CN1302254A - 低k介电无机/有机复合薄膜及其制造方法 - Google Patents

低k介电无机/有机复合薄膜及其制造方法 Download PDF

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CN1302254A
CN1302254A CN99806506A CN99806506A CN1302254A CN 1302254 A CN1302254 A CN 1302254A CN 99806506 A CN99806506 A CN 99806506A CN 99806506 A CN99806506 A CN 99806506A CN 1302254 A CN1302254 A CN 1302254A
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dielectric film
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P·罗斯
E·洛帕塔
J·费尔茨
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Exxon Mobil
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Abstract

公开了一种在半导体或集成电路衬底上的介电薄膜及其制造方法,其中,所述介电薄膜具有基本由无机基团和有机基团构成的骨架结构和结合在所述骨架结构上的有机侧基,形成一种无机和有机材料的复合材料,从而提供了具有小于4.0的介电常数并表现出在氮气中在400℃失重小于每小时2%的所述薄膜。所述介电薄膜通过等离子体CVD法沉积在位于支架(16)上的衬底(14)上,所述支架通过射频电源(18)偏置。通过气体进口(26)或(28)把有机硅前体引入到沉积室(11)中。

Description

低κ介电无机/有机复合薄膜及其制造方法
本发明涉及具有低介电常数的材料。更具体地，本发明涉及用有机硅前体生产的用于半导体的具有低介电常数的无机/有机复合(即杂合)薄膜，及其制造方法。
未来几年，微电子工业面临的最大挑战之一是寻找代替二氧化硅的先进介电材料，作为金属层间和层内的电介质。介电薄膜层是集成电路和半导体的基本元件。这样的薄膜提供元件之间的电隔离。随着器件密度增大，一般使用多层电介质膜隔离器件的部件。在形成介电薄膜时，重要的是所述薄膜表现出某些性能，例如良好的空隙填充、热稳定性和有利的电性能。通过各种方法形成最广泛使用的介电层，即二氧化硅(SiO2)。最常用的方法是化学气相沉积(CVD)和等离子体CVD。
随着器件密度收缩，线路之间的空隙变得更小，对介电薄膜的要求变得更严格。当临界部件尺寸小于0.25微米时，介电材料的介电常数(κ)的重要性提高。例如，随着工业向着更小的互连线路和器件各部件发展，互连线路的实际长度增大，在其间的空隙减小。这些趋势增大了电路的RC延迟。
对于给定的几何尺寸，一般有两种方法降低RC延迟：(1)通过使用不同的金属可以降低互连线路的电阻；或者(2)通过改进或使用不同介电材料可以降低介电常数。增大RC延迟对于器件的速度具有有害的作用，这具有巨大的商业价值。此外，更窄的线间隙由于更高的电容损耗和更大的串扰导致效率降低。这种降低的效率使得器件对某些应用吸引力降低，如电池供电的计算机、移动电话和其它装置。降低介电常数对于电容损耗和串扰具有有利的影响。因此，非常希望降低器件的RC延迟。
目前，器件可以引入5或6个介电层，所有的介电层由二氧化硅构成。二氧化硅(SiO2)具有较高的介电常数，约为4.0。用合适的低介电常数(低κ材料)材料代替SiO2将导致器件速度的巨大提高和功率消耗的降低。这样的先进低介电材料在使半导体工业发展到下一代器件方面起重要作用。
已经研究了各种材料作为半导体制备中的低κ介电层。为了降低薄膜的介电常数，已经向SiO2薄膜中加入了氟。通过等离子体CVD法形成的稳定的氟掺杂SiO2典型的介电常数为3.5-3.7；然而，要求明显更低的κ值。
产生低κ薄膜的另一种等离子体CVD法是沉积高度交联的碳氟化合物薄膜，通常称为氟化的无定型碳。一般已经报道，这种薄膜更有希望的型式的介电常数在第一次退火后在2.5-3.0之间。氟化的无定型碳的问题仍然存在，最显著的是结合性；热稳定性，包括尺寸稳定性；以及薄膜的集成性能。
也已经研究了聚合物材料。例如，已经使用了旋涂聚合物材料。尽管它们的κ值低，但是由于加工和材料的限制，这些聚合物不能完全令人满意。在约400-450℃的标准加工条件下，聚合物一般是热不稳定和尺寸不稳定的。虽然已经认为这些材料用于包埋结构，但是通常它们不适合于完全堆叠空隙填充或镶嵌结构。
由于旋涂聚合物的缺点，已经探索了汽相聚合作为低κ材料制备的替代方法。已经通过汽相聚合制备的一类特定的聚合物是聚对二甲苯(也称为聚对亚苯基二甲基)如聚对二甲苯N(ppx-N)和聚对二甲苯F(ppx-F)。聚对二甲苯的κ值范围为2.3-2.7，因此作为用于集成电路的低介电材料是有吸引力的。然而，到目前为止已经制备的聚对二甲苯，作为ppx-N呈现较差的热稳定性，而ppx-F昂贵，或者具有机械稳定性的问题。
到目前为止，先进的低κ材料还没有成功地应用于半导体工业。同样，在寻找新材料及其制造方法方面有持续的需要，所述新材料具有低κ值、高热稳定性、完全是可制造的并且产生成本低的可靠器件。
因此，本发明的一个目的是提供一种具有电介电常数的介电材料。
更特别地，本发明的一个目的是提供一种介电薄膜，由用于半导体和集成电路的、具有低介电常数和良好热稳定性的无机/有机复合材料构成。
本发明的另一个目的是使用有机硅前体，如硅氧烷，形成一种具有低κ和良好热稳定性的无机/有机复合介电材料，用于半导体和/或集成电路。
本发明的另一个目的是提供一种沉积介电层的方法，所述介电层用于半导体和集成电路领域，并含有低介电常数的无机/有机复合材料。
通过本发明的一种改进的介电薄膜达到这些和其它目的及优点，所述介电薄膜具有低介电常数，在半导体和/或集成电路中形成为薄膜，并且由无机和有机官能团结合构成。更具体地，所述薄膜包括基本由Si-O-Si构成的骨架结构和结合到所述骨架结构上的有机侧基。在一个另一实施方案中，所述薄膜包括基本由Si-N-Si基团构成的骨架结构和结合到所述骨架结构上的有机侧基。
在本发明的另一个实施方案中，使用有机硅前体形成介电薄膜，用于半导体和/或集成电路中，所述介电薄膜具有基本由Si-O-Si或Si-N-Si基团构成的骨架和有机侧基。
在本发明的另一个实施方案中，提供一种通过化学气相沉积(CVD)在半导体和/或集成电路中沉积介电薄膜的方法。所述薄膜的沉积方式使得所述薄膜包括基本由Si-O-Si或Si-N-Si基团形成的骨架以及连接在所述骨架上的有机侧基。
在本发明的另一个实施方案中，提供一种制造具有多层结构的薄膜的方法。所述方法包括下列步骤，形成由下列层组成的薄膜：在半导体或集成电路器件中的至少一种具有无机和有机材料组合的低κ介电层，具有低介电常数；直接在每个低κ介电层之上和/或直接在每个低κ介电层之下原位形成至少一种氧化物层，形成所述多层薄膜。可以简单地改变工艺条件原位形成所述氧化物层。
在阅读下面提供的本发明的详细描述并参考附图时，本发明的其他目的和优点将会更清楚，其中：
图1是根据本发明的一个实施方案的薄膜结构的示意图。
图2是表示用于实施本发明的反应器的实例的示意图。
图3是表示根据本发明的一个实施方案的薄膜组成的FTIR扫描。
图4a是说明根据文献的FTIR峰范围及其归属的表。
图4b是表示根据本发明的薄膜的FTIR曲线的一种解释的表。
提供了用于半导体工业中的低介电常数(κ)的薄膜，及其制造方法。术语“低κ电介质”、“低介电常数”和“低κ”可以互换使用，一般是指介电常数小于4.0的电介质。术语“非常低介电常数”(vlκ)一般认为是等于或小于3.0的介电常数。根据本发明，低κ和非常低κ介电薄膜具有无机和有机性能的组合。更特别地，所述无机/有机复合薄膜由硅、氧和/或氮、碳和氢构成；或者作为替换，由硅、氧和/或氮、碳和氟构成。所述薄膜的结构是随机混合的有机和无机基团。所述基团可以交联。所述基团可以存在于三维基质中。优选的是，该薄膜具有基本由无机Si-O-Si基团构成的骨架结构，有机侧基结合在所述骨架上。在一个备选的实施方案中，该薄膜具有基本由Si-N-Si构成的骨架结构，有机侧基结合在所述骨架结构上。更优选的是，所述骨架以具有通过无机链连接的环状Si-O-Si基团的三维网络的形式存在，形成环状(或其它三维结构，如球、立方体等)和链状结构。所述无机链可以基本由Si-O-Si基团构成，或者由Si-N-Si基团构成。所述无机链的长度和组成可以变化。有机侧基结合到所述环状和链状基团中的至少之一上。
在一个备选的实施方案中，所述薄膜由一系列连有有机侧基的硅氧烷链(没有环状基团)构成。所述链可以交联。上述有机侧基一般由碳链组成。更具体地，所述有机侧基选自由脂肪族、烯属和芳香族的碳氢化合物，以及脂肪族、烯属和芳香族的碳氟化合物组成的组中。所述侧基不必由相同的单元构成，而是可以是不同有机基团的混合。优选的是，所述有机侧基基本由甲基(CH3)或碳三氟(CF3)基团构成。
参考图1，表示了本发明的一部分低κ薄膜的示例性实施方案。在该实例中，表示了所述环状和链状结构。所述环在该实例中是由四个硅原予构成的环状部分。所述环通过无机链连接。所述链的长度可变，在本例中该链为Si-O-Si基团。如图所示，所述结构的骨架由Si-O-Si环状环和链状基团构成。有机侧基结合在所述环和链基团两者上，且在该实例中，所述有机侧基由甲基构成。
所述薄膜的结构是无规网络。再参考图1，只表示了薄膜的一部分。在每个端部，所述结构连续且可以连接到更多的环、长链或短链上，或者连接到所有以上这些的组合上。一般来说，在所述薄膜中，硅与碳的比例在约0.25∶1-4∶1范围内。估计在所述链基团中的硅与所述环状基团中的硅的密度之比在约10∶1-0.1∶1范围内。
在所述优选的实施方案中，本发明的低κ薄膜具有由环状和链状基团组成的结构。这种环状和链状基团的混合提供了比现有技术薄膜明显的先进性。本发明人已经发现了一种在薄膜中保持环状单元存在的方法，这降低了薄膜的介电常数。此外，本发明人已经发现使所述薄膜结构中的C-C键合最小化，容许把有机物添加到所述薄膜中，而对所述薄膜在450℃的温度下的热稳定性没有明显的不利影响。如图1所示，没有碳与碳的键合。
通过本发明生产的薄膜表现出理想的介电常数同时保持良好的热稳定性。所述薄膜的介电常数小于4.0，优选小于3.0，介电常数在约小于3.0至1.5的范围内是最优选的。例如，用介电常数为3.0试验的薄膜表现出良好的热稳定性，在氮气环境中425℃下，测量的失重为每8小时小于1％。
为了形成本发明的无机/有机复合薄膜，使用有机硅前体化学组成，或者可以使用含有有机硅前体的混合物。在一个实施方案中，可以使用下列分子式的有机硅前体来形成本发明的薄膜：
RnSi(OSi)mX(2m-n+4)
其中，n为0-(2m+4)；m为0-4；所述有机硅可以是线性的或支链的；X是选自由H和卤素组成的组中；R选自由脂肪族、烯属和芳香族的碳氢化合物以及脂肪族、烯属和芳香族的碳氟化合物组成的组中，可以有和没有氧连接。合适的脂肪族、烯属和芳香族的碳氢化合物基团的实例包括甲基、乙基、丙基、丁基和苯基等。
在另一个实施方案中，所述有机硅前体可以由具有下列分子式的环状有机硅氧烷构成：
Rn(SiO)mX(2m-n)
其中，n为0-2m；m为3-10；X选自由H和卤素组成的组中；R选自由脂肪族、烯属和芳香族的碳氢化合物以及脂肪族、烯属和芳香族的碳氟化合物组成的组中，如上所列举的。
在本发明的另一个实施方案中，所述有机硅前体由下列分子式的有机硅氮烷构成：
RnSi(NSi)mX(3m-n+4)
其中，所述有机硅氮烷可以是线性的或支链的；n为0-(3m+4)；m为1-4；X选自由H和卤素组成的组中；R选自由脂肪族、烯属和芳香族的碳氢化合物以及脂肪族、烯属和芳香族的碳氟化合物组成的组中。
在本发明的另一个实施方案中，所述有机硅前体由下列分子式的有机硅氮烷构成：
Rn(SiN)mX(3m-n)
其中，n为0-3m；m为3-10；X选自由H和卤素组成的组中；R选自由脂肪族、烯属和芳香族的碳氢化合物以及脂肪族、烯属和芳香族的碳氟化合物组成的组中。
因此，根据本发明的合适的前体包括：有机硅氧烷、氟硅氧烷、环硅氧烷、含氟的环硅氧烷、有机硅氮烷、氟硅氮烷、环硅氮烷、硅酸盐、TEOS和TMS及其混合物。合适的侧基实例包括：-H、-CH3、-F、-C2H5、-CF3、-C2F5、-C6H5、-C6F5、-CF2CF3、和C-H2CF3。在反应器中混合时可以以最后的形式产生与上述前体类似化学成分的化学品的混合也是适用的，例如，硅烷、硅四氟化物和有机前体的混合物。
特别有利的是，本发明提供了使所述前体的碎裂最小化，因此保持了在薄膜中沉积的大致结构。这样，可以使用具有形成包括带有有机侧基的无机骨架的薄膜结构的组分的前体，因此，为了形成由SiOC构成的无机/有机复合薄膜，在本发明的一个实施方案中，优选的是在等离子体CVD反应器中用有机硅前体沉积所述薄膜。也可以使用上述材料的氟取代物。所述有机硅前体可以是饱和的或不饱和的。根据本发明，合适的有机硅前体的实例包括六甲基二硅氧烷(HMDSO)、1,1,3,3-四甲基二硅氧烷(TMDSO)等。也可以使用其它有机前体，如四乙氧基硅烷(TEOS)。所提到的材料一般是便宜的且容易获得。这些材料在加热时是挥发性的，因此可以引入到等离子体CVD反应器系统中。
在一个备选的实施方案中，通过环状有机硅或环状有机硅氮烷前体形成具有环状和链状结构的本发明的薄膜。所述环状有机硅或有机硅氮烷可以用一个或多个氟原子取代。此外，它们可以是饱和的或不饱和的。合适的环状有机硅的实例包括：环硅氧烷如八甲基环四硅氧烷(OMCTS)、六甲基环三硅氧烷、六苯基环三硅氧烷、八苯基环四硅氧烷、1,3,5-三甲基-1,3,5-三-3,3,3-三氟丙基环三硅氧烷，含氟环硅氧烷，以及产生上述相同化学成分的化学物质的混合物。也可以使用有机硅氮烷前体。
最优选的是，所述前体是八甲基环四硅氧烷(OMCTS)。使用这种环状硅氧烷前体具有特别的优点，因为如上所述，本发明提供了保持部分前体结构的薄膜形成方法。通过保持环状前体的部分结构，形成具有环状和链状结构的薄膜，所述结构是一种三维网络结构。这种三维网络结构降低了所述薄膜的密度，这又进一步降低了介电常数并提高了所述薄膜的热稳定性。重要的是注意，虽然所述三维网络结构在本文中典型的是称为环，但可以存在任何三维结构，如球结构或立方体结构。
通过向体系中加入氟化的材料，利用本发明可以形成氟化的薄膜。这可以用两种方式完成。第一种，向所述反应器中的等离子体中加入氟化的气体。合适的氟化气体是NF3、CF4、SiF4等。第二种，可以向所述反应器中加入氟化的前体。例如，氟硅氧烷或环氟硅氧烷前体可以单独使用，或者与线型或环状有机硅或有机硅氮烷混合使用，形成氟化的薄膜。
为了制备用于半导体工业中的低κ介电薄膜，本发明提供了一种沉积同时具有无机和有机性质的低κ介电薄膜的方法，所述介电薄膜用于半导体和集成电路领域中。所述薄膜由带有有机侧基的无机骨架构成。所述骨架可以是线型的，或者由三维结构(如环、球、立方体等)和链的组合构成。所述薄膜通过化学气相沉积(CVD)形成，优选的是所述薄膜通过在等离子体CVD反应器中的等离子体CVD沉积。具有特别的优点的是，本发明提供了一种改进的CVD法，这是一种保留了前体材料部分结构的薄膜的沉积方法。当所述前体本质上为环状的时候，本发明的方法沉积一种保留所述前体的部分环状结构的薄膜。如上所述，由于这样一种结构提高了在所沉积的薄膜中的低κ性能，所以这是特别有利的。
可以使用各种等离子体CVD反应器实施本发明。在一个示例性的实施方案中，使用图2所示的反应器沉积本发明的薄膜。如图2所示，反应器5包括一个等离子体室10和一个工艺室11。所述等离子室10包括一个等离子源12，用于耦合范围从直流到微波的能量通过发生器13送入等离子体室10，把气体激发成等离子体。在该图中，等离子体源12用排列在等离子室10周围的线圈表示并用rf能量激发，然而，熟悉该领域的技术人员将会理解的是，可以使用该领域中已知的各种类型的等离子体源产生等离子体。
把衬底14放在支架16上，并定位在工艺室11内。支架16可以利用rf能源和/或直流电机18加偏置。支架16可以是一个静电卡盘。室10和11通过口22抽真空。为了在该示例性实施方案中形成薄膜，通过气体进口管24，把所述化学前体注入工艺室11中。另外，可以把所述前体或其它气体通过气体进口26注入等离子体室10中。如果根据本发明的有机硅前体在大气压下以液态存在，所述液体通过汽化器28，使所述前体在引入到室11中之前汽化。此外，可以通过扩散器(bubbler)把所述液体有机硅前体引入到所述室中。同时，可以通过进口27向反应器5中加入稀释的气体和/或氧化性气体。
在前体注入体系中时，所述等离子源使所述前体部分离子化。重要的是控制等离子体条件，使得所述前体不会高度碎裂，也不会过分氧化。这与现有技术的CVD过程正好相反，在现有技术的CVD过程中，人们一般希望在沉积介电薄膜时，所述前体尽可能多地碎裂。有机硅前体的高度碎裂一般将导致沉积具有高介电常数的二氧化硅型材料。如果在所述等离子体中存在一定浓度的氧尤其如此。
所述半导体衬底位于工艺室中，其中，所述半导体衬底暴露于前体中，所述前体反应并通过CVD在表面上沉积薄膜。优选的是，所述前体靠近衬底表面注入工艺室，例如，通过气环来提高所沉积的薄膜的均匀性。
所述前体可以是一种单一的化学物质，或者多种化学物质。已经发现氧的加入可以提高所述薄膜的热稳定性。加入氧的准确浓度取决于工艺条件和系统的结构。
一般来说，与现有技术的体系相反，不向体系中加入惰性气体。已经发现，氩气的加入一般对薄膜有不利影响。氩气被离子化到很高的程度并导致前体碎裂。这又导致薄膜具有高介电常数。相反，已经发现加入氦在某些情况下对介电常数的影响很小，并且可以进一步提高所述薄膜的热稳定性。
如上所述，工艺条件对沉积本发明的薄膜是重要的。最重要的因素是系统的功率和压力、以及有机硅流量、氧与有机硅流量比。重要的是注意，在上述教导中，准确的工艺条件将随所用反应器的种类和结构而变化。在本发明的一个示例性实施方案中，所述等离子体室包括等离子体源，激发是在200-20,000W/ft3范围内的功率密度下进行的。所述工艺条件与所用的前体和反应器的结构密切相关。例如，在等离子体系统的情况下，低激发功率一般产生有机薄膜，高激发功率一般产生热稳定性更高的薄膜。如果所述激发功率太高，所述薄膜变成类SiO2薄膜，介电常数太高。如果所述激发功率太低，那么，热稳定性将非常差。此外，当功率太低时，或者没有适当地确定等离子体的化学组成时，在某些情况下有可能在薄膜中产生不希望存在的基团。在这样的条件下，在FTIR谱图中已经观察到与Si-OH有关的峰，并且介电常数高于希望值。同时，氧在所述方法中的作用是改善薄膜的热稳定性。氧的量随着所用的反应器和工艺条件而变化。例如，所用的氧的百分比浓度是工艺条件的函数，例如rf功率、压力、以及有机硅前体的流量。太多的氧将导致形成类SiO2材料的薄膜。太少的氧一般形成比希望值的有机成分更多有机成分的薄膜，这降低了所述薄膜的热稳定性并可能导致在所述薄膜中形成不希望的基团，如-OH。
虽然已经描述了一种反应器，但是，熟悉该领域的技术人员将会理解可以使用不同种类的反应器来沉积本发明的薄膜。例如，可以使用在大气压、低于大气压的压力或者在低压下操作的热CVD反应器。在热CVD系统中，在氧化剂的存在下，有机硅被热降解。对所述室的温度、氧化剂(如臭氧、过氧化氢和/或氧)的性质、以及氧化剂浓度的控制对于生产低κ薄膜是重要的。
在半导体和集成电路器件的制造中，本发明的另一个实施方案提供了一种具有多层结构薄膜的制备方法。在某些应用中提供多层的薄膜是有利的，其中，与低κ介电薄膜一起形成一种氧化物(如SiO2或类SiO2)，来形成所述多层的薄膜。可以在所述低κ介电层之上或之下形成所述氧化物层，来提供一个防护层，或者改进结合性。根据本发明，可以直接在低κ介电层之上和/或直接在低κ介电层之下原位形成至少一种氧化物、或类氧化物层。所述低κ介电层由无机和有机材料的混合物组成。如上所述来形成所述低κ介电薄膜。所述氧化物或二氧化硅层可以简单地通过改变反应器中的工艺条件原位形成。可以用两种方式使用工艺条件。第一种，可以使用现有技术已知的SiO2沉积方法。第二种，可以改变本发明的方法，使得所述前体大量发生碎裂，导致SiO2或SiO2型薄膜的沉积。可以用多种方式改变所述方法，引起所述前体的大量碎裂，例如把所述前体暴露于更高的等离子体功率密度下、增大氧的流量、加入氩气、或者任何这些方法的组合。
如上所述，可以在所述多层薄膜中的任何合适位置形成所述SiO2层。然后在半导体器件中的任何合适位置形成所述多层薄膜。例如，所述SiO2层可以直接在所要求的低κ薄膜之下形成，来改善结合性，即所述低κ薄膜直接在所述SiO2层之上。另外，可以形成所述SiO2层作为器件中的顶层，以提供一个防护层，或者有助于进一步加工，例如化学机械平面化或腐蚀。
                           实验
通过说明而不是限制的方式提供下列实施例。
实施例1
使用在13.56MHz的频率下产生的等离子体放电中混合的八甲基环四硅氧烷(OMCTS)和氧，在圆筒形等离子体反应器中的4"硅晶片上形成根据本发明的非常低κ介电薄膜。把所述硅晶片放在铜制的衬底夹具上，所述铜制衬底夹具在沉积过程中是电绝缘的。晶片用能适应真空的粘合剂固定在所述衬底夹具上，并放入所述沉积室内。所述沉积室直径8”，长8”，含有其中心与所述硅晶片中心一致的中空阴极电极系统。所述沉积室用旋转真空泵抽真空到小于20毫乇的压力。一旦所述沉积室抽真空后，把OMCTS液体注入到加热的不锈钢汽化系统中，把所述物料汽化形成蒸气流，然后以约8seem(标准立方厘米每分钟)的流量可控地流入等离子体反应器。在OMCTS流稳定后，以5sccm的流量通过与所述OMCTS相同的气体进口使氧气(来自压缩气体气瓶，纯度为99.95％)可控地流入所述反应器。在反应器中的所得压力约为150毫乇(mTorr)。然后用13.56MHz的电源，用300瓦的功率点燃等离子体，并保持等离子体放电约5分钟，其间，在所述晶片表面沉积薄膜。使薄膜沉积到5000埃的厚度。用椭圆计测量薄膜厚度，使用铝点技术(aluminum dot techniques)测量介电常数。所述实验获得2.6的介电常数。用上述相同的条件和方法在晶片上沉积另外的薄膜，然后在400℃加热1小时测量热失重。所述薄膜表现出2.0重量％的失重。然后使所述薄膜经过425℃ 1小时和450℃ 1小时的热循环。在每种情况中的失重约为每小时0.4％，从而表明有理想的介电常数和热稳定性。
实施例2
在第二组实验中，根据本发明方法的另一个实施方案沉积低κ薄膜，其中，改变所述前体的流量和等离子体条件。所用的反应器与实施例1中所述的反应器一样，并使用相同的前体，然而，在本实验中，氧的流量约为2.5sccm。OMCTS的流量相同，约为8sccm。所述等离子条件也不同，在这种情况下，所述等离子体用13.56MHz的电源，用275瓦的功率点火，并保持所述等离子体放电约5分钟。用标准铝点电容实验法(alminum dot capacitance test method)测量所得的5000埃厚的薄膜，获得3.3的介电常数。用上述相同的条件和方法在晶片上沉积本发明另外的薄膜，然后在400℃加热1小时测量热失重。所述薄膜表现出0.3重量％的失重。然后使所述薄膜经过425℃ 1小时和450℃ 1小时的热循环，分别产生0.3％和0.4％的失重，再次表明有理想的介电常数和热稳定性。
实施例3
在第三组实验中，根据本发明的另一个实施方案沉积非常低к介电薄膜。在这组实验中，使用Watkins-Johnson Company HDP工具组(cluster tool)反应器型号WJ-2000H(有一个感应耦合等离子体源)在下列条件下在8英寸硅晶片上沉积低κ薄膜：把汽化的OMCTS以0.300ccm的液体流量(在室温下测定)注入所述反应器。此外，以20sccm的流量加入氧。所述等离子体源在13.56MHz频率下约600瓦的RF输入功率(功率密度为1200瓦/立方英尺)下操作。在所述反应器中所得的压力约为25毫乇。在两种工艺时间下沉积薄膜；即约2分45秒，和6分30秒。用椭圆计测量，较短的工艺时间获得约5000埃的薄膜。用Hg探针技术在1MHz下测量该薄膜的介电常数为2.97。然后在氮环境中通过热失重分析(TGA)测量所述薄膜的热稳定性。较厚的薄膜(用较长工艺时间沉积的)在以10℃/分钟的速度从室温加热到425℃、然后在425℃保温140分钟、再冷却到室温时，表现出3.65％的失重。这样的结果表明了有理想的介电常数和热稳定性。
图3表示根据本发明的、由无机和有机材料构成的介电层的Fourier变换红外吸收(FTIR)谱图。作为参考，图4a是表示根据文献的FTIR峰范围及其归属的表。虽然FTIR谱图的解释并不是准确的科学方法，但是本发明人认为在本发明的薄膜的FTIR扫描中描述的吸收峰对应于图4b所示的结构。
如所述FTIR谱图所示，并参考图4a和图4b的解释，本发明的薄膜不呈现出明显的碳-碳键合。所述FTIR谱图和图4a和4b还表明主要存在有机硅骨架，具有在约1060-1080cm-1波数的Si-O-Si环状结构，其峰肩在约1080cm-1；具有在约1020-1060cm-1波数的Si-O-Si链，主峰在1026cm-1。在该插图中，表明有机侧基主要在1265cm-1和888cm-1，分别由Si-(CH3)3和Si(CH3)2构成。虽然表示了一个实施例的FTIR谱图，但是，应该理解所述FTIR谱图将会变化并且仍然落在本
发明的说明范围内。
因此，已经提供了一种用于半导体和集成电路中的改进的介电薄膜，由具有低介电常数的无机/有机复合材料构成。还提供了本发明的前体化学组成和沉积方法。所述薄膜表现出在约1.5-4.0范围内的低介电常数、高热稳定性、且完全能以可靠的器件产量制造。
虽然结合特定的实施方案描述了本发明，但是，很明显，根据上述描述和说明，熟悉该领域的技术人员可以进行各种变化、取代、替换和改进。因此，本说明书意图包括在所附权利要求的精神范围内的所有这种变化、取代、替换和改进。

Claims (50)

1．一种在半导体或集成电路上的低介电常数介电薄膜，包括：
一种基本由无机基团构成的骨架结构；和
连接在所述骨架结构上的有机侧基，形成无机和有机材料的复合材料，提供了具有小于4.0的介电常数并表现出在氮气中在400℃失重小于每小时2％的所述薄膜。
2．根据权利要求1的介电薄膜，其中，所述介电常数小于3.0。
3．根据权利要求1的介电薄膜，其中，所述介电薄膜由多层组成，其中，至少一个氧化硅层在所述介电薄膜之上和/或之下原位形成。
4．根据权利要求1的介电薄膜，其中，所述骨架结构在Si-O-Si基团的三维、交联基质中形成。
5．根据权利要求1的介电薄膜，其中，所述骨架结构在Si-N-Si基团的三维、交联基质中形成。
6．根据权利要求1的介电薄膜，其中，所述骨架结构由Si-O-Si基团构成，并且通过等离子体化学气相沉积形成。
7．根据权利要求1的介电薄膜，其中，所述薄膜使用有机硅前体通过等离子体化学气相沉积形成。
8．根据权利要求1的介电薄膜，其中，所述薄膜通过化学气相沉积形成。
9．根据权利要求1的介电薄膜，其中，所述薄膜使用有机硅前体通过化学气相沉积形成。
10．根据权利要求1的介电薄膜，其中，所述骨架结构进一步基本由环状Si-O-Si基团和链构成。
11．根据权利要求1的介电薄膜，其中，所述有机侧基基本没有C-C键合。
12．根据权利要求10的介电薄膜，其中，所述环状基团由环、球、立方体或其任何组合构成。
13．根据权利要求10的介电薄膜，其中，在所述无机链中的Si与在所述环状Si-O-Si基团中的Si的比例在约10∶1-0.1∶1的范围内。
14．根据权利要求1的介电薄膜，其中，所述有机侧基选自由-H、-CH3、-F、-C2H5、-CF3、-C2F5、-C6H5、-CF2CF3和CH2CF3组成的组中。
15．一种具有低介电常数的在半导体或集成电路上的介电薄膜的制造方法，包括下列步骤：
提供至少一种有机硅前体；
通过化学气相沉积进行沉积，其中，所述前体反应并在所述衬底表面沉积所述介电薄膜；
其中，所述介电薄膜具有一种基本由无机基团构成的骨架结构和结合在所述骨架结构上的有机侧基，形成一种无机和有机材料的复合材料，提供了具有小于4.0的介电常数并表现出在氮气中在400℃失重小于每小时2％的所述薄膜。
16．根据权利要求15的方法，其中，所述沉积步骤通过等离子体化学气相沉积进行。
17．根据权利要求15的方法，其中，所述介电薄膜具有小于3.0的介电常数。
18．根据权利要求15的介电薄膜，其中，所述骨架结构进一步基本由环状Si-O-Si基团和链构成。
19．根据权利要求15的介电薄膜，其中，所述骨架结构进一步基本由环状Si-N-Si基团和无机链构成。
20．根据权利要求18的介电薄膜，其中，所述环状基团由环、球、立方体、或其任何组合构成。
21．根据权利要求15的介电薄膜，其中，所述前体是环状有机硅化合物。
22．根据权利要求15的方法，其中，所述前体选自由硅氧烷、氟硅氧烷、环硅氧烷、含氟环硅氧烷、有机硅氮烷、氟硅氮烷、环状有机硅氮烷、环氟硅氮烷、及其混合物组成的组中。
23．根据权利要求15的介电薄膜，其中，所述有机侧基选自由-H、-CH3、-F、-C2H5、-CF3、-C2F5、-C6H5、-CF2CF3和CH2CF3组成的组中。
24．根据权利要求15的方法，其中，所述前体具有下列分子式：
RnSi(OSi)mX(2m-n+4)
其中，所述前体可以是线型的或支链的；n为0-(2m+4)；m为0-4；X选自由H和卤素组成的组中；R选自由脂肪族、烯属和芳香族的碳氢化合物以及脂肪族、烯属和芳香族的碳氟化合物组成的组中。
25．根据权利要求15的方法，其中，所述前体具有下列分子式：
Rn(SiO)mX(2m-n)
其中，n为0-2m；m为3-10；X选自由H和卤素组成的组中；R选自由脂肪族、烯属和芳香族的碳氢化合物以及脂肪族、烯属和芳香族的碳氟化合物组成的组中。
26．根据权利要求15的方法，其中，所述前体具有下列分子式：
RnSi(NSi)mX(3m-n+4)
其中，所述前体可以是线型的或支链的；n为0-(3m+4)；m为1-4；X选自由H和卤素组成的组中；R选自由脂肪族、烯属和芳香族的碳氢化合物以及脂肪族、烯属和芳香族的碳氟化合物组成的组中。
27．根据权利要求15的方法，其中，所述前体具有下列分子式：
Rn(SiN)mX(3m-n)
其中，n为0-3m；m为3-10；X选自由H和卤素组成的组中；R选自由脂肪族、烯属和芳香族的碳氢化合物以及脂肪族、烯属和芳香族的碳氟化合物组成的组中。
28．根据权利要求15的方法，其中，所述前体是八甲基环四硅氧烷。
29．根据权利要求15的方法，其中，在所述有机侧基中的碳-碳键合最少化。
30．根据权利要求15的方法，还包括下列步骤：
提供与所述前体混合的氧气。
31．根据权利要求15的方法，还包括下列步骤：
在所述介电薄膜之上和/或之下原位沉积至少一层氧化硅，形成多层的薄膜。
32．一种通过等离子体化学气相沉积在半导体或集成电路上沉积低κ介电薄膜的方法，包括下列步骤：
把所述衬底定位在所述工艺室内；
向所述工艺室内注入至少一种有机硅前体；
向所述等离子体室内提供功率，产生等离子体；
在所述衬底表面沉积所述介电薄膜，所述介电薄膜具有基本由环状和线型Si-O-Si基团构成的骨架结构和结合在所述骨架结构上的有机侧基，提供了具有小于4.0的介电常数并表现出在氮气中在400℃失重小于每小时2％的所述薄膜。
33．根据权利要求32的方法，其中，所述介电薄膜具有小于3.0的介电常数。
34．根据权利要求32的方法，还包括使所述前体在等离子体条件下暴露于所述等离子体，从而使所述介电薄膜的结构部分保留所述前体的结构。
35．根据权利要求32的方法，其中，所述前体是环状有机硅烷化合物。
36．根据权利要求32的方法，其中，所述前体选自由硅氧烷、氟硅氧烷、环硅氧烷、含氟环硅氧烷、有机硅氮烷、环硅氮烷、氟硅氮烷、环氟硅氮烷、及其混合物组成的组中。
37．根据权利要求32的方法，其中，所述前体具有下列分子式：
Rn(SiO)mX(2m-n)
其中，n为0-2m；m为3-10；X选自由H和卤素组成的组中；R选自由脂肪族、烯属和芳香族的碳氢化合物以及脂肪族、烯属和芳香族的碳氟化合物组成的组中。
38．根据权利要求32的方法，其中，所述前体具有下列分子式：
Rn(SiN)mX(3m-n)
其中，n为0-3m；m为3-10；X选自由H和卤素组成的组中；R选自由脂肪族、烯属和芳香族的碳氢化合物以及脂肪族、烯属和芳香族的碳氟化合物组成的组中。
39．根据权利要求32的方法，其中，所述前体是八甲基环四硅氧烷。
40．根据权利要求32的方法，其中，所述等离子体室包括一个等离子体源，所述暴露还包括把所述前体暴露于在200-20,000瓦/立方英尺范围内的功率密度下的所述等离子体中。
41．根据权利要求32的方法，还包括下列步骤：
在所述介电薄膜之上和/或之下原位沉积至少一层氧化硅，形成多层的薄膜。
42．根据权利要求32的方法，其中，在所述有机侧基中的碳-碳键合最少化。
43．根据权利要求32的方法，还包括下列步骤：
提供与所述有机硅前体混合的氧气。
44．根据权利要求32的方法，还包括下列步骤：
向所述反应器中引入稀释气体。
45．根据权利要求32的方法，还包括下列步骤：
向所述反应器中引入氦。
46．根据权利要求32的薄膜，其中，所述无机链中的Si与所述环状Si-O-Si基团中的Si的比例在约10∶1-0.1∶1范围内。
47．根据权利要求32的方法，其中，所述介电薄膜具有基本由环状和线型Si-N-Si基团构成的骨架结构和结合在所述骨架结构上的有机侧基。
48．根据权利要求32的方法，其中，所述环状基团由环、球、立方体、或其任何组合构成。
49．根据权利要求32的方法，其中，所述有机硅前体是选自由八甲基环四硅氧烷(OMCTS)、六甲基环三硅氧烷、六苯基环三硅氧烷、八苯基环四硅氧烷、1,3,5-三甲基-1,3,5-三-3,3,3-三氟丙基环三硅氧烷、含氟环硅氧烷、及其混合物组成的组中的环硅氧烷。
50．根据权利要求15的方法，其中，所述有机硅前体是选自由八甲基环四硅氧烷(OMCTS)、六甲基环三硅氧烷、六苯基环三硅氧烷、八苯基环四硅氧烷、1,3,5-三甲基-1,3,5-三-3,3,3-三氟丙基环三硅氧烷、含氟环硅氧烷、及其混合物组成的组中的环硅氧烷。
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