CR2)3-nSi-SiR3 m(O(O)CR4)3-m,其中R1和R3能独立地为H、或C1-C4直链或支链的、饱和的、单或多不饱和的、环状的、部分或完全氟化的;R2和R4能独立地为H、或C1-C6直链或支链的、饱和的、单或多不饱和的、环状的、芳香族的、部分或完全氟化的,n是1-3并且m是1-3。
-实例:1,2-二甲基-1,1,2,2-四乙酰氧基乙硅烷
-R1 n(O(O)CR2)3-nSi-O-SiR3 m(OR4)3-m,其中R1和R3能独立地为H、或C1-C4直链或支链的、饱和的、单或多不饱和的、环状的、部分或完全氟化的;R2能独立地为H、C1-C6直链或支链的、饱和的、单或多不饱和的、环状的、芳香族的、部分或完全氟化的;R4能独立地为C1-C6直链或支链的、饱和的、单或多不饱和的、环状的、芳香族的、部分或完全氟化的,n是1-3和m是1-3。
-实例:1,3-二甲基-1-乙酸基-3-乙氧基二硅氧烷
-R1 n(O(O)CR2)3-nSi-SiR3 m(OR4)3-m,其中R1和R3能独立地为H、或C1-C4直链或支链的、饱和的、单或多不饱和的、环状的、部分或完全氟化的;R2能独立地为H、C1-C6直链或支链的、饱和的、单或多不饱和的、环状的、芳香族的、部分或完全氟化的;R4能独立地为C1-C6直链或支链的、饱和的、单或多不饱和的、环状的、芳香族的、部分或完全氟化的,n是1-3并且m是1-3。
-实例:1,2-二甲基-1-乙酰氧基-2-乙氧基乙硅烷
-R1 n(OR2)p(O(O)CR4)4-(n+p)Si,其中R1能独立地为H、或C1-C4直链或支链的、饱和的、单或多不饱和的、环状的、部分或完全氟化的;R2能独立地为H、或C1-C6直链或支链的、饱和的、单或多不饱和的、环状的、芳香族的、部分或完全氟化的,和R4能独立地为H、或C1-C6直链或支链的、饱和的、单或多不饱和的、环状的、芳香族的、部分或完全氟化的,n是1-3并且p是1-3。
-实例:甲基乙酰氧基-叔丁氧基硅烷
-R1 n(OR2)p(O(O)CR4)4-n-pSi-O-SiR3 m(O(O)CR5)q(OR6)3-m-q,其中R1和R3能独立地为H、或C1-C4直链或支链的、饱和的、单或多不饱和的、环状的、部分或完全氟化的;R2和R6能独立地为C1-C6直链或支链的、饱和的、单或多不饱和的、环状的、芳香族的、部分或完全氟化的,以及R4和R5能独立地为H、或C1-C6直链或支链的、饱和的、单或多不饱和的、环状的、芳香族的、部分或完全氟化的,n是1-3、m是1-3、p是1-3并且q是1-3。
-实例:1,3-二甲基-1,3-二乙酰氧基-1,3-二乙氧基二硅氧烷
-R1 n(OR2)p(O(O)CR4)4-n-pSi-SiR3 m(O(O)CR5)q(OR6)3-m-q,其中R1和R3能独立地为H、或C1-C4直链或支链的、饱和的、单或多不饱和的、环状的、部分或完全氟化的;R2、R6能独立地为C1-C6直链或支链的、饱和的、单或多不饱和的、环状的、芳香族的、部分或完全氟化的,以及R4和R5能独立地为H、或C1-C6直链或支链的、饱和的、单或多不饱和的、环状的、芳香族的、部分或完全氟化的,n是1-3、m是1-3、p是1-3并且q是1-3。
-实例:1,2-二甲基-1,2-二乙酰氧基-1,2-二乙氧基乙硅烷
-式(OSiR1R3)x的环状硅氧烷,其中R1和R3能独立地为H、或C1-C4直链或支链的、饱和的、单或多不饱和的、环状的、部分或完全氟化的,并且x可以是2-8之间的任意整数。
-实例:1,3,5,7-四甲基环四硅氧烷、八甲基环四硅氧烷
能用于SiO2或OSG沉积的其它前体例如是TEOS、三乙氧基硅烷、二-叔丁氧基硅烷、硅烷、乙硅烷、二叔丁氧基二乙酰氧基硅烷等。
本发明指向使用通过电子制备工业中多种已知常规方法中的任一方法沉积的牺牲材料,作为牺牲层在空隙空间制备中的用途。该层在微电子工业的气隙结构制备中和在纳米技术制备中用于“释放”结构或用于空隙空间制备中特别有用。
将在这里对在其中含有一个或多个气隙结构的半导体和形成其的方法进行描述。在一个实施方式中,在层状基底中在导线间的至少部分空间中形成一个或多个气隙。这里所使用的术语“导线”通常指的是金属线、迹线、丝、互连导线、信息通路或为基底中耦合或互连电路提供信号通路的信号介质。结构易于放大到多层和适于单或双层镶嵌处理。在某些实施方式中,介电层可以是固体材料或可替代地可以为多孔和/或含有空隙、空穴或气隙。
第一种实施方式:有机不稳定的牺牲材料
在这个实施方式中,使用牺牲有机层来产生空隙空间。通过使用至少一种相同的有机前体用于沉积牺牲层和作为复合层中的成孔剂,例如PDEMSTM层,它允许在器件中建造梯度。因为使用相同的前体作为牺牲层前体和作为有机成孔剂前体,所以能最初仅使用至少一种有机前体、然后添加至少一种OSG前体进行PECVD过程的操作,在牺牲层和多孔层之间能形成无缝梯度。美国专利号6,583,048和6,846,515、6,054,206、6,054,379、6,171,945和WO99/41423提供了一些实例性的可用于形成本发明的有机硅酸盐薄膜的CVD方法。
不受限于理论,用于复合层中的成孔剂和作为牺牲层沉积的有机前体的本质具有某些希望的属性。有机前体应能够以气体形式输送到反应室中,因此希望有机前体在50℃或更高温度具有可测量的蒸气压。希望有机前体应在反应室中以这样一种方式反应使得它形成在100℃或更高温度不具有显著蒸气压的材料,更优选的,希望成孔剂反应而形成在高于200℃不具有明显蒸气压的材料。
有机分子中的不饱和度数目被定义为分子中多键数量或环结构的数量。因此,分子中单个双键或单个环结构为一个不饱和度,而三键或环结构中的双键为两个不饱和度。有机前体中不饱和度数目将影响沉积反应,不饱和度数目较高通常导致较高的沉积速率。然而,不受限于理论,通常观察到由具有较高不饱和度的有机前体沉积的材料更难于被完全除去,因此必须在沉积和除去间找到平衡。
在一些情况下,在分子中可具有可提高成孔剂或牺牲材料沉积的杂原子(例如氧、单或硫)是有利的。相信在等离子体环境中,杂原子将增加电子俘获的截面,因此增加气相中中性自由基的数目。中性自由基数量的增加将增加沉积效率,因为相信沉积基于中性自由基的反应。
下面是适于本发明有机前体的非限制性的材料实例。
1)通式CnH2n的环烃,其中你=4-14,其中环状结构中的碳原子数在4到10之间,其中能在环状结构上具有多个取代的简单烃或支链烃。
实例包括环已烷、1,2,4,-三甲基环己烷、1-甲基-4-(1-甲基乙基)环己烷,环辛烷、甲基环辛烷等。
2)通式CnH(2n+2)-2y的直链或支链的、饱和的、单或多不饱和烃,其中n=2-20,y=0-n。
实例包括:乙烯、丙烯、乙炔、新己烷、1,3-丁二烯、2-甲基-1,3-丁二烯、2,3-二甲基-2,3-丁二烯、取代的二烯烃等。
3)通式CnH2n-2x的单或多不饱和环烃,其中x是分子中不饱和位置的数目,n=4-14,其中环状结构上的碳原子数在4和10之间,其中在环状结构中能具有多个取代的简单烃或支链烃。不饱和度能位于环内或环状结构的一个烃取代基上。
实例包括:辛烷、1,5-辛二烯、己烯、乙烯-环己烷、二甲基环己烷、α-萜品烯、萜烯、1,8-萜二烯、乙烯-环己烯。
4)通式CnH2n-2的双环烃,其中n=4-14,其中双环中的碳原子数在4-12之间,其中在环状结构中能具有多个取代的简单烃或支链烃。
实例包括:降莰烷、螺环壬烷、十氢化萘等。
5)通式CnH2n-(2+2x)的多不饱和双环烃,其中x是分子中不饱和位置数,n=4-14,其中双环结构中的碳原子数在4和12之间,其中在环状结构中能具有多个取代的简单烃或支链烃。不饱和度能位于环内或环结构的一个烃取代基上。
实例包括莰烯、降冰片烯、降冰片二烯、5-亚乙基-2-降冰片烯等。
6)烃通式CnH2n-4的三环烃,其中n=4-14,其中三环结构中的碳原子数在4和12之间,在环结构中能具有多个取代的简单烃或支链烃。
实例包括金刚烷。
7)包含一个或多个醇基并且通式为CnH2n+2-2x-2y-z(OH)z的烃结构,其中n=1-12,x是所述结构中环的数目并且在0-4之间,y是所述结构中不饱和键的数目并且在0和n之间,z是所述化合物中醇基的数目并且在1和4之间,并且其中醇官能团可以在环外和/或环内。其实例有:丙醇(n=3,x=0,z=1)、乙二醇(n=2,x=0,y=0,z=2)、己醇(n=6,x=0,y=0,z=1)、环戊醇(n=5,x=1,y=0,z=1)、1,5-己二烯-3,4-二醇(n=6,x=0,y=2,z=2)、甲酚(n=7,x=1,y=3,z=1)和间苯二酚(n=6,x=1,y=3,z=2)等。
8)包含一个或多个醚基并且通式为CnH2n+2-2x-2yOz的烃结构,其中n=1-12,x是所述结构中环的数目并且在0-4之间,y是所述结构中不饱和键的数目并且在0和n之间,z是所述结构中醚键的数目并且在1和4之间,并且其中醚键可以在环外和/或环内。其实例有:乙醚(n=4,x=0,y=0,z=1)、2-甲基-四氢呋喃(n=5,x=1,y=0,z=1)、2,3-苯并呋喃(n=8,x=2,y=4,z=1)、乙二醇二乙烯基醚(n=6,x=0,y=2,z=2)、桉树脑(桉叶油素)(n=10,x=2,y=0,z=1)等。
9)包含一个或多个环氧基团并且通式为CnH2n+2-2x-2y-2zOz的烃结构,其中n=1-12,x是所述结构中环的数目并且在0-4之间,y是所述结构中不饱和键的数目并且在0和n之间,z是所述结构中环氧基团的数目并且在1和4之间,并且其中环氧基团可连接在环上或直链上。其实例有:1,2环氧-3-甲基丁烷(n=5,x=0,y=0,z=1)、1,2-环氧-5-己烯(n=5,x=0,y=1,z=1)、氧化环己烯(n=6,x=1,y=0,z=1)、9-氧杂二环[6.1.0]壬-4-烯(n=8,x=1,y=1,z=1)等。
10)包含一个或多个醛基并且通式为CnH2n+2-2x-2y-2zOz的烃结构,其中n=1-12,x是所述结构中环的数目并且在0-4之间,y是所述结构中不饱和键的数目并且在0和n之间,z是所述结构中醛基的数目并且在1和4之间。其实例有:环戊烷甲醛(n=5,x=1,y=0,z=1)等。
11)包含一个或多个酮基并且通式为CnH2n+2-2x-2y-2zOz的烃结构,其中n=1-12,x是所述结构中环的数目并且在0-4之间,y是所述结构中不饱和键的数目并且在0和n之间,z是所述结构中酮基的数目并且在1和4之间,并且其中酮基可以在环外和/或环内。其实例有:3,4-己二酮(n=6,x=0,y=0,z=2))、环戊酮(n=5,x=1,y=0,z=1))、2,4,6-三甲苯基氧化物(n=6,x=0,y=1,z=1)等。
12)包含一个或多个羧基并且通式为CnH2n+2-2x-2y-3z(OOH)z的烃结构,其中n=1-12,x是所述结构中环的数目并且在0-4之间,y是所述结构中不饱和键的数目并且在0和n之间,z是所述结构中羧基的数目并且在1和4之间。其实例有:环戊烷甲酸(n=6,y=1,x=0,z=1)等。
13)包含偶数个羧基并且酸官能团被脱水以形成环状酸酐基团的烃结构,其中所述结构的通式为CnH2n+2-2x-2y-6z(O3)z,其中n=1-12,x是所述结构中环的数目并且在0-4之间,y是所述结构中不饱和键的数目并且在0和n之间,z是所述结构中酸酐基的数目并且为1或2。其实例有:马来酸酐(n=2,x=0,y=1,z=1)等。
14)包含酯基并且通式为CnH2n+2-2x-2y-2z(O2)z的烃结构,其中n=1-12,x是所述结构中环的数目并且在0-4之间,y是所述结构中不饱和键的数目,其中没有不饱和键与酯的羰基共轭,z是所述结构中酸酐基的数目并且为1或2。其实例有:等。
15)包含丙烯酸酯官能团并且通式为CnH2n+2-2x-2y-2z(O2)z的烃结构,其中所述官能团由酯基和至少一个与酯基的羰基共轭的不饱和键组成,n=1-12,x是所述结构中环的数目并且在0-4之间,y是所述结构中不饱和键的数目并且大于或等于1,其中至少一个不饱和键与酯的羰基共轭,z是所述结构中酯基的数目并且为1或2。其实例有:甲基丙烯酸乙酯(n=6,x=0,y=1,z=1)等。
16)包含醚基和羰基官能团并且通式为CnH2n+2-2w-2x-2z(O)y(O)z的烃结构,其中n=1-12,w是所述结构中环的数目并且在0-4之间,x是所述结构中不饱和键的数目并且在0和n之间,y是所述结构中羰基的数目,其中羰基可以为酮和/或醛,z是所述结构中醚基的数目并且为1或2,并且醚基可以在环外和/或环内。其实例有:乙氧基异丁烯醛(n=6,w=0,x=1,y=1,z=1)等。
17)包含醚和醇官能团并且通式为CnH2n+2-2w-2x-2z(OH)y(O)z的烃结构,其中n=1-12,w是所述结构中环的数目并且在0-4之间,x是所述结构中不饱和键的数目并且在0和n之间,y是所述结构中醇基的数目z是所述结构中醚基的数目并且为1或2,并且其中醚基可以在环外和/或环内。其实例有:3-羟基四氢呋喃等。
18)包含选自下面官能团:醇、醚、羰基和羧酸的任何组合并且通式为CnH2n+2-2u-2v-w-2y-3z(OH)w(O)x(O)y(OOH)z的烃结构,其中n=1-12,u是所述结构中环的数目并且在0-4之间,v是所述结构中不饱和键的数目并且在0和n之间,w为通式中醇基的数目并且在0和4之间,x是所述结构中醚基的数目且在0和4之间并且其中醚基可以是环外或环内的,y是所述结构中羰基的数目并且在0和3之间,其中所述羰基可以是酮和/或醛,z是所述结构中羧基的数目并且在0和2之间。
19)包含一个或多个伯胺基并且并且通式为CnH2n+2-2x-2y-z(NH2)z的烃结构,其中n=1-12,x是所述结构中环的数目并且在0-4之间,y是所述结构中不饱和键的数目并且在0和n之间,z是所述化合物中胺基的数目并且在1和4之间,并且其中胺官能团可以是环外和/或环内的。其实例有:环戊胺(n=5,x=1,y=0,z=1)等。
20)包含一个或多个仲胺基并且通式为CnH2n+2-2x-2y-2z(NH)z的烃结构,其中n=1-12,x是所述结构中环的数目并且在0-4之间,y是所述结构中不饱和键的数目并且在0和n之间,z是所述化合物中仲胺基的数目并且在1和4之间,并且其中胺官能团可以是环外和/或环内的。其实例有:二异丙胺(n=6,x=0,y=0,z=1)、哌啶(n=5,x=1,y=0,z=1)、吡啶(n=5,x=1,y=3,z=1)等。
21)包含一个或多个叔胺并且通式为CnH2n+2-2x-2y-3z(N)z的烃结构,其中n=1-12,x是所述结构中环的数目并且在0-4之间,y是所述结构中不饱和键的数目并且在0和n之间,z是所述化合物中叔胺基的数目并且在1和4之间,并且其中胺官能团可以是环外和/或环内的。其实例有:三乙胺(n=6,x=0,y=0,z=1)、N-甲基吡咯烷(n=5,x=1,y=0,z=1)、N-甲基吡咯(n=5,x=1,y=2,z=1)等。
22)包含一个或多个硝基并且通式为CnH2n+2-2x-2y-z(NO2)z的烃结构,其中n=1-12,x是所述结构中环的数目并且在0-4之间,y是所述结构中不饱和键的数目并且在0和n之间,z是所述化合物中硝基的数目并且在1和4之间,并且其中硝基官能团可以是环外和/或环内的。其实例有:硝基环戊烷(n=5,x=1,y=0,z=1)、硝基苯(n=6,x=1,y=3,z=1)等。
23)包含胺和醚官能团并且通式为CnH2n+2-2u-2v-w-2x-3y-z(NH2)w(NH)x(N)y(OH)z的烃结构,其中n=1-12,u是所述结构中环的数目并且在0-4之间,v是所述结构中不饱和键的数目并且在0和n之间,w是伯胺基的数目,x是仲胺基的数目,y是叔胺基的数目,并且1<w+x+y<4,z是所述化合物中醇基的数目并且在1和4之间,并且其中醇基和/或胺基官能团可以是环外和/或环内的。其实例有:2-(2-氨基乙基氨基)乙醇(n=4,u=0,v=0,w=1,x=1,y=0,z=1),N-甲基吗啉(n=5,u=1,v=0,w=0,x=0,y=1,z=1)等。
24)包含胺和醇官能团并且通式为CnH2n+2-2u-2v-w-2x-3y-z(NH2)w(NH)x(N)y(OH)z的烃结构,其中n=1-12,u是所述结构中环的数目并且在0-4之间,v是所述结构中不饱和键的数目并且在0和n之间,w是伯胺基的数目,x是仲胺基的数目,y是叔胺基的数目,并且1<w+x+y<4,z是所述化合物中醚基的数目并且在1和4之间,并且其中醚基和/或胺基可以是环外和/或环内的。其实例有:四氢糖胺(n=5,u=1,v=0,w=1,x=0,y=0,z=1)等。
25)包含胺和羰基官能团并且通式为CnH2n+2-2u-2v-w-2x-3y-2z(NH2)w(NH)x(N)y(O)z的烃结构,其中n=1-12,u是所述结构中环的数目并且在0-4之间,v是所述结构中不饱和键的数目并且在0和n之间,w是伯胺基的数目,x是仲胺基的数目,y是叔胺基的数目,并且1<w+x+y<4,z是所述化合物中羰基的数目并且在1和4之间,其中羰基可以醛和/或酮,羰基和/或胺基可以是环外和/或环内的。其实例有:N,N-二乙基甲酰胺(n=5,u=0,v=0,w=0,x=0,y=1,z=1)、(二甲胺)丙酮(n=5,u=0,v=0,w=0,x=0,y=1,z=1)、N-甲基吡咯烷酮(n=5,u=1,v=1,w=0,x=0,y=l,z=1)等。
在图3A-H中和实施例4中举例说明了该技术,使用至少一种相同的有机前体沉积复合层中的牺牲层和成孔剂。在图3A中,提供裸硅晶片,尽管可以在微电子或纳米技术器件制备中的任意阶段制备该硅晶片。第一步骤是如图3B所述的通过PECVD利用至少一种有机前体沉积牺牲层。在该牺牲层顶部沉积硬掩膜,该硬掩膜可以是具有对光刻胶和牺牲层好的刻蚀选择性的任何材料,在图3C中描述使用由DEMS和Limonen沉积的复合薄膜作为硬掩膜。如图3D所示,下一步骤是应用图案转移层,这能通过多种技术获得,例如通过应用、曝光和光刻胶显影或通过纳米压印转移,或根据应用可通过喷墨技术。图3E描述在刻蚀硬掩膜后的结构,例如能通过RIE或湿刻蚀。接下来如图3E所示,通过例如O2RIE将图案转移到牺牲层上,在该步骤中,将图案转移材料(即光刻胶)的刻蚀速度和厚度工程化,使得当牺牲层刻蚀(这限制了可对牺牲层具有负面影响的灰化步骤)时硬掩膜上的图案转移材料被完全除去是有利的。在将牺牲层图案化后,然后如图3G所示利用与沉积牺牲层相同的至少一种有机前体、通过PECVD在该结构顶部沉积PDEMSTM复合层,因此确保牺牲层能够通过多孔OSG层。最后,通过任意技术除去成孔剂和牺牲层,在图3H中描述了热退火技术。
通过SEM测试薄膜的截面以确定通过多孔OSG层除去牺牲有机材料的效果。图9A显示在热退火除去牺牲材料后并在多孔OSG网络中留有“孔道”的SEM照片。
第二种实施方式:选择性地刻蚀的硅的牺牲材料
已知气态的含氟选择性刻蚀气体(例如XeF2或BrF3),将相对于二氧化硅选择性地刻蚀硅,例如参见Lopez等人Micro Total Analysis Systems2002,Proceedings of the μTAS 2002 Symposium,6th,Nara,Japan,Nov.3-7,2002(2002),934-936。刻蚀选择性由单晶-多晶-或无定形硅与使用的XeF2、BrF3等间增加的化学活性获得。这种类型制备的一个实例是形成悬臂,通过在硅上沉积多晶硅层为SiO2,然后在多晶硅顶部涂覆第二层SiO2,在图案化和刻蚀顶层SiO2层和多晶硅层后,通过使用XeF2来选择性地刻蚀多晶硅层而形成悬臂。
在本发明的第二实施方式中,含氟的选择性刻蚀气体通过在多晶硅或无定形硅层上形成的多孔硅酸盐或多孔OSG加帽层进行扩散以刻蚀下层的多晶或无定形硅,并刻蚀顶层周围的下面的层而无需对结构进行开口(即无需侧向扩散)。以这种方式,能除去硅层而无需制备通道以用于刻蚀气体的扩散。
能够使用该技术的实例是:在半导体制备中气隙的形成、用于气体或液体输送通道的形成,例如用于通过微毛细管制备的药物输送,或用于先进光纤光缆制备中中空芯的形成。在除去硅前,能够制备多层多孔SiO2或多孔OSG和硅将允许能够制备微毛细管的互连层,微毛细管能以与微芯片中电路相似的方式相互作用,特别是对于芯片上的化学物质。
图4A-I显示了典型的形成孔隙的途径。在该方法中,在氧环境中对硅晶片(图4A)进行热氧化以形成对于阻止选择性的含氟刻蚀气体与硅晶片反应是必要的SiO2层(图4B),如果使用非硅下层,那么该步骤不是必须的。在该SiO2上,能例如使用高温热CVD由硅烷沉积多晶硅层(图4C)。如图4D所述的下一步骤是应用图案转移层,这能通过各种技术例如通过应用、曝光和光刻胶显影而获得,或通过纳米压印转移或依靠所述应用能够通过喷墨技术获得。图4E描述了硅层被刻蚀后的结构,例如能通过RIE或使用例如Cl2或HBr进行刻蚀。接着,在灰化步骤除去图案转移材料(即光刻胶),在灰化步骤中能使用多种不同方法,即O2活性离子刻蚀步骤、O2下游灰化、还原灰化例如H2或NH3下游灰化,或UV辅助的灰化等。然后如图4G所示,给这些导线涂覆了复合氧化硅或OSG。能利用任意方法形成复合层,例如:使用旋涂器和Meso-ELK产品(Air Products and Chemicals,Inc,Allentown,PA),如美国专利6,365,266;6,592,980;6,818,289和6,942,918所描述的,这些专利在这里通过参考进行引用;或通过PSEMTM方法的PECVD进行沉积(Air Products and Chemicals,Inc,Allentown,PA),如美国专利6,583,048和美国专利6,846,515描述的。然后如图4H所示在退火步骤中除去用于形成多孔氧化硅或多孔OSG的成孔剂,该退火步骤能是任意过程,例如在惰性气氛下的热退火、在氧化气氛下的热退火、在真空的热退火、活性离子例如O2等离子体、在气氛下或还原压力下的UV退火等。然后如图4I所示这些样品在10托和室温下暴露于BeF3一段时间。
用于本发明形成气隙的其它硅选择性刻蚀剂包括:HF、惰性气体卤化物、卤间化合物,例如IF5、BrCl3、IF7和ClF3。
BrF3和XeF2在SiO2或OSG上刻蚀硅的选择性依赖于温度,较低的温度导致较高的选择性。
图9B显示将结构暴露于BrF3以除去牺牲硅材料并在多孔OSG网络中留下“通道”后的SEM照片。
不受限于理论,能够制备在适当位置具有硅的整体半导体器件,然后在切割晶片后,将芯片暴露于选择性含氟刻蚀气体以除去硅和选择性的产生气隙,这可在封装过程中提供机械完整性的优点,这对于具有差机械完整性的材料是主要问题。
能够预见,用于制备具有液体或气体通道的器件能将多晶或无定形硅层刻蚀成图案,通过允许多层通道允许在沿晶片的特定位置进行化学物质的混合,能在单芯片上进行分子多步合成。一旦制备希望结构的多孔氧化硅或OSG和多晶或无定形硅层,将器件暴露于选择性的含氟刻蚀气体中以刻蚀硅并留下开口通道。如果需要,在多孔氧化硅或OSG层中进行填充是有利的,以阻止气体或液体通过多孔层从一个通道扩散到另一通道。可进行的一种方式是给孔填充可聚合的有机物,例如能被活化进行聚合以有效填充孔的液体。能使孔中的液体比通道中的材料更少程度挥发的毛细管作用促进该过程。
中空芯光纤光缆的制备是有利的,因为空气(RI=1)和多孔氧化硅或OSG(RI=1.2-1.46)间反射指数(RI’s)的大的差异,与常规实芯光纤光缆相比,这种差异将允许更大的信号密度并降低信号损失。为了制备中空芯光纤光缆,可预见,首先形成多晶或无定形硅的薄丝,然后涂覆复合氧化硅或OSG层,接着在退火步骤中除去成孔剂。然后使用选择性含氟刻蚀气体刻蚀硅芯。然后再给中空芯光纤涂覆另一层以提供机械强度是有利的。
第三实施方式:在极性溶剂中溶解的牺牲材料
也希望使用多孔硅酸盐层和水溶性金属氧化物例如氧化锗(GeO2)以制备结构作为本发明的实施方式。已知GeO2是水溶性氧化物材料,能通过任何技术例如化学气相沉积或PECVD由容易获得的前体材料或由使用预氧化物的旋涂技术然后进行退火步骤沉积GeO2。形成水溶性金属氧化物的前体的实例是例如但不限制于选自四甲基锗烷、锗烷、四甲氧基锗和四乙氧基锗的锗(Ge)基前体;和选自三甲基硼、三甲氧基硼烷、三乙氧基硼烷和乙硼烷的硼(B)基前体。尽管SiO2和OSG薄膜不是水溶性的,但它们允许水通过它们扩散,因此允许例如被多孔硅酸盐或多孔OSG层覆盖的GeO2的溶解。
本发明还打算在水溶性金属氧化层上使用多孔硅酸盐涂层以允许水通过多孔层进行扩散并刻蚀下层的水溶性金属氧化物层而无需刻蚀结构以暴露下层的边缘。
可能使用该技术的实例是:在半导体制备中气隙的形成、用于输送气体或液体例如用于药物输送的通道的形成或用于先进光纤光缆制备中中空芯的形成。
图5A-I显示形成空隙空间的典型途径。在该方法中,给硅晶片涂覆一层水溶性金属氧化物层,例如GeO2(图5A)。在该水溶性金属氧化物层上,能使用例如PECVD方法沉积阻挡层例如SiO2层(图4B),在这种情况下使用阻挡层来在光刻以显影抗蚀剂图案过程中阻止水溶性金属氧化物在氢氧化四甲基铵中的溶解(5C图),如果使用其它图案转移技术例如喷墨或压印技术,那么该层不是必需的。图5D描述刻蚀水溶性金属氧化物后的结构,这能通过例如RIE或使用任何碳氟化合物包括CF4、C4F6/C4F8等进行刻蚀。如图5F所示,下一步骤是在灰化步骤中除去图案转移材料(即光刻胶),在灰化步骤中能使用许多不同的方法,即O2活性离子刻蚀步骤、O2下游灰化、还原灰化例如H2或NH3下游灰化,或UV辅助的灰化等。然后如图5G所示,这些导线涂覆复合氧化硅或OSG。能利用任意方法形成复合层,例如:使用旋涂器和Meso-ELK产品(Air Products and Chemicals,Inc,Allentown,PA),如美国专利6,365,266;6,592,980;6,818,289和6,942,918描述的,这些专利在这里通过参考进行引用;或通过PSEMTM方法中的PECVD进行沉积(Air Products and Chemicals,Inc,Allentown,PA),如美国专利6,583,048和美国专利6,846,515描述的。然后如图4H所示,在退火步骤中除去用于形成多孔氧化硅或多孔OSG的成孔剂,该退火步骤能是任意过程,例如在惰性气氛下的热退火、在氧化气氛下的热退火、在真空的热退火、活性离子例如O2等离子体、在气氛下或还原压力下的UV退火等。然后如图5I中所示,将这些样品在10托和室温下暴露于BeF3一段时间。
图9C显示用水溶解GeO2部分以除去牺牲的水溶性金属氧化物并在多孔OSG网络中留下“通道”的SEM照片。
用于气隙制备时,模式将与使用纯成孔剂作为牺牲层的方法相似,除了在该方法中使用GeO2作为牺牲层外,实际上,能够在气隙制备前制备整个半导体器件,这可在封装中提供机械完整性的优点,这对于具有差机械完整性的材料是主要问题。
用于液体或气体通道,能预见,能将GeO2层刻蚀成图案,通过允许多层通道允许在沿晶片的特定位置上进行化学物质的混合,能在单芯片上进行分子多步合成。一旦制备希望结构的多孔氧化硅或OSG和GeO2层,将器件暴露于水中以刻蚀GeO2并留下开口通道。如果需要,在多孔氧化硅或OSG层中进行填充是有利的,以阻止气体或液体通过多孔层从一个通道扩散到另一通道。可进行的一种方式是给孔填充可聚合的有机物,例如能被活化进行聚合以有效填充孔的液体。通过能使孔中的液体比通道中的材料更少程度挥发的毛细管作用促进该过程。
中空芯光纤光缆的制备是有利的,因为空气(RI=1)和多孔氧化硅或OSG(RI=1.2-1.4)间反射指数(RI)的大的差异,与常规实芯光纤光缆相比,这种差异将允许更大的信号密度并降低信号损失。为了制备中空芯纤维光缆,可预见,首先形成GeO2的薄丝,然后涂覆多孔氧化硅或OSG层,然后使用水溶解硅芯。然后再给中空芯光纤涂覆另一层以提供机械强度是有利的。
能使用B2O3代替GeO2作为水溶性金属氧化物。能使用各种极性溶剂,例如乙醇、乙醚、含有杂原子的分子、酯、酮、醛和这些溶剂的混合物来代替水。
也能够共沉积GeO2和或B2O3连同SiO2和或OSG以通过无机成孔剂的溶解来形成多孔层,以这种方式,能通过在水中溶解GeO2和或B2O3完成器件的制备。
沉积方法
如在前提及的,使用各种不同的方法在至少部分基底上由前体组合物或混合物来沉积牺牲材料和复合层。这些方法可各自使用或组合使用。一些可用于形成有机硅酸盐玻璃的方法的实例包括:热化学气相沉积、等离子增强的化学气相沉积(“PECVD”)、高密度PECVD、光辅助的CVD、等离子-光辅助的(“PPECVD”)、低温化学气相沉积、化学辅助的气相沉积、热丝化学气相沉积(aka iCVD或cat-CVD)、光诱发的化学气相沉积、液体聚合物前体的CVD、由超临界流体的沉积,或传输聚合(“TP”)。在某些优选的实施方式中,在100-425℃、优选200-425℃、更优选200-350℃温度范围内进行沉积。尽管有时这里使用的化学试剂可被描述为“气态”,但应理解为化学试剂可直接以气体输送到反应器中,以蒸发的液体、升华的固体输送和/或通过惰性载气输送到反应器。
在本发明的某些实施方式中,通过等离子辅助的化学气相沉积方法形成牺牲材料和复合材料。简单地说以PECVD方法,将化学试剂流入反应室中例如真空室,并且等离子体能量使化学试剂活化,因此在至少部分基底上形成薄膜。在这些实施方式中,能通过共沉积形成基底的层,或可替换地,通过气态混合物依次沉积,该混合物包括至少一种形成牺牲层的等离子体聚合有机材料和至少一层形成复合层的含有氧化硅的前体例如有机硅烷或有机硅氧烷。在某些实施方式中,应用于试剂的等离子体能量可以在0.02-7瓦特/cm2、更优选在0.3-3瓦特/cm2范围。每种试剂的流速可以在10-5000sccm范围。本发明PECVD过程沉积中的真空室中压力可在0.01-600托范围、优选在1-10托的范围。然而应理解的是,工艺参数例如等离子体能量、流速和压力可以依靠多种因素例如基底表面积、在PECVD过程中使用的设备等进行变化。
除了一种或多种化学试剂外,能在沉积反应前、过程中和/或后在真空室中充入附加材料。这种材料包括例如惰性气体(例如,He、Ar、N2、Kr、Xe、等,可用于较少挥发的前体的载气和/或能促进所沉积材料的固化和提供更稳定的最终薄膜)和活性物质,例如气态或液体有机物、NH3、H2、CO2、CO、O2或N2O。CO2是优选的载气。
对气态试剂应用能量以促使气体反应和在基底上形成薄膜。能通过例如热、热丝、等离子体、脉冲等离子体、螺旋(helicon)等离子、高密度等离子体、感应耦合等离子和远程等离子方法提供这种能量。能使用二级射频频率源调整基底表面上的等离子体特性。优选地,通过等离子体增强的化学气相沉积形成薄膜。特别优选的在13.56MHz频率产生电容耦合等离子。
基于基底的表面积,等离子体功率优选0.02-7瓦特/cm2、更优选0.3-3瓦特/cm2。使用具有低电离能以降低等离子体中电子温度的载气是有利的,这又将引起OSG前体中较少的碎裂。这种类型的低电离气体的实例包括CO2、NH3、CO、CH4、Ar、Xe和Kr。
对于每单个200mm晶片,每种气态试剂的流速优选为10-5000sccm,更优选为30-1000sccm。选择各自的速率以提供薄膜中希望的结构形成体和气孔形成体的量。实际需要的流速可依据晶片尺寸和腔室的构造,并不限制于200mm晶片或单个晶片腔室。在某些实施方式中,可以以至少50nm/分钟的沉积速度沉积薄膜。
在沉积过程中,真空室的压力优选为0.01-600托,更优选为1-15托。
薄膜优选被沉积到0.002-10微米厚度,尽管厚度能根据需要进行变化。在没有图案化的表面上沉积的覆盖薄膜具有优异的均匀性,除去适当的边缘以外,其中例如基底5mm最外边缘不包括在均匀性的统计计算中,在横跨基底的1个标准偏差厚度上,其厚度变化小于2%。
如同上面描述的气相沉积方法,在某些实施方式中能够够使用旋涂技术应用复合薄膜,例如Air Product and Chemicals Meso-ELKTM薄膜,例如根据美国专利7,122,880沉积的薄膜。
通常利用旋涂技术使用混合物形成这些薄膜。混合物通常包括至少一种氧化硅源和至少一种成孔剂。混合物还可包括其它组分,例如但不限于水、溶剂、催化剂和/或离子添加剂。
如前面描述的,混合物包括至少一种氧化硅源。这里使用的“氧化硅源”是具有硅(Si)和氧(O)的化合物,并且可能附加取代基例如但不限制为其它元素例如H、B、C、P或卤化物原子和有机基团例如烷基基团或芳基基团。这里使用的术语“烷基”包括直链、支链或环状烷基基团,含有1-24碳原子,优选1-12碳原子和更优选1-5碳原子。该术语也应用于含有其它基团的烷基部分,例如卤代烷基、芳烷基。术语“烷基”也应用于被取代的烷基部分,例如用羰基官能团取代的烷基部分。这里使用的术语“芳基”是指具有芳族特征的6-12碳环。术语“芳基”也应用于被取代的芳基部分。氧化硅源可包括具有多个Si-O键的材料,但也能包括Si-O-Si桥、Si-R-Si桥、Si-C键、Si-H键、Si-F键或C-H键。优选至少一个氧化硅源赋予了介电材料中最小量的Si-OH键。
用于形成本发明薄膜的混合物还包括成孔剂。这里使用的“成孔剂”是用于在所得薄膜中产生空隙体积的试剂。用于本发明复合材料的适合成孔剂包括不稳定的有机基团、溶剂、可分解的聚合物、表面活性剂、枝状体(dendrimers)、高度枝化的聚合物、聚氧化烯化合物、有机大分子或其组合。适合的成孔剂的另外实例包括已经转让给本发明受让人的待审专利申请代理人案号06274P2中描述的成孔剂。
在本发明的某些实施方式中,成孔剂可包括不稳定的有机基团。当在反应混合物中具有一些不稳定的有机基团时,不稳定的有机基团可含有充分的氧并在固化步骤中转变为气态产物。含有不稳定有机基团的化合物的一些实例包括在美国专利号6,171,945中公开的化合物,该专利在这里通过参考进行全部引用。
在本发明的一些实施方式中,成孔剂可以是溶剂。在这方面,该溶剂通常存在于与基质材料的至少一部分发生交联的过程中。典型的用来帮助气孔形成的溶剂具有相对较高的沸点,即高于175℃或高于200℃。适于在本发明混合物中用于成孔剂的溶剂包括例如在美国专利号6,231,989中提供的那些溶剂。
在某些实施方式中,成孔剂可以是小分子,例如在参考文献Zheng等人“Synthsis of Mesoporous Silica Materials with Hydroxyacetic Acid Derivatives asTemplates via a Sol-Gel Process”,J.Inorg.Organomet.Polymers,1,103-113(2000)中描述的那些。
成孔剂也可以是可分解的聚合物。可分解的聚合物可以是可辐射分解的,或者更优选是可热分解的。除非有相反的明确表述,这里所用的术语“聚合物”也包括术语低聚物和/或共聚物。可辐射分解的聚合物是在暴露于例如紫外线、X-射线、电子束等辐射时分解的聚合物。可热分解的聚合物在接近氧化硅源材料缩合温度的温度下进行热分解并且在至少一部分发生交联的过程中存在。这样的聚合物是可以培育玻璃固化反应的模板、可以控制和确定气孔的尺寸和可以在加工过程的适合时间分解并从基质中扩散出来的那些聚合物。这些聚合物的实例包括具有三维结构的聚合物,例如但不限于,嵌段共聚物、即二嵌段、三嵌段和多嵌段共聚物;星形嵌段共聚物;放射状二嵌段共聚物;接枝二嵌段共聚物;共接枝共聚物;枝形接枝共聚物;递变嵌段共聚物;和这些构造的组合。可分解聚合物的其它实例见于美国专利号6,204,202中,该专利通过参考全部进行引用。
成孔剂可以是高度支化的或枝状的聚合物。高度支化和枝状的聚合物通常具有低的溶液和熔体粘度,由于表面官能团而具有高化学反应性,并且即使在较高分子量中也具有提高的溶解度。适合的可分解的高度支化聚合物和枝状聚合物的一些非限制性实例在“Comprehensive Polymer Science”,2ndSupplement,Aggarwal,pp.71-132(1996)中提供,通过参考全部进行引用。
在形成薄膜的混合物中的成孔剂也可包括聚氧化烯化合物,例如聚氧化烯非离子表面活性剂、聚氧化烯聚合物、聚氧化烯共聚物、聚氧化烯低聚物和它们的组合。其中一个实例是包括C2-C6烷基部分的聚氧化烯,例如聚氧化乙烯、聚氧化丙烯和它们的共聚物。
本发明的成孔剂也可以包括表面活性剂。对于其中通过加入表面活性剂(所述表面活性剂随后被除去)而引入孔的氧化硅溶胶-凝胶基薄膜改变表面活性剂的量可以改变孔隙率。典型的表面活性剂表现出两亲性质,意味着它们同时是亲水的和疏水的。两亲性表面活性具有对水有强亲和性的亲水头基和长的疏水尾部,该疏水尾部是亲有机的并且排斥水。表面活性剂可以是阴离子的、阳离子的、非离子的或两性的。表面活性剂的进一步分类包括硅氧烷表面活性剂、聚(氧化烯)表面活性剂和氟化学品表面活性剂。
在其中通过旋涂方法形成薄膜的实施方式中,所述混合物包括,除其它外,至少一种氧化硅源、成孔剂、催化剂、离子添加剂和水。在某些优选的实施方式中,混合物还包括溶剂和表面活性剂。总之,在基底上分散混合物和蒸发溶剂和水能形成薄膜。通常通过将涂覆的基底固化到一个或多个温度并且持续足够的时间而除去表面活性剂和剩余的溶剂和水以产生复合物薄膜。
然后进一步对涂覆的基底进行加热或固化到以形成多孔SiO2或OSG薄膜。具体的温度和持续的时间将依赖于混合物的组分、基底和希望的孔体积进行变化。在某些实施方式中,在两个或多个温度下而不是受控的升温或热渗透下进行固化步骤。典型的低于300℃的第一温度可以从混合物中除去水和/或溶剂并还发生交联反应。第二温度可以除去成孔剂,并基本上但不必完全使材料交联。
有机成孔剂和牺牲材料的除去
通过能包括热退火、化学处理、原位或间接等离子体处理、电子束处理、光固化和/或微波的固化步骤来除去有机成孔剂和牺牲材料。也可使用其它原位或沉积后处理以提高剩余多孔SiO2或多孔OSG的材料性能,例如硬度、稳定性(相对于收缩、暴露于空气中、刻蚀、湿刻蚀等)、整体性、一致性以及粘附性。所述处理可使用除去成孔剂的相同或不同的手段在除去成孔剂之前、期间和/或之后应用于所述薄膜。因此在这里使用的术语“”后处理”指的是:利用能量(例如加热、等离子体、光量子、电子、微波等)或化学物质对薄膜的处理,以除去成孔剂、稳定薄膜和/或提高材料性能。
后处理的条件能进行明显变化。例如,能在高压或在真空环境下进行后处理。
在下面条件下进行退火。
环境可为惰性的(例如氮气、CO2、稀有气体(He、Ar、Ne、Kr、Xe)等)、氧化性的(例如氧气、空气、稀氧环境、富氧环境、臭氧、一氧化二氮等)或还原性的(稀或浓氢、烃(饱和的、不饱和的和直链或支链的、芳香烃)等)。压力优选为约1-约1000托。然而,对于热退火和任何其它的后处理方式,真空环境也是可能的。温度优选为200-500℃,升温速率为0.1-100℃/分钟。总的退火时间优选为0.01分钟至12小时。
在下面条件下进行等离子体处理以选择性地除去不稳定基团和可能对OSG薄膜进行化学物质改性。
环境可为惰性的(例如氮气、CO2、稀有气体(He、Ar、Ne、Kr、Xe)等)、氧化性的(例如氧气、空气、稀氧环境、富氧环境、臭氧、一氧化二氮等)或还原性的(稀或浓氢、烃(饱和的、不饱和的和直链或支链的、芳香烃)等)。等离子体的功率优选为0-5000W。温度优选为室温到500℃。压力优选为10毫托至大气压力。总的固化时间优选为0.01分钟至12小时。
在下面条件下通过暴露于UV而除去成孔剂和牺牲有机材料。
环境可为惰性的(例如氮气、CO2、稀有气体(He、Ar、Ne、Kr、Xe)等)、氧化性的(例如氧气、空气、稀氧环境、富氧环境、臭氧、一氧化二氮等)或还原性的(稀或浓氢、烃(饱和的、不饱和的和直链或支链的、芳香烃)等)。温度优选为室温到500℃。功率优选为0-5000W。波长优选为IR、可见光、UV或远UV(波长<200nm)。总的固化时间优选为0.01分钟至12小时。
在下面条件下通过暴露于微波而除去成孔剂和牺牲有机材料。
环境可为惰性的(例如氮气、CO2、稀有气体(He、Ar、Ne、Kr、Xe)等)、氧化性的(例如氧气、空气、稀氧环境、富氧环境、臭氧、一氧化二氮等)或还原性的(稀或浓氢、烃(饱和的、不饱和的和直链或支链的、芳香烃)等)。温度优选为室温到500℃。功率和波长可以变化,并且可以被调至特定值。总的固化时间优选为0.01分钟至12小时。
在下面条件下通过暴露于电子束而除去成孔剂和牺牲有机材料。
环境可为真空、惰性(例如氮气、CO2、稀有气体(He、Ar、Ne、Kr、Xe)等)、氧化性的(例如氧气、空气、稀氧环境、富氧环境、臭氧、一氧化二氮等)或还原性的(稀或浓氢、烃(饱和的、不饱和的和直链或支链的、芳香烃)等)。温度优选为室温到500℃。电子密度和能量可以被改变并可被调至特定值。总的固化时间优选为0.001分钟至12小时,并且可以是连续或脉冲的。电子束的一般性使用的其它指导可以参考出版物:S.Chattoradhyay等人,Journal of Materials Science,36(2001)4323-4330;G.Koster等人,Proceedings ofIITC,June3-5,2002,SF,CA;以及美国专利号6,207,555B1、6,204,201B1和6,132,814A1。利用电子束处理可以除去成孔剂并通过基质中键的形成来提高薄膜的机械性能。
本发明的薄膜也可含有呈无机氟形式的氟(例如Si-F)。当存在时,氟优选含量为0.5-7原子%。
所述薄膜可与化学机械平面化(CMP)和各向同性刻蚀相容,并且能够粘附在各种材料上,例如粘附硅、SiO2、Si3N4、OSG、FSG、碳化硅、氢化碳化硅、氮化硅、氢化氮化硅、碳氮化硅、氢化碳氮化硅、氮化硼、防反射涂层、光刻胶、有机聚合物、多孔有机和无机材料、例如铜和铝的金属、以及例如但不限于TiN、Ti(C)N、TaN、Ta(C)N、Ta、W、WN或W(C)N的扩散阻挡层上。薄膜优选能够粘附在至少一种前述材料上,并足以通过常规的拉力试验,如ASTM D3359-95a带拉力试验。如果没有可察觉的薄膜除去,那么就认为试样通过了试验。
能以能够通过CVD沉积的各种形式提供本发明的产品,例如涂层、多层构件、无需平或薄的其它类型物体、不需用于集成电路的各种物品。优选基底是半导体。
除了用于气隙结构牺牲材料的本发明材料外,本发明包括制备产品的方法、使用产品的方法,使用用于制备产品的化合物和复合物的方法
图6A-G显示了说明用于形成本发明半导体基底的方法步骤的截面图。图6A显示在牺牲材料(30)层上的多孔SiO2或OSG和成孔剂的层(40)。这些层下面是已经制备的气隙互连的层级,该层级包括在基底(50)上的至少一空隙空间(10)、多孔氧化硅或OSG层(20)、金属化层(60)和铜金属(70)。在图6B中,由至少成孔剂和氧化硅或OSG构成的顶层(40)优选使用光刻技术进行刻蚀。如图6C所示,在顶层(40)图案化后,层级能使用标准光刻技术刻蚀出牺牲层(30)。然后如图6D所示沉积包括至少一种Ta、TaN、Ru、Ti、TiN、TiSiN的铜阻挡层(60)。然后如图6E通过例如电镀或化学镀沉积铜(70),接着通过铜和阻挡层的CMP形成二维结构图6F。最后如图6G所示除去成孔剂和牺牲层。
如图7A-7K所示的单嵌入式方法允许在金属线间形成牺牲层。在该方法中,分别沉积和刻蚀每一层。首先在图7A和7B中沉积和刻蚀牺牲层(30)。然后如图7C所示沉积包括至少一种Ta、TaN、Ru、Ti、TiN、TiSiN的铜阻挡层(60)。然后如图7D所示,通过例如电镀或化学镀沉积铜(70),接着通过铜和阻挡层的CMP形成二维结构图7E。然后沉积(图7F)并刻蚀(图7G)具有成孔剂(40)的复合氧化硅或OSG。然后如图7H所示沉积包括至少一种Ta、TaN、Ru、Ti、TiN、TiSiN的铜阻挡层(60)。然后如图7I通过例如电镀或化学镀沉积铜(70),接着通过铜和阻挡层的CMP形成二维结构图7J。最后如图7K所示除去成孔剂和牺牲层。
图8A-I示意性地显示如何通过双层镶嵌方法在金属线间形成气隙。最初,如图8A所示在基底50上沉积具有成孔剂(40)的复合氧化硅或OSG层。然后如图8B所示除去成孔剂以产生多孔氧化硅或OSG层(20)。然后如图8C所示在多孔层(20)上沉积牺牲层(30)。然后使用光刻技术刻蚀牺牲层和多孔层(图8D-E),在该步骤中必须使用硬掩膜以提高在牺牲层和光刻胶间的刻蚀和灰化效率,特别是如果牺牲层是有机材料。然后如图8F所示沉积包括至少一种Ta、TaN、Ru、Ti、TiN、TiSiN的铜阻挡层(60)。然后如图8G通过例如电镀或化学镀沉积铜(70),接着通过铜和阻挡层的CMP形成二维结构图8H。然后在图8I顶层上沉积具有成孔剂(40)的氧化硅或OSG的复合层。
前面的描述旨在示例性地进行描述,可需要附加的步骤和或层以完成所描述的完整方案。也可在某些实施方式中包括层例如刻蚀停止层、防反射涂层、SiO2硬掩膜层、TiN或其它金属硬掩膜、导线、阻挡层、Cu扩散阻挡层、金属晶种层、金属粘附层、碳硬掩膜等以帮助描述和制备所述结构是有利的。用于通孔优先中的沟槽优先(trech-first of via first)双层镶嵌刻蚀等的其它实例还包括但不限于硬掩膜层、刻蚀停止阻挡层、粘附层、粘附促进层、应力阻挡层、刻蚀后处理、修复化学物、牺牲层。
将参考下面实施例更为详细的说明本发明,但应理解为本发明并不限制于此。
实施例
通过等离子体增强的CVD方法使用Applied Materials Precision-5000系统在200mm真空室中形成实施例薄膜,该真空室配备有用于各种不同化学前体和过程条件的Advance Energy200射频发生器。CVD过程通常包括下面基本步骤:最初气流的充入和稳定、沉积、在除去晶片前腔室的吹扫/抽空。在SCI Filmtek 2000反射仪上测量每层薄膜的厚度和反射指数。使用标准RIE刻蚀剂在AMAT平台上进行RIE刻蚀。使用KarlSuss MA6接触式光刻机在365nm处进行光刻,使用标准TMAH显影方法进行显影。在结构RIE刻蚀后,剩余光刻胶在O2下游灰化过程中被除去。
当应用时,在装配有4英寸直径吹扫石英管并且氮流速为2-4slpm的Applied Test Systems,Inc.3210系列管式炉中进行热沉积后处理或退火。从25到425℃的升温速率为13℃/分钟。在425℃,将薄膜进行热渗透4小时。在从炉中取出前允许薄膜冷却到低于100℃。
实施例1-3
使用有机前体的牺牲层的沉积
通过这里描述的等离子增强的CVD方法在基底表面上沉积三种示例性的牺牲层。表1中提供三种示例性的牺牲层的沉积条件。
表1-各种有机前体的沉积参数
沉积参数 | 实施例1:十氢萘(DHN) | 实施例2:1,5-二甲基-环辛二烯(DM-COD) | 实施例3:α-萜品烯(ATP) | 实施例4:1,8-萜二烯(Limo) |
液体流速(m/gm) | 600 | 600 | 600 | 600 |
载气流速 | 500sccm(CO2) | 500sccm(CO2) | 220sccm(CO2) | 200sccm(CO2) |
沉积温度 | 200℃ | 200℃ | 250℃ | 250℃ |
室压 | 10托 | 8托 | 8托 | 8托 |
间距(毫英寸) | 400 | 400 | 350 | 350 |
等离子体功率 | 600W | 600W | 600W | 600W |
沉积速率 | 87nm/分钟 | 126nm/分钟 | 87nm/分钟 | 45nm/分钟 |
实施例4
具有DEMS/Limo复合层的Limo牺牲层的沉积
使用下面参数沉积牺牲层:800mg/分钟Limo液体流速、200sccmCO2、载气流速、350毫英寸喷淋头/晶片间距、250℃晶片温度、8托腔室压力、360秒以产生具有下面性质的薄膜:薄膜厚度289nm和反射指数1.568。
使用下面参数在Limo牺牲层顶部上沉积复合层:800mg/分钟液体流速(20/80DEMS/Limo摩尔混合物)、220sccmCO2载气流速、350毫英寸喷淋头/晶片间距、250℃晶片温度、8托腔室压力、60秒以产生具有下面性质的薄膜:薄膜厚度114nm和反射指数1.439。
然后给该晶片涂覆500nm Schipley 1805抗蚀剂并使用KarlSuss MA6接触式光刻机在365nm、12mW/cm2曝光1秒进行显影。然后使用TMAH显影图案。
然后使用下面顺序刻蚀该图案:首先6秒高密度O2等离子体以清除图案,接着使用C4F4/O2/Ar刻蚀配比进行60秒刻蚀,刻蚀速率140nm/分钟以清除硬掩膜,接着第二O2等离子体24秒以刻蚀除去在硬掩膜上的光刻胶并刻蚀牺牲1,8-萜二烯层。然后使用下面参数沉积加帽的复合层:800mg/分钟液体流速(20/80DEMS/Limo摩尔混合物)、220sccmCO2载气流速、350毫英寸喷淋头/晶片间距250℃晶片夹温度、8托腔室压力、180秒以产生具有下面性能的薄膜:薄膜厚度362nm和反射指数1.439。
然后对该结构进行热退火以除去成孔剂和牺牲层以形成气隙。在图9A中显示热退火后的该叠层的扫描电镜(SEM)照片。
实施例5
使用选择性刻蚀硅特征的气隙制备,首先进行裸硅晶片的热氧化,以提供XeF2/BrF3选择性刻蚀的刻蚀停止。在热氧化物的顶部,通过高温(900℃)CVD方法使用硅烷生长0.5微米厚的多晶硅层,也能使用其它类型的硅例如无定形硅。使用标准光刻技术对多晶硅和BCl3基的RIE方法进行图案化。在刻蚀多晶硅后,在O2等离子体中灰化光刻胶,然后使用Air Products’proprietary Meso-ELKTM旋涂多孔OSG方法给图案化的多晶硅结构涂覆复合OSG层。然后将叠层在400℃空气中煅烧以除去成孔剂。将样品在室温下暴露于10托的BeF31小时。BrF3通过Meso-ELK结构进行扩散并且选择性地刻蚀硅结构。图9B显示在使用BrF3选择性地刻蚀硅层后形成气隙的SEM照片,XeF2也能用于该制备过程。
实施例6
使用水溶性牺牲层的气隙制备,首先在硅晶片上沉积1.2微米GeO2层。我们使用PECVD由Me4Ge和O2沉积GeO2,尽管也能使用其它锗基前体例如Ge(OEt)4。使用Me4Si和O2在GeO2上沉积SiO2层作为在光刻胶TMAH显影过程中的水分阻挡层,也能使用多种不同的SiO2或OSG前体作为水分阻挡层。一旦光刻胶进行图案化和显影,在CF4/Ar/O2RIE过程中对SiO2/GeO2叠层进行刻蚀。在O2等离子体灰化过程除去光刻胶后,能保留SiO2帽或在定时的CF4/Ar/O2RIE过程中除去,在该实施例中,在定时的刻蚀中除去帽。然后使用Air Products’proprietary Meso-ELKTM旋涂多孔OSG方法给图案化的GeO2涂覆复合OSG层。然后在400℃空气中煅烧复合层以除去成孔剂。在涂覆多孔OSG后,将薄膜在水中浸渍10分钟,期间GeO2溶解。在图9C中显示多孔OSG层下部分溶解的GeO2牺牲层的SEM截面。也能使用B2O3或其它水溶性金属氧化物材料作为牺牲层使用相同的方法进行该过程。
本发明的技术使用三种不同的牺牲材料成功地制备了气隙结构。第一种材料是与在多孔OSG层中产生孔的不稳定材料相同的不稳定有机牺牲材料,这种一致性允许产生结构。通过使用相同的牺牲材料和成孔剂,对于所述两层能使用相同的PECVD腔室,能使用一个退火步骤以产生气隙和产生多孔OSG,通过多孔OSG,由气隙产生的副产物进行扩散。该方法的另一优点是PECVD沉积过程能在>250℃的温度下进行,相对于旋涂聚合物,这允许更大尺寸稳定的牺牲材料。
第二牺牲材料是水溶性的GeO2结构。使用无机材料作为牺牲材料提供了更高的结构强度,在制备结构中允许使用更为标准的刻蚀过程。在气隙制备中使用GeO2或B2O3的一个困难是对湿过程,例如:显影、剥离、Cu沉积和CMP的选择性。如果能通过硬掩膜或Cu阻挡层对GeO2/B2O3结构相对于这些过程进行保护,那么因为热强度和机械强度,GeO2/B2O3将提供独特的优点。
最后成功的牺牲材料是硅。能使用硅,因为XeF2或BrF3相对于SiO2或OSG对硅进行热刻蚀的选择性特性,能够沉积任何数量的多孔OSG层,例如使用PECVDTM或Meso-ELK多孔介电材料。再次,使用无机牺牲层在制备中提供结构更高的机械强度并允许更标准的各向同性刻蚀过程。
尽管参考具体的实施例更为详细的描述了本发明,但对本领域技术人员而言能在没有脱落其实质和范围内进行各种变化和改变是显而易见的。
Claims (38)
1.形成气隙的方法,方法包括:
(a)提供基底;
(b)在基底上沉积具有至少一种有机前体的牺牲层;
(c)在牺牲层上沉积具有成孔剂和至少一种含有氧化硅的前体或有机硅酸盐玻璃(OSG)前体的复合层,所述成孔剂是(b)中的至少一种有机前体;和
(d)对具有牺牲层和复合层的基底应用能量以除去牺牲层而提供气隙和除去成孔剂而形成多孔层。
2.权利要求1中所述的形成气隙的方法,其中至少一种有机前体是选自下面的至少一种:
(1)至少一种具有环状结构和通式CnH2n的环烃,其中n=4-14,并且环状结构中的碳原子数在4到10之间,并且至少一种环烃在环状结构上含有或不含有多个取代的简单烃或支链烃;
2)至少一种通式CnH(2n+2)-2y的直链或支链的、饱和的、单或多不饱和的烃,其中n=2-20,y=0-n;
3)至少一种具有环状结构和通式CnH2n-2x的单或多不饱和环烃,其中x是不饱和位置数,n=4-14,环状结构上的碳原子数在4和10之间,所述的至少一种单或多不饱和环烃任选地在环状结构上含有多个取代的简单烃或支链烃取代基,并且含有环内不饱和度或位于一个烃取代基上的不饱和度;
4)至少一种具有双环结构和通式CnH2n-2的双环烃,其中n=4-14,其中所述双环中的碳原子数为4-12,并且所述的至少一种双环烃任选地在双环结构中含有多个取代的简单烃或支链烃;
5)至少一种具有双环结构和通式CnH2n-(2+2x)的多不饱和双环烃,其中x是分子中不饱和位置数,n=4-14,其中双环结构中的碳原子数在4和12之间,并且所述的至少一种多不饱和双环烃任选地在双结构上含有多个取代的简单烃或支链烃取代基,并且含有环内不饱和度或位于一个烃取代基上的不饱和度;
6)至少一种具有三环结构和通式CnH2n-4的三环烃,其中n=4-14,所述 三环结构上的碳原子数在4和12之间,并且所述的至少一种三环烃任选地在环结构上含有多个取代的简单烃或支链烃;
7)至少一种含有一个或多个羟基并且具有通式CnH2n+2-2x-2y-z(OH)z的结构,其中n=1-12,并且其中x是所述结构中环的数目并且在0-4之间,并且其中y是所述结构中不饱和键的数目并且在0和n之间,并且其中z为所述化合物中所述的醇基的数目并且在1和4之间,并且其中所述的醇官能团在环外和/或环内;
8)至少一种包含一个或多个醚基并且具有通式CnH2n+2-2x-2yOz的结构,其中n=1-12,并且其中x是所述结构中环的数目并且在0-4之间,并且其中y是所述结构中不饱和键的数目并且在0和n之间,并且其中z为所述结构中醚键的数目并且在1和4之间,并且其中醚键在环外和/或环内;
9)至少一种包含一个或多个环氧基团并且具有通式CnH2n+2-2x-2y-2zOz的结构,其中n=1-12,并且其中x是所述结构中环的数目并且在0-4之间,并且其中y是所述结构中不饱和键的数目并且在0和n之间,并且其中z是所述结构中环氧基团的数量并且在1和4之间,并且其中环氧基团连接在环上或直链上;
10)至少一种包含一个或多个醛基并且通式为CnH2n+2-2x-2y-2zOz的结构,其中n=1-12,并且其中x是所述结构中环的数目并且在0-4之间,并且其中y是所述结构中不饱和键的数目并且在0和n之间,并且其中z是所述结构中醛基的数目并且在1和4之间;
11)至少一种包含一个或多个酮基并且通式为CnH2n+2-2x-2y-2zOz的结构,其中n=1-12,并且其中x是所述结构中环的数目并且在0-4之间,并且其中y是所述结构中不饱和键的数目并且在0和n之间,并且其中z是所述结构中酮基的数目并且在1和4之间,并且其中酮基在环外和/或环内;
12)至少一种包含一个或多个羧基并且通式为CnH2n+2-2x-2y-3z(OOH)z的结构,其中n=1-12,并且其中x是所述结构中环的数目并且在0-4之间,并且其中y是所述结构中不饱和键的数目并且在0和n之间,并且其中z是所述结构中羧基的数目并且在1和4之间;
13)至少一种包含偶数个羧基并且其中酸官能团被脱水以形成环状酸酐基团的结构,其中所述结构的通式为CnH2n+2-2x-2y-6z(O3)z,其中n=1-12,并且 其中x是所述结构中环的数目并且在0-4之间,并且其中y是所述结构中不饱和键的数目并且在0和n之间,并且其中z是所述结构中酸酐基的数目并且为1或2;
14)至少一种包含酯基并且通式为CnH2n+2-2x-2y-2z(O2)z的结构,其中n=1-12,并且其中x是所述结构中环的数目并且在0-4之间,并且其中y是所述结构中不饱和键的数目,其中没有不饱和键与酯的羰基共轭,并且其中z是所述结构中酸酐基的数目并且为1或2;
15)至少一种包含丙烯酸酯官能团并且通式为CnH2n+2-2x-2y-2z(O2)z的结构,其中所述官能团由酯基和至少一个与酯基的羰基共轭的不饱和键组成,其中n=1-12,其中x是所述结构中环的数目并且在0-4之间,其中y是所述结构中不饱和键的数目并且大于或等于1,其中至少一个所述的不饱和键与所述酯的羰基共轭,z是所述结构中酯基的数目并且为1或2;
16)至少一种包含醚基和羰基官能团并且通式为CnH2n+2-2w-2x-2z(O)y(O)z的结构,其中n=1-12,其中w是所述结构中环的数目并且在0-4之间,其中x是所述结构中不饱和键的数目并且在0和n之间,其中y是所述结构中羰基的数目,其中羰基是酮和/或醛,其中z是所述结构中醚基的数目并且为1或2,并且醚基在环外和/或环内 ;
17)包含醚和醇官能团并且通式为CnH2n+2-2w-2x-2z(OH)y(O)z的结构,其中n=1-12,其中w是所述结构中环的数目并且在0-4之间,其中x是所述结构中不饱和键的数目并且在0和n之间,其中y是所述结构中醇基的数目,并且其中z是所述结构中醚基的数目并且为1或2,并且其中醚基在环外和/或环内;
18)至少一种包含选自下列官能团:醇、醚、羰基和羧酸的任何组合并且通式为CnH2n+2-2u-2v-w-2y-3z(OH)w(O)x(O)y(OOH)z的结构,其中n=1-12,并且其中u是所述结构中环的数目并且在0-4之间,并且其中v是所述结构中不饱和键的数目并且在0和n之间,并且其中w是所述结构中醇基的数目并且在0和4之间,其中x是所述结构中醚基的数目且在0和4之间并且其中所述醚基是环外或环内的,其中y是所述结构中羰基的数目并且在0和3之间,其中所述羰基是酮和/或醛,其中z是所述结构中羧基的数目并且在0和2之间;
19)至少一种包含一个或多个伯胺基并且并且通式为CnH2n+2-2x-2y-z(NH2)z的结构,其中n=1-12,其中x是所述结构中环的数目并且在0-4之间,其中y是所述结构中不饱和键的数目并且在0和n之间,其中z为所述化合物中胺基的数目并且在1和4之间,并且其中所述胺官能团是环外和/或环内的;
20)至少一种包含一个或多个仲胺基并且通式为CnH2n+2-2x-2y-2z(NH)z的结构,其中n=1-12,并且其中x是所述结构中环的数目并且在0-4之间,并且其中y是所述结构中不饱和键的数目并且在0和n之间,并且其中z为所述化合物中仲胺基的数目并且在1和4之间,并且其中所述胺官能团是环外和/或环内的;
21)至少一种包含一个或多个叔胺基并且通式为CnH2n+2-2x-2y-3z(N)z的结构,其中n=1-12,并且其中x是所述结构中环的数目并且在0-4之间,并且其中y是所述结构中不饱和键的数目并且在0和n之间,z是所述化合物中叔胺基的数目并且在1和4之间,并且其中所述胺官能团是环外和/或环内的;
22)至少一种包含一个或多个硝基并且通式为CnH2n+2-2x-2y-z(NO2)z的结构,其中n=1-12,并且其中x是所述结构中环的数目并且在0-4之间,并且其中y是所述结构中不饱和键的数目并且在0和n之间,并且其中z是所述化合物中硝基的数目并且在1和4之间,并且其中所述硝基官能团是环外和/或环内的;
23)至少一种包含胺和醚官能团并且通式为CnH2n+2-2u-2v-w-2x-3y-z(NH2)w(NH)x(N)y(OH)z的结构,其中n=1-12,并且其中u是所述结构中环的数目并且在0-4之间,并且其中v是所述结构中不饱和键的数目并且在0和n之间,并且其中w是伯胺基的数目,并且其中x是仲胺基的数目,并且其中y是叔胺基的数目,并且其中1<w+x+y<4,并且其中z是所述化合物中醇基的数目并且在1和4之间,并且其中所述醇基和/或胺基官能团是环外和/或环内的;
24)至少一种包含胺和醇官能团并且通式为CnH2n+2-2u-2v-w-2x-3y-z(NH2)w(NH)x(N)y(OH)z的结构,其中n=1-12,其中u是所述结构中环的数目并且在0-4之间,其中v是所述结构中不饱和键的数目并且在0和n之间, 其中w是伯胺基的数目,其中x是仲胺基的数目,其中y是叔胺基的数目,并且其中1<w+x+y<4,其中z是所述化合物中醚基的数目并且在1和4之间,并且其中所述醚基和/或胺基是环外和/或环内的;
25)至少一种包含胺和羰基官能团并且通式为CnH2n+2-2u-2v-w-2x-3y-2z(NH2)w(NH)x(N)y(O)z的结构,其中n=1-12,其中u是所述结构中环的数目并且在0-4之间,其中v是所述结构中不饱和键的数目并且在0和n之间,其中w是伯胺基的数目,其中x是仲胺基的数目,其中y是叔胺基的数目,并且其中1<w+x+y<4,其中z是所述化合物中羰基的数目并且在1和4之间,其中所述羰基是醛和/或酮,其中所述羰基和/或胺基是环外和/或环内的。
3.权利要求1中所述的形成气隙的方法,其中所述的至少一种有机前体是选自下面的至少一种:α-萜品烯、1,8-萜二烯、环己烷、1,2,4,-三甲基环己烷、1,5-二甲基-1,5-环辛二烯、莰烯、金刚烷、1,3-丁二烯、取代的二烯烃、十氢化萘、1,5-环辛二烯、环辛烷、环辛烯、降冰片二烯、5-亚乙基-2-降冰片烯、环戊烯氧化物和环戊酮。
4.权利要求1中所述的形成气隙的方法,还包括将选自所述的牺牲层、复合层、多孔层及其组合的层图案化。
5.权利要求1中所述的形成气隙的方法,其中通过化学气相沉积(CVD)沉积所述的牺牲层和复合层两者。
6.权利要求1中所述的形成气隙的方法,其中通过等离子体增强的化学气相沉积(PECVD)沉积所述的牺牲层和复合层两者。
7.权利要求1中所述的形成气隙的方法,其中在一个化学气相沉积(CVD)步骤中沉积所述的牺牲层和复合层。
8.权利要求1中所述的形成气隙的方法,其中在一个等离子体增强的化学气相沉积(PECVD)步骤中沉积所述的牺牲层和复合层。
9.权利要求1中所述的形成气隙的方法,其中在步骤(d)中应用的能量包括选自下面的至少一种:α-粒子、β-粒子、γ-射线、x-射线、高能电子、电子束、可见光、红外光、微波频率、射频、等离子体及其组合。
10.权利要求1中所述的形成气隙的方法,其中在步骤(d)中应用的能量是紫外光。
11.权利要求10中所述的形成气隙的方法,其中当紫外光功率在0-5000W范围内;气氛条件选自惰性的、氧化的和还原的;温度为从室温到500℃以及暴露时间为0.01分钟到12小时时应用步骤(d)。
12.权利要求1中所述的形成气隙的方法,其中在步骤(d)中应用的能量是热能。
13.权利要求12中所述的形成气隙的方法,其中当压力为从10毫托到大气压力;气氛条件选自惰性的、氧化的和还原的;温度为从室温到500℃以及暴露时间为0.01分钟到12小时时应用步骤(d)。
14.权利要求1中所述的形成气隙的方法,还包括填充多孔层中的孔。
15.权利要求14中所述的形成气隙的方法,通过采用能够被活化聚合的可聚合的有机物填充所述孔来进行所述的填充过程。
16.权利要求1中所述的形成气隙的方法,还包括重复步骤(a)-(d)至少一次以制备多层结构。
17.权利要求16中所述的形成气隙的方法,还包括填充多孔层中的孔。
18.权利要求17中所述的形成气隙的方法,通过采用能够被活化聚合的可聚合的有机物填充所述孔来进行所述的填充过程。
19.形成气隙的方法,该方法包括:
(a)提供基底;
(b)沉积包括多晶硅或无定形硅的牺牲层;
(c)沉积具有成孔剂和至少一种含有氧化硅前体或有机硅酸盐玻璃(OSG)前体的复合层;
(d)对具有牺牲层和复合层的基底应用能量以除去成孔剂而形成多孔层;和
(e)使具有牺牲层和多孔层的基底与能够通过多孔层扩散的含氟试剂在减少压力条件下接触,以选择性地除去牺牲层而形成气隙。
20.权利要求19中所述的形成气隙的方法,其中所述的含氟试剂是XeF2或BrF3。
21.权利要求19中所述的形成气隙的方法,其中所述的含氟试剂是选自HF、稀有气体卤化物、卤间化合物、ClF3和其混合物的气体。
22.权利要求19中所述的形成气隙的方法,其中当温度低于150℃时进 行步骤(e)。
23.权利要求19中所述的形成气隙的方法,还包括形成刻蚀停止层以保护基底的基层。
24.权利要求23中所述的形成气隙的方法,其中刻蚀停止层是通过热氧化硅基底而形成的SiO2层。
25.权利要求19中所述的形成气隙的方法,还包括将选自牺牲层、复合层、多孔层及其组合的层图案化。
26.权利要求19中所述的形成气隙的方法,其中在步骤(b)中通过化学气相沉积(CVD)来沉积牺牲层。
27.权利要求19中所述的形成气隙的方法,其中在步骤(b)中通过等离子体增强的化学气相沉积(PFCVD)来沉积牺牲层。
28.权利要求19中所述的形成气隙的方法,其中在步骤(c)中通过选自化学气相沉积、旋涂、浸渍涂覆和喷雾沉积的方法来沉积复合层。
29.权利要求19中所述的形成气隙的方法,其中在步骤(d)中应用的能量包括选自下面的至少一种:α-粒子、β-粒子、γ-射线、x-射线、高能电子、电子束、可见光、红外光、微波频率、射频、等离子体及其组合。
30.权利要求19中所述的形成气隙的方法,其中在步骤(d)中应用的能量是紫外光。
31.权利要求30中所述的形成气隙的方法,其中当紫外光功率为0-5000W;气氛条件选自惰性的、氧化的和还原的;温度为从室温到500℃以及暴露时间为0.01分钟到12小时时应用步骤(d)。
32.权利要求19中所述的形成气隙的方法,其中在步骤(d)中应用的能量是热能。
33.权利要求32中所述的形成气隙的方法,其中当压力为从10毫托到大气压力;气氛条件选自惰性的、氧化的和还原的;温度为从室温到500℃以及暴露时间为0.01分钟到12小时时应用步骤(d)。
34.权利要求19中所述的形成气隙的方法,还包括填充多孔层中的孔。
35.权利要求34中所述的形成气隙的方法,通过用能够被活化聚合的可聚合的有机物填充所述的孔来进行所述的填充过程。
36.权利要求19中所述的形成气隙的方法,还包括重复步骤(a)-(e)至少 一次以制备多层结构。
37.权利要求36中所述的形成气隙的方法,还包括填充多孔层中的孔。
38.权利要求37中所述的形成气隙的方法,通过用能够被活化聚合的可聚合的有机物填充所述的孔来进行所述的填充过程。
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CN102569179A (zh) | 2012-07-11 |
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US9293361B2 (en) | 2016-03-22 |
CN101060095A (zh) | 2007-10-24 |
JP2011233926A (ja) | 2011-11-17 |
TWI395268B (zh) | 2013-05-01 |
EP1848032A3 (en) | 2012-02-29 |
EP1848032B1 (en) | 2017-03-01 |
JP2007311777A (ja) | 2007-11-29 |
EP1848032A2 (en) | 2007-10-24 |
CN102569179B (zh) | 2016-08-03 |
JP5485953B2 (ja) | 2014-05-07 |
US20140363950A1 (en) | 2014-12-11 |
KR100859178B1 (ko) | 2008-09-19 |
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