CN111197159A - 通过循环沉积工艺在衬底上沉积过渡金属硫族化物膜的方法 - Google Patents

通过循环沉积工艺在衬底上沉积过渡金属硫族化物膜的方法 Download PDF

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CN111197159A
CN111197159A CN201911099680.6A CN201911099680A CN111197159A CN 111197159 A CN111197159 A CN 111197159A CN 201911099680 A CN201911099680 A CN 201911099680A CN 111197159 A CN111197159 A CN 111197159A
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transition metal
precursor
film
deposition
less
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M·马蒂内恩
M·瑞塔拉
M·雷斯克拉
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ASM IP Holding BV
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ASM IP Holding BV
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Abstract

公开了通过循环沉积工艺在衬底上沉积过渡金属硫族化物膜的方法。所述方法可以包括使所述衬底与含有至少一种过渡金属的气相反应物接触，所述含有至少一种过渡金属的气相反应物包含铪前体或锆前体中的至少一种；以及使所述衬底与含有至少一种硫族化物的气相反应物接触，其中所述衬底在接触步骤期间的温度低于约450℃。还提供了包括通过本公开的方法沉积的过渡金属硫族化物膜的半导体装置结构。

Description

通过循环沉积工艺在衬底上沉积过渡金属硫族化物膜的方法
联合研究协议的合作对象
本文中要求保护的本发明是根据或代表和/或结合赫尔辛基大学(theUniversity of Helsinki)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
本公开大体上涉及通过循环沉积工艺在衬底上沉积过渡金属硫族化物膜的方法，且尤其涉及包含铪或锆的过渡金属硫族化物的循环沉积。本公开还涉及包括通过循环沉积工艺沉积的过渡金属硫族化物膜的半导体装置结构。
背景技术
近年来，二维(2D)材料由于在改善新一代电子装置的性能方面的潜力而引起广泛关注。例如，石墨烯是迄今研究最多的2D材料并且展现出高迁移率、透射率、机械强度和柔性。不过，纯石墨烯中带隙的缺乏限制了其在半导体装置结构，如晶体管中的性能。石墨烯的此类限制激励了作为石墨烯类似物的替代性2D材料的研究。近来，以过渡金属硫族化物，且尤其是过渡金属二硫族化物作为石墨烯的替代选择引起了相当大的研究关注。过渡金属二硫族化物可以具有MX2的化学计算量，其描述过渡金属(M)被夹在两层硫族元素原子(X)之间，并且在金属-硫族元素之间具有较强的平面内共价键且在各层之间具有较弱的平面外范德华键(van der Waals bonding)。
然而，用于制造2D材料的可缩放的低温方法极少。目前，机械剥离块状晶体是最常用的形成方法，不过，尽管这种方法制造出质量良好的晶体，但所述方法无法制造出连续膜并且劳动量非常大，使得此类方法不适用于工业制造。化学气相沉积(CVD)已被用于沉积2D材料，但目前用于一些金属硫族化物，如二硫化铪(HfS2)的CVD工艺的操作温度在900℃与1000℃之间，而且无法制造出连续的大面积2D材料。
因此，需要能够在较低沉积温度下且在原子水平上控制膜厚度下制造出2D材料的方法。
发明内容
提供本概述是为了以简化的形式引入一系列概念。下文在本公开的示例性实施例的详细描述中更详细地描述这些概念。本概述不打算标识所要求保护的主题的关键特征或必要特征，也不打算用于限制所要求保护的主题的范围。
在一些实施例中，提供了通过循环沉积工艺在衬底上沉积过渡金属硫族化物膜的方法。所述方法可包含：使所述衬底与含有至少一种过渡金属的气相反应物接触，所述含有至少一种过渡金属的气相反应物包含铪前体或锆前体中的至少一种；以及使所述衬底与含有至少一种硫族化物的气相反应物接触，其中所述衬底在接触步骤期间的温度低于约450℃。
本公开的实施例还提供了包含通过本文中所描述的方法沉积的过渡金属硫族化物膜的半导体装置结构。
出于概述本发明以及所实现的优于现有技术的优势的目的，上文中描述了本发明的某些目的和优势。当然，应当理解，未必所有这些目的或优势都可以根据本发明的任何特定实施例来实现。因此，例如，所属领域的技术人员将认识到，本发明可以按实现或优化如本文中所教示或建议的一种优势或一组优势但不一定实现如本文中可能教示或建议的其它目的或优势的方式来实施或进行。
所有这些实施例都旨在落入本文中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是工艺流程图，示出了根据本公开的实施例的示例性循环沉积方法；
图2示出了根据本公开的实施例在各种沉积温度下沉积的示例性铪硫族化物膜的生长速率、结晶度和组成；
图3示出了根据本公开的实施例在各种沉积温度下沉积的示例性锆硫族化物膜的生长速率、结晶度和组成；
图4示出了根据本公开的实施例在各种沉积温度下沉积的示例性铪硫族化物膜的掠入射x射线衍射(GIXRD)数据；
图5示出了根据本公开的实施例在各种沉积温度下沉积的示例性锆硫族化物膜的掠入射x射线衍射(GIXRD)数据；
图6示出了根据本公开的实施例的裸锆硫族化物膜和覆盖有金属硅酸盐覆盖层的锆硫族化物膜两者随时间推移的环境稳定性；
图7A示出了根据本公开的实施例的利用不同数目的沉积循环沉积且硫族化物膜上方没有沉积覆盖层的示例性锆硫族化物膜的掠入射x射线衍射(GIXRD)数据；
图7B示出了根据本公开的实施例的利用不同数目的沉积循环沉积且硫族化物膜上方沉积覆盖层的示例性锆硫族化物膜的掠入射x射线衍射(GIXRD)数据；
图8示出了包括根据本公开的实施例沉积的过渡金属硫族化物膜的示例性半导体装置结构；
图9示出了可以根据本公开的实施例用于沉积过渡金属硫族化物膜的示例性反应系统。
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。
如本文中所使用，术语“衬底”可以指可以使用的，或在上面可以形成装置、电路或膜的任何底层材料。
如本文所使用，术语“循环沉积”可以指将前体(反应物)依序引入反应室中以在衬底上方沉积膜并且包括沉积技术，如原子层沉积和循环化学气相沉积。
如本文中所使用，术语“原子层沉积(ALD)”可以指在处理室中进行沉积循环，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，将前体用化学方法吸附到沉积表面(例如衬底表面或先前沉积的底层表面，如来自先前ALD循环的材料)，由此形成不易与额外前体反应的单层或亚单层(即，自限性反应)。此后，必要时，可以随后将反应物(例如另一种前体或反应气体)引入到处理室中，以用于将用化学方法吸附的前体转换成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，在每个循环期间，还可以利用吹扫步骤以在转换用化学方法吸附的前体之后从处理室移除过量前体和/或从处理室移除过量反应物和/或反应副产物。此外，当使用前体组合物、反应性气体和吹扫(例如惰性载体)气体的交替脉冲进行时，如本文所使用的术语“原子层沉积”还意图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。
如本文所使用，术语“循环化学气相沉积”可以指使衬底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/或分解以产生所需沉积。
如本文所使用，术语“含有硫族元素的气相反应物”可以指含有硫族元素的反应物(前体)，其中硫族元素是来自周期表第VI族的元素，包括硫、硒和碲。
如本文所使用，术语“膜”和“薄膜”可以指由本文所公开的方法沉积的任何连续或非连续结构和材料。举例来说，“膜”和“薄膜”可包括2D材料、纳米层合物、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/或分子的簇。“膜”和“薄膜”可以包含具有针孔的材料或层，但仍然是至少部分连续的。
如本文所使用，术语“2D材料”或“二维材料”可以指一个、两个或三个原子厚度的纳米级结晶材料。此外，“2D材料”或“二维材料”还可以指由每个单层约三个原子厚度的多个单层的结晶材料构成的有序纳米级结晶结构。
如本文所用，术语“卤化物前体”可以指包含包括氯、碘或溴中的至少一种的卤化物组分的过渡金属卤化物前体。
如本文所用，术语“金属有机前体”可以指过渡金属有机金属前体，其中“金属有机”或“有机金属”可互换使用，并且可以指含有金属物种的有机化合物。有机金属化合物可被认为是具有直接金属-碳键的金属有机化合物亚类。
在本公开的整个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。
本公开的实施例可包括用于通过循环沉积工艺在衬底上沉积过渡金属硫族化物的方法，且特别是通过原子层沉积工艺沉积包含铪组分或锆组分的过渡金属硫族化物膜的方法。作为非限制性实例，二硫化铪(HfS2)和二硫化锆(ZrS2)是新兴的材料，具有2D晶体结构，类似于众所周知的过渡金属二硫族化物(TMDC)，例如二硫化钼(MoS2)。与被研究最多的2D材料石墨烯相比，二硫化铪和二硫化锆可具有可调整大小的带隙，这使得此类示例性过渡金属硫族化物膜更适合于半导体装置结构，如场效应晶体管(FET)。
当前用于形成过渡金属硫族化物膜的方法不适于形成高质量、共形、低温薄膜。过渡金属硫族化物晶体可通过机械剥离块状过渡金属硫族化晶体而形成，但此类方法不适合于在合适的衬底上以原子级的厚度精度形成过渡金属硫族化物膜。此外，已展示出一些过渡金属硫族化物膜的化学气相沉积，但此类工艺上在高沉积温度(例如，对于HfS2高于900℃)下操作并且不适合制造纳米级共形薄膜。
循环沉积方法，如循环化学气相沉积和原子层沉积技术，本质上是可缩放的并且提供原子级准确膜厚度控制，这对于沉积高质量2D材料至关重要。此外，具有反应表面控制的循环沉积方法，如原子层沉积，在特征上是共形的，由此能够均匀地涂布三维结构。
另外，过渡金属硫族化物膜在沉积工艺期间或在暴露于环境条件下可能易于氧化。因此，循环沉积方法可能是合乎需要的，其在沉积期间不将过渡金属氧化物相并入到硫族化物膜中。另外，对于防止过渡金属硫族化物膜在暴露于环境条件下时氧化，方法极为合乎需要。
因此，需要能够在低温下、保形地且以原子级厚度准确度沉积过渡金属硫族化物膜的方法。此外，包含过渡金属硫族化物膜的半导体装置结构是合乎需要的。
循环沉积工艺的非限制性示例性实施例可以包括ALD，其中ALD通常是基于自限性反应，由此每个沉积循环，使用反应物的依序和交替脉冲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，交替脉冲的反应物的每个循环通常留下所需材料的不超过约一个单层。然而，如上文所提到的，熟练技术人员应认识到，在一个或多个ALD循环中可以沉积材料的超过一个单层，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。
在用于沉积过渡金属硫族化物膜的ALD型工艺中，一个沉积循环可以包含：使衬底暴露于第一气相反应物，从反应空间去除任何未反应的第一反应物和反应副产物，以及使衬底暴露于第二气相反应物，随后进行第二去除步骤。第一反应物可以包含含有过渡金属的前体，如铪前体或锆前体，并且第二反应物可以包含含有硫族元素的前体。
前体可以利用如氩气(Ar)或氮气(N2)的惰性气体分离，以防止反应物之间发生气相反应并实现自饱和表面反应。然而，在一些实施例中，可以移动衬底以分别接触第一气相反应物和第二气相反应物。由于所述反应自饱和，故可能不需要对衬底进行严格的温度控制以及对前体进行精确的剂量控制。不过，衬底温度优选地使得附带的气体物种既不冷凝成单层，也不在衬底表面上分解。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，从衬底表面去除过剩的化学品和反应副产物(如果存在的话)。可以借助于惰性吹扫气体从反应空间中有效地排出不合需要的气态分子。可以使用真空泵来辅助吹扫程序。
能够用于沉积或生长薄膜的反应器可以被用来进行沉积。此类反应器包括ALD反应器以及配备有用于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。在一些实施例中，反应器是空间ALD反应器，在所述反应器中，衬底在加工期间移动或旋转。
在一些实施例中，可以使用间歇反应器。在一些实施例中，利用供舟皿在加工期间旋转的竖直式间歇反应器。因此，在一些实施例中，晶片在加工期间旋转。在其它实施例中，间歇反应器包含被配置成容纳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2个晶片的小型间歇反应器。在使用间歇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％。
本文中所描述的沉积工艺可以任选地在连接到丛集工具的反应器或反应室中进行。在丛集工具中，因为每一个反应室专门用于一种工艺类型，故每个模块中反应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，有可能减少将反应空间用泵增压到衬底之间所需的工艺压力水平的时间。
独立反应器可配备装载锁。在此情况下，不必在每次运行之间冷却反应室。在一些实施例中，用于沉积包含过渡金属硫族化物膜的膜的沉积工艺可以包含多个沉积循环，例如ALD循环。
在一些实施例中，使用循环沉积工艺在衬底上沉积过渡金属硫族化物膜，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。例如，在一些实施例中，相较于CVD工艺，ALD工艺的沉积速率可能较低。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衬底温度下操作，从而引起化学气相沉积工艺，但仍利用前体的依序引入，此类工艺可被称作循环CVD。在一些实施例中，循环CVD工艺可包含向反应室中引入两种或更多种前体，其中反应室中所述两种或更多种前体之间可能存在重叠的时间段，从而产生ALD沉积组分和CVD沉积组分。例如，循环CVD工艺可包含进入反应室内的第一前体的连续流动和第二前体的周期性脉冲。
根据本公开的一些实施例，使用ALD工艺在如集成电路工件的衬底上沉积过渡金属硫族化物膜。在一些实施例中，每一个ALD循环可以包含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，期望在其上进行沉积的衬底表面与用化学方法吸附到衬底表面上的第一气相反应物接触，所述第一气相反应物包含铪前体或锆前体中的至少一种，从而在衬底的表面上形成反应物物种的不超过约一个单层。在沉积循环的第二阶段(“硫族元素阶段”)中，使期望在上面进行沉积的衬底表面接触与先前用化学方法吸附的物种反应的第二气相反应物，所述第二气相反应物包含含有至少一种硫族元素的气相反应物，从而形成过渡金属硫族化物膜。
在本公开的一些实施例中，所述含有过渡金属的气相反应物包含铪前体或锆前体中的至少一种。在一些实施例中，铪前体或锆前体包含卤化物前体或金属有机前体中的至少一种。在一些实施例中，所述金属有机前体可以包含烷基酰胺前体或含有环戊二烯基配体的前体中的至少一种。在一些实施例中，铪前体或锆前体可包含混配前体。
在一些实施例中，铪前体可包含铪卤化物前体、铪金属有机前体或有机金属铪前体中的至少一种。
在一些实施例中，铪卤化物前体可以包含至少一个卤化物配体，而其余的配体是不同的，如本文稍后所述的金属有机或有机金属配体。在一些实施例中，铪卤化物前体可包含一个、两个、三个或四个卤化物配体，如氯化物配体。
在一些实施例中，铪卤化物前体可以包含氯化铪、碘化铪或溴化铪中的至少一种。在一些实施例中，氯化铪可包含四氯化铪(HfCl4)。在一些实施例中，碘化铪可包含四碘化铪(HfI4)。在一些实施例中，溴化铪可包含四溴化铪(HfBr4)。
在一些实施例中，铪金属有机前体可包含铪烷基酰胺前体、含有铪环戊二烯基配体的前体或其它金属有机铪前体中的至少一种。
在一些实施例中，铪烷基酰胺前体可以选自包含以下的群组：四(乙基甲基酰胺基)铪(Hf(NEtMe)4)、四(二甲基酰胺基)铪(Hf(NMe2)4)或四(二乙基酰胺基)铪(Hf(NEt2)4)。
在本公开的一些实施例中，含有铪环戊二烯基配体的前体可以选自包含以下的群组：(三(烷基酰胺基)环戊二烯基铪，如(三(二甲基酰胺基)环戊二烯基铪HfCp(NMe2)3、或双(甲基环戊二烯基)甲氧基甲基铪(MeCp)2Hf(CH)3(OCH3)或那些前体的衍生物，如其中一个或多个碳氢化合物(如烷基)连接到那些前体的环戊二烯基配体、或烷基酰胺基配体中的其它烷基的前体。
在一些实施例中，铪前体可具有式；
HfL1L2L3L4
其中经由L1-L4的每个L配体可以独立地选择为
a)卤化物，如氯化物、溴化物或碘化物
b)烷基酰胺基，如二甲基酰胺基(-NMe2)、二乙基胺基(-NEt2)、乙基甲基酰胺基(-NEtMe)
c)脒基，如N,N'-二甲基甲脒基
d)胍基，如N,N'-二异丙基-2-乙基甲基酰胺基胍基
e)环戊二烯基或那些的衍生物，如环戊二烯基或甲基环戊二烯基或其它烷基取代的环戊二烯基配体
f)环庚二烯基或环庚三烯基类，如环庚三烯基或环庚二烯基
g)烷基，如C1-C5烷基，例如甲基，主要在混配前体的情况下
h)醇盐，如甲醇盐(-OMe)、乙醇盐(-OEt)、异丙醇盐(-OiPr)、正丁醇盐(-OBu)或叔丁醇盐(-OtBu)
i)β二酮化物，如(2,2,6,6-四甲基-3,5-庚二酮基)(thd)
j)供体官能化醇盐，如二甲基乙醇胺
在本公开的一些实施例中，铪前体包含经由氮和/或氧原子键合于Hf的一个或多个双齿配体。在一些实施例中，铪前体包含经由氮、氧和/或碳键合于Hf的一个或多个配体。
在一些实施例中，锆前体可包含锆卤化物前体、锆金属有机前体或有机金属锆前体中的至少一种。
在一些实施例中，锆卤化物前体可以包含氯化锆、碘化锆或溴化锆中的至少一种。在一些实施例中，氯化锆可包含四氯化锆(ZrCl4)。在一些实施例中，锆卤化物前体可以包含至少一个卤化物配体，而其余的配体是不同的，如本文稍后所述的金属有机或有机金属配体。在一些实施例中，锆卤化物前体可包含一个、两个、三个或四个卤化物配体，如氯化物配体。在一些实施例中，碘化锆可包含四碘化锆(ZrI4)。在一些实施例中，溴化锆可包含四溴化锆(ZrBr4)。
在一些实施例中，锆金属有机前体可包含锆烷基酰胺前体、含有锆环戊二烯基配体的前体或其它金属有机锆前体中的至少一种。
在一些实施例中，锆烷基酰胺前体可以选自包含以下的群组：四(乙基甲基酰胺基)锆(Zr(NEtMe)4)、四(二甲基酰胺基)锆(Zr(NMe2)4)或四(二乙基酰胺基)锆(Zr(NEt2)4)。
在本公开的一些实施例中，含有锆环戊二烯基配体的前体可以选自包含以下的群组：(三(烷基酰胺基)环戊二烯基锆，如(三(二甲基酰胺基)环戊二烯基锆ZrCp(NMe2)3、或双(甲基环戊二烯基)甲氧基甲基锆(MeCp)2Zr(CH)3(OCH3)或那些前体的衍生物，如其中一个或多个碳氢化合物(如烷基)连接到那些前体的环戊二烯基配体、或烷基酰胺基配体中的其它烷基的前体。
在一些实施例中，锆前体可具有式；
ZrL1L2L3L4
其中经由L1-L4的每个L配体可以独立地选择为
k)卤化物，如氯化物、溴化物或碘化物
l)烷基酰胺基，如二甲基酰胺基(-NMe2)、二乙基胺基(-NEt2)、乙基甲基酰胺基(-NEtMe)
m)脒基，如N,N'-二甲基甲脒基
n)胍基，如N,N'-二异丙基-2-乙基甲基酰胺基胍基
o)环戊二烯基或那些的衍生物，如环戊二烯基或甲基环戊二烯基或其它烷基取代的环戊二烯基配体
p)环庚二烯基或环庚三烯基类，如环庚三烯基或环庚二烯基
q)烷基，如C1-C5烷基，例如甲基，主要在混配前体的情况下
r)醇盐，如甲醇盐(-OMe)、乙醇盐(-OEt)、异丙醇盐(-OiPr)、正丁醇盐(-OBu)或叔丁醇盐(-OtBu)
s)β二酮化物，如(2,2,6,6-四甲基-3,5-庚二酮基)(thd)
t)供体官能化醇盐，如二甲基乙醇胺
在本公开的一些实施例中，锆前体包含经由氮和/或氧原子键合于Zr的一个或多个双齿配体。在一些实施例中，锆前体包含经由氮、氧和/或碳键合于Zr的一个或多个配体。
在一些实施例中，使衬底暴露于含有过渡金属的气相反应物可以包含在衬底上方对过渡金属前体进行脉冲，持续在约0.01秒与约60秒之间、在约0.05秒与约10秒之间或在约0.1秒与约5.0秒之间的时段。此外，在衬底上方对过渡金属前体进行脉冲期间，过渡金属前体的流动速率可以小于2000sccm、或小于500sccm、或甚至小于100sccm。此外，在衬底上方对过渡金属前体进行脉冲期间，过渡金属前体的流动速率可以是约1到约2000sccm、约5到约1000sccm或约10到约500sccm。
在一些实施例中，含有过渡金属的气相反应物的纯度可以影响所沉积膜的组成，并且因此可以利用含有过渡金属的气相反应物的高纯度源。例如，在一些实施例中，过渡金属气相反应物可以包含具有大于或等于99.99％的纯度的铪前体或锆前体。
在一些实施例中，含有过渡金属的气相反应物可以容纳于容器中，并且一个或多个加热器可以与所述容器相关联以控制所述金属前体的温度并且随后对所述金属前体的分压进行控制。在本公开的一些实施例中，所述容器内的所述金属前体可以被加热到介于约20℃与约300℃之间的温度。在一些实施例中，所述金属前体可以被加热到约30℃至约250℃、或约40℃至约225℃、或约50℃至约150℃的温度，取决于前体选择。
在一些实施例中，含有所述金属前体的容器可以连接到一种或多种载气源。载气可以被引入到容器中并且吸入到容器内所容纳的金属前体上或鼓泡通过容器内所容纳的金属前体。所引起的金属前体蒸发使得金属前体的蒸气变得夹带于载气中，进而产生可分配至反应室的过渡金属气相反应物。
在一些实施例中，除了使用高纯度过渡金属前体，载气可进一步纯化以去除不需要的杂质。因此，本公开的一些实施例可进一步包含：使载气流过容器，所述容器含有所述含有过渡金属的气相反应物的源，从而将含有过渡金属的气相反应物输送到所述反应室。本公开的其它实施例可以包含：在进入含有过渡金属的气相反应物的源之前使载体流过气体纯化器，从而降低载气中的水或氧气中的至少一种的浓度。
在一些实施例中，载气中的水浓度可以降低至低于百万分之十、或低于百万分之一、或低于十亿分之一百、或低于十亿分之十、或低于十亿分之一或甚至低于万亿分之一。
在一些实施例中，载气中的氧气浓度可以降低至百万分之十、或低于百万分之一、或低于十亿分之一百、或低于十亿分之十、或低于十亿分之一或甚至低于万亿分之一。
在一些实施例中，载气中的氢气(H2)浓度可降低至低于万亿分之一百。在一些实施例中，载气中的二氧化碳(CO2)浓度可降低至低于万亿分之一百。在一些实施例中，载气中的一氧化碳(CO)浓度可降低至低于万亿分之一百。
在一些实施例中，载气可包含氮气(N2)且载气纯化器可包括氮气纯化器。
在本公开的一些实施例中，含有过渡金属的气相反应物可以在进入反应室之前通过气体纯化器进料，以便降低含有过渡金属的气相反应物中的水或氧气中的至少一种的浓度。
在一些实施例中，含有过渡金属的气相反应物中的水浓度可以降低至低于1原子％、或低于百万分之一千、或低于百万分之一百、或低于百万分之十、或低于百万分之一、或低于十亿分之一百或甚至低于万亿分之一百。
在一些实施例中，含有过渡金属的气相反应物中的氧气浓度可以降低至低于1原子％、或低于百万分之一千、或低于百万分之一百、或低于百万分之十、或低于百万分之一、或低于十亿分之一百或甚至低于万亿分之一百。
不受任何理论或机制约束，但是据信载气和/或含有过渡金属的气相反应物中的水浓度或氧气浓度中的至少一种降低可允许以所需组成沉积过渡金属硫族化物膜，同时防止过渡金属氧化物相在适当沉积温度下沉积。
过量过渡金属气相反应物，如铪前体或锆前体和反应副产物(如果存在的话)可以例如通过泵送惰性气体而从衬底表面去除。举例来说，在本公开的一些实施例中，所述方法可包括其中衬底表面被吹扫不到约5.0秒、或不到约2.0秒或甚至不到约1.0秒的时间的吹扫循环。在一些实施例中，对衬底表面进行吹扫持续在约0.01秒与约60秒之间、或在约0.05秒与约10秒之间或在约0.1秒与约5秒之间的时段。可以借助于由泵送系统产生的真空来去除过量的过渡金属气相反应物和任何反应副产物。
在沉积循环的第二阶段(“硫族元素阶段”)中，使衬底与第二气相反应物接触，所述第二气相反应物包含含有至少一种硫族元素的气相反应物。在本公开的一些实施例中，含有至少一种硫族化物的气相反应物可以包含硫化氢(H2S)、硒化氢(H2Se)、二甲硫醚((CH3)2S)或二甲基碲((CH3)2Te)。
本领域的技术人员应了解，在本文所公开的循环沉积工艺中可以使用任意数量的硫族元素前体。在一些实施例中，硫族元素前体选自以下清单：H2S、H2Se、H2Te、(CH3)2S、(NH4)2S、二甲亚砜((CH3)2SO)、(CH3)2Se、(CH3)2Te、元素或原子S、Se、Te、含有硫族元素-氢键的其它前体，如H2S2、H2Se2、H2Te2或具有式R-Y-H的硫族醇，其中R可以是被取代或未被取代的烃，优选地是C1-C8烷基或被取代的烷基，如烷基硅烷基，更优选地是直链或支链C1-C5烷基，并且Y可以是S、Se或Te。在一些实施例中，硫族元素前体是具有式R-S-H的硫醇，其中R可以是被取代或未被取代的烃，优选地是C1-C8烷基，更优选直链或支链C1-C5烷基。在一些实施例中，硫族元素前体具有式(R3Si)2Y，其中R3Si是烷基硅烷基并且Y可以是S、Se或Te。在一些实施例中，硫族元素前体包含S或Se。在一些实施例中，硫族元素前体包含S。在一些实施例中，硫族元素前体不包含S。在一些实施例中，硫族元素前体可以包含元素硫族元素，如元素硫。在一些实施例中，硫族元素前体包含Te。在一些实施例中，硫族元素前体不包含Te。在一些实施例中，硫族元素前体包含Se。在一些实施例中，硫族元素前体不包含Se。在一些实施例中，硫族元素前体选自包含S、Se或Te的前体。在一些实施例中，硫族元素前体包含H2Sn，其中n是4到10。
在一些实施例中，合适的硫族元素前体可以包括任意数量的含硫族元素化合物。在一些实施例中，硫族元素前体可以包含至少一个硫族元素-氢键。在一些实施例中，硫族元素前体可以包含硫族元素等离子体、硫族元素原子或硫族元素自由基。在需要高能硫族元素前体的一些实施例中，可以在反应室中或反应室上游产生等离子体。在一些实施例中，硫族元素前体不包含高能硫族元素前体，如等离子体、原子或自由基。在一些实施例中，硫族元素前体可以包含由如H2S的含硫族元素-氢键的硫族元素前体形成的硫族元素等离子体、硫族元素原子或硫族元素自由基。在一些实施例中，硫族元素前体可以包含硫族元素等离子体、硫族元素原子或硫族元素自由基，如包含硫、硒或碲的等离子体，优选包含硫的等离子体。在一些实施例中，等离子体、原子或自由基包含碲。在一些实施例中，等离子体、原子或自由基包含硒。在一些实施例中，硫族元素前体不包含碲前体。
在一些实施例中，含有硫族元素的气相反应物的纯度可以影响所沉积膜的组成，并且因此可以利用含有硫族元素的气相反应物的高纯度源。在一些实施例中，含有硫族元素的气相反应物可具有大于或等于99.5％的纯度。作为非限制性实例，含有硫族元素的气相反应物可包含具有大于或等于99.5％的纯度的硫化氢(H2S)。
在一些实施例中，除了使用高纯度含有硫族元素的气相反应物，硫族元素前体气体可进一步纯化以去除不需要的杂质。因此，本公开的一些实施例可进一步包含：在进入反应室之前使含有硫族元素的气相反应物流过气体纯化器，从而降低含有硫族元素的气相反应物中的水或氧气中的至少一种的浓度。
在一些实施例中，含有硫族元素的气相反应物中的水或氧气浓度可以降低至低于5原子％、或低于1原子％、或低于百万分之一千、或低于百万分之一百、或低于百万分之十、或低于百万分之一、或低于十亿分之一百、或低于十亿分之十、或甚至低于十亿分之一。
不受任何理论或机制约束，但是据信含有硫族元素的气相反应物中的水浓度或氧气浓度中的至少一种降低可允许以所需组成沉积过渡金属硫族化物膜，同时防止过渡金属氧化物相在适当沉积温度下沉积。
在一些实施例中，使衬底暴露于含有硫族元素的气相反应物可以包含在衬底上方对硫族元素前体(例如硫化氢)进行脉冲，持续在0.1秒与2.0秒之间、或约0.01秒到约10秒、或不到约20秒、或不到约10秒、或不到约5秒的时段。在衬底上方对硫族元素前体进行脉冲期间，硫族元素前体的流动速率可以小于2000sccm、或小于500sccm、或甚至小于100sccm。此外，在衬底上方对硫族元素前体进行脉冲期间，硫族元素前体的流动速率可以是约1sccm到约2000sccm、或约5sccm到约1000sccm、或约10sccm到约500sccm。
包含含有硫族元素的前体的第二气相反应物可以与留在衬底上的含金属的分子反应。在一些实施例中，第二阶段硫族元素前体可以包含硫化氢，并且反应可以在衬底的表面上沉积过渡金属二硫化物。
可以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源化学品和反应副产物(如果存在的话)。吹扫气体优选地是任何惰性气体，如但不限于氩气(Ar)、氮气(N2)或氦气(He)。如果吹扫(即，吹扫气体脉冲)或其它反应物去除步骤介于两个阶段之间，那么一个阶段一般被视为紧接着另一阶段。
使衬底替代地与第一气相反应物(即，含有过渡金属的前体)和第二气相反应物(即，含有硫族元素的前体)接触的沉积循环可以重复一次或多次，直至沉积所需厚度的过渡金属硫族化物。应了解，在本公开的一些实施例中，衬底与第一气相反应物和第二气相反应物接触的次序可以是这样的：先使衬底与第二气相反应物接触，随后与第一气相反应物接触。此外，在一些实施例中，循环沉积工艺可以包含使衬底与第一气相反应物(即，含有过渡金属的前体)接触一次或多次，随后使衬底与第二气相反应物(即，含有硫族元素的前体)接触一次或多次，并且类似地，可以替代地包含使衬底与第二气相反应物接触一次或多次，随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。
本文所描述的利用含有过渡金属的前体和含有硫族元素的前体形成过渡金属硫族化物膜的循环沉积工艺可以在ALD或CVD沉积系统中，在加热的衬底的情况下进行，即，在衬底与化学前体接触的工艺期间，可以控制衬底的温度。
例如，在一些实施例中，方法可以包含将衬底加热到在约200℃与约500℃之间的温度，或甚至将衬底加热到在约350℃与约450℃之间的温度。当然，用于任何给定循环沉积工艺，如用于ALD反应的适当温度窗口将取决于所涉及的表面终止状态和反应物物种。这里，温度取决于所使用的前体而变化，并且通常处于或低于约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℃与约600℃之间，并且在一些实施例中，沉积温度在约300℃与约500℃之间。在一些实施例中，沉积温度低于约500℃，或低于约475℃，或低于约450℃，或低于约425℃或低于约400℃，或低于约375℃，或低于约350℃，或低于约325℃或低于约300℃。在某些情况下，例如，如果在所述工艺中使用额外的反应物或还原剂，那么沉积温度可以低于约250℃，或低于约200℃，或低于约150℃，或低于约100℃。在一些情况下，沉积温度可以高于约20℃、高于约50℃并且高于约75℃。在本公开的一些实施例中，沉积温度，即沉积期间衬底的温度，是约400℃。
在一些实施例中，过渡金属硫族化物膜的生长速率是约
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本公开的实施例可以包含循环沉积工艺，所述循环沉积工艺可以通过图1的示例性方法100更详细地示出。方法100可以工艺方块110开始，其包含向反应室中提供衬底以及将衬底加热至沉积温度。
在本公开的一些实施例中，衬底可包含平面衬底或者包括高纵横比特征如沟槽结构和/或鳍结构的图案化衬底。衬底可以包含一种或多种材料，包括但不限于硅(Si)、锗(Ge)、锗锡(GeSn)、硅锗(SiGe)、硅锗锡(SiGeSn)、碳化硅(SiC)，或III-V族半导体材料，例如砷化镓(GaAs)、磷化镓(GaP)或氮化镓(GaN)。在一些实施例中，衬底可包含一种或多种介电材料，包括但不限于氧化物、氮化物、或氮氧化物。例如，衬底可包含氧化硅(例如，SiO2)、金属氧化物(例如，Al2O3)、氮化硅(例如，Si3N4)或氮氧化硅。在本公开的一些实施例中，衬底可包含工程化衬底，其中表面半导体层安置在块体支撑件上方，其间安置有介入的隐埋氧化物(BOX)。
图案化衬底可以包含如下衬底，所述衬底可包括形成于衬底中或衬底表面上的半导体装置结构，例如图案化衬底可包含部分制造的半导体装置结构，例如晶体管和/或存储器元件。在一些实施例中，衬底可以含有单晶表面和/或一个或多个次表面，所述次表面可以包含非单晶表面，例如多晶表面和/或非晶表面。单晶表面可以包含例如以下中的一种或多种：硅(Si)、硅锗(SiGe)、锗锡(GeSn)、锗(Ge)或III-V族材料。多晶或非晶表面可以包括电介质材料，如氧化物、氧氮化物或氮化物，例如氧化硅和氮化硅。
用于示例性循环沉积工艺100的反应室可以是原子层沉积反应室或化学气相沉积反应室或如本文先前所述的任何反应室。在本公开的一些实施例中，反应室可以在将衬底装载于反应室内之前或在衬底预装载到反应室中的情况下经受预退火工艺。例如，预退火工艺可用于降低反应室中的水和/或氧中至少一种的浓度。因此，本公开的一些实施例可进一步包含在膜沉积之前在高于400℃、或高于500℃、或高于600℃或甚至高于700℃的温度下对反应室进行预退火。在一些实施例中，可以在不到60分钟、或不到30分钟、或不到15分钟、或不到10分钟、或甚至不到5分钟的时间段内进行高温下的反应室的预退火。
(图1的)工艺方块110可通过将衬底加热到所需沉积温度来继续，如本文先前所公开。作为非限制性实例，可将衬底加热到介于约300℃与约450℃之间的沉积温度，或加热到约400℃的温度。
示例性方法100可以循环沉积阶段140继续，所述循环沉积阶段140可借助于工艺方块120开始，所述工艺方块120包含使衬底与含有过渡金属的气相反应物接触，如本文先前所公开。作为非限制性实例，衬底可以与四氯化铪(HfCl4)或四氯化锆(ZrCl4)接触持续约1秒的时间段。在使衬底与含有过渡金属的前体接触后，可以通过吹扫/泵送工艺从反应室去除过量的含有过渡金属的前体和任何副产物。
示例性方法100的循环沉积阶段140可借助于工艺方块130继续，所述工艺方块130包含使衬底与含有硫族元素的气相反应物接触，如本文先前所公开。作为非限制性实例，衬底可以与硫化氢(H2S)接触持续约1秒的时间段。在使衬底与含有硫族元素的前体接触后，可以通过吹扫/泵送工艺从反应室去除过量的含有硫族元素的前体和任何副产物。
其中使衬底交替并依序与含有至少一种过渡金属的气相反应物接触并与含有至少一种硫族元素的气相反应物接触的方法可以构成一个单位沉积循环。例如，单位沉积循环可包含：使衬底与过渡金属气相反应物接触，吹扫反应室，使所述衬底与含有硫族元素的气相反应物接触，且再次吹扫反应室。
在本公开的一些实施例中，沉积过渡金属硫族化物的方法可以包含重复单位沉积循环一次或多次。例如，示例性方法100的循环沉积阶段140可借助于决策门150继续，所述决策门150判定示例性方法100的循环沉积阶段140是继续还是退出。工艺方块150的决策门可基于沉积的过渡金属硫族化物膜的厚度来判定。例如，如果过渡金属硫族化物膜的厚度不足以用于所需应用，那么示例性方法100的循环沉积阶段140可以返回到工艺方块120，并且使衬底与含有过渡金属的气相反应物接触以及使衬底与含有硫族元素的气相反应物接触的工艺可以重复一次或多次。在沉积过渡金属硫族化物膜达到所需厚度后，示例性方法100就可以经由工艺方块160退出，并且过渡金属硫族化物膜可以经历额外的工艺以形成装置结构。
在本公开的一些实施例中，过渡金属硫族化物膜的沉积温度可影响硫族化物膜的生长速率、硫族化物膜的结晶度和硫族化物膜的组成。作为非限制性实例，图2示出了利用四氯化铪(HfCl4)和硫化氢(H2S)作为前体化学品在各种沉积温度下沉积的示例性二硫化铪膜的生长速率、结晶度和组成。图2的检验示出了在约200℃的沉积温度到约350℃沉积之间，示例性二硫化铪膜的沉积速率减小，并且二硫化铪膜的晶体结构是非晶的，即，没有通常与结晶材料有关的晶体结构的长程有序度。在约350℃与约400℃的沉积温度之间，示例性二硫化铪膜的生长速率提高，且二硫化铪膜的晶体结构变得结晶，即，存在硫族化物膜的结晶结构的长程有序度。另外，在约350℃与约400℃的沉积温度之间，示例性二硫化铪膜表现出二硫化铪(HfS2)的组成。然而，随着沉积温度进一步升高高于约400℃的温度，示例性膜的生长速率再次降低，并且所沉积膜的组成变成硫化铪与氧化铪之间的混合物。在以上非限制性实例中利用的反应室中剩余的残余氧和/或水可能产生高于约400℃温度的氧化铪相沉积。在另外的非限制性实例中，反应室内的残余氧和/或水浓度可进一步降低，并且沉积高于约400℃的温度可引起二硫化铪(HfS2)膜沉积，而不沉积氧化铪相。
因此，在本公开的一些实施例中，过渡金属硫族化物膜可以包含硫化铪，且特别是二硫化铪(HfS2)。另外，在一些实施例中，过渡金属硫族化物膜可以与包含二硫化铪(HfS2)的组合物在约350℃与约400℃之间的沉积温度下、且特别是在约400℃的沉积温度下结晶。在一些实施例中，结晶二硫化铪(HfS2)膜可以在高于400℃的沉积温度下沉积。
作为另一非限制性实例，图3示出了利用四氯化锆(ZrCl4)和硫化氢(H2S)作为前体化学品在各种沉积温度下沉积的示例性硫化锆膜的生长速率、结晶度和组成。图3的检验示出了在约200℃的沉积温度到约350℃沉积之间，示例性硫化锆膜的沉积速率减小，并且硫化锆膜的晶体结构是非晶的，即，没有通常与结晶材料有关的晶体结构的长程有序度。在约350℃与约400℃的沉积温度之间，示例性硫化锆膜的生长速率提高，且硫化锆膜的晶体结构变得结晶，即，存在硫族化物膜的结晶结构的长程有序度。另外，在约350℃与约400℃的沉积温度之间，示例性硫化锆膜表现出二硫化锆(ZrS2)的组成。然而，随着沉积温度进一步升高高于约400℃的温度，示例性膜的生长速率初始降低，并且接着再次升高，且所沉积膜的组成变成硫化锆与氧化锆之间的混合物。在以上非限制性实例中利用的反应室中剩余的残余氧和/或水可能产生高于约400℃温度的氧化锆相沉积。在另外的非限制性实例中，反应室内的残余氧和/或水浓度可进一步降低，并且沉积高于约400℃的温度可引起二硫化锆(ZrS2)膜沉积，而不沉积氧化锆相。
因此，在本公开的一些实施例中，过渡金属硫族化物膜可以包含硫化锆，且特别是二硫化锆(ZrS2)。另外，在一些实施例中，过渡金属硫族化物膜可以与包含二硫化锆(ZrS2)的组合物在约350℃与约400℃之间的沉积温度下、且特别是在约400℃的沉积温度下结晶。在一些实施例中，结晶二硫化锆(ZrS2)膜可以在高于400℃的沉积温度下沉积。
根据本公开的实施例沉积的过渡金属硫族化物膜的另外的非限制性实例，图4和图5示出了在介于200℃与500℃之间的各种沉积温度下沉积的，利用四氯化铪(HfCl4)和硫化氢(H2S)作为化学前体沉积的硫化铪膜(图4)和利用四氯化锆(ZrCl4)和硫化氢(H2S)作为化学前体沉积的硫化锆膜(图5)的掠入射x射线衍射(GIXRD)数据。
图4的检验示出了对于约200℃的沉积温度到约350℃沉积温度，GIXRD数据不包括数据中的任何可辨别峰值，对应于非结晶膜，即，示例性硫化铪膜是非晶的。对于400℃的沉积温度到450℃的沉积温度，GIXRD数据具有可辨别的主峰值，对应于结晶硫化铪膜，且特别是具有组成(HfS2)的二硫化铪膜。另外，对于介于400℃与450℃之间的沉积温度，示例性二硫化铪膜具有主导(001)结晶取向，如由GIXRD数据中的峰的位置所展示。对于500℃的沉积温度，与二硫化铪相关的GIXRD数据中的峰值是不可辨别的，但实际上存在对应于氧化铪(例如，HfO2)的许多较小峰，指示所沉积膜包含氧化铪膜。如本文先前描述，在500℃下沉积存在氧化铪相可能是由于在用于沉积图4的示例性硫化铪膜的反应室内残留的水和/或氧。在另外的非限制性实例中，用于沉积硫化铪膜的反应室可具有降低的水和/或氧气浓度，以及在500℃和更高温度下沉积可产生结晶硫化铪膜，而不存在氧化铪相。
因此，在本公开的一些实施例中，过渡金属硫族化物膜可以包含硫化铪，且特别是二硫化铪(HfS2)。另外，在一些实施例中，对于在约350℃与约400℃之间的沉积温度，且特别是约400℃的沉积温度，过渡金属硫族化物膜可包含具有主要(001)结晶取向的结晶二硫化铪(HfS2)。在一些实施例中，对于高于400℃的沉积温度，过渡金属硫族化物膜可包含具有主要(001)结晶取向的结晶二硫化铪(HfS2)。
另外，来自示例性硫化锆膜的GIXRD数据在图5中示出，并且图5的检验示出了对于200℃的沉积温度到300℃的沉积温度，GIXRD数据不包括数据中的任何可辨别峰值，对应于非结晶膜，即，示例性硫化锆膜是非晶的。对于350℃的沉积温度到450℃的沉积温度，GIXRD数据具有单个可辨别的峰，对应于结晶硫化锆膜，且特别是具有组成(ZrS2)的二硫化锆膜。另外，对于在350℃与450℃之间的沉积温度，示例性二硫化锆膜具有主导(001)结晶取向，如由GIXRD数据中的峰的位置所展示。对于500℃的沉积温度，存在与二硫化锆相关的GIXRD数据中的峰值，但也存在对应于氧化锆(例如，ZrO2)的许多较小峰，指示所沉积膜包含硫化锆和氧化锆两者的混合物。如本文先前描述，在500℃的沉积温度下氧化锆相的存在可归因于用于沉积图5的示例性硫化锆膜的反应室内的残余水和/或氧。在另外的非限制性实例中，用于沉积硫化锆膜的反应室可具有降低的水和/或氧气浓度，且在500℃和更高的温度下沉积可产生结晶硫化锆膜，而不存在氧化锆相。
因此，在本公开的一些实施例中，过渡金属硫族化物膜可包含硫化锆且特别是二硫化锆(ZrS2)。另外，在一些实施例中，对于在约300℃与约450℃之间的沉积温度，且特别是约400℃的沉积温度，过渡金属硫族化物膜可包含具有(001)结晶取向的结晶二硫化锆(ZrS2)。在一些实施例中，对于高于400℃的沉积温度，过渡金属硫族化物膜可包含具有主要(001)结晶取向的结晶二硫化锆(ZrS2)。
在本公开的一些实施例中，所沉积的过渡金属硫族化物膜可以经历沉积后退火工艺以改良过渡金属硫族化物膜的结晶度。例如，在一些实施例中，沉积过渡金属硫族化物膜的方法可进一步包含：金属硫族化物在高于过渡金属硫族化物膜的沉积温度的温度下的沉积后退火。例如，在一些实施例中，过渡金属硫族化物的退火可以包含：将过渡金属硫族化物膜加热到约低于800℃、或约低于600℃、或约低于500℃、或甚至约低于400℃的温度。在一些实施例中，过渡金属硫族化物薄膜的沉积后退火可以在包含硫族元素的气氛中执行，例如，沉积后退火工艺可以在包含硫族化物，例如硫化合物，如硫化氢(H2S)气氛的环境中执行。在一些实施例中，金属硫族化物薄膜的沉积后退火可以执行持续不到1小时、或不到30分钟、或不到15分钟、或甚至是不到5分钟的时段。在一些实施例中，过渡金属硫族化物膜膜的沉积后退火可以在不包含硫族元素，如S、Se或Te的气氛中，例如在惰性气体环境如N2，或稀有气体如Ar或He中，或在含氢气环境，如H2或H2/N2环境中执行。
根据本公开的一些实施例沉积的过渡金属硫族化物膜的薄膜，如二硫化铪薄膜可以是包括2D材料的连续薄膜。在一些实施例中，包含根据一些本公开实施例沉积的过渡金属硫族化物膜的膜可以是厚度低于约100纳米、或低于约60纳米、或低于约50纳米、或低于约40纳米、或低于约30纳米、或低于约25纳米、或低于约20纳米、或低于约15纳米、或低于约10纳米、或低于约5纳米或更低的连续膜。
在一些实施例中，根据本公开的实施例沉积的过渡金属硫族化物膜在具有大于100毫米、或大于200毫米、或大于300毫米或甚至大于400毫米直径的衬底上可以是连续的。本文提及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。
在本公开的一些实施例中，通过本文所公开的方法沉积的过渡金属硫族化物膜可包含硫化铪、硒化铪、碲化铪、硫化锆、硒化锆或碲化锆中的至少一种。
在本公开的一些实施例中，通过本文公开的方法沉积的过渡金属硫族化物膜可以包含铪硫族化物且特别是具有通式HfSx的硫化铪，其中x可以在约0.75到约2.8范围内，或其中x可以在约0.8到约2.5范围内，或其中x可以在0.9到约2.3范围内，或替代地，其中x可以在约0.95到约2.2范围内。HfSx的元素组成范围可以包含约30原子％到约60原子％、或约35原子％到约55原子％或甚至是约40原子％到约50原子％的Hf。或者，HfSx的元素组成范围可以包含约25原子％到约75原子％的S、或约30原子％到约60原子％的S或甚至是约35原子％到约55原子％的S。
在本公开的一些实施例中，通过本文公开的方法沉积的过渡金属硫族化物膜可以包含锆硫族化物且特别是具有通式ZrSx的硫化锆，其中x可以在约0.75到约2.8范围内，或其中x可以在约0.8到约2.5范围内，或其中x可以在0.9到约2.3范围内，或替代地，其中x可以在约0.95到约2.2范围内。ZrSx的元素组成范围可以包含约30原子％到约60原子％，或约35原子％到约55原子％或甚至是约40原子％到约50原子％的Zr。或者，ZrSx的元素组成范围可以包含约25原子％到约75原子％的S、或约30原子％到约60原子％的S或甚至是约35原子％到约55原子％的S。
在另外的实施例中，本公开的过渡金属硫族化物膜可以包含低于约20原子％的氧、或低于约10原子％的氧、或低于约5原子％的氧或甚至是低于约2原子％的氧。在其它实施例中，过渡金属硫族化物膜可以包含低于约25原子％的氢，或低于约10原子％的氢，或低于约5原子％的氢，或低于约2原子％的氢，或甚至是低于约1原子％的氢。在又其它实施例中，过渡金属硫族化物膜可以包含低于约20原子％的碳，或低于约10原子％的碳，或低于约5原子％的碳，或低于约2原子％的碳，或低于约1原子％的碳，或甚至是低于约0.5原子％的碳。在本文概述的实施例中，元素的原子浓度可以利用卢瑟福背散射(Rutherfordbackscattering，RBS)和/或弹性反冲检测分析(elastic recoil detection analysis，ERDA)测定。
在本公开的一些实施例中，可以将过渡金属硫族化物膜沉积于三维结构上。在一些实施例中，在纵横比(高度/宽度)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，过渡金属硫族化物膜的阶梯覆盖率可以等于或大于约50％、或大于约80％、或大于约90％、或约95％、或约98％，或约99％或更高百分比。
在一些实施例中，本公开的过渡金属硫族化物膜，如铪和锆二硫族化物膜，可以沉积到约20纳米至约100纳米的厚度。在一些实施例中，根据一些本文所述的实施例沉积的过渡金属硫族化物膜的厚度可以是约20纳米到约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过渡金属硫族化物薄膜的厚度可以大于约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纳米或甚至更大。在一些实施例中，根据一些本文所述的实施例沉积的过渡金属硫族化物薄膜的厚度可以小于约50纳米、或小于约30纳米、或小于约20纳米、或小于约15纳米、或小于约10纳米、或小于约5纳米、或小于约3纳米、或小于约2纳米、或小于约1.5纳米或甚至小于约1纳米。
在一些实施例中，根据一些本文所述的实施例沉积的过渡金属硫族化物膜，如铪或锆二硫族化物膜的厚度可以等于或小于约10个单层的过渡金属硫族化物材料、或等于或小于约7个单层的过渡金属硫族化物材料、或等于或小于约5个单层的过渡金属硫族化物材料、或等于或小于约4个单层的过渡金属硫族化物材料、或等于或小于约3个单层的过渡金属硫族化物材料、或等于或小于约2个单层的过渡金属硫族化物材料，或甚至等于或小于约1个单层的过渡金属硫族化物材料。
在本公开的一些实施例中，根据本文所公开的方法沉积的过渡金属硫族化物膜可以包括保护性覆盖层，从而基本上防止、或甚至防止过渡金属硫族化物膜的不合需要的氧化。例如，在完成过渡金属硫族化物的沉积后，硫族化物膜可从反应室卸载，并暴露于其中周围环境中的氧和/或水可氧化所沉积的过渡金属硫族化物膜的环境条件。
因此，在一些实施例中，覆盖层可沉积在过渡金属硫族化物膜上方，并且特别是直接沉积在过渡金属硫族化物膜上方。另外，为了防止过渡金属硫族化物膜的任何潜在氧化，覆盖层可沉积在用于沉积过渡金属硫族化物的同一反应室内，即，覆盖层可在用于沉积过渡金属硫族化物膜的同一反应室内原位沉积。因此，在本公开的一些实施例中，所述方法可进一步包含：在过渡金属硫族化物膜上原位沉积覆盖层，从而在暴露于环境条件下基本上防止过渡金属硫族化物膜氧化。
在一些实施例中，覆盖层可以包含金属硅酸盐膜。在一些实施例中，金属硅酸盐膜可以包含硅酸铝(AlxSiyOx)、硅酸铪(HfxSiyOx)、或硅酸锆(ZrxSiyOx)中的至少一种。有关金属硅酸盐膜沉积的更详细信息可见于2000年10月13日提交的标题为“用于生长氧化膜的方法(METHOD FOR GROWING THIN OXIDE FILMS)”的美国专利第6,632,279号，所述专利均以引用的方式并入本文并且作为本说明书的一部分。
在一些实施例中，覆盖层可通过循环沉积工艺，如原子层沉积工艺或循环化学气相沉积工艺直接沉积在过渡金属硫族化物膜上，如本文所公开的。作为非限制性实例，覆盖层可以包含金属硅酸盐，并且金属硅酸盐可以通过循环沉积工艺，如原子层沉积进行沉积。在一些实施例中，覆盖层可以使用包含非氧化反应物/前体的工艺或含有非氧反应物(例如，没有O2、H2O、O3、H2O2、含O等离子体、自由基或原子)的工艺沉积。因此，在一些实施例中，覆盖层可以在不使用H2O、O3或H2O2的情况下沉积。在一些实施例中，覆盖层可以在不使用氧类等离子体的情况下沉积，即，没有含O等离子体、氧自由基、氧原子或氧激发物种。覆盖层可使用包含非氧化反应物/前体或非氧反应物的工艺沉积，从而防止或基本上防止下层过渡金属硫族化物膜的氧化。因此，在一些实施例中，在过渡金属硫族化物膜上方原位沉积覆盖层可在过渡金属硫族化物膜没有额外氧化的情况下进行。
在其它实施例中，覆盖层可以包含金属，如过渡金属。在一些实施例中，覆盖层可包含氮化物、硫化物、碳化物或其混合物，或例如含硅层，如非晶硅层。在其它实施例中，覆盖层可以是电介质层。在其它实施例中，覆盖层可以是导电层。在其它实施例中，覆盖层可以是半导体层。
用于沉积覆盖层的示例性ALD方法可以包含一个或多个重复单位沉积循环，其中单位沉积循环可包含：使衬底与金属气相反应物接触，吹扫反应室中的过量金属前体和反应副产物，使衬底与包含硅组分和氧组分的前体接触，以及第二次吹扫反应室。作为非限制性实例，覆盖层可以包含硅酸铝膜(AlxSiyOz)，且金属气相反应物可包含三氯化铝(AlCl3)，而包含硅组分和氧组分的前体可包含四正丁氧基硅烷Si(OnBu)4。在本公开的一些实施例中，覆盖层可包含在不使用氧化前体的情况下沉积的金属硅酸盐，如O2、H2O、O3、H2O2、含O等离子体、自由基或原子。
在一些实施例中，覆盖层可以在用于沉积过渡金属硫族化物膜的相同温度下沉积。例如，覆盖层可以在低于500℃、或低于450℃、或低于400℃、或低于300℃、或低于200℃的温度下沉积。在一些实施例中，覆盖层可以在介于约200℃与500℃之间的温度下，且特别是在约400℃的沉积温度下沉积。
在一些实施例中，覆盖层可以沉积为小于50纳米、或小于40纳米、或小于30纳米、或小于20纳米、或小于10纳米、或小于7纳米、或小于5纳米、或小于3纳米、或小于2纳米或甚至小于1纳米的厚度。在一些实施例中，覆盖层是连续膜，并且直接安置在金属硫族化物膜上方，从而基本上防止金属硫族化物膜氧化。
作为非限制性实例，图6示出了根据本公开的实施例沉积的裸锆硫族化物膜和覆盖有硅酸铝覆盖层的锆硫族化物膜两者随时间推移的环境稳定性。更详细地说，图6示出了硅酸铝覆盖的二硫化锆膜(由三角形数据标记表示)和未覆盖的裸二硫化锆膜(由方形数据标记表示)随着暴露于环境条件的时间推移的主要(001)峰的归一化x射线衍射(XRD)强度的变化。裸二硫化锆膜的数据的检验示出了XRD数据中的(001)峰强度随时间推移降低，指示裸二硫化锆在暴露于环境条件时随时间推移氧化。相比之下，硅酸铝覆盖的二硫化锆膜的数据的检验示出了XRD数据中的(001)峰强度随时间推移不降低，指示被覆盖的二硫化锆膜基本上不氧化。
在本公开的一些实施例中，覆盖层直接在过渡金属硫族化物膜的表面上的原位沉积在提高薄过渡金属硫族化物膜作为覆盖层的质量方面可能有益，因为覆盖层可防止在沉积之后在反应室冷却期间硫族化物膜的氧化。
更详细地说，图7A示出了利用不同数目的沉积循环沉积且没有覆盖层的示例性二硫化锆膜的掠入射x射线衍射(GIXRD)数据，而图7B示出了利用不同数目的沉积循环沉积且硫族化物膜上方直接沉积有原位覆盖层的示例性锆硫族化物膜的掠入射x射线衍射(GIXRD)数据。图7A的检验，即，未覆盖的二硫化锆，示出了对应于结晶二硫化锆的XRD峰在已完成1000个沉积循环之前不会出现，其对应于约8纳米的厚度。相比之下，图7B的检验，即，覆盖的二硫化锆，示出了在500个沉积循环处对应于结晶二硫化锆的XRD峰出现，其对应于约4纳米的厚度。因此，在本公开的一些实施例中，所述金属硫族化物膜可以由原位覆盖层覆盖，并且所述金属硫族化物膜可以是在小于约5纳米、或小于约4纳米、或小于约2纳米、或小于1.5纳米、或甚至小于1纳米的厚度下的结晶。
通过本文所公开的循环沉积工艺沉积的金属硫族化物膜可以用于多种情形中，如用于半导体装置结构的形成。本领域的技术人员应认识到，本文所描述的方法适用于许多情形，包括但不限于晶体管的制造。
作为非限制性实例，并且参看图8，半导体装置结构800可以包含场效应晶体管(FET)，所述场效应晶体管可以包括硅衬底802和安置于硅衬底802上的二氧化硅(SiO2)层804。半导体装置结构800可进一步包含源极区806和漏极区808。在源极区与漏极区之间安置有根据本公开的实施例沉积的过渡金属硫族化物膜810。过渡金属硫族化物膜810可包含二硫化铪或二硫化锆的膜，并且可由FET结构的通道区组成。在本公开的一些实施例中，所述过渡金属硫族化物膜810可具有小于10纳米、或小于5纳米、或甚至小于1纳米的厚度。直接安置在过渡金属硫族化物膜810上方的可以是覆盖层811。例如，覆盖层811可以包含金属硅酸盐膜，且特别是硅酸铝膜。半导体装置结构800可进一步包含安置于过渡金属硫族化物膜810上方的栅极电介质层812，其中所述栅极电介质层812可以包含二氧化铪(HfO2)。半导体装置结构800可进一步包含安置在过渡金属硫族化物膜810上方的栅电极814。
本公开的实施例还可以包括被配置成用于沉积本公开的过渡金属硫族化物膜的反应系统。更详细地，图9示意性地示出了包括反应室902的反应系统900，所述反应系统进一步包括用于将衬底(未图示)保持在预定压力、温度和环境条件下并且用于将衬底选择性暴露于各种气体的机构。前体反应物源904可以通过导管或其它适当的构件904A联接到反应室902，并且可以进一步联接到歧管、阀门控制系统、质量流量控制系统或用以控制来源于前体反应物源904的气态前体的机构。由前体反应物源904供应的前体(未图示)、反应物(未图示)在室温和标准大气压条件下可以是液态或固态的。可以在反应物源真空容器内汽化此类前体，所述反应物源真空容器可以维持处于或高于前体源室内的汽化温度。在此类实施例中，可以用载气(例如不活泼或惰性气体)输送汽化的前体，且接着经由导管904A将汽化的前体进料到反应室902中。在其它实施例中，在标准条件下，前体可以是蒸气。在此类实施例中，不需要汽化的前体，并且前体可能不需要载气。例如，在一个实施例中，前体可以储存在气瓶中。导管904A可进一步包含用于从进料到反应室902的蒸汽基本上去除不需要的污染物的气体纯化器905A。
反应系统900还可以包括额外的前体反应物源，如还可如上文所描述，借助于导管906A和额外的气体纯化器905B联接到反应室902的前体反应物源906。
吹扫气体源908还可经由导管908A联接到反应室902，并且选择性地将各种惰性或稀有气体供应到反应室902，以帮助从反应室去除前体气体或废气。可以供应的各种惰性或稀有气体可以来源于固态、液态或储存的气态形式。
图9的反应系统900还可包含系统操作和控制机构910，所述系统操作和控制机构910提供电子电路和机械组件以选择性地操作包括在反应系统900中的阀门、歧管、泵和其它设备。此类电路和组件操作以引入前体，吹扫来自相应前体源904、906和吹扫气体源908的气体。系统操作和控制机构910还控制气体脉冲序列的时序、衬底和反应室的温度，及反应室的压力，以及实现反应系统900的适当操作所必需的各种其它操作。操作和控制机构910可以包括控制软件和电控制或气动控制的阀门，用以控制前体、反应物和吹扫气体进出反应室902的流动。控制系统可包括执行某些任务的模块，如软件或硬件组件，例如FPGA或ASIC。模块可以有利地配置成驻留在控制系统的可寻址存储媒体上，并且可以有利地被配置成执行一个或多个工艺。
相关领域的技术人员应了解，本发明的反应系统的其它配置是可能的，包括不同数目和种类的前体反应物源和吹扫气体源。此外，这些人还应了解，存在可以用于实现将气体选择性供给到反应室902中的目标的阀门、导管、前体源、吹扫气体源的许多布置。此外，作为反应系统的示意性图示，为了简化说明，省去了许多组件，并且此类组件可以包括例如各种阀门、歧管、纯化器、加热器、容器、通风孔和/或旁路。
上文所描述的本公开的示例性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。任何等效实施例都希望在本发明的范围内。实际上，所属领域的技术人员根据说明书可以了解除本文中所示出和描述的内容外的对本公开的各种修改，例如，所描述元件的替代有用组合。此类修改和实施例也希望在所附权利要求书的范围内。

Claims (20)

1.一种通过循环沉积工艺在衬底上沉积过渡金属硫族化物膜的方法，所述方法包含：
使所述衬底与含有至少一种过渡金属的气相反应物接触，所述含有至少一种过渡金属的气相反应物包含铪前体或锆前体中的至少一种；以及
使所述衬底与含有至少一种硫族化物的气相反应物接触，其中所述衬底在接触步骤期间的温度低于约450℃。
2.根据权利要求1所述的方法，其中所述循环沉积工艺包含原子层沉积。
3.根据权利要求1所述的方法，其中所述循环沉积工艺包含循环化学气相沉积。
4.根据权利要求1所述的方法，其中所述铪前体或所述锆前体包含卤化物前体或金属有机前体中的至少一种。
5.根据权利要求4所述的方法，其中所述卤化物前体包含四氯化铪(HfCl4)或四氯化锆(ZrCl4)中的至少一种。
6.根据权利要求4所述的方法，其中所述金属有机前体包含烷基酰胺前体或含有环戊二烯基配体的前体中的至少一种。
7.根据权利要求6所述的方法，其中所述烷基酰胺前体包含四(乙基甲基酰胺基)铪(Hf(NEtMe)4)或四(乙基甲基酰胺基)锆(Ze(NEtMe)4)中的至少一种。
8.根据权利要求6所述的方法，其中所述含有环戊二烯基配体的前体包含以下中的至少一种：三(二甲基酰胺基)环戊二烯基铪(HfCp(NMe2)3)、双(甲基环戊二烯基)甲氧基甲基铪((MeCp)2Hf(CH)3(OCH3))、三(二甲基酰胺基)环戊二烯基锆(ZrCp(NMe2)3)或双(甲基环戊二烯基)甲氧基甲基锆((MeCp)2Zr(CH)3(OCH3))。
9.根据权利要求1所述的方法，其中所述含有至少一种硫族元素的气相反应物包含硫化氢(H2S)、硒化氢(H2Se)、二甲硫醚((CH3)2S)或二甲基碲(CH3)2Te。
10.根据权利要求1所述的方法，其进一步包含在进入所述反应室之前使所述含有硫族化物的气相反应物流过气体纯化器，从而降低所述含有硫族化物的气相反应物中的水或氧气中的至少一种的浓度。
11.根据权利要求10所述的方法，其中所述含有硫族化物的气相反应物中的水或氧气中的至少一种的浓度降低至低于百万分之一。
12.根据权利要求1所述的方法，其进一步包含使载气流过含有所述含有过渡金属的气相反应物的源的容器，从而将所述含有过渡金属的气相反应物输送到所述反应室，并且进一步包含在进入所述含有过渡金属的气相反应物的源之前使所述载气流过气体纯化器，从而降低所述载气中的水或氧气中的至少一种的浓度。
13.根据权利要求12所述的方法，其中所述载气中的水或氧气中的至少一种的浓度降低至低于百万分之一。
14.根据权利要求1所述的方法，其进一步包含在膜沉积之前在高于500℃的温度下预退火所述反应室。
15.根据权利要求1所述的方法，其中所述过渡金属硫族化物膜包含主要(001)结晶取向。
16.根据权利要求1所述的方法，其进一步包含在所述过渡金属硫族化物膜上方原位沉积覆盖层，从而在暴露于环境条件时基本上防止所述过渡金属硫族化物膜氧化。
17.根据权利要求16所述的方法，其中在所述过渡金属硫族化物膜上方原位沉积覆盖层，其进一步包含使用非氧化性前体或非氧反应物沉积所述覆盖层。
18.根据权利要求16所述的方法，其中所述覆盖层包含金属硅酸盐膜。
19.根据权利要求18所述的方法，其中所述金属硅酸盐膜包含硅酸铝膜(AlxSiyOz)。
20.一种半导体装置结构，其包含通过根据权利要求1所述的方法沉积的过渡金属硫族化物膜。
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