CN111684105A - 通过循环沉积工艺在衬底上形成含过渡金属的膜的方法、向反应腔室供给过渡金属卤化物化合物的方法以及相关的气相沉积装置 - Google Patents

通过循环沉积工艺在衬底上形成含过渡金属的膜的方法、向反应腔室供给过渡金属卤化物化合物的方法以及相关的气相沉积装置 Download PDF

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CN111684105A
CN111684105A CN201980011788.7A CN201980011788A CN111684105A CN 111684105 A CN111684105 A CN 111684105A CN 201980011788 A CN201980011788 A CN 201980011788A CN 111684105 A CN111684105 A CN 111684105A
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transition metal
precursor
substrate
halide compound
metal halide
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T.哈坦帕
K.韦尔南
M.里塔拉
M.莱斯克拉
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Abstract

公开了一种通过循环沉积工艺在衬底上形成含过渡金属的膜的方法。所述方法可包括：使衬底与第一气相反应物接触，所述第一气相反应物包含过渡金属卤化物化合物，所述过渡金属卤化物化合物包含二齿含氮加合物配体；以及使衬底与第二气相反应物接触。公开了一种向反应腔室供给包含二齿含氮配体的过渡金属卤化物化合物的方法及相关的气相沉积装置。

Description

通过循环沉积工艺在衬底上形成含过渡金属的膜的方法、向 反应腔室供给过渡金属卤化物化合物的方法以及相关的气相 沉积装置
相关专利申请的交叉引用
本公开要求2018年2月15日提交的标题为“A METHOD OF FORMING A TRANSITIONMETAL CONTAINING FILM ON A SUBSTRATE BY A CYCLICAL DEPOSITION PROCESS,AMETHOD FOR SUPPLYING A TRANSITION METAL HALIDE COMPOUND TO A REACTIONCHAMBER,AND RELATED VAPOR DEPOSITION APPARATUS”的美国专利申请号15/897,578的权益，该专利申请以引用的方式并入本文。
联合研究协议的合作对象
本文要求保护的发明是根据或代表和/或结合赫尔辛基大学(University ofHelsinki)与ASM微量化学公司(ASM Microchemistry Oy.)之间的联合研究协议进行的。所述协议在作出所要求保护的本发明的日期当天和之前有效，并且所要求保护的本发明是作为在所述协议的范围内进行的活动的结果而作出。
技术领域
本公开总的涉及通过循环沉积工艺在衬底上形成含过渡金属的膜的方法以及形成含钴、铜和镍的膜的特定方法。本公开还总的涉及向气相沉积工具和相关的气相沉积装置供给过渡金属卤化物化合物的方法。
背景技术
在先进的技术节点中，半导体器件制造工艺通常需要最先进的沉积方法来形成含过渡金属的膜，例如元素过渡金属、过渡金属氧化物、过渡金属氮化物、过渡金属硅化物、过渡金属磷化物、过渡金属硒化物或过渡金属硼化物。
沉积含过渡金属的膜的一个常见要件是沉积过程要非常保形。例如，常需要保形沉积以在包括高纵横比特征的三维结构上方均匀地沉积含过渡金属的膜。沉积含过渡金属的膜的另一常见要求是沉积工艺能够在大的衬底区域上方沉积连续的超薄膜。在其中含过渡金属的膜是导电的这一特定情况下，可能需要优化沉积工艺以产生低电阻膜。
循环沉积工艺，例如原子层沉积(ALD)和循环化学气相沉积(CCVD)，向反应腔室中依序引入一种或多种前体(反应物)，在这里，这些前体以依序、自限性的方式一次一种在衬底的表面上反应。已经证实循环沉积工艺产生具有优异保形性的含金属膜，具有原子级厚度控制。
可利用循环沉积工艺来沉积含过渡金属的膜，例如含铜膜、含镍膜、特别是含钴膜。然而，适合于含过渡金属的膜、特别是含钴膜的循环沉积的化学前体是不常见的且成本高昂。例如，用于含钴膜的循环沉积的现有化学前体可能需要不期望的高温沉积工艺和/或使用等离子体增强沉积工艺。另外，由于沉积工艺对下面的衬底的材料的敏感性，故使用现有的钴化学前体的循环沉积工艺可能不合需要。相应地，需要用于形成含过渡金属的膜、特别是含钴、铜和镍的膜的循环沉积方法、适用于循环沉积工艺中的化学前体和相关的气相沉积装置。
发明内容
提供此概述是为了以简化的形式引入一系列概念。下文在本公开的实例实施例的详细描述中更详细地描述这些概念。本概述并非旨在标识所要求保护的主题的关键特征或必要特征，也并非旨在用于限制所要求保护的主题的范围。
在本公开的一些实施例中，提供了通过循环沉积工艺在衬底上形成含金属的膜的方法。所述方法可包括：使衬底与第一气相反应物接触，所述第一气相反应物包含过渡金属卤化物化合物，所述过渡金属卤化物化合物包含二齿含氮加合物配体；和使衬底与第二气相反应物接触。
在本公开的一些实施例中，提供了通过循环沉积工艺在衬底上形成含金属的膜的另外的方法。所述方法可包括：使衬底与第一气相反应物接触，所述第一气相反应物包含过渡金属化合物，所述过渡金属化合物包含加合物形成配体；和使衬底与第二气相反应物接触；其中所述过渡金属选自铜(Cu)、镍(Ni)和钴(Co)。
在本公开的一些实施例中，提供了向反应腔室供给过渡金属卤化物化合物的方法，其中所述过渡金属卤化物化合物包含二齿含氮加合物配体。所述方法可包括：提供配置为用于容纳过渡金属卤化物化合物的前体源容器，将前体源容器流体连接到反应腔室；将前体源容器中容纳的过渡金属卤化物化合物加热到高于150℃的温度；产生至少0.001毫巴的过渡金属卤化物化合物蒸气压；和向反应腔室供给过渡金属卤化物化合物。
在本公开的一些实施例中，提供了利用反应性挥发性化学品的气相沉积装置。所述装置可包含：反应腔室；设置在反应腔室中的衬底；与反应腔室流体连通的前体源容器；和设置在前体源容器中的过渡金属卤化物化合物，所述过渡金属卤化物化合物包含二齿含氮加合物配体。
出于概述本发明和所实现的优于现有技术的优势的目的，在本文上述内容中描述了本发明的某些目标和优势。当然，应理解，未必所有此类目标或优势都可根据本发明的任一特定实施例实现。因此，举例来说，所属领域的技术人员将认识到，本发明可按实现或优化本文中教示或表明的一个优势或一组优势的方式体现或实行，而未必实现本文中可能教示或表明的其它目标或优势。
所有这些实施例均意在包括在所公开的本发明的范围内。对于所属领域的技术人员来说，这些和其它实施例将根据参考附图的某些实施例的以下详细描述而变得显而易见，本发明不限于所公开的任何特定实施例。
附图说明
虽然本说明书以具体地指出并明确地要求保护被视为本发明实施例的内容的权利要求书结束，但在结合附图阅读时，可以根据本公开的实施例的某些实例的描述更容易地确定本公开的实施例的优势，在附图中：
图1示意了根据本公开的实施例的一种示例性循环沉积方法的工艺流程；
图2示意了包含根据本公开的实施例沉积的含过渡金属的膜的示例性器件结构的示意图；
图3示意了在本公开的循环沉积工艺中利用的过渡金属卤化物化合物的实例；
图4示意了根据本公开的实施例的一种示例性气相沉积装置的示意图。
具体实施方式
尽管下文公开了某些实施例和实例，但所属领域的技术人员将理解，本发明延伸超出了本发明具体公开的实施例和/或用途以及显而易见的修改和其等效物。因此，希望本发明所公开的范围不应受下文所描述特定公开实施例的限制。
本文中呈现的图解不打算作为任何特定材料、结构或装置的实际视图，而仅仅是用以描述本公开的实施例的理想化图示。
如本文所用，术语“循环沉积”可指向反应腔室中依序引入前体(反应物)以在衬底上方沉积膜并包括沉积技术如原子层沉积和循环化学气相沉积。
如本文所用，术语“循环化学气相沉积”可指其中衬底被依序暴露于两种或更多种挥发性前体的任何工艺，所述挥发性前体在衬底上反应和/或分解以产生所希望的沉积。
如本文所用，术语“衬底”可指可使用的或上面可形成器件、电路或膜的任何一种或多种下层材料。
如本文所用，术语“原子层沉积(ALD)”可指在工艺腔室中进行沉积循环、优选地多个连续沉积循环的气相沉积工艺。通常，在每个循环期间，将前体化学吸附到沉积表面(例如，衬底表面或先前沉积的下层表面，如来自前一ALD循环的材料)，由此形成不易与额外的前体反应的单层或亚单层(即，自限性反应)。其后，如果必要，可随后将反应物(例如，另一前体或反应气体)引入到工艺腔室中以用于将被化学吸附的前体转化为沉积表面上的所需材料。通常，此反应物能够与前体进一步反应。此外，还可在每个循环期间利用吹扫步骤来在被化学吸附的前体的转化之后从工艺腔室去除过量的前体和/或从工艺腔室去除过量的反应物和/或反应副产物。此外，当使用前体组合物、反应性气体和吹扫气体(例如，惰性载气)的交替脉冲进行时，如本文所用，术语“原子层沉积”还意在包括由相关术语如“化学气相原子层沉积”、“原子层外延”(ALE)、分子束外延(MBE)、气体源MBE或有机金属MBE和化学束外延所指定的工艺。
如本文所用，术语“膜”、“薄膜”、“层”和“薄层”可指通过本文公开的方法沉积的任何连续或非连续结构和材料。例如，“膜”、“薄膜”、“层”和“薄层”可包括2D材料、纳米棒、纳米管或纳米颗粒或甚至部分或完整分子层或者部分或完整原子层或者原子和/或分子的团簇。“膜”、“薄膜”、“层”和“薄层”可包含具有针孔的材料或层，但仍然是至少部分连续的。
如本文所用，术语“含过渡金属的膜”可指含有过渡金属物种的膜，包括但不限于元素过渡金属、过渡金属氧化物、过渡金属氮化物、过渡金属硅化物、过渡金属硒化物、过渡金属磷化物、过渡金属硼化物及其混合物。另外，术语“含过渡金属的膜”可指含有过渡金属物种以及含有碳和/或氢的膜。
在整个本公开的实施例中给出了大量的实例材料，应指出，针对每一实例材料给出的化学式不应理解为限制性的，并且给出的非限制性实例材料不应受限于所给实例化学计量。
本公开包括用于在衬底上形成含过渡金属的膜的方法和在衬底上循环沉积含过渡金属的膜的特定方法。本公开的实施例可包括含过渡金属的膜例如含铜膜、含镍膜、特别是含钴膜的循环沉积方法。
在本公开的特定实施例中，可利用循环沉积方法来沉积含钴膜，例如元素钴、钴氧化物、钴氮化物、钴硅化物、钴磷化物、钴硒化物或钴硼化物。在新兴的半导体器件制造工艺中，钴金属膜在应用如衬里层和覆盖层中可能是重要的以抑制铜互连材料向周围的介电材料中的电迁移。实际上，随着先进技术节点中器件特征尺寸的减小，可利用钴金属膜作为互连材料，替代常用的铜互连。钴金属膜也可能在巨磁阻应用和磁存储应用中引起人们的兴趣。另外，也可将钴薄膜沉积到集成电路中的硅栅接触件上以在退火时形成硅化钴。钴的氧化物可在新兴能源相关的技术中具有应用，例如锂离子电池和电化学水氧化，以及用作催化材料。
通常已利用溅射技术以及利用金属有机前体的CVD方法实现了元素钴和含钴膜的沉积。然而，由于其固有的不保形性，故用于沉积含钴膜的此类已知方法可能不适合于先进技术节点。循环沉积方法如原子层沉积是特征性地保形的沉积方法并高度适合于在包括高纵横比特征的三维结构上方沉积保形的含过渡金属的膜。因此，高度需要用于沉积含过渡金属的膜、特别是用于沉积含钴膜的循环沉积方法。
另外，由于缺乏合适的化学前体和成本有效的化学前体，故用于含钴膜的循环沉积方法的发展受到了阻碍。例如，利用已知的化学前体进行的含钴膜的循环沉积可能需要不期望的高温沉积工艺，例如高于300℃。可利用等离子体增强原子层沉积工艺来在较低沉积温度下沉积含钴膜，但由于高能等离子体反应性物种对下面的半导体器件结构的潜在损伤，故基于等离子体的工艺的利用在一些器件应用中可能是不期望的。因此，需要适合于通过循环沉积工艺沉积含过渡金属的膜的化学前体、特别是沉积含钴膜的化学前体。另外，需要用于向合适的气相沉积系统例如原子层沉积装置供给化学前体的方法和相关装置。
因此，本公开的一些实施例可包括通过循环沉积工艺在衬底上形成含过渡金属的膜的方法。所述方法可包括：使衬底与第一气相反应物接触，所述第一气相反应物包含过渡金属卤化物化合物，所述过渡金属卤化物化合物包含二齿含氮加合物配体；和使衬底与第二气相反应物接触。
在本公开的一些实施例中，可通过利用过渡金属卤化物化合物作为金属前体的循环沉积工艺来沉积含过渡金属的层(或膜)。循环沉积工艺的非限制性实例实施例可包括原子层沉积(ALD)，其中ALD基于通常自限性反应，由此使用反应物的依序和交替脉冲来在每一个沉积循环沉积材料的约一个原子(或分子)单层。通常选择沉积条件和前体以提供自饱和反应，使得一种反应物的吸附层留下不与同一反应物的气相反应物反应的表面终止状态(termination)。随后，使衬底与不同的反应物接触，所述不同的反应物与先前的终止状态反应而实现继续沉积。因此，交替脉冲的每个循环通常留下所要材料的不多于约一个单层。然而，如上文所提到，熟练技术人员应认识，在一个或多个ALD循环中可沉积材料的不止一个单层(例如如果发生了一些气相反应的话)而不管工艺的交替性如何。
在用于沉积含过渡金属的膜的ALD型工艺中，一个沉积循环可包括：使衬底与第一反应物接触，从反应空间去除任何未反应的第一反应物和反应副产物，和使衬底与第二反应物接触，然后是第二去除步骤。第一反应物可包含过渡金属卤化物化合物(“金属前体”)，第二反应物可包含氧前体、氮前体、硅前体、硫前体、硒前体、磷前体、硼前体或还原剂中的至少之一。
前体可通过惰性气体如氩气(Ar)或氮气(N2)分开，以防止反应物之间的气相反应并实现自饱和表面反应。然而，在一些实施例中，可移动衬底以分别接触第一气相反应物和第二气相反应物。由于反应自饱和，故可能不需要严格控制衬底的温度和精确控制前体的剂量。然而，衬底温度优选地使得附带的气体物种既不冷凝成单层，也不在表面上分解。在使衬底与下一反应性化学品接触之前，如通过吹扫反应空间或通过移动衬底，从衬底表面去除剩余的化学品和反应副产物(如果存在)。可以借助于惰性吹扫气体从反应空间中有效地排出不合期望的气态分子。可以使用真空泵来辅助吹扫。
可以使用能够用来沉积含过渡金属的膜的反应器来进行沉积。此类反应器包括ALD反应器以及配备有提供前体的适宜设备和措施的CVD反应器。根据一些实施例，可使用喷淋头反应器。根据一些实施例，可使用错流、批量、小批量或空间ALD反应器。
可使用的合适反应器的实例包括可商购获得的单衬底(或单晶片)沉积设备，如可得自美国亚利桑那州菲尼克斯的ASM America,Inc.和荷兰阿尔梅勒的ASM Europe B.V.的
Figure BDA0002618661280000071
反应器(如
Figure BDA0002618661280000072
2000和
Figure BDA0002618661280000073
3000及
Figure BDA0002618661280000074
XP ALD)以及
Figure BDA0002618661280000075
XP和
Figure BDA0002618661280000076
反应器。其它可商购的反应器包含来自ASM Japan K.K.(日本东京)，商品名为
Figure BDA0002618661280000077
XP和XP8的反应器。在一些实施例中，反应器为空间ALD反应器，在所述反应器中，衬底在加工过程中移动或旋转。
在本公开的一些实施例中，可使用批量反应器。合适的批量反应器包含但不限于可自ASM Europe B.V.(荷兰阿尔梅勒)商购获得的商品名为A400和A412 PLUS的
Figure BDA0002618661280000078
400系列反应器。在一些实施例中，晶片在加工过程中旋转。在其他实施例中，批量反应器包括配置为容纳10个或更少晶片、8个或更少晶片、6个或更少晶片、4个或更少晶片或者2个或更少晶片的小批量反应器。在使用批量反应器的一些实施例中，晶片间的不均匀性小于3％(1西格玛)、小于2％、小于1％或甚至小于0.5％。
本文描述的沉积工艺可任选地在连接到丛集工具的反应器或反应腔室中进行。在丛集工具中，因为每一个反应腔室专门用于一种工艺类型，故每个模块中反应腔室的温度可保持恒定，与其中在每次运行前加热衬底直至工艺温度的反应器相比，这将提高生产量。另外，在丛集工具中可以缩短将反应腔室压力变至衬底之间所需工艺压力水平的时间。在本公开的一些实施例中，可在包含多个反应腔室的丛集工具中进行沉积工艺，其中可利用每个单独的反应腔室来将衬底暴露于单独的前体气体并且衬底可在不同的反应腔室之间转移以暴露于多种前体气体，衬底的转移在受控的周围环境下进行以防止衬底的氧化/污染。在本公开的一些实施例中，沉积工艺可在包括多个反应腔室的丛集工具中进行，其中每个单独的反应腔室都可配置为将衬底加热到不同的沉积温度。
独立反应器可配备负载锁。在此情况下，不必在每次运行之间冷却反应空间。在一些实施例中，用于沉积含过渡金属的膜的沉积工艺可包括多个沉积循环，例如ALD循环或循环CVD循环。
在一些实施例中，使用循环沉积工艺来在衬底上形成含过渡金属的膜并且循环沉积工艺可以是ALD型工艺。在一些实施例中，循环沉积可以是混合式ALD/CVD或循环CVD工艺。举例来说，在一些实施例中，相比于CVD工艺，ALD工艺的生长速率可能较低。增大生长速率的一个方法可以是相比于通常在ALD工艺中所用的温度在更高的基材温度下操作，从而导致化学气相沉积工艺，但仍利用前体的依序引入，此类工艺可被称作循环CVD。
根据本公开的一些实施例，可使用ALD工艺来在衬底上沉积含过渡金属的膜，如部分制造的半导体器件结构。在本公开的一些实施例中，每一个ALD循环包括两个不同的沉积步骤或阶段。在沉积循环的第一阶段(“金属阶段”)中，使期望在其上沉积的衬底表面与包含化学吸附到衬底表面上的金属前体的第一气相反应物接触，从而在衬底的表面上形成反应物物种的不多于约一个单层。在沉积的第二阶段中，使期望在其上沉积的衬底表面与包含氧前体、氮前体、硅前体、硫前体、硒前体、磷前体、硼前体或还原剂中的至少之一的第二气相反应物接触，其中所述第二气相反应物可与衬底表面上的过渡金属物种反应而在衬底上形成含过渡金属的膜，例如元素过渡金属、过渡金属氧化物、过渡金属氮化物、过渡金属硅化物、过渡金属硒化物、过渡金属磷化物、过渡金属硼化物及其混合物，以及还包含碳和/或氢的含过渡金属的膜。
在本公开的一些实施例中，第一气相反应物可包含含金属的前体，这里也称“金属化合物”。在一些实施例中，第一气相反应物可包含具有加合物形成配体的过渡金属化合物。在一些实施例中，第一气相反应物可包含过渡金属化合物。在一些实施例中，第一气相反应物可包含过渡金属卤化物化合物。在一些实施例中，第一气相反应物可包含具有加合物形成配体的过渡金属化合物，如单齿、二齿或多齿加合物形成配体。在一些实施例中，第一气相反应物可包含具有加合物形成配体的过渡金属卤化物化合物，如单齿、二齿或多齿加合物形成配体。在一些实施例中，第一气相反应物可包含具有加合物形成配体的过渡金属化合物，如包含氮的单齿、二齿或多齿加合物形成配体。在一些实施例中，第一气相反应物可包含具有包含磷、氧或硫的加合物形成配体的过渡金属化合物，如包含磷、氧或硫的单齿、二齿或多齿加合物形成配体。例如，在一些实施例中，过渡金属卤化物化合物可包含过渡金属氯化物、过渡金属碘化物、过渡金属氟化物或过渡金属溴化物。在本公开的一些实施例中，过渡金属卤化物化合物可包含过渡金属物种，包括但不限于钴、镍或铜中的至少之一。在本公开的一些实施例中，过渡金属卤化物化合物可包含氯化钴、氯化镍或氯化铜中的至少之一。在一些实施例中，过渡金属卤化物化合物可包含二齿含氮加合物形成配体。在一些实施例中，过渡金属卤化物化合物可包含包括两个氮原子的加合物形成配体，其中所述氮原子中的每一个键合到至少一个碳原子。在本公开的一些实施例中，过渡金属卤化物化合物包含键合到中心过渡金属原子的一个或多个氮原子，由此形成金属络合物。
在本公开的一些实施例中，第一气相反应物可包含具有式(I)的过渡金属化合物：
(加合物)n-M-Xa (I)
其中所述“加合物”中的每一个为加合物形成配体并可独立地选择为单齿、二齿或多齿加合物形成配体或其混合物：在单齿形成配体的情况下，n为1至4，在二齿或多齿加合物形成配体的情况下，n为1至2；M为过渡金属，例如钴(Co)、铜(Cu)或镍(Ni)；其中Xa中的每一个为另一配体，并可独立地选择为卤化物或其他配体；其中a为1至4，在一些情况下a为2。
在本公开的一些实施例中，过渡金属化合物如过渡金属卤化物化合物中的加合物形成配体可包含单齿、二齿或多齿加合物形成配体，其通过氮原子、磷原子、氧原子或硫原子中的至少之一与过渡金属化合物的过渡金属原子配位。在本公开的一些实施例中，过渡金属化合物中的加合物形成配体可包含环状加合物配体。在本公开的一些实施例中，过渡金属化合物中的加合物形成配体可包含单胺、二胺或多胺。在本公开的一些实施例中，过渡金属化合物中的加合物形成配体可包含单醚、二醚或多醚。在一些实施例中，过渡金属化合物中的加合物形成配体可包含单膦、二膦或多膦。在一些实施例中，过渡金属化合物中的加合物形成配体可包含碳和/或除加合物形成配体中的氮、氧、磷或硫之外还包含碳。
在本公开的一些实施例中，过渡金属化合物中的加合物形成配体可包含一个单齿加合物形成配体。在本公开的一些实施例中，过渡金属化合物中的加合物形成配体可包含两个单齿加合物形成配体。在本公开的一些实施例中，过渡金属化合物中的加合物形成配体可包含三个单齿加合物形成配体。在本公开的一些实施例中，过渡金属化合物中的加合物形成配体可包含四个单齿加合物形成配体。在本公开的一些实施例中，过渡金属化合物中的加合物形成配体可包含一个二齿加合物形成配体。在本公开的一些实施例中，过渡金属化合物中的加合物形成配体可包含两个二齿加合物形成配体。在本公开的一些实施例中，过渡金属化合物中的加合物形成配体可包含一个多齿加合物形成配体。在本公开的一些实施例中，过渡金属化合物中的加合物形成配体可包含两个多齿加合物形成配体。
在本公开的一些实施例中，加合物形成配体包含氮，如胺、二胺或多胺加合物形成配体。在这样的实施例中，过渡金属化合物可包含以下中的至少之一：三乙胺(TEA)、N,N,N’,N’-四甲基-1,2-乙二胺(CAS:110-18-9)(TMEDA)、N,N,N′,N′-四乙基乙二胺(CAS:150-77-6)(TEEDA)、N,N’-二乙基-1,2-乙二胺(CAS:111-74-0)(DEEDA)、N,N’-二异丙基乙二胺(CAS:4013-94-9)、N,N,N’,N’-四甲基-1,3-丙二胺(CAS:110-95-2)(TMPDA)、N,N,N’,N’-四甲基甲二胺(CAS:51-80-9)(TMMDA)、N,N,N’,N”,N”-五甲基二亚乙基三胺(CAS:3030-47-5)(PMDETA)、二亚乙基三胺(CAS:111-40-0)(DIEN)|、三亚乙基四胺(CAS:112-24-3)(TRIEN)、三(2-氨基乙基)胺(CAS:4097-89-6)(TREN,TAEA)、1,1,4,7,10,10-六甲基三亚乙基四胺(CAS:3083-10-1)(HMTETA)、1,4,8,11-四氮杂环十四烷(CAS:295-37-4)(Cyclam)、1,4,7-三甲基-1,4,7-三氮杂环壬烷(CAS:96556-05-7)或1,4,8,11-四甲基-1,4,8,11-四氮杂环十四烷(CAS:41203-22-9)。
在本公开的一些实施例中，加合物形成配体包含磷，如膦、二膦或多膦加合物形成配体。例如，过渡金属化合物可包含三乙基膦(CAS：554-70-1)、亚磷酸三甲酯(CAS：121-45-)、1,2-双(二乙基膦基)乙烷(CAS：6411-21-8)(BDEPE)或1,3-双(二乙基膦基)丙烷(CAS：29149-93-7)中的至少之一。
在本公开的一些实施例中，加合物形成配体包含氧，如醚、二醚或多醚加合物形成配体。例如，过渡金属化合物可包含1,4-二氧六环(CAS：123-91-1)、1,2-二甲氧基乙烷(CAS：110-71-4)(DME，单甘醇二甲醚)、二乙二醇二甲醚(CAS：111-96-6)(二甘醇二甲醚)、三乙二醇二甲醚(CAS：112-49-2)(三甘醇二甲醚)或1,4,7,10-四氧杂环十二烷(CAS：294-93-9)(12-冠-4)中的至少之一。
在本公开的一些实施例中，加合物形成配体可包含硫醚或混合醚胺，例如1,7-二氮杂-12-冠-4：1,7-二氧杂-4,10-二氮杂环十二烷(CAS：294-92-8)或1,2-双(甲硫基)乙烷(CAS：6628-18-8)中的至少之一。
在一些实施例中，过渡金属卤化物化合物可包含氯化钴N,N,N’,N’-四甲基-1,2-乙二胺(CoCl2(TMEDA))。在一些实施例中，过渡金属卤化物化合物可包含溴化钴四甲基乙二胺(CoBr2(TMEDA))。在一些实施例中，过渡金属卤化物化合物可包含碘化钴四甲基乙二胺(CoI2(TMEDA))。在一些实施例中，过渡金属卤化物化合物可包含氯化钴N,N,N’,N’-四甲基-1,3-丙二胺(CoCl2(TMPDA))。在本公开的一些实施例中，过渡金属卤化物化合物可包含氯化钴N,N,N’,N’-四甲基-1,2-乙二胺(CoCl2(TMEDA))、氯化镍四甲基-1,3-丙二胺(NiCl2(TMPDA))或碘化镍四甲基-1,3-丙二胺(NiI2(TMPDA))中的至少之一。
在本公开的一些实施例中，使衬底与包含过渡金属卤化物化合物即包含加合物形成配体的过渡金属卤化物的第一气相反应物接触可包括将衬底暴露于过渡金属卤化物化合物、即使衬底与过渡金属卤化物化合物接触约0.01秒至约60秒之间、约0.05秒至约10秒之间或约0.1秒至约5.0秒之间的时间段。另外，在对过渡金属卤化物化合物进行脉冲期间，过渡金属卤化物化合物的流率可小于2000sccm、或小于500sccm、或甚至小于100sccm。另外，在衬底上方对过渡金属卤化物化合物进行脉冲期间，过渡金属卤化物化合物的流率可在约1至2000sccm、约5至1000sccm、或约10至约500sccm的范围内。
可例如通过用惰性气体吹扫来从表面去除过量的过渡金属卤化物化合物和反应副产物(如果存在)。例如，在本公开的一些实施例中，所述方法可包括吹扫循环，其中将衬底表面吹扫不到大约2.0秒的时间段。可借助于真空去除过量的过渡金属卤化物化合物和任何反应副产物，所述真空由与反应腔室流体连通的泵送系统产生。
在沉积循环的第二阶段中，可使衬底与第二气相反应物接触，所述第二气相反应物包含氧前体、氮前体、硅前体、硫前体、硒前体、磷前体、硼前体或还原剂中的至少之一。在一些实施例中，第二气相反应物可包含氧前体并且通过本文公开的循环沉积方法沉积的含过渡金属的膜可包含过渡金属氧化物。在一些实施例中，第二气相反应物可包含还原剂(这将在下文更详细地描述)并且通过这里公开的循环沉积方法沉积的含过渡金属的膜可包含元素过渡金属。在一些实施例中，第二气相反应物可包含氮前体并且通过本文公开的循环沉积方法沉积的含过渡金属的膜可包含过渡金属氮化物。在一些实施例中，第二气相反应物可包含硅前体并且通过本文公开的循环沉积方法沉积的含过渡金属的膜可包含过渡金属硅化物。在一些实施例中，第二气相反应物可包含硫前体并且通过本文公开的循环沉积方法沉积的含过渡金属的膜可包含过渡金属硫化物。在一些实施例中，第二气相反应物可包含硒前体并且通过本文公开的循环沉积方法沉积的含过渡金属的膜可包含过渡金属硒化物。在一些实施例中，第二气相反应物可包含磷前体并且通过本文公开的循环沉积方法沉积的含过渡金属的膜可包含过渡金属磷化物。在一些实施例中，第二气相反应物可包含硼前体并且通过本文公开的循环沉积方法沉积的含过渡金属的膜可包含过渡金属硼化物。
在其中第二气相反应物包含氧前体的本公开实施例中，所述氧前体可包含臭氧(O3)、分子氧(O2)、氧原子(O)、氧等离子体、氧自由基、氧激发物种、水(H2O)或过氧化氢(H2O2)中的至少之一。
在其中第二气相反应物包含氮前体的本公开实施例中，氮前体可包含氨(NH3)、肼(N2H4)、三氮烷(N3H5)、叔丁基肼(C4H9N2H3)、甲基肼(CH3NHNH2)、二甲肼((CH3)2N2H2)或氮等离子体或包含氢的氮等离子体中的至少之一。
在一些实施例中，第二气相反应物可包含烃取代的肼前体。在沉积循环的第二阶段(“取代的肼阶段”)中，使衬底与包含烃取代的肼前体的第二气相反应物接触。在本公开的一些实施例中，方法还可包括选择取代的肼以包含具有至少四(4)个碳原子的烷基基团，其中“烷基基团”是指长度为至少四(4)个碳原子的饱和或不饱和烃链，如但不限于丁基、戊基、己基、庚基和辛基及其异构体，如这些烷基基团的正-、异-、仲-和叔-异构体。烷基基团可以是直链或支链的并可包括烷基基团的所有结构异构体形式。在一些实施例中，烷基链可以被取代。在本公开的一些实施例中，烷基-肼可包含至少一个键合到氮的氢。在本公开的一些实施例中，烷基-肼可包含至少两个键合到氮的氢。在本公开的一些实施例中，烷基-肼可包含至少一个键合到氮的氢和至少一个键合到氮的烷基链。在本公开的一些实施例中，第二反应物可包含烷基-肼并还可包含叔丁基肼(C4H9N2H3)、二甲基肼或二乙基肼中的一者或多者。在本公开的一些实施例中，取代的肼具有至少一个连接到氮的烃基团。在本公开的一些实施例中，取代的肼具有至少两个连接到氮的烃基团。在本公开的一些实施例中，取代的肼具有至少三个连接到氮的烃基团。在本公开的一些实施例中，取代的肼具有至少一个连接到氮的C1-C3烃基团。在本公开的一些实施例中，取代的肼具有至少一个连接到氮的C4-C10烃基团。在本公开的一些实施例中，取代的肼具有连接到氮的直链、支链或环状或芳族烃基团。在本公开的一些实施例中，取代的肼包含连接到氮的取代的烃基团。
在本公开的一些实施例中，取代的肼具有下式II：
RIRII-N-NRIIIRIV, (II)
其中RI可选自烃基团，如直链、支链、环状、芳族或取代的烃基团，并且RII、RIII、RIV基团中的每一个可独立地选择为氢或烃基团，如直链、支链、环状、芳族或取代的烃基团。
在一些实施例中，在式(II)中，RI、RII、RIII、RIV可为C1-C10烃、C1-C3烃、C4-C10烃或氢，如直链、支链、环状、芳族或取代的烃基团。在一些实施例中，RI、RII、RIII、RIV基团中的至少之一包含芳族基团如苯基基团。在一些实施例中，RI、RII、RIII、RIV基团中的至少之一包含甲基、乙基、正丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基基团或苯基基团。在一些实施例中，各个RI、RII、RIII、RIV基团中的至少两者可独立地选择为包含甲基、乙基、正丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基基团或苯基基团。在一些实施例中，RII、RIII和RIV基团为氢。在一些实施例中，RII、RIII和RIV基团中的至少两者为氢。在一些实施例中，RII、RIII和RIV基团中的至少之一为氢。在一些实施例中，RII、RIII和RIV基团中的全部为烃。
在其中第二气相反应物包含硅前体的本公开实施例中，硅前体可包含硅烷(SiH4)、乙硅烷(Si2H6)、丙硅烷(Si3H8)、丁硅烷(Si4H10)、异戊硅烷(Si5H12)或新戊硅烷(Si5H12)中的至少之一。在其中第二气相反应物包含硅前体的本公开实施例中，硅前体可包含C1-C4烷基硅烷。在其中第二气相反应物包含硅前体的本公开实施例中，硅前体可包含来自硅烷家族的前体。
在其中第二气相反应物包含硼前体的本公开实施例中，硼前体可包含硼烷(BH3)、乙硼烷(B2H6)或其他硼烷如癸硼烷(B10H14)中的至少之一。
在其中第二气相反应物包含氢前体的本公开实施例中，氢前体可包含H2、H离子、H等离子体或H自由基中的至少之一。
在本公开的一些实施例中，第二气相反应物包含磷前体、硫前体或硒化物前体。在一些实施例中，硫前体包含氢和硫。在一些实施例中，硫前体为烷基硫化合物。在一些实施例中，第二反应物包含元素硫、H2S、(CH3)2S、(NH4)2S、((CH3)2SO)和H2S2中的一者或多者。在一些实施例中，硒前体为烷基硒化合物。在一些实施例中，第二反应物包含元素硒、H2Se、(CH3)2Se和H2Se2中的一者或多者。在一些实施例中，硒前体包含氢和硒。在一些实施例中，第二反应物可包含Te、Sb、Se的烷基甲硅烷基化合物，如(Me3Si)2Te、(Me3Si)2Se或(Me3Si)3Sb。在一些实施例中，磷前体为烷基磷化合物。在一些实施例中，第二反应物包含元素磷、PH3或烷基膦如甲基膦中的一者或多者。在一些实施例中，磷前体包含氢和磷。
在其中第二气相反应物包含有机前体如还原剂的本公开实施例中，可利用例如醇、醛或羧酸或其他有机化合物，例如不具有金属或半金属但包含-OH基团的有机化合物。醇可以是伯醇、仲醇、叔醇、多羟基醇、环醇、芳族醇以及醇的其他衍生物。
伯醇具有连接到碳原子的-OH基团，所述碳原子与另一个碳原子键合，特别地，根据通式(III)的伯醇：
R1-OH (III)
其中R1为直链或支链C1-C20烷基或烯基基团，如甲基、乙基、丙基、丁基、戊基或己基。伯醇的实例包括甲醇、乙醇、丙醇、丁醇、2-甲基丙醇和2-甲基丁醇。
仲醇具有连接到碳原子的-OH基团，所述碳原子与两个其他碳原子键合。特别地，仲醇具有通式(IV)：
Figure BDA0002618661280000151
其中每个R1独立地选自直链或支链C1-C20烷基和烯基基团，如甲基、乙基、丙基、丁基、戊基或己基。仲醇的实例包括2-丙醇和2-丁醇。
叔醇具有连接到碳原子的-OH基团，所述碳原子与三个其他的碳原子键合。特别地，叔醇具有通式(V)：
Figure BDA0002618661280000152
其中每个R1独立地选自直链或支链C1-C20烷基和烯基基团，如甲基、乙基、丙基、丁基、戊基或己基。叔醇的实例为叔丁醇。
多羟基醇，如二醇和三醇，具有如上所述的伯醇、仲醇和/或叔醇基团。多羟基醇的实例有乙二醇和甘油。
环醇具有连接到至少一个碳原子的-OH基团，所述至少一个碳原子为1至10个、如5-6个碳原子的环的一部分。
芳族醇具有至少一个连接到苯环或连接到侧链中的碳原子的-OH基团。
有机前体可包含至少一个醛基团(-CHO)，其选自具有通式(VI)的化合物、具有通式(VII)的烷二醛化合物、卤代醛及醛的其他衍生物。
因此，在一个实施例中，有机前体为具有通式(VI)的醛：
R3-CHO (VI)
其中R3选自氢和直链或支链C1-C20烷基和烯基基团，如甲基、乙基、丙基、丁基、戊基或己基。在一些实施例中，R3选自甲基或乙基。根据式(VI)的示例性化合物有但不限于甲醛、乙醛和丁醛。
在另一个实施例中，有机前体为具有通式(VII)的醛：
OHC-R4-CHO (VII)
其中R4为直链或支链C1-C20饱和或不饱和烃。或者，醛基团可直接彼此键合(R4不存在)。
含至少一个-COOH基团的有机前体可选自通式(VIII)的化合物、多羧酸、卤代羧酸及羧酸的其他衍生物。
因此，在一个实施例中，有机前体为具有通式(VIII)的羧酸：
R5-COOH (VIII)
其中R5为氢或者直链或支链C1-C20烷基或烯基基团，如甲基、乙基、丙基、丁基、戊基或己基，例如甲基或乙基。在一些实施例中，R5为直链或支链C1-C3烷基或烯基基团。根据式(VII)的化合物的实例有甲酸、丙酸和乙酸，在一些实施例中为甲酸(HCOOH)。
在本公开的一些实施例中，将衬底暴露于第二气相反应物、即使衬底与第二气相反应物接触包括在衬底上方对第二气相反应物进行脉冲，持续0.1秒至2.0秒、或约0.01秒至约10秒之间、或不到约20秒、不到约10秒或不到约5秒的时间段。在衬底上方对第二气相反应物进行脉冲期间，第二气相反应物的流率可小于50sccm、或小于25sccm、或小于15sccm、或甚至小于10sccm。
可例如通过吹扫气体脉冲和/或由泵送系统产生的真空从衬底表面去除过量的第二气相反应物和反应副产物(如果有的话)。吹扫气体优选任何惰性气体，如但不限于氩气(Ar)、氮气(N2)、氦气(He)，或在一些情况下可使用氢气(H2)。如果有吹扫(即，吹扫气体脉冲)或其他反应物去除步骤介入，则通常认为一个阶段紧接在另一个阶段之后。
可将其中衬底交替地与第一气相反应物(即，金属卤化物化合物)和第二气相反应物(例如，氧前体)接触的沉积循环重复一次或多次，直至沉积了所需厚度的含过渡金属的膜。应理解，在本公开的一些实施例中，使衬底与第一气相反应物和第二气相反应物接触的顺序可以是这样的：先使衬底与第二气相反应物接触，然后与第一气相反应物接触。此外，在一些实施例中，循环沉积工艺可包括使衬底与第一气相反应物接触一次或多次，然后使衬底与第二气相反应物接触一次或多次，并且类似地，作为替代方案，可包括使衬底与第二气相反应物接触一次或多次，然后使衬底与第一气相反应物接触一次或多次。
此外，本公开的一些实施例可以包含非等离子体反应物，例如第一和第二气相反应物大体上不含离子化反应性物种。在一些实施例中，第一和第二气相反应物大体上不含离子化反应性物种、受激物种或自由基物种。例如，第一气相反应物和第二气相反应物可以包含非等离子体反应物以防止底层衬底的离子化损坏和由此产生的相关缺陷。当下面的衬底含有易碎的制造或至少部分制造的半导体器件结构时，非等离子体反应物的使用可能尤其有用，因为高能等离子体物种可能损伤和/或降低器件性能特性。
在本公开的一些实施例中，本公开的示例性循环沉积方法可包括另外的工艺步骤，其包括使衬底与包含还原剂的第三气相反应物接触。在一些实施例中，还原剂可包含以下中的至少之一：氢气(H2)、氢(H2)等离子体、氨气(NH3)、氨(NH3)等离子体、肼(N2H4)、硅烷(SiH4)、乙硅烷(Si2H6)、丙硅烷(Si3H8)、锗烷(GeH4)、乙锗烷(Ge2H6)、硼烷(BH3)、乙硼烷(B2H6)、叔丁基肼(C4H12N2)、硒前体、硼前体、磷前体、硫前体、有机前体(例如，醇、醛或羧酸)或氢前体。在本公开的一些实施例中，本公开的示例性循环沉积方法可包括使衬底与为还原剂的第二气相反应物接触(无任何另外的前体/反应物接触步骤)。
在一种示例性的循环沉积方法中，可向反应腔室中引入包含还原剂的第三气相反应物并在多个工艺阶段与衬底接触。在本公开的一些实施例中，可向反应腔室中引入还原剂并使衬底单独地与第一气相反应物和单独地与第二气相反应物接触。例如，可在使衬底与第一气相反应物接触之前、在使衬底与第一气相反应物接触之后并在使衬底与第二气相反应物接触之前、和/或在使衬底与第二气相反应物接触之后向反应腔室中引入还原剂并与衬底接触。在本公开的一些实施例中，可与第一气相反应物同时和/或与第二气相反应物同时向反应腔室中引入还原剂并与衬底接触。例如，可使还原剂和第一气相反应物共同流动到反应腔室中并同时与衬底接触，和/或可使还原剂和第二气相反应物共同流动到反应腔室中并同时与衬底接触。
在本公开的一些实施例中，第一气相反应物可包含过渡金属卤化物化合物，第二气相反应物可包含氧前体。在这样的实施例中，循环沉积工艺可在衬底上沉积过渡金属氧化物。作为一个非限制性实例，第一气相反应物可包含CoCl2(TMEDA)，第二气相反应物可包含水(H2O)，并且沉积在衬底上的膜可包含氧化钴。在一些实施例中，过渡金属氧化物可通过将过渡金属氧化物暴露于还原剂来进一步加工。在一些实施例中，可将过渡金属氧化物暴露于至少一种还原剂，所述还原剂包含合成气体(H2+N2)、氨气(NH3)、肼(N2H4)、分子氢(H2)、氢原子(H)、氢等离子体、氢自由基、氢激发物种、醇、醛、羧酸、硼烷或胺。
在一些实施例中，将过渡金属氧化物暴露于还原剂可将过渡金属氧化物还原为元素过渡金属。作为一个非限制性实例，可利用本公开的循环沉积工艺来沉积氧化钴膜至50纳米的厚度，并可在1000毫巴的压力和大约250℃的温度下将氧化钴膜暴露于10％的合成气体以将氧化钴膜还原为元素钴。在本公开的一些实施例中，过渡金属氧化物可具有小于500纳米、或小于100纳米、或小于50纳米、或小于25纳米、或小于20纳米、或小于10纳米、或甚至小于5纳米的厚度。在一些实施例中，可将过渡金属氧化物暴露于还原剂不到5小时、或不到1小时、或不到30分钟、或不到15分钟、或不到10分钟、或不到5分钟、或甚至不到1分钟。在一些实施例中，可在低于500℃、或低于400℃、或低于300℃、或低于250℃、或低于200℃或甚至低于150℃的衬底温度下将过渡金属氧化物暴露于还原剂。在一些实施例中，可在减压气氛中将过渡金属氧化物暴露于还原剂，其中所述压力可为约0.001毫巴至约10巴、或约1毫巴至约1000毫巴。
本文描述的利用包含过渡金属卤化物化合物的第一气相反应物和第二气相反应物来沉积含过渡金属的膜的循环沉积工艺可在ALD或CVD沉积系统中用经加热的衬底进行。例如，在一些实施例中，方法可以包括将衬底加热到在约80℃与约150℃之间的温度，或甚至将衬底加热到在约80℃与约120℃之间的温度。当然，用于任何给定循环沉积工艺，如用于ALD反应的适当温度范围将取决于所涉及的表面终止状态和反应物物种。这里，温度随使用的前体而异并通常处于或低于约700℃。在一些实施例中，对于气相沉积工艺，沉积温度通常处于或高于约100℃，在一些实施例中，沉积温度在约100℃至约300℃之间，并且在一些实施例中，沉积温度在约120℃至约200℃之间。在一些实施例中，沉积温度低于约500℃、或低于约400℃、或低于约350℃、或低于约300℃。在一些情况下，沉积温度可低于约300℃、低于约200℃或低于约100℃。在一些情况下，沉积温度可高于约20℃、高于约50℃、高于约75℃。在本公开的一些实施例中，沉积过程中的沉积温度即衬底的温度为大约275℃。
在一些实施例中，含过渡金属的膜的生长速率为约
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/循环至约
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/循环、约
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/循环至约
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/循环。在一些实施例中，含过渡金属的膜的生长速率大于约
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/循环、大于约
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/循环、大于约
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/循环、大于约
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/循环、大于约
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/循环、或大于约
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/循环。在一些实施例中，含过渡金属的膜的生长速率小于约
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/循环、小于约
Figure BDA0002618661280000198
/循环、小于约
Figure BDA0002618661280000199
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Figure BDA00026186612800001910
/循环、或小于约
Figure BDA00026186612800001911
/循环。在本公开的一些实施例中，含过渡金属的膜的生长速率可为大约
Figure BDA00026186612800001912
/循环。
本公开的实施例可包括循环沉积，所述循环沉积可由图1的示例性循环沉积方法100更详细地示意。方法100可以工艺框110开始，其包括向反应腔室中提供至少一个衬底和将衬底加热到沉积温度。例如，衬底可包含一个或多个部分制造的半导体器件结构，反应腔室可包括原子层沉积反应腔室，并可将衬底加热到大约低于275℃的沉积温度。另外，可控制反应腔室内的压力以在反应腔室中提供减压气氛。例如，在循环沉积工艺期间反应腔室内的压力可低于1000毫巴、或低于100毫巴、或低于10毫巴、或低于5毫巴、或甚至在一些情况下低于1毫巴。
方法100可以工艺框120继续，其包括使衬底与过渡金属卤化物化合物接触，例如，可使衬底与过渡金属卤化物化合物接触大约1秒的时间段。在本公开的一些实施例中，过渡金属化合物可与衬底接触约0.01秒至约60秒之间、约0.05秒至约10秒之间、或约0.1秒至约5秒之间的时间段。另外，在衬底上方对过渡金属前体进行脉冲期间，过渡金属前体的流率可小于2000sccm、或小于1000sccm、或小于500sccm、或小于200sccm、或甚至小于100sccm。
在使衬底与过渡金属卤化物化合物接触后，可通过吹扫/抽吸工艺从反应腔室去除过量的金属前体和任何反应副产物。
方法100可以工艺框130继续，其包括使衬底与第二气相反应物如氧前体、氮前体、硅前体、磷前体、硒前体、硼前体或还原剂接触。第二气相反应物(例如，水)可与衬底接触大约4秒的时间段。在本公开的一些实施例中，第二气相反应物可与衬底接触约0.01秒至约60秒之间、约0.05秒至约10秒之间、或约0.1秒至约5.0秒之间的时间段。另外，在衬底上方对第二气相反应物进行脉冲期间，第二气相反应物的流率可小于2000sccm、或小于1000sccm、或小于500sccm、或小于200sccm、或甚至小于100sccm。
在使衬底与第二气相反应物前体接触后，可通过吹扫/抽吸工艺从反应腔室去除过量的第二气相反应物和任何反应副产物。
其中使衬底交替且依序地与过渡金属卤化物化合物接触(工艺框120)和与第二气相反应物接触(工艺框130)的示例性循环沉积方法100可构成一个沉积循环。在本公开的一些实施例中，沉积含过渡金属的膜的方法可包括将沉积循环重复一次或多次。例如，方法100可以决策门140继续，其决定循环沉积方法100是继续还是经由工艺框150退出。决策门140基于沉积的含过渡金属的膜的厚度作决定，例如，如果含过渡金属的膜的厚度对于所需的器件结构不够，则方法100可返回到工艺框120并可将使衬底与过渡金属卤化物化合物接触和使衬底与第二气相反应物接触的工艺重复一次或多次。在含过渡金属的膜已沉积到所需的厚度后，方法可经由工艺框150退出并可使含过渡金属的膜和下面的半导体结构经受另外的工艺以形成一个或多个器件结构。
根据一些本文所述的实施例沉积的包含过渡金属的膜或层可以是连续的薄膜。在一些实施例中，根据一些本文所述的实施例沉积的包含过渡金属的薄膜可在低于大约100纳米、或低于大约60纳米、或低于大约50纳米、或低于大约40纳米、或低于大约30纳米、或低于大约25纳米、或低于大约20纳米、或低于大约15纳米、或低于大约10纳米、或低于大约5纳米或更低的厚度下是连续的。本文中提到的连续性可以是物理连续性或电连续性。在一些实施例中，使膜可以具有物理连续性的厚度可能与使膜具有电连续性的厚度不相同，并且使膜可以具有电连续性的厚度可能与使膜具有物理连续性的厚度不相同。
在一些实施例中，根据一些本文所述的实施例沉积的含过渡金属的膜的厚度可为约20纳米至约100纳米。在一些实施例中，根据一些本文所述的实施例沉积的含过渡金属的膜的厚度可为约20纳米至约60纳米。在一些实施例中，根据一些本文所述的实施例沉积的含过渡金属的膜的厚度可大于约20纳米、或大于约30纳米、或大于约40纳米、或大于约50纳米、或大于约60纳米、或大于约100纳米、或大于约250纳米、或大于约500纳米或更大。在一些实施例中，根据一些本文所述的实施例沉积的含过渡金属的膜的厚度可小于约50纳米、小于约30纳米、小于约20纳米、小于约15纳米、小于约10纳米、小于约5纳米、小于约3纳米、小于约2纳米、或甚至小于约1纳米。
在本公开的一些实施例中，可在三维结构例如包含高纵横比特征的非平面衬底上沉积含过渡金属的膜。在一些实施例中，在纵横比(高/宽)大于约2、大于约5、大于约10、大于约25、大于约50或甚至大于约100的结构中，含过渡金属的膜的台阶覆盖率可等于或高于约50％、或高于约80％、或高于约90％、或高于约95％、或高于约98％、或高于约99％或更高。
在本公开的一些实施例中，根据本公开的实施例沉积的含过渡金属的膜可包含低于约50原子％的氧、低于约25原子％的氧、低于约10原子％的氧、低于约5原子％的氧、低于约2原子％的氧、或甚至低于约1原子％的氧。在进一步的实施例中，含过渡金属的膜可包含低于约5原子％的氢、或低于约2原子％的氢、或低于约1原子％的氢、或甚至低于约0.5原子％的氢。在还进一步的实施例中，含过渡金属的膜可包含低于约5原子％的碳、或低于约2原子％的碳、或低于约1原子％的碳、或甚至低于约0.5原子％的碳。在还进一步的实施例中，含过渡金属的膜可包含低于约5原子％的卤化物物种、或低于约2原子％的卤化物物种、或低于约1原子％的卤化物物种、或甚至低于约0.5原子％的卤化物物种。在一些实施例中，可利用飞行弹性反冲检测分析(ToF-ERDA)的时间来确定含过渡金属的材料的原子％。
在本公开的一些实施例中，可利用本公开的循环沉积工艺来沉积过渡金属氧化物，例如氧化钴等。用于循环沉积工艺如原子层沉积的现有钴前体已证明对水(H2O)不活跃，因此通常已利用臭氧(O3)作为氧前体。然而，将臭氧用于氧化钴的循环沉积通常会导致氧化钴(II,III)(Co3O4)而不是氧化钴(II)(CoO)的形成。在一些实施例中，可能有利的是沉积CoO而不是Co3O4，例如，CoO形式的钴的较低氧化态可更容易地还原为钴金属。因此，在本公开的一些实施例中，可利用本公开的循环沉积工艺来沉积基本上氧化钴(II)(CoO)的膜，即其中钴与氧的比率基本上等于1:1。在本公开的一些实施例中，循环沉积工艺期间的沉积温度可影响所沉积的膜的化学计量。例如，当利用本文公开的循环沉积工艺沉积氧化钴膜时，衬底温度可影响沉积膜中钴与氧的比率(Co:O)。因此，作为本公开的一个非限制性实例实施例，可利用CoCl2(TMEDA)作为钴前体和水(H2O)作为氧前体来沉积氧化钴膜。在这样的循环沉积工艺期间，可将衬底温度控制在大约275℃下，这可导致氧化钴(II)(CoO)的沉积，其中钴与氧的比率(Co:O)为大约1:1。
通过本文公开的循环沉积工艺沉积的含过渡金属的膜可用于多种场合，例如衬里层、覆盖层、间隙填充层、沟槽填充层、种子层、接触层/接触填充层、电迁移改进层、后道(BEOL)应用中的导电互连和用于半导体器件接触件的硅化物形式。在一些实施例中，可利用本公开的含过渡金属的膜作为电极或电极的至少一部分，所述电极配置为向一个或多个器件结构提供电流。在本公开的一些实施例中，可将本公开的含过渡金属的膜用在CMOS器件应用中作为一个或多个CMOS器件的电极的至少一部分。
作为一个非限制性的实例实施例，可将含过渡金属的膜例如钴用作后道(BEOL)金属化应用中的屏障材料和/或覆盖层，如图2中所示。更详细地，图2示意了部分制造的半导体器件结构200，其包含衬底202，该衬底可包含部分制造和/或制造的半导体器件结构如晶体管和存储器元件(未示出)。部分制造的半导体器件结构200可包括形成在衬底202上方的介电材料204，该介电材料可包含低介电常数材料，即低-k电介质，如含硅电介质或金属氧化物。沟槽可形成于介电材料204中，屏障材料206可设置于沟槽的表面上，其防止或基本上防止金属互连材料208向周围介电材料204中的扩散。在本公开的一些实施例中，屏障材料206可包含通过本文所述的循环沉积工艺沉积的钴。在本公开的一些实施例中，钴膜的厚度可小于35埃、或25埃、或甚至15埃。部分制造的半导体结构200还可包含用于将设置在衬底202中的多个器件结构电互连的金属互连材料208。在一些实施例中，金属互连材料208可包含铜或钴中的一者或多者。除了使用钴作为屏障材料外，还可利用钴作为覆盖层。因此，参考图2，部分制造的半导体器件结构200还可包括直接设置在金属互连材料208的上表面上的覆盖层210。可利用覆盖层210来防止金属互连材料208的氧化，并且重要的是防止金属互连材料208向后续制造工艺中在部分制造的半导体结构200上方形成的另外的介电材料中的扩散，即，用于多级互连结构。在本公开的一些实施例中，覆盖层210也可包含钴，其厚度小于20埃、或小于15埃、或甚至小于10埃。在一些实施例中，金属互连材料208、屏障材料206和覆盖层210可共同形成用于设置在衬底202中的多个半导体器件的电互连的电极。
还可利用本公开的实施例来合成可用于气相沉积工艺如原子层沉积、化学气相沉积和循环化学气相沉积的化学前体。因此，本公开的实施例可包括合成如本文前文所述的包含加合物形成配体的过渡金属卤化物化合物例如包含二齿含氮加合物配体的过渡金属卤化物的方法。在一些实施例中，可利用本公开的方法来合成氯化钴(II)(TMEDA)、氯化镍(II)(TMEDA)或氯化铜(II)(TMEDA)中的一种或多种。在一些实施例中，可利用本公开的方法来合成碘化钴(II)(TMEDA)、碘化镍(II)(TMEDA)或碘化铜(II)(TMEDA)中的一种或多种。在一些实施例中，可利用本公开的方法来合成溴化钴(II)(TMEDA)、溴化镍(II)(TMEDA)或溴化铜(II)(TMEDA)中的一种或多种。另外，在一些实施例中，可利用本公开的方法来合成氯化钴(II)(TMPDA)、氯化镍(II)(TMPDA)和氯化铜(II)(TMPDA)。
以下描述公开了一种用于合成CoCl2(TMEDA)的方法，应理解，所公开的用于合成CoCl2(TMEDA)的方法同样适用于本文公开的另外的过渡金属卤化物化合物的合成方法并且不应理解为限制性的。
化学前体合成方法可使用标准的Schlenk技术和惰性气体(例如，N2或Ar)手套箱在严格排除空气和水分的条件下进行所有处理和操作。利用无水CoCl2(99％)和N,N,N`,N`-四甲基乙二胺(TMEDA)(99％)作为反应物。另外，利用二氯甲烷(CH2Cl2)作为合适的溶剂，工艺包括用
Figure BDA0002618661280000231
分子筛对CH2Cl2脱氧和干燥。
在本公开的一些实施例中，可称取一定量的CoCl2并加到合适的容器如Schlenk瓶中。可向CoCl2中加入一定量的CH2Cl2。随后，可向溶液中逐滴加入化学计量量的TMEDA。在一些实施例中，可以超过卤化物化合物的量加入加合物形成配体(例如，TMEDA)，如以比卤化物化合物的量大2倍、或大5倍、或甚至大10倍的量。所得悬浮液可在室温下搅拌大约1小时。作为一个非限制性实例，可称取6.00g(46.211mmol)CoCl2并与100ml CH2Cl2一道加入Schlenk瓶中。向溶液中加入5.37g(46.211mmol)TMEDA并在室温下搅拌1小时。可将所得蓝色溶液蒸发至干，产生蓝色粗产物。可将所得粗产物转移到升华器，在其中，产品可在大约150-200℃之间的温度下升华，由此产生CoCl2(TMEDA)。在本公开的一些实施例中，所得挥发性过渡金属卤化物化合物例如CoCl2(TMEDA)的杂质浓度百分数可小于5原子％、或小于2原子％、或小于1原子％、或小于0.1原子％、或甚至小于0.01原子％。在本公开的一些实施例中，与有机过渡金属前体相比，挥发性过渡金属卤化物化合物可具有更高的分解温度。例如，本公开的过渡金属卤化物化合物可具有高于150℃或甚至高于200℃的分解温度。
因此，在本公开的一些实施例中，可合成可用于气相沉积含过渡金属的膜的过渡金属卤化物化合物。在一些实施例中，可利用一步合成工艺合成包含加合物形成配体的金属卤化物化合物，所述一步合成工艺包括在低于大约50℃、或低于大约30℃、或甚至低于大约15℃的温度下合并过渡金属卤化物化合物与加合物形成配体，其中整个合成工艺可在不到5小时、或不到2小时、或不到1小时、或甚至不到30分钟的时间段内完成。
本公开的实施例还可包含气相沉积装置，所述气相沉积装置包括一个或多个前体源容器，所述前体源容器配置为容纳过渡金属卤化物化合物和向反应腔室供给过渡金属卤化物化合物。因此，在本公开的一些实施例中，提供了利用反应性挥发性化学品的气相沉积装置。所述装置可包含：反应腔室；设置在反应腔室内的衬底；与反应腔室流体连通的前体源容器；和设置在前体源容器中的过渡金属卤化物化合物，所述过渡金属卤化物化合物包含二齿含氮配体。
更详细地，图4示意性地示出了包括反应腔室400的气相沉积装置400。应指出，图4为气相沉积装置400的简化示意版本而不含本公开的气相沉积装置400中可能利用的每一个元件，即，如但不限于阀、电连接、质量流量控制器、密封件和气体导管。在本公开的一些实施例中，反应腔室402可包括配置为用于将衬底406支承在反应腔室内的衬托器404。反应腔室中还设置了喷淋头气体分配器408，其用于将衬底选择性地暴露于各种气体。
在本公开的一些实施例中，前体源容器410A可经由导管或其他适宜的措施412A与反应腔室402流体连通，并可进一步耦接到歧管、阀控制系统、质量流量控制系统或用以控制源自前体源容器410A的气态前体的机构。前体源容器410A可配置为用于贮存包含二齿含氮配体的过渡金属卤化物化合物。在一些实施例中，前体源容器410A可包含石英材料，所述石英材料对贮存在前体源容器410A内的过渡金属卤化物化合物可以是基本上化学惰性的。在本公开的替代实施例中，前体源容器410A可由耐腐蚀金属或金属合金如哈氏合金(Hastelloy)、蒙乃尔合金(Monel)或其组合制成。
在本公开的一些实施例中，前体源容器410A可还包含一个或多个加热单元414，所述加热单元配置为用于加热贮存在前体源容器410A中的过渡金属卤化物化合物。在一些实施例中，可利用所述一个或多个加热单元400来将过渡金属卤化物化合物加热到大约高于0℃、或大约高于20℃、或大约高于100℃、或大约高于150℃、或大约高于200℃、或大约高于200℃、或大约高于300℃、或甚至大约高于400℃的温度。在一些实施例中，所述一个或多个加热单元414可配置为将贮存在前体源容器410A中的过渡金属卤化物化合物加热到大约170℃的温度。
在一些实施例中，与前体源容器410A相关联的所述一个或多个加热单元414配置为用于将过渡金属卤化物化合物从固体转化为液体或气体。在一些实施例中，可利用与前体源容器410A相关联的所述一个或多个加热单元414来控制贮存在前体贮存容器410A中的过渡金属卤化物化合物的粘度。在一些实施例中，与前体源容器410A相关联的所述一个或多个加热单元414可配置为用于控制由贮存在前体源容器内的过渡金属卤化物化合物生成的蒸气压。在本公开的一些实施例中，过渡金属卤化物化合物可在高于25℃、或高于50℃、或甚至高于100℃的温度下具有高于0.01毫巴的蒸气压。在本公开的一些实施例中，过渡金属卤化物化合物可在低于350℃、或低于250℃、或低于200℃、或甚至低于150℃的温度下具有高于0.01毫巴的蒸气压。在本公开的一些实施例中，过渡金属卤化物化合物可在高于25℃、或甚至高于100℃的温度下具有高于0.1毫巴的蒸气压。在本公开的一些实施例中，过渡金属卤化物化合物可在低于400℃、或低于200℃、或甚至低于100℃的温度下具有高于0.1毫巴的蒸气压。在本公开的一些实施例中，过渡金属卤化物化合物可在高于25℃、或甚至高于100℃的温度下具有高于1毫巴的蒸气压。例如，可将过渡金属卤化物化合物加热到高于150℃的温度，从而生成高于0.001毫巴的蒸气压。
在一些实施例中，贮存在前体源容器410A内的过渡金属卤化物416可包含氯化钴(TMEDA)或氯化镍(TMEDA)中的至少之一。在一些实施例中，贮存在前体源容器410A内的过渡金属卤化物416可包含碘化钴(TMEDA。在一些实施例中，贮存在前体源容器410A内的过渡金属卤化物416可包含。另外，在一些实施例中，贮存在前体源容器410A内的过渡金属卤化物416可包含氯化钴(TMPDA)和氯化镍(TMPDA)。
在本公开的一些实施例中，气相通道418可连接到前体源容器410A使得一种或多种载气可经由气相通道418从载气贮存容器(未示出)输送到前体源容器中。在一些实施例中，可将质量流量控制器(未示出)布置在气相通道418上并靠近前体源容器410A设置。例如，可校准质量流量控制器以控制进入前体源容器410A的载气的质量通量，从而允许更好地控制过渡金属卤化物化合物蒸气从前体源容器410A流出并进入反应腔室402的后续流动。
在一些实施例中，载气(例如，氢气、氮气、氦气、氩气及其混合物)可在过渡金属卤化物化合物416的暴露表面上方流动，从而从过渡金属卤化物化合物416拾取一部分蒸气并与载气一道将过渡金属卤化物化合物输送到反应腔室402。在本公开的替代实施例中，载气可例如由任选的气相通道418`通过过渡金属卤化物化合物416“鼓泡”，从而搅动和拾取过渡金属卤化物化合物416的一部分并经由气体导管412A将过渡金属卤化物化合物蒸气输送到反应腔室402。
在本公开的一些实施例中，气相沉积装置400可包括另外的前体源容器和一个或多个用于惰性吹扫气体的源容器。例如，前体源容器410B可配置为容纳第二气相反应物，例如氧前体、氮前体、硫前体、硒前体、磷前体、硼前体、硅前体或还原剂中的一者或多者。容纳在前体源容器410B中的第二气相反应物可经由气体导管412B输送到反应腔室402。在一些实施例中，前体源容器410B还可具有用于控制贮存在前体源容器410B内的前体的温度的关联加热器414。另外，可利用源容器410C来容纳惰性吹扫气体，例如但不限于氩气(Ar)、氮气(N2)或氦气(He)。尽管气相沉积系统400包括三个源容器，但应理解，可配置含有另一化学前体的另一源容器与反应腔室402一起使用。
在本公开的一些实施例中，气相沉积装置400还可包括系统操作和控制机构420，其提供电子电路和机械部件以选择性地操作阀、歧管、泵以及与气相沉积装置400相关联的其他设备。这样的电路和部件用以从相应的前体源容器410A、410B和吹扫气体容器410C引入前体、吹扫气体。系统操作和控制机构420还可控制气体脉冲序列的时序、衬底和反应腔室的温度、反应腔室的压力以及提供气相沉积装置400的适当操作所必需的各种其他操作。操作和控制机构420可包括控制软件和电控制或气动控制的阀以控制前体、反应物和吹扫气体进出反应腔室402的流动。控制系统可包括执行某些任务的模块，如软件和/或硬件部件，例如FPGA或ASIC。模块可有利地配置为位于控制系统的可寻址存储介质上并配置为执行一个或多个工艺。
相关领域技术人员应理解，本发明的气相沉积装置的其他配置是可能的，包括不同数目和种类的前体反应物源和吹扫气体源。此外，相关领域技术人员还应理解，存在阀、导管、前体源、吹扫气体源的许多布置，其可用来实现向反应腔室402中选择性地进给气体的目标。此外，作为气相沉积装置的示意性图示，为了简化说明，省去了许多部件，这样的部件可包括例如各种阀、歧管、纯化器、加热器、容器、通风孔和/或旁路。
可利用图4的气相沉积装置400来向气相沉积工具供给包含二齿含氮加合物配体的过渡金属卤化物化合物。所述方法可包括：提供配置为用于容纳过渡金属卤化物化合物的前体源容器；将前体源容器流体连接到反应腔室；将前体源容器中容纳的过渡金属卤化物化合物加热到高于150℃的温度；产生至少0.001毫巴的过渡金属卤化物化合物蒸气压；和向反应腔室供给过渡金属卤化物化合物。在本公开的一些实施例中，过渡金属卤化物化合物可在高于25℃、或高于50℃、或甚至高于100℃的温度下具有高于0.01毫巴的蒸气压。在本公开的一些实施例中，过渡金属卤化物化合物可在低于350℃、或低于250℃、或低于200℃、或甚至低于150℃的温度下具有高于0.01毫巴的蒸气压。在本公开的一些实施例中，过渡金属卤化物化合物可在高于25℃、或甚至高于100℃的温度下具有高于0.1毫巴的蒸气压。在本公开的一些实施例中，过渡金属卤化物化合物可在低于400℃、或低于200℃、或甚至低于100℃的温度下具有高于0.1毫巴的蒸气压。在本公开的一些实施例中，过渡金属卤化物化合物可在高于25℃、或甚至高于100℃的温度下具有高于1毫巴的蒸气压。
在一些实施例中，过渡金属卤化物化合物可包含氯化钴(TMEDA)或氯化镍(TMPDA)中的至少之一。
上文所描述的本公开的实例实施例不限制本发明的范围，因为这些实施例仅仅是本发明实施例的实例，本发明由所附权利要求书和其合法等效物限定。任何等同的实施例均意在包括在本发明的范围内。实际上，所属领域的技术人员根据说明书可以清楚了解除本文中所展示和描述的内容外的对本公开的各种修改，如所描述要素的替代性适用组合。这样的修改和实施例也意在落在附随的权利要求书的范围内。

Claims (28)

1.一种通过循环沉积工艺在衬底上形成含过渡金属的膜的方法，所述方法包括：
使所述衬底与第一气相反应物接触，所述第一气相反应物包含过渡金属卤化物化合物，所述过渡金属卤化物化合物包含二齿含氮加合物配体；以及
使所述衬底与第二气相反应物接触。
2.根据权利要求1所述的方法，其中所述加合物配体包含两个氮原子，每个氮原子与至少一个碳原子键合。
3.根据权利要求1所述的方法，其中所述过渡金属卤化物化合物包含过渡金属氯化物。
4.根据权利要求3所述的方法，其中所述过渡金属氯化物化合物包含氯化钴、氯化镍或氯化铜中的至少之一。
5.根据权利要求4所述的方法，其中所述过渡金属氯化物化合物包含氯化钴(TMEDA)或氯化镍(TMPDA)中的至少之一。
6.根据权利要求1所述的方法，其中所述第二气相反应物包含氧前体，所述氧前体选自臭氧(O3)、分子氧(O2)、氧原子(O)、氧等离子体、氧自由基、氧激发物种、水(H2O)和过氧化氢(H2O2)。
7.根据权利要求6所述的方法，其中所述含过渡金属的膜包含过渡金属氧化物。
8.根据权利要求7所述的方法，其中所述过渡金属氧化物基本上包含氧化钴(II)(CoO)。
9.根据权利要求7所述的方法，所述方法还包括使所述过渡金属氧化物与还原剂前体接触，从而形成元素过渡金属。
10.根据权利要求9所述的方法，其中所述还原剂前体包含合成气体(H2+N2)、氨气(NH3)、肼(N2H4)、分子氢(H2)、氢原子(H)、氢等离子体、氢自由基、氢激发物种、醇、醛、羧酸、硼烷或胺中的至少之一。
11.根据权利要求1所述的方法，所述方法还包括使所述衬底与第三气相反应物接触，所述第三气相反应物包含选自以下的还原剂前体：叔丁基肼(C4H12N2)、氢气(H2)、氢(H2)等离子体、氨气(NH3)、氨(NH3)等离子体、肼(N2H4)、硅烷(SiH4)、乙硅烷(Si2H6)、丙硅烷(Si3H8)、锗烷(GeH4)、乙锗烷(Ge2H6)、硼烷(BH3)和乙硼烷(B2H6)。
12.根据权利要求1所述的方法，其中所述含过渡金属的膜包含元素钴、元素镍或元素铜中的至少之一。
13.根据权利要求1所述的方法，其中所述循环沉积工艺包括原子层沉积工艺。
14.根据权利要求1所述的方法，其中所述循环沉积工艺包括循环化学气相沉积工艺。
15.根据权利要求1所述的方法，其中所述含过渡金属的膜包含元素过渡金属、过渡金属氮化物、过渡金属硅化物、过渡金属硫化物、过渡金属硒化物、过渡金属磷化物或过渡金属硼化物中的至少之一。
16.一种通过循环沉积工艺在衬底上形成含过渡金属的膜的方法，所述方法包括：
使所述衬底与第一气相反应物接触，所述第一气相反应物包含过渡金属化合物，所述过渡金属化合物包含加合物形成配体；以及
使所述衬底与第二气相反应物接触；
其中所述过渡金属选自铜(Cu)、镍(Ni)和钴(Co)。
17.根据权利要求16所述的方法，其中所述加合物形成配体包含氮、磷、氧或硫中的至少之一。
18.根据权利要求16所述的方法，其中所述过渡金属化合物包含过渡金属卤化物化合物，所述过渡金属卤化物化合物选自过渡金属氯化物、过渡金属碘化物、过渡金属氟化物或过渡金属溴化物。
19.根据权利要求18所述的方法，其中所述过渡金属卤化物化合物包含二齿氮加合物形成配体。
20.根据权利要求16所述的方法，其中所述过渡金属化合物包含氯化钴(TMEDA)、溴化钴(TMEDA)、碘化钴(TMEDA)、氯化钴(TMPDA)或氯化镍(TMPDA)中的至少之一。
21.根据权利要求16所述的方法，其中包含加合物形成配体的所述过渡金属化合物利用一步合成工艺合成，所述一步合成工艺包括在低于50℃的温度下合并过渡金属卤化物化合物与加合物形成配体。
22.根据权利要求16所述的方法，其中所述第二气相反应物包含氧前体、氮前体、硅前体、硫前体、硒前体、磷前体、硼前体或还原剂中的至少之一。
23.一种器件结构，所述器件结构包括根据权利要求1所述的方法形成的含过渡金属的膜。
24.一种向反应腔室供给过渡金属卤化物化合物的方法，其中所述过渡金属卤化物化合物包含二齿含氮加合物配体，所述方法包括：
提供配置为用于容纳所述过渡金属卤化物化合物的前体源容器；
将所述前体源容器流体连接到所述反应腔室；
将所述前体源容器中容纳的所述过渡金属卤化物化合物加热到高于50℃的温度；
产生至少0.001毫巴的所述过渡金属卤化物化合物蒸气压；以及
向所述反应腔室供给所述过渡金属卤化物化合物。
25.根据权利要求24所述的方法，其中所述过渡金属卤化物化合物包含氯化钴(TMEDA)、氯化镍(TMPDA)中的至少之一。
26.一种利用反应性挥发性化学品的气相沉积装置，所述装置包含：
反应腔室；
设置在所述反应腔室中的衬底；
与所述反应腔室流体连通的前体源容器；和
设置在所述前体源容器中的过渡金属卤化物化合物，所述过渡金属卤化物化合物包含二齿含氮加合物配体。
27.根据权利要求26所述的装置，其中所述过渡金属卤化物化合物包含氯化钴(TMEDA)或氯化镍(TMPDA)中的至少之一。
28.根据权利要求26所述的装置，其中所述过渡金属化合物在低于150℃的过渡金属化合物温度下表现出高于0.001毫巴的蒸气压。
CN201980011788.7A 2018-02-15 2019-02-11 通过循环沉积工艺在衬底上形成含过渡金属的膜的方法、向反应腔室供给过渡金属卤化物化合物的方法以及相关的气相沉积装置 Pending CN111684105A (zh)

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