CN107104036B - 用于在沟槽侧壁或平整表面上选择性形成氮化硅膜的方法 - Google Patents

用于在沟槽侧壁或平整表面上选择性形成氮化硅膜的方法 Download PDF

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CN107104036B
CN107104036B CN201710086406.XA CN201710086406A CN107104036B CN 107104036 B CN107104036 B CN 107104036B CN 201710086406 A CN201710086406 A CN 201710086406A CN 107104036 B CN107104036 B CN 107104036B
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dielectric film
film
plasma
sidewall portions
portions
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CN107104036A (zh
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石川大
深泽笃毅
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ASM IP Holding BV
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Abstract

一种用于在沟槽中制备层结构的方法，其包括：同时在沟槽的上表面和底表面以及侧壁上形成含有Si‑N键的介电膜，其中通过由在两个电极之间施加电压激发的等离子体的轰击使在上表面和底表面上形成的膜的顶部/底部部分和在侧壁上形成的膜的侧壁部分具有不同的耐化学性，所述在电极之间将基材平行于两个电极放置；并且通过湿蚀刻基本去除所述膜的顶部/底部部分和侧壁部分中的任一个但不同时去除两个，所述湿蚀刻根据不同的耐化学性，相对于所述膜的顶部/底部部分和侧壁部分中的一个，更主要地去除所述膜的顶部/底部部分和侧壁部分中的另一个。

Description

用于在沟槽侧壁或平整表面上选择性形成氮化硅膜的方法
背景
发明领域
本发明涉及一种用于在基材的上表面中形成的沟槽中制备由含有Si-N键的介电膜组成的层结构的方法。
背景技术
在大规模集成电路(LSI)的生产过程中，有一些工艺用于在沟槽中形成侧壁。侧壁被用作间隔体或被用于阻挡从沟槽的侧边表面上蚀刻结构。通常，通过以下方法来形成侧壁：在沟槽的表面上形成共形膜，并随后通过不对称蚀刻去除在形成沟槽的上表面上形成的所述膜的部分和在所述沟槽的底表面上形成的所述膜的部分。不过，当使用这样的形成方法时，需要过蚀刻从而去除侧壁的基脚(footing)，在所述基脚处侧壁的厚度在底部和底部附近增加，形成斜坡。过蚀刻引起了下方层的蚀刻并且造成层结构破坏。
本发明中包括的与背景技术相关的任何问题和方案的讨论仅用于为本发明提供背景的目的，不应作为对发明本发明时已知任何或所有讨论的认同。
概述
在一些实施方式中，在形成有沟槽的基材的顶表面上和在所述沟槽的底表面上形成的膜与在所述沟槽的侧壁上形成的膜具有与湿蚀刻相关的不同的膜性质(即膜性质的方向控制)。通过使基材湿蚀刻，可选择性去除在沟槽的顶/底表面上形成的膜或在沟槽的侧壁上形成的膜，即，在沟槽结构中选择性地形成水平方向上延伸的膜或在垂直方向上延伸的膜。根据上述方法，可仅通过湿蚀刻而不需要干蚀刻作为蚀刻方式选择性地形成沟槽结构中的水平或垂直层(即膜形成的方向控制)。
在一些实施方式中，具有方向控制的膜性质的膜可以是通过等离子体增强化学气相沉积(PECVD)或等离子体增强原子层沉积(PEALD)沉积的氮化硅膜。或者，在一些实施方式中，沉积氮化硅膜而不需要方向控制，并且随后处理所述膜以提供膜性质的方向性。也即是，当在膜沉积过程中或在膜沉积之后在氮化硅膜上进行离子轰击时，可从膜中去除杂质，从而使所述膜致密化并改善所述膜的质量；不过当在与所述膜垂直的方向上在介电膜上增强并不对称地进行离子轰击时，膜的质量会降级，从而断开Si-N键，降低所述膜的密度并增加湿蚀刻速率。由于通常相信离子轰击引起膜的致密化并降低湿蚀刻速率，因此上述现象是完全意想不到的。离子轰击的强度可通过使用可控制离子的入射方向、离子的剂量和离子的能量的平行板电极构造形成的等离子体(例如电容耦合等离子体)来方向控制。根据不旨在限制本发明的上述理论，可控制膜性质的方向性。
出于总结本发明各方面和相对于背景技术所取得的益处的目的，在本文中描述本发明的某些目标和益处。当然，应理解本发明的任意具体实施方式不必然能实现所有的这些目的或优点。因此，例如本领域普通技术人员将理解可以下述方式实施或进行本发明：取得或优化本文所教导的一种或更多种优点，而不必然取得本文所可能教导或暗示的其它目的或优点。
本发明的其它方面、特征和优点会在以下详细说明中变得显而易见。
附图简要说明
现结合优选的实施方式的附图说明本发明的这些或其它特征，这旨在说明本发明而不是限制本发明。为了说明目的，附图被大大简化并且不一定按比例绘制。
图1A是示意图，说明了用于沉积能在本发明的实施方式中使用的保护膜的PEALD(等离子体增强原子层沉积)设备。
图1B说明了示意图，表示使用流动通过系统(FPS)的能在本发明的实施方式中使用的前体供应系统。
图2是流程图，说明了制备根据本发明的一个实施方式的层结构的步骤。
图3是流程图，说明了制备根据本发明的另一个实施方式的层结构的步骤。
图4是流程图，说明了制备根据本发明的另一个实施方式的层结构的步骤。
图5是流程图，说明了制备根据本发明的另一个实施方式的层结构的步骤。
图6是流程图，说明了制备根据本发明的不同实施方式的层结构的步骤。
图7的图显示了根据本发明的一个实施方式，RF功率与在沟槽的顶表面上形成的膜和在沟槽的侧壁上形成的膜的湿蚀刻速率之间的关系，显示了阈值(参考)RF功率。
图8显示了根据本发明的一些实施方式形成的氮化硅膜的截面图的扫描电子显微镜(SEM)照片。
图9显示了根据本发明的一个实施方式形成的氮化硅膜的截面图的扫描电子显微镜(SEM)照片。
图10说明了根据本发明的一个实施方式形成的氮化硅膜的截面图。
图11说明了根据本发明的另一实施方式形成的氮化硅膜的截面图。
图12是显示了RF功率与根据本发明的一个实施方式的SiN膜的Si-N峰强度[au]之间的关系的图。
图13是显示了RF功率与根据本发明的一个实施方式的SiN膜的密度[g/cm3]之间的关系的图。
图14的图显示了等离子体密度与根据本发明的一个实施方式在沟槽的顶表面上形成的膜和沟槽的侧壁上形成的膜的湿蚀刻速率之间的一般关系。
具体实施方式
本文中，“气体”可包括蒸发的固体和/或液体并可由单一气体或气体混合物构成。在本文中，通过喷淋头被引入到反应腔室中的处理气可包含前体气体和添加气体、基本由或由前体气体和添加气体组成。前体气体和添加气体通常以混合的气体或分别被引入到反应空间中。可使用载气(例如惰性气体)来引入前体气体。所述添加气体可包含反应气体和稀释气体(例如惰性气体)、基本由或由反应气体和稀释气体(例如惰性气体)组成。所述反应气体和稀释气体可作为混合的气体或分别被引入到反应空间中。前体可包含两种或多种前体，反应气体可包含两种或多种反应气体。所述前体是在基材上化学吸收的气体并且通常含有准金属或金属元素，所述准金属或金属元素构成了介电膜基质的主要结构，所述用于沉积的反应气体是当所述气体被激发成将原子层或单层固定在基材上时与在基材上化学吸收的前体反应的气体。“化学吸收”是指化学饱和吸收。可使用除了处理气体之外的气体，即不通过喷淋头引入的气体来例如密封反应空间，所述除了处理气体之外的气体包括密封气体，例如稀有气体。在一些实施方式中，“膜”是指基本没有针孔的，在垂直于厚度方向的方向上连续延伸以覆盖整个目标物或相关表面的层，或简单来说是覆盖目标物或相关表面的层。在一些实施方式中，“层”指在表面或膜的同义词或非膜结构上形成的具有特定厚度的结构。膜或层可由具有某些特征的离散的单一膜或层或多层的膜或层构成，相邻膜或层之间的边界可清晰或不清晰并且所述边界可根据相邻膜或层的物理、化学、和/或任何其它特征、形成方法或顺序、和/或功能或目的建立。
在本发明中，“含有Si-N键”可指通过一个或多个Si-N键表征，具有基本上由一个或多个Si-N键构成的主骨架，和/或具有基本上由一个或多个Si-N键构成的取代基。含有Si-N键的介电膜包括但不限于SiN膜和SiON膜，其具有约2-10，通常为约4-8的介电常数。
在本发明中，“退火”表示在该过程中处理材料以达到其稳定形式，例如组分中存在的封端基团(例如醇基和羟基)被更稳定的基团(例如Si-Me基团)取代和/或形成更稳定的形式(例如Si-O键)，通常导致膜致密化。
此外，在本文中，除非另外说明，“一”或“一个”是指一个种或包括多个种的一个类。在一些实施方式中，术语“由……构成“和“具有”独立地指“通常或广泛地包含”、“包含”、“基本由……组成”或“由……组成”。同样，在本文中，任何限定的含义并不必排除在一些实施方式中普通和自定义含义。
此外，在本文中，当可行范围可根据常规作业决定时，变量的任意两个数字可构成变量的可行范围，并且任何显示的范围可包括或排除端点。另外，在一些实施方式中，表示的变量的任何值(无论它们是否与“约”一起出现)可指精确值或近似值并包括等效值，可指均值、中值、代表值、大多数等。
在本发明中，当没有说明条件和/或结构时，本领域技术人员可从本发明的角度出发，按常规试验容易地提供所述条件和/或结构。在所有公开的实施方式中，出于预期的目的，实施方式中使用的任何元素可用与其等效的任何元素替代，包括本文明确地、必需地或固有地公开的那些。另外，本发明可等同地应用于设备和方法。
借助优选的实施方式来解释这些实施方式。然而，本发明不局限于这些优选的实施方式。
一些实施方式提供了一种用于在基材的上表面中形成的沟槽中制备由含有Si-N键的介电膜构成的层结构的方法，所述方法包括：(i)同时在沟槽的上表面和底表面以及侧壁上形成含有Si-N键的介电膜，其中通过由在两个电极之间施加电压激发的等离子体的轰击而使在上表面和底表面上形成的介电膜的顶部/底部部分和在侧壁上形成的介电膜的侧壁部分具有不同的耐化学性，在所述两个电极之间将基材平行于两个电极放置；并且(ii)通过湿蚀刻基本去除所述介电膜的顶部/底部部分和侧壁部分中的任一个但不同时去除两个，所述湿蚀刻根据不同的耐化学性，相对于所述介电膜的顶部/底部部分和侧壁部分中的另一个，更主要地去除所述介电膜的顶部/底部部分和侧壁部分中的一个。术语“同时形成”可表示大致或基本在相同时间、相同工艺中或相同步骤中形成，这包括大致或基本在相同时间、相同工艺中或相同步骤中沉积，和/或大致或基本在相同时间、相同工艺中或相同步骤中处理。在本发明中，术语“基本”或“基本上”可以指足够的、相当大量的由本领域技术人员认为足以用于预期的目的或功能的材料量，尺寸，时间或空间(例如，相对于总的或参考的值，至少70％，80％，90％或95％)。
图2是流程图，说明了制备根据本发明的一个实施方式的层结构的步骤。步骤S1和步骤S2分别对应于步骤(i)和(ii)。在步骤S1中，通过使用等离子体轰击，在沟槽上形成了具有膜性质的方向性的介电膜。可在沉积膜的过程中或在沉积膜完成后施加等离子体轰击。在步骤S2中，根据所述膜的顶部/底部部分与所述膜的侧壁部分之间膜性质的不同，所述膜的所述部分中的一个相对于另一个通过湿蚀刻而被更主要地蚀刻，在层结构中仅留下所述部分中的一个。
在步骤S2中，使用例如氟化氢(HF)溶液进行湿蚀刻。
通过调整通过在两个电极之间施加电压激发的等离子体的轰击，可赋予在上表面和下表面上形成的介电膜的顶部/底部部分和在侧壁上形成的介电膜的侧壁部分不同的耐化学性，其中在所述电极之间将基材平行于两个电极放置。等离子体是具有高游离电子含量(约50％)的部分离子化的气体，当通过在平行电极之间施加AC电压来激发等离子体时，通过由在等离子体壳层与较低电极之间形成的自dc偏压(VDC)加速离子，并轰击在沿与膜垂直的方向上(离子入射方向)放置在较低电极上的基材上的膜。等离子体的轰击可由等离子体密度或离子的动能表示。可主要通过调节压力和RF功率来调整等离子体密度(压力越低且功率越高，则等离子体密度变得越高)。还可通过施加具有为离子跟踪设置的较低频率(<1MHz)的AC压或dc偏压来调整等离子体密度。可使用探针法(例如“使用杂化朗格缪尔探针和微波干涉法的高精确性等离子体密度测量(High accuracy plasma densitymeasurement using hybrid Langmuir probe and microwave interferometermethod)”，Deline C等，Rev.Sci.Instrum.2007年11月；78(11):113504，其公开的内容通过引用全文结合入本文)测定等离子体密度。当在等离子体中插入探针并在其上施加电压时，电流流过探针，这被称为“离子饱和电流”(Ii)，其可以如下计算，并随后可如下计算等离子体密度(Np)：
Ii＝e x Ne√(kTe/M)x exp(1/2)eA；Np＝Ii√(M/kTe)/exp(1/2)eA，其中Ii：离子饱和电流[A]；A：探针的表面积[m2]；e：电子电荷[C]；Ne：电子密度[m-3]；k：波尔兹曼常数[J/K]；Te：电子温度[K]；M：离子质量[kg]。
图14的图显示了等离子体密度与根据本发明的一个实施方式在沟槽的顶表面上形成的膜和沟槽的侧壁上形成的膜的湿蚀刻速率之间的一般关系。在该图中，由蚀刻速率表示耐化学性。在所述膜的顶部/底部表面上，等离子体轰击通常沿垂直于膜表面的方向上发挥作用，而在所述膜的侧壁表面上，等离子体轰击通常沿平行于膜表面的方向上发挥作用。当等离子体密度低时，由于包含在在所述膜上发挥作用的等离子体中的离子去除了杂质并导致所述膜的致密化，因此在沟槽的顶部/底部表面上形成的膜的湿蚀刻速率是低的。然而，如图14所示，当等离子体密度增加时，在顶部/底部表面上形成的膜的湿蚀刻速率增加，这是因为离子的剂量太高从而增强了Si-N键的断裂。另一方面，当等离子体密度低时，由于包含在在所述膜上发挥作用的等离子体中的离子剂量不足以去除杂质并导致所述膜的致密化，因此在沟槽的侧壁表面上形成的膜的湿蚀刻速率是高的。然而，如图14所示，当等离子体的密度增加时，在侧壁表面上形成的膜的湿蚀刻速率降低。换而言之，当等离子体密度增加时，在顶部/底部表面上形成的膜的膜质量降级，而当等离子体密度增加时，在侧壁表面上形成的膜的膜质量得到改善。因此，等离子体密度中有阈值点，在该点上顶部/底部表面上的膜的膜质量(或膜性质)和在侧壁上的膜的膜质量(或膜性质)基本相当，即显示在顶部/底部表面上形成的膜的湿蚀刻速率与等离子体密度之间的关系的线与显示在侧壁上形成的膜的湿蚀刻速率与等离子体密度之间的关系的线在如图14所示的阈值点处相交。在顶部/底部表面上的膜的膜性质和在侧壁表面上的膜的膜性质在阈值点处反转。因此，通过调节等离子体密度，可形成具有膜性质的方向性的膜。当将等离子体密度设置为低于阈值点时，相对于在顶部/底部表面上的膜，可通过湿蚀刻更主要地去除在侧壁上的膜，而当将等离子体密度设置为高于阈值点时，相对于在侧壁上的膜，可通过湿蚀刻更主要地去除顶部/底部表面上的膜。因此，可制备所需的层结构。
在图14中，根据施加电压的持续时间、频率、压力、电极间的距离、温度等改变相交点(阈值点)，其中，一般地，施加电压的时间越长，且压力越低，则交点处的等离子体密度变得越低。应注意，当压力、RF功率、电压等恒定时，可在湿蚀刻速率与在平行电极之间的RF功率之间得到基本与图14相似的关系。可根据本发明和常规实验在步骤(i)和(ii)之前确定阈值点。因此，在一些实施方式中，制备层结构的方法还包括，在步骤(i)和(ii)之前，重复以下步骤以确定阈值点(参考点)：(a)在与步骤(i)相同的条件下同时形成介电膜，不同之处在于改变电压作为可变量；以及(b)在与步骤(ii)相同的条件下，通过湿蚀刻基本去除介电膜的顶部/底部部分和侧壁部分中的一个但不同时去除两个。
图3是流程图，说明了制备根据本发明的一个实施方式的层结构的步骤。步骤S11对应于步骤(a)和(b)，步骤S12和S13分别对应于步骤(i)和(ii)。在步骤S11中，确定用于反转顶部/底部部分和侧壁部分的膜性质的等离子体轰击的阈值电压。在步骤12中，通过使用在参考确定的阈值电压调节的电压下的等离子体轰击，在沟槽上形成具有膜性质的方向性的介电膜。例如，当在步骤S12中在电极之间施加高于阈值电压的电压时，所述膜的顶部/底部部分的湿蚀刻速率变得比所述膜的侧壁部分的湿蚀刻速率高，使得在步骤S13中通过湿蚀刻主要去除了所述膜的顶部/底部部分而不是所述膜的侧壁部分。另一方面，当在步骤S12中在电极之间施加低于阈值电压的电压时，所述膜的侧壁部分的湿蚀刻速率变得比所述膜的顶部/底部部分的湿蚀刻速率高，使得在步骤S13中通过湿蚀刻主要去除了所述膜的侧壁部分而不是所述膜的顶部/底部部分。
当离子轰击在膜上发挥作用而不使用平行电极构造时，例如通过使用在低压化学气相沉积(LPCVD)中的反应物，不会得到阈值点(例如如图14所显示的)，因为LPCVD中的反应物不会形成不对称的离子轰击，即不会形成膜性质的方向性。例如，美国专利申请公开第2003/0029839号公开了LPCVD，其中注入含氮离子例如N2 +以形成富氮层，随后通过热退火以促进层中的Si-N和N-H键从而降低所述层的湿蚀刻速率。相反，在本发明的一些实施方式中，使用氮的不对称等离子体轰击在顶部/底部层上发挥作用，在所述层中并不富含氮，但打断了Si-N键并降低了所述层的密度，从而相对于在沟槽的侧壁上形成的层的湿蚀刻速率，增加了在顶部/底部表面上形成的层的蚀刻速率。在上文中，当Si-N键断裂时，形成Si悬空键和N悬空键，它们最终被氢封端，形成N-H键和Si-H键。作为Si-N键断裂的结果，所述层的密度降低，且湿蚀刻速率增加。因此，在一些实施方式中，在步骤(i)和(ii)之间不进行热退火(例如在900℃)从而避免顶部/底部层的致密化(即避免降低顶部/底部层的湿蚀刻速率)。此外，在一些实施方式中，离子的入射能小于约200eV(等离子体电位约100-200V)，这比美国专利申请公开第2003/0029839号中公开的(0.5-20keV)低。对于LPCVD中的反应物，热原子层沉积(ALD)中的反应物和远程等离子体沉积的等离子体不能形成如图14所示的阈值点，这是因为热ALD和远程等离子体沉积的等离子体同样不能形成不对称的离子轰击，即不能形成膜性质的方向性。此外，当使用一种等离子体，例如具有入射离子的低离子动能和低电子温度的表面波等离子体(SWP)时，离子轰击的作用非常有限，因此不发生膜降级，并且因此很难形成膜性质的方向性。另外，即使当等离子体轰击在由氧化硅构成的膜上发挥作用时，氧化硅膜的膜质量不降级，并因此难以形成膜性质的方向性。
在一些实施方式中，等离子体是通过对两个电极中的一个施加RF功率而激发的电容耦合等离子体(CCP)。此外，在一些实施方式中，电感偶合等离子体(ICP)、电子回旋共振(ECR)等离子体、微波表面波等离子体、螺旋波等离子体等可用作等离子体，其中根据需要对电极施加偏压以增加等离子体与电极之间的dc偏压。
在一些实施方式中，RF功率比所述介电膜的顶部/底部部分和所述介电膜的侧壁部分的耐化学性基本相当时的参考RF功率高，其中相对于所述介电膜的侧壁部分，所述湿蚀刻选择性地去除了所述介电膜的顶部/底部部分。
在一些实施方式中，等离子体是Ar、N2和/或O2或具有比氢或氦高的原子数的其它原子的等离子体。
在一些实施方式中，沟槽的宽度为10-50nm(通常为15-30nm)(其中当沟槽的长度基本与宽度相等时，其被认为是孔/通孔(via)，直径为10-50nm)，深度为30-200nm(通常为50-150nm)，纵横比为3-20(通常为3-10)。
在一些实施方式中，介电膜可用作蚀刻终止物、低-k间隔物或间隙填充物。例如，当只留下侧壁部分时，所述部分可用作用于间隔物限定的双重图案化(SDDP)的间隔物，或者当只留下顶部/底部部分时，所述部分可用作专门用于侧壁层的固态掺杂(SSD)的掩模。
在一些实施方式中，步骤(i)包括：(ia)将在其上表面中具有沟槽的基材放置在电极之间；和(ib)通过使用氮气作为反应气体的等离子体增强原子层沉积(PEALD)在所述基材上沉积介电膜，其中所述等离子体是在PEALD的每个循环中通过对两个电极中的一个施加RF功率激发的电容耦合等离子体(CCP)，其中所述RF功率比所述介电膜的顶部/底部部分和所述介电膜的侧壁部分的耐化学性基本相当时的参考RF功率高，从而相对于所述介电膜的侧壁部分，在步骤(ii)中湿蚀刻选择性地去除了所述介电膜的顶部/底部部分。在上文中，具有膜性质的方向性的膜在沉积膜时形成，而不是在膜沉积完成之后形成。
图4是流程图，说明了制备根据本发明的另一个实施方式的层结构的步骤。步骤S21对应于步骤(ib)，步骤S22对应于步骤(ii)。在步骤S21中，通过使用在比阈值电压高的电压下的等离子体轰击将具有膜性质的方向性的介电膜沉积在沟槽上，在步骤S22中，相对于膜的侧壁部分，更主要地去除膜的顶部/底部部分，从而在层结构中仅留有侧壁部分。
在一些实施方式中，步骤(i)包括：(ia)将在其上表面中具有沟槽的基材放置在电极之间；和(ic)通过使用氮气作为反应气体的等离子体增强原子层沉积(PEALD)在所述基材上沉积介电膜，其中所述等离子体是在PEALD的每个循环中通过对两个电极中的一个施加RF功率激发的电容耦合等离子体(CCP)，其中所述RF功率比所述介电膜的顶部/底部部分和所述介电膜的侧壁部分的耐化学性基本相当时的参考RF功率低，从而相对于所述介电膜的顶部/底部部分，在步骤(ii)中湿蚀刻选择性地去除了所述介电膜的侧壁部分。在上文中，具有膜性质的方向性的膜在沉积膜时形成，而不是在膜沉积完成之后形成。
图5是流程图，说明了制备根据本发明的另一个实施方式的层结构的步骤。步骤S31对应于步骤(ic)，步骤S32对应于步骤(ii)。在步骤S31中，通过使用在比阈值电压低的电压下的等离子体轰击将具有膜性质的方向性的介电膜沉积在沟槽上，在步骤S32中，相对于膜的顶部/底部部分，更主要地去除膜的侧壁部分，从而在层结构中仅留有顶部/底部部分。
在一些实施方式中，介电膜是SiN膜或SiON膜或其它含有Si-N键的膜。
在一些实施方式中，PEALD或其它沉积方法使用一种或多种选自下组的化合物作为前体：氨基硅烷、卤化硅烷、甲硅烷或乙硅烷。氨基硅烷和卤化硅烷包括但不限于Si2Cl6、SiCl2H2、SiI2H2、双二乙基氨基硅烷、双二甲基氨基硅烷、六乙基氨基硅烷、四乙基氨基硅烷、叔丁基氨基硅烷、双叔丁基氨基硅烷、三甲基甲硅烷基二乙胺、三甲基甲硅烷基二乙胺和双二甲基氨基二甲基硅烷。
在一些实施方式中，步骤(i)包括：(iA)在其上表面具有沟槽的基材上沉积介电膜；(iB)将所述基材放置在两个电极之间；和(iC)在电极之间激发等离子体以处理沉积的介电膜的表面而不沉积膜，其中所述等离子体是通过对两个电极中的一个施加RF功率激发的电容耦合等离子体(CCP)，其中所述RF功率比所述介电膜的顶部/底部部分和所述介电膜的侧壁部分的耐化学性基本相当时的参考RF功率高，从而相对于所述介电膜的侧壁部分，在步骤(ii)中湿蚀刻选择性地去除了所述介电膜的顶部/底部部分。在上文中，通过处理所述膜，在膜沉积完成后形成具有膜性质的方向性的膜。在上文中，步骤(ii)是沉积后处理，其不需要循环。
图6是流程图，说明了制备根据本发明的不同实施方式的层结构的步骤。步骤S41对应于步骤(iA)，步骤S42对应于步骤(iB)和(iC)，步骤S43对应于步骤(ii)。在步骤S41中，将介电膜沉积在沟槽上，所述膜不需要具有膜性质的方向性，但所述膜可以是已经具有膜性质的方向性。在步骤S42中，作为沉积后处理的等离子体轰击在高于阈值电压的电压下在膜上发挥作用，从而所述膜的顶部/底部部分的湿蚀刻速率比所述膜的侧壁部分的湿蚀刻速率高。在步骤S43中，通过湿蚀刻所述膜的顶部/底部部分比所述膜的侧壁部分被更主要地去除，从而基本只有所述膜的侧壁部分留在层结构中。如上文讨论的在图14中说明的，由于在沉积后处理之前已经沉积了膜，比阈值电压低的电压的使用可能不起作用，因为侧壁部分的湿蚀刻速率没有变得比通过在膜上进行等离子体轰击沉积的膜的湿蚀刻速率高。
在一些实施方式中，沉积的介电膜的厚度约为10nm或更小(通常约为5nm或更小)。如果将膜处理成比约10nm厚，等离子体轰击不能到达膜的底部，即难以在厚度方向上完全调节膜的湿蚀刻速率。
可通过任何合适的沉积方法，包括等离子体增强原子层沉积(PEALD)、热ALD、低压化学气相沉积(PCVD)、远程等离子体沉积、PECVD等在基材上沉积经过沉积后处理的介电膜。优选地，由于ALD可提供高共形性，例如大于约70％(或大于80％或90％)，因此通过ALD沉积介电膜。
在一些实施方式中，在沉积介电膜之后和在步骤(ii)之前不进行退火。
在一些实施方式中，沉积循环可通过PEALD进行，其一个循环在下述表1所示的条件下进行。
表1(数字是近似值的)
在一些实施方式中，可在如下表2中所示的条件下进行沉积后处理。
表2(数字是近似值的)
在上文中，虽然在反应腔室中没有输入前体，但载气持续流动。
在一些实施方式中，可在如下表3中所示的条件下进行湿蚀刻。
表3(数字是近似值的)
对于湿蚀刻，可以使用包括任何常规装置的任何合适的单晶片型或间歇型装置。同样，可使用包括任何常规溶液的任何合适的用于湿蚀刻的溶液。
在一些实施方式中，如下所述，可仅在沟槽的一个侧壁上形成绝缘膜：
1)在具有沟槽图案的基材上形成SiN膜，其中输送前体的脉冲和将基材暴露于含有由等离子体激发的氮物质的环境气氛中的脉冲重复进行，其中在膜的侧壁部分的湿蚀刻速率低于膜的顶部/底部部分的湿蚀刻速率的条件下，以使等离子体轰击在基材上沿垂直于基材的方向(离子的入射角垂直于基材)发挥作用的方式激发等离子体；以及
2)通过湿蚀刻去除膜的顶部/底部部分。
在上述过程顺序中，使用持续供应的载气在脉冲中供应前体。这可通过使用流动-通过系统(FPS)来完成，其中，用含有具有前体储器(瓶)的迂回管线提供载气管线，主管线和迂回管线可进行切换，其中，当希望只将载气输送至反应腔室时，关闭迂回管线，而当有意将载气和前体气体都输送至反应腔室时，关闭主管线，载气流动通过迂回管线并且与前体气体一起从瓶中流出。以这种方式，载气可持续流入反应腔室中，并可通过切换主管线和迂回管线使载气以脉冲方式携带前体气体。图1B说明了根据本发明的一个实施方式的使用流动-通过系统(FPS)的前体供应系统(黑色阀说明该阀是关闭的)。如在图1B中的(a)中所示的，当向反应腔室(未显示)中输送前体时，首先，载体气体，例如Ar(或He)流过具有阀b和c的气体管线，随后进入瓶(储器)30。载气从瓶30流出的同时携带了与在瓶30内部蒸气压相对应的量的前体气体，并且流过具有阀f和e的气体管线，随后与前体一起被输送至反应腔室中。上文中，阀a和d是关闭的。当向反应腔室中仅输送载气(惰性气体)时，如图1B中的(b)所示，所述载气流过具有阀a的气体管线，同时绕过瓶30。在上述情况中，阀b、c、d、e和f是关闭的。
可在载气的协助下提供前体。由于ALD是自限制的吸附反应过程，沉积的前体分子的数量由反应性表面位点的数量决定，且不受饱和后的前体暴露的影响，并且前体的供应使得反应性表面位点在每个循环中都是饱和的。用于沉积的等离子体可原位形成，例如，在整个沉积循环中持续流过的氨气中形成。在另一些实施方式中，等离子体可远程形成并被提供至反应腔室中。
如上所述，每个沉积循环中的各脉冲或阶段优选都是自限制的。在各阶段中供给过量的反应物以使易受影响的结构表面饱和。表面的饱和确保了反应物占据所有可用的反应性位点(受制于例如物理尺寸或“空间位阻”的限制)，从而确保优异的阶差覆盖。在一些实施方式中，可减少一种或多种反应物的脉冲时间，从而不实现完全饱和，并且吸附至基材表面上的物质不足以形成单层。
处理循环可使用任何合适的设备进行，包括例如图1A中所示的设备。图1A是PEALD设备的示意图，理想的是与程序化的控制相连以进行下述顺序，用于本发明的一些实施方式中。在该图中，通过提供一对平行放置且在反应腔室3的内腔11(反应区域)中相对的导电平板电极4、2，并且对一侧施加HRF功率(13.56MHz或27MHz)20并将另一侧12电接地，在电极之间激发等离子体。在较低平台2(下电极)提供温度调节器，将设置于其上的基材1的温度以给定的温度保持恒定。上电极4也用作喷淋板，分别通过气体管线21和气体管线22并通过喷淋板4将反应气体(和稀有气体)和前体气体引入反应腔室3中。另外，在反应腔室3中，提供具有排气管线7的环状输送管13，反应腔室3的内腔11中的气体通过环状输送管13排出。此外，通过气体管线23将稀释气体引入到反应腔室3中。此外，设置在反应腔室3下方的转移腔室5具有密封气体管线24以通过转移腔室5的内腔16(转移区域)将密封气体引入到反应腔室3的内腔11中，其中，提供用于分隔反应区域和转移区域的分隔板14(该图中省略了闸门阀，通过该闸门阀可将晶片转入或转出转移腔室5)。转移腔室还具有排气管线6。在一些实施方式中，多元素膜的沉积和表面处理在同一反应空间内进行，从而所有步骤可持续进行而不需要将基材暴露于空气或其它含氧气氛中。在一些实施方式中，远程等离子体单元可用于激发气体。
在一些实施方式中，在图1A中所示的设备中，图1B中显示的惰性气体流和前体气体流的开关系统(之前描述过)可用于将前体气体引入脉冲中而不使反应腔室的压力显著波动。
在一些实施方式中，可使用双腔室反应器(相互之间紧密设置的用于处理晶片的两个部分或隔室)，其中反应气体和稀有气体可通过共用的管线供应，而前体气体通过非共用的管线供应。
本领域技术人员应理解，所述设备包括一个或多个程序化或者以其他方式设置成能进行本文其它部分所述的沉积和反应器清洁处理的控制器(未显示)。本领域技术人员应理解，所述控制器与各种动力源、加热系统、泵、机器人和气流控制器或反应器的阀连接。
参考以下工作实施例对本发明做进一步解释。然而，这些实施例并非旨在限制本发明。在实施例中，当没有说明条件和/或结构时，本领域技术人员可从本发明的角度出发，按常规实验容易地提供所述条件和/或结构。而且，在一些实施方式中，具体实施例中所用的数字可在至少±50％的范围内修改，并且所述数字是近似值。
在一些实施方式中，如下所述，可仅在沟槽的一个侧壁上形成绝缘膜：
1)在具有沟槽图案的基材上形成SiN膜(所述膜可具有或不具有膜性质的方向性)；
2)在膜的侧壁部分的湿蚀刻速率比膜的顶部/底部部分的湿蚀刻速率低的条件下，用以使等离子体轰击在基材上沿垂直于基材的方向(离子的入射角垂直于基材)发挥作用的方式激发的等离子体来处理所述膜；以及
3)通过湿蚀刻去除膜的顶部/底部部分。
实施例
实施例1
通过PEALD在具有沟槽的Si基材(Ф300mm)上形成的SiN膜，在如下表4所示的条件下使用图1A中说明的PEALD装置和图1B中说明的气体供给系统(FPS)进行PEALD的一个循环(沉积循环)。
基材从反应腔室中取出之后，在下表4所示的条件下使所述基材经过湿蚀刻。
表4(数字是近似值的)
在图7中显示结果。图7的图显示了RF功率与在沟槽的顶表面上形成的膜和在沟槽的侧壁上形成的膜的湿蚀刻速率之间的关系，显示了阈值(参考)RF功率。如图7所示，侧壁部分的湿蚀刻速率随着RF功率的增加而降低，而顶部/底部部分的湿蚀刻速率随着RF功率增加而增加，其中表示前者的线和表示后者的线在RF功率约为600W处交叉。也即是，阈值RF功率约为600W，应理解，当在电极之间施加的RF功率高于约600W时，相对于膜的侧壁部分可选择性地去除膜的顶部/底部部分，而当在电极之间施加的RF功率低于约600W时，相对于膜的顶部/底部部分可选择性去除膜的侧壁部分。
此外，在湿蚀刻之前，将膜的顶部部分经过额外的分析：Si-N峰强度和密度。图12的图显示了RF功率与SiN膜的Si-N峰强度[au]之间的关系。图13的图显示了RF功率与SiN膜的密度[g/cm3]之间的关系。如从图12和13中所看到的，与常规技术知识(即当增加RF功率时，发生膜的致密化)相反，当RF功率增加时，对于SiN膜的不对称的等离子体轰击打断了Si-N键，作为Si-N键断裂的结果，膜的密度降低(密度通常为2.6-3.2g/cm3)，其中要通过湿蚀刻去除的膜部分的密度比湿蚀刻中仍保留的膜部分的密度低。
实施例2
在如表5所示的条件下沉积SiN膜，其中以与实施例1中相同的方式测得阈值RF功率为大约400W。随后在表5所示的条件下使所述SiN膜经过湿蚀刻。图8显示氮化硅膜截面图的扫描透射电子显微镜(STEM)照片。如从图8所见，当RF功率为700W时，通过湿蚀刻选择性地去除膜的顶部/底部部分，并且在沟槽的顶表面上和底部基本没有保留膜(没有观察到剩余膜)。当RF功率为500W时，相对于膜的侧壁部分，通过湿蚀刻更主要地去除膜的顶部/底部部分，但在沟槽的顶表面和底部保留了剩余膜，而膜的侧壁部分绝大多数被保留。当RF功率为300W时，相对于膜的顶部/底部部分，通过湿蚀刻更主要地去除膜的侧壁部分，并且在侧壁的一些区域没有保留剩余膜，而膜的顶部/底部部分绝大多数被保留。
表5(数字是近似值的)
实施例3
以与实施例1相同的方式沉积SiN膜，不同之处在于RF功率为880W。随后在与实施例1相同的条件下使所述SiN膜经过湿蚀刻。图9显示了湿蚀刻后SiN膜的截面图的扫描透射电子显微镜(STEM)照片。如在图9中可见，在沟槽的顶表面和底部基本没有膜保留(没有观察到剩余膜)。
实施例4(预测实施例)
以与实施例1相同的方式通过PEALD在具有沟槽的Si基材(Ф300mm)上形成SiN膜，不同之处在于RF功率为600W。随后，在同一反应器中，在下表6所示的条件下用等离子体处理所述膜，其中RF功率是800W，这比阈值RF功率高，从而引起了基材的顶表面和沟槽的底表面的破坏并使膜的质量降级。基材从反应腔室中取出之后，在下表6所示的条件下使所述基材经过湿蚀刻。
表6(数字是近似值的)
图10说明了氮化硅膜的截面图。由于在基材51中形成的沟槽的侧壁51上形成的膜的部分52没有受到显著的等离子体轰击，因此部分52保持了膜性质并在湿蚀刻后保留。相反，由于在顶表面51b上形成的膜的部分和在底表面51a上形成的膜的部分受到等离子体轰击，所述部分降低了膜性质的等级并在湿蚀刻后被去除。
实施例5(预测实施例)
通过PEALD在具有沟槽的Si基材(Ф300mm)上形成SiN膜，在如下表7所示的条件下使用图1A中说明的PEALD装置和图1B中说明的气体供给系统(FPS)进行PEALD的一个循环(沉积循环)。
基材从反应腔室中取出之后，在下表7所示的条件下使所述基材经过湿蚀刻。
表7(数字是近似值的)
图11说明了氮化硅膜的截面图。由于RF功率是100W，这比阈值RF功率(预期为600W)低，因此相对于膜的顶部部分53b和底部部分53a，通过湿蚀刻选择性地去除膜的侧壁部分，其中在湿蚀刻之后只有顶部/底部部分53a、53b保留。所述膜可用作盖层。
本领域技术人员应理解，可进行大量和各种改进而不背离本发明的精神。因此，应清楚地理解，本发明的形式仅用于说明而不是为了限制本发明的范围。

Claims (16)

1.一种用于在基材中形成的沟槽中制备由含有Si-N键的介电膜组成的层结构的方法，所述方法包括：
(i)同时在沟槽的上表面和底表面以及侧壁上形成含有Si-N键的介电膜，其中在沉积介电膜的过程中，通过由在两个电极之间反应空间中施加电压激发的等离子体的轰击而使在上表面和底表面上形成的介电膜的顶部/底部部分和在侧壁上形成的介电膜的侧壁部分具有不同的耐化学性，在所述两个电极之间将基材平行于两个电极放置；并且
(ii)通过湿蚀刻基本去除所述介电膜的顶部/底部部分和侧壁部分中的任一个但不同时去除两个，所述湿蚀刻根据不同的耐化学性，相对于所述介电膜的顶部/底部部分和侧壁部分中的一个，更主要地去除所述介电膜的顶部/底部部分和侧壁部分中的另一个；
其中步骤(i)中所述等离子体是通过对两个电极中的一个施加RF功率而激发的电容耦合等离子体(CCP)，施加RF功率使得由此产生的等离子体密度比所述介电膜的顶部/底部部分和所述介电膜的侧壁部分的耐化学性基本相当时的参考等离子体密度高，其中相对于所述介电膜的侧壁部分，步骤(ii)所述湿蚀刻选择性地去除了所述介电膜的顶部/底部部分。
2.如权利要求1所述的方法，其中，步骤(i)中，所述的介电膜通过等离子体增强原子层沉积(PEALD)形成。
3.如权利要求1所述的方法，其中所述等离子体是Ar、N2或O2的等离子体。
4.如权利要求1所述的方法，其中，所述介电膜是SiN膜。
5.如权利要求4所述的方法，其中，步骤(i)中，卤化硅烷用作前体。
6.如权利要求1所述的方法，其中，所述的湿蚀刻是使用氟化氢(HF)溶液进行的。
7.如权利要求1所述的方法，其中，所述等离子体密度通过调节反应空间中的压力进行调节，所述的等离子体密度随压力的降低而增加。
8.如权利要求7所述的方法，其中，还包括，在步骤(i)和(ii)之前，重复以下步骤以确定参考等离子体密度：
在与步骤(i)相同的条件下同时形成介电膜，不同之处在于改变压力作为可变量；并且
在与步骤(ii)相同的条件下，通过湿蚀刻基本去除所述介电膜的顶部/底部部分和侧壁部分中的一个但不同时去除两个。
9.如权利要求2所述的方法，其中在步骤(i)中，前体包含氨基硅烷、卤化硅烷、甲硅烷或乙硅烷。
10.如权利要求1所述的方法，其中在步骤(i)中，所述的介电膜通过原子层沉积(ALD)形成。
11.如权利要求1所述的方法，其中，所沉积的介电膜的厚度为10nm或更薄。
12.如权利要求1所述的方法，其中，步骤(i)完全在同一腔室中进行。
13.如权利要求1所述的方法，其中，所述等离子体是氮等离子体。
14.如权利要求1所述的方法，其中，在沉积所述介电膜之后和步骤(ii)之前不进行退火。
15.如权利要求1所述的方法，其中在步骤(i)和(ii)之间不进行退火。
16.一种用于在基材的上表面中形成的沟槽中制备由含有Si-N键的介电膜组成的层结构的方法，所述方法包括：
(i)同时在沟槽的上表面和底表面以及侧壁上形成含有Si-N键的介电膜，其中在沉积介电膜的过程中，通过由在两个电极之间施加电压激发的等离子体的轰击而使在上表面和底表面上形成的介电膜的顶部/底部部分和在侧壁上形成的介电膜的侧壁部分具有不同的耐化学性，在所述两个电极之间将基材平行于两个电极放置；并且
(ii)通过湿蚀刻基本去除所述介电膜的顶部/底部部分和侧壁部分中的任一个但不同时去除两个，所述湿蚀刻根据不同的耐化学性，相对于所述介电膜的顶部/底部部分和侧壁部分中的一个，更主要地去除所述介电膜的顶部/底部部分和侧壁部分中的另一个；
其中步骤(i)中所述等离子体是通过对两个电极中的一个施加RF功率而激发的电容耦合等离子体(CCP)，RF功率被施加使得由此产生的等离子体密度比所述介电膜的顶部/底部部分和所述介电膜的侧壁部分的耐化学性基本相当时的参考等离子体密度低，其中相对于所述介电膜的顶部/底部部分，步骤(ii)所述湿蚀刻选择性地去除了所述介电膜的侧壁部分。
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