CN108411281B - 通过热ald和peald沉积氧化物膜的方法 - Google Patents

通过热ald和peald沉积氧化物膜的方法 Download PDF

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CN108411281B
CN108411281B CN201810116717.0A CN201810116717A CN108411281B CN 108411281 B CN108411281 B CN 108411281B CN 201810116717 A CN201810116717 A CN 201810116717A CN 108411281 B CN108411281 B CN 108411281B
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oxide film
gas
reaction chamber
thermal ald
peald
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CN108411281A (zh
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深泽笃毅
福田秀明
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ASM IP Holding BV
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Abstract

一种用于通过热ALD和PEALD将氧化物膜沉积于衬底上的方法，其包括：在反应室中提供衬底；通过热ALD在所述反应室中将第一氧化物膜沉积于所述衬底上；和在不中断真空的情况下，通过PEALD在所述反应室中将第二氧化物膜连续沉积于所述第一氧化物膜上。

Description

通过热ALD和PEALD沉积氧化物膜的方法
技术领域
本发明大体上涉及一种通过热原子层沉积(热ALD)和等离子体增强原子层沉积(PEALD)来沉积氧化物膜的方法。
背景技术
随着半导体装置微型化的发展，在半导体制造工艺期间引起的对凹槽图案或底层的损坏变得更加难以解决。这是因为当使装置微型化时，由凹槽图案或底层的受损所引起的尺寸变化更大程度地影响图案化精密性，导致功能下降。常规地，SiO膜用于图案化或用作通过PEALD沉积的功能膜；然而，使用直接等离子体即电容耦合等离子体(CCP)的PEALD导致凹槽图案或底层受损，并且损坏程度往往取决于等离子体功率，并且因此，已使用低RF功率用于构造微型化半导体装置。确切地说，由于基于碳的底层对氧化的耐性较低，因此通常施加低RF功率以便使对底层的损坏降到最低。当损坏通过膜的收缩率表现时，常规地，底膜通常显示约2％到5％的收缩率。然而，在微型化装置中越来越需要较小的膜收缩率。
对与相关技术相关的问题和解决方案的任何论述已仅出于向本发明提供背景的目的包括于本公开中，并且不应被视为承认论述中的任一项或全部在创作本发明时是已知的。
发明内容
在一些实施例中，使用连续两步法形成氧化物膜，所述方法包含热ALD作为第一步骤和PEALD作为第二步骤，以避免将衬底的底层暴露于等离子体，从而抑制底层的尺寸降级和/或氧化。在一些实施例中，第一步骤和第二步骤在同一反应室中连续进行。在一些实施例中，由于用于热ALD的反应物和前体的反应性高于用于PEALD的反应物和前体的反应性，即使当其处于非激发态时也如此，因此将反应物以针对热ALD与针对PEALD的流动路径不同的流动路径供应到反应室。用于热ALD的前体可以与用于PEALD的前体不同或相同。
出于概述本发明的方面和优于相关技术而实现的优势的目的，本发明的某些目标和优势描述于本公开中。当然，应理解，未必所有这类目标或优势可以根据本发明的任何特定实施例来实现。因此，举例来说，所属领域的技术人员将认识到本发明可以按实现或优化如本文中教示的一种优势或一组优势的方式实施或进行，而不必须获得如本文中可以教示或表明的其它目标或优势。
本发明的其它方面、特征和优势将从之后的实施方式变得显而易见。
附图说明
现将参考优选实施例的图式来描述本发明的这些和其它特征，所述优选实施例在于说明并且不限制本发明。所述图式出于说明性目的被大大简化并且未必按比例。
图1A是可用于本发明的一个实施例的用于热ALD和等离子体增强ALD(PEALD)沉积氧化物膜的ALD(原子层沉积)设备的示意性图示。
图1B说明可用于本发明的一个实施例的使用流通系统(FPS)的前体供应系统的示意性图示，其中(a)表示运载气体流过瓶以从那里携带前体的状态，并且(b)表示运载气体绕过瓶的状态。
图2显示根据本发明的一个实施例的一个循环的热ALD的示意性过程顺序，其中灰色单元表示开启状态而白色单元表示断开状态，并且每栏的宽度不表示每一过程的持续时间。
图3显示根据本发明的一个实施例的与一个循环的PEALD的示意性过程顺序组合的一个循环的热ALD的示意性过程顺序，其中灰色单元表示开启状态而白色单元表示断开状态，并且每栏的宽度不表示每一过程的持续时间。
图4显示根据本发明的一个实施例的一个循环的PEALD的示意性过程顺序，其中灰色单元表示开启状态而白色单元表示断开状态，并且每栏的宽度不表示每一过程的持续时间。
图5显示根据本发明的另一个实施例的一个循环的热ALD的示意性过程顺序，其中灰色单元表示开启状态而白色单元表示断开状态，并且每栏的宽度不表示每一过程的持续时间。
图6显示根据本发明的另一个实施例的与一个循环的PEALD的示意性过程顺序组合的一个循环的热ALD的示意性过程顺序，其中灰色单元表示开启状态而白色单元表示断开状态，并且每栏的宽度不表示每一过程的持续时间。
图7是可用于本发明的另一个实施例的用于热ALD和等离子体增强ALD(PEALD)沉积氧化物膜的ALD(原子层沉积)设备的示意性图示。
具体实施方式
在本公开中，取决于背景，“气体”可以包括气化固体和/或液体并且可以由单一气体或气体混合物构成。同样，取决于背景，冠词“一(a/an)”是指一种物种或包括多种物种的属。在本公开中，通过喷头或另一端口引入到反应室的工艺气体可以包含含硅或金属前体和添加剂气体、主要由其组成或由其组成。添加剂气体可以包括用于氧化前体的反应气体，和当向添加剂气体施加RF功率时用于激发前体的惰性气体(例如，稀有气体)。惰性气体可以作为运载气体和/或稀释气体馈送到反应室。前体和添加剂气体可以作为混合气体或单独地引入到反应空间。前体可以用运载气体如稀有气体引入。不为工艺气体的气体，即，在不穿过喷头的情况下引入的气体，可以用于例如密封反应空间，其包括密封气体如稀有气体。在一些实施例中，术语“前体”一般是指参与产生另一化合物的化学反应的化合物，并且尤其是指构成膜基质或膜的主要构架的化合物，然而术语“反应物”是指不为前体的活化前体、使前体改性或催化前体反应的化合物，其中当施加RF功率时反应物可以向膜基质提供元素(如O)并且变成膜基质的一部分。术语“惰性气体”是指当施加RF功率时激发前体的气体，但不同于反应物，其不变成膜基质的一部分。
在一些实施例中，“膜”是指在垂直于厚度方向的方向上连续延伸的层，基本上无针孔覆盖整个目标或相关表面；或简单地覆盖目标或相关表面的层。在一些实施例中，“层”是指形成于表面上的具有某一厚度的结构或膜或非膜结构的同义词。膜或层可以由具有某些特征的离散单一膜或层或多个膜或层构成，并且邻近膜或层之间的边界可以透明或可以不透明，并且可以基于物理、化学和/或任何其它特征，形成过程或顺序和/或邻近膜或层的功能或目的而确立。此外，在本公开中，由于可工作范围可以基于常规工作确定，因此变数的任何两个数字可以构成变数的可工作范围，并且所指示的任何范围可以包括或排除端点。另外，所指示的变数的任何值(与它们是否用“约”指示无关)可以指精确值或近似值并且包括等同物，并且在一些实施例中可以指平均值、中值、代表值、大部分值等。此外，在本公开中，在一些实施例中，术语“由……构成”和“具有”独立地是指“通常或广泛地包含”、“包含”、“基本上由……组成”或“由……组成”。在本公开中，在一些实施例中，任何所定义的含义未必排除普通和惯用含义。
在未指定条件和/或结构的本公开中，鉴于本公开，所属领域的技术人员可以按照常规实验容易地提供这类条件和/或结构。
在所有的所公开实施例中，出于既定目的，实施例中所使用的任何元素可以用与其同等的任何元素替换，包括本文中明确、必须或本质上所公开的那些元素。此外，本发明可以同等地应用于设备和方法。
实施例将参照优选实施例而阐述。然而，本发明不限于优选实施例。
在一个实施例中，一种通过热ALD和PEALD将氧化物膜沉积于衬底上的方法，其包含：在反应室中提供衬底；通过热ALD在反应室中将第一氧化物膜沉积于衬底上；和在不中断真空的情况下，通过PEALD在反应室中将第二氧化物膜连续沉积于第一氧化物膜上。
在上文中，取决于实施例，词语“连续”是指以下中的至少一项：空间不间断(例如，不移动衬底)、流动不间断(例如，至少一次不间断的流入)、不暴露于周围大气、和无任何物质插入步骤(除了辅助步骤如净化或其它可忽略的步骤以外)。在本公开中，“连续的”流动具有恒定的流动速率(替代地，即使流动是“连续的”，其流动速率仍可以随时间的推移而改变)。
在一些实施例中，由于作为反应物，含有H2O或OH基团的气体可以用于热ALD，但残余湿气可以保持在反应室内部，并且因此，为降低反应室内部的湿气的分压，通过使用还原气体如H2，可以在热ALD与PEALD之间从反应室中去除残余湿气，同时维持热ALD和PEALD的连续性。
由于第一氧化物膜通过热ALD沉积于衬底的底层上而不暴露于等离子体，因此可以有效抑制对底层的损坏，例如，由于在例如约100℃温度下进行的热ALD期间可以有效地抑制用于图案化的底层(例如，减小底层的收缩率)，因此含碳膜(例如，通过旋涂或CVD工艺制备的非晶碳)的尺寸降低；或由于在例如约300℃温度下进行的热ALD期间可以有效地抑制底层(例如，减小底层的氧化部分的厚度)，因此硅衬底氧化。在通过热ALD沉积第一氧化物膜后，通过PEALD将第二氧化物膜连续沉积于第一氧化物膜上。由于底层受到第一氧化物膜的保护而免遭用于PEALD的等离子体的损害，因此通过PEALD，底层不受损。
在一些实施例中，氧化物膜有效地沉积于具有图案化凹槽例如沟槽的衬底上。在本公开中，邻近垂直间隔物之间的凹槽和任何其它凹槽图案被称作“沟槽”。也就是说，沟槽是包括由垂直间隔物形成的图案的任何凹槽图案并且其在一些实施例中具有约20nm到约100nm(通常约30nm到约50nm)的宽度(其中当沟槽具有基本上与宽度相同的长度时，其被称作孔/通孔，并且其直径是约20nm到约100nm)、约30nm到约100nm(通常约40nm到约60nm)的深度和约1到约10(通常约2到约5)的纵横比。沟槽的适当尺寸可以取决于工艺条件、膜组成、既定应用等而改变。
通过热ALD沉积的第一氧化物膜的膜质量不如通过PEALD沉积的第二氧化物膜的膜质量那么好，并且因此，通过在同一反应室中连续进行热ALD和PEALD，避免了将第一氧化物膜暴露到周围大气(例如，空气)，从而保护第一氧化物膜的表面。通常，与第二氧化物膜相比，第一氧化物膜具有更高的湿润蚀刻速率和更低的密度。由于第一和第二氧化物膜是连续沉积的，因此由第一和第二氧化物膜构成的膜被视为通过ALD沉积的单一氧化物膜，其中第一氧化物膜充当保护层，而第二氧化物膜充当确定或控制组合氧化物膜的总体特性的块体层。在一些实施例中，第一氧化物膜具有约1nm到约7nm(例如，约2nm到5nm)的厚度，并且第二膜具有约5nm到约30nm(例如，约8nm到20nm)的厚度，其中第二膜比第一膜更厚。
尽管通过热ALD沉积的第一氧化物膜和通过PEALD沉积的第二氧化物膜是连续沉积的，但其间的边界或界面可以通过组成分析通过SIMS(次级离子质谱分析)来显现或鉴别，例如，所述分析显示边界或界面处Si、O、H、C等的浓度变化。举例来说，当通过热ALD沉积的第一氧化物膜和通过PEALD沉积的第二氧化物膜均在同一温度(例如，100℃)下沉积时，由于与在PEALD中相比在热ALD中的反应性较弱，因此与第二氧化物膜相比，第一氧化物膜具有更高浓度的碳和湿气，甚至当使用同一前体时也如此。通过STEM(扫描透射电子显微镜)的结构性观测可能不能够显现边界或界面。
在一些实施例中，热ALD的循环包含将前体馈送到反应室，所述前体是至少一种选自由以下组成的群组的化合物的气体：氨基硅烷、硅烷胺、异氰酸酯硅烷、isothonatesilane、无机硅烷、含硅烷氢氧化物和含硅烷醇盐。在一些实施例中，前体含有金属而非硅，如Ti、Zr和Hf，形成例如由TiO、ZrO和HfO构成的膜。
在一些实施例中，热ALD的循环包含将反应物馈送到反应室，所述反应物是至少一种选自由以下组成的群组的气体：H2O、醚、醇(例如，甲醇、乙醇等)、H2与O2的混合物以及H2O2。这种反应物可以在无等离子体的情况下被激发以便与吸附在衬底表面上的前体反应。因此，尽管通常存在三种方式来将反应物馈送到反应室(即，通过将反应物引入到反应室内部所提供的喷头的上游的歧管管道，通过在喷头处引入反应物，和/或通过将反应物引入喷头与上面放置衬底的基座之间，来将反应物馈送到反应室)，但取决于反应物的反应性，应选择适当的馈送方法。
在一些实施例中，PEALD的循环包含使用连续流动到反应室的运载气体以脉冲形式馈送前体，和将反应物连续馈送到反应室。在一些实施例中，反应物是至少一种选自由以下组成的群组的气体：O2、CO2和N2O。
在一些实施例中，热ALD的循环包含将反应物馈送到反应室，所述反应物是连续通过循环的至少一种选自由以下组成的群组的气体：乙醇、H2O和O3。当反应物的反应性不高时，反应物可以连续地流动通过反应室。然而，由于反应性较低，因此花费较长时间来完全沉积具有所期望厚度的膜。因此，在一些实施例中，热ALD的循环包含将催化气体以脉冲形式馈送到反应室，所述催化气体是不为前体和反应物的并且在循环中能够促进氧化物膜沉积的气体。针对热ALD，通过馈送催化气体，可以显著提高膜的沉积速率，并且可能使得反应性会较低的反应气体连续流动。当反应物不仅在PEALD中并且还在热ALD中连续流动时，尽管热ALD和PEALD可能需要不同的反应物，但反应室内部的压力基本上会贯穿热ALD的循环和PEALD的循环而恒定。
在一些实施例中，催化气体是至少一种选自由以下组成的群组的化合物的气体：吡啶、烷基金属、吡啶基硅烷、硅烷胺和硅氮烷。
在一些实施例中，沉积方法进一步包含在通过热ALD和PEALD沉积后清洗反应室。可以在热ALD和PEALD后进行同一清洗过程。在一些实施例中，使用清洗气体通过将清洗气体馈送在前体和反应物在气体混合室中混合的位置的上游，来进行清洗，使得可以清洗气体混合室、喷头的通道、反应室、排气通道。在一些实施例中，清洗气体通过反应室上游的远程等离子体单元来激发，或使用含氟气体(例如，ClF3)原位激发。在一些实施例中，在由热ALD的循环和PEALD的循环构成的每n数目的重复沉积循环后，进行清洗，其中重复的n数目少于沉积于反应室内壁等上的非想要膜开始从内壁剥离的重复的数目，从而产生污染物颗粒。
实施例将参照图式而阐述。然而，本发明不限于图式。
图2显示根据本发明的一个实施例的一个循环的热ALD的示意性过程顺序，其中灰色单元表示开启状态而白色单元表示断开状态，并且每栏的宽度不表示每一过程的持续时间。在图2中所说明的顺序中，前体使用连续供应的运载气体和稀释气体(共同称为“惰性气体”)以脉冲形式供应(“馈送”)。这可以使用流通系统(FPS)实现，其中运载气体管线具备具有前体储存器(瓶)的绕道管线，并且主管线和绕道管线经切换，其中当打算仅将运载气体馈送到反应室时，关闭绕道管线，而当打算将运载气体和前驱气体馈送到反应室时，关闭主管线，并且运载气体流过绕道管线并且与前驱气体一起从瓶中流出。通过这种方式，运载气体可以连续流入反应室中，并且可以通过切换主管线和绕道管线携带呈脉冲形式的前驱气体。图1B说明根据本发明的一个实施例的使用流通系统(FPS)的前体供应系统(黑色阀指示阀是关闭的)。如图1B中的(a)中所显示，当将前体馈送到反应室(未显示)时，首先，运载气体如Ar(或He)流过具有阀b和c的气体管线，并且接着进入瓶(储存器)20。运载气体从瓶20中流出，同时携载量对应于瓶20内部的蒸气压的前驱气体，并且流过具有阀f和e的气体管线，并且接着与前体一起馈送到反应室。在上文中，阀a和d是关闭的。当仅将运载气体(稀有气体)馈送到反应室时，如图1B中的(b)中所显示，运载气体流过具有阀a的气体管线，同时绕过瓶20。在上文中，阀b、c、d、e和f是关闭的。
在图2中，前体借助运载气体(“惰性气体”)提供。由于ALD是自限制吸附反应工艺，因此所沉积前体分子的数目通过反应性表面位点的数目测定，并且饱和后与前体暴露无关，并且由此每一循环对前体的供应使得反应性表面位点是饱和的。将用于沉积反应的反应物以脉冲形式供应到反应室(“反应”)，其中反应物经过热活化(例如，蒸气H2O)以与暴露在吸附于衬底上的前体的表面上的位点(例如，-CH3)反应，同时在不馈送前体的情况下将惰性气体连续馈送到反应室，从而形成单层。
如上文所提及，每一沉积循环的每一脉冲或阶段优选是自限制的。在每个阶段供应过量的前体以使敏感的结构表面饱和。表面饱和确保了前体占据所有可用的反应性位点(例如，受到物理大小或“位阻”限制)，并且因此确保了极佳的步阶覆盖。在一些实施例中，可以减少一种或多种前体的脉冲时间，使得不实现完全饱和并且少于一单层吸附于衬底表面上。在“馈送”后，净化反应室(“净化1”)，其中不将前体馈送到反应室，同时在不供应反应物的情况下将惰性气体连续馈送到反应室，从而从衬底的表面去除非化学吸附的前体和过量气体。在“反应”后，净化反应空间(“净化2”)，其中在不将前体和反应物馈送到反应室的情况下，将惰性气体连续馈送到反应室，从而从衬底的表面去除副产物和过量气体。由于进入反应室的惰性气体作为恒定流(前体间歇地或以脉冲形式注射于其中)连续流动，因此可以有效地进行净化以从层表面快速去除过量气体和副产物，从而有效地继续多个热ALD循环直到获得所期望的层厚度。
图4显示根据本发明的一个实施例的一个循环的PEALD的示意性过程顺序，其中灰色单元表示开启状态而白色单元表示断开状态，并且每栏的宽度不表示每一过程的持续时间。在图4中所说明的顺序中，前体使用连续供应的运载气体和稀释气体(共同称为“惰性气体”)以脉冲形式供应(“馈送”)。这可以使用如上文相关于图2的过程顺序所描述的流通系统(FPS)来实现。
在图4中，借助运载气体(“惰性气体”)提供前体。由于ALD是自限制吸附反应工艺，因此所沉积前体分子的数目通过反应性表面位点的数目测定，并且饱和后与前体暴露无关，并且由此每一循环对前体的供应使得反应性表面位点是饱和的。通过在贯穿沉积循环连续流动的反应气体(“反应物”)(例如，O2)中以脉冲形式原位施加RF功率(“RF”)产生用于沉积的等离子体，同时在不馈送前体的情况下将惰性气体和反应物连续馈送到反应室，从而形成单层。
如上文相关于图2的顺序所提及，供应过量的前体以使敏感的结构表面饱和。在一些实施例中，可以减少一种或多种前体的脉冲时间，使得不实现完全饱和并且少于一单层吸附于衬底表面上。在“馈送”后，净化反应空间(“净化1”)，其中不将前体馈送到反应空间，同时在不施加RF功率的情况下将惰性气体和反应气体连续馈送到反应空间，从而从衬底的表面去除非化学吸附的前体和过量气体。在“RF”后，净化反应空间(“净化2”)，其中在不馈送前体并且在不施加RF功率到反应空间的情况下，将惰性气体和反应气体连续馈送到反应空间，从而从衬底的表面去除副产物和过量气体。由于反应气体连续流动，并且也由于进入反应空间的惰性气体作为恒定流(前体间歇地或以脉冲形式注射于其中)连续流动，因此可以有效地进行净化以从层表面快速去除过量气体和副产物，从而有效地继续多个PEALD循环直到获得所期望的层厚度。
图3显示根据本发明的一个实施例的与一个循环的PEALD的示意性过程顺序组合的一个循环的热ALD的示意性过程顺序，其中灰色单元表示开启状态而白色单元表示断开状态，并且每栏的宽度不表示每一过程的持续时间。在一个循环的热ALD和PEALD的这一连续的组合过程顺序中，热ALD包含“馈送1”、“净化1”、“反应”和“净化2”，这基本上分别对应于图2中所说明的“馈送”、“净化1”、“反应”和“净化2”。在重复以上循环m次(m是1到3000、优选1到500的整数)后，开始PEALD，其包含“馈送2”、“净化3”、“RF”和“净化4”，这基本上分别对应于图4中所说明的“馈送”、“净化1”、“RF”和“净化2”。以上循环可以重复n次(n是1到1000、优选1到150的整数)。n/m的比可以在0.1到3、优选0.2到1的范围内。
在热ALD中，反应物的反应性通常较低，并且因此，沉积速率相比于PEALD的沉积速率通常较低，除非使用具有高反应性的反应物，如硅烷醇盐。当使用具有低反应性的反应物时，通过添加催化剂如吡啶，可以显著提高反应性，其中例如暴露在单层表面上的SiO-H键因催化剂而弱化，从而增加反应物物种的反应性和吸附前体的暴露位点。图5显示根据本发明的另一个实施例的一个循环的热ALD的示意性过程顺序，其中灰色单元表示开启状态而白色单元表示断开状态，并且每栏的宽度不表示每一过程的持续时间。在图5中所说明的顺序中，前体使用连续供应的运载气体和稀释气体(共同称为“惰性气体”)以脉冲形式供应(“馈送1”)。这可以使用如上文相关于图2的过程顺序所描述的流通系统(FPS)来实现。
在图5中，前体借助运载气体(“惰性气体”)提供。由于ALD是自限制吸附反应工艺，因此所沉积前体分子的数目通过反应性表面位点的数目测定，并且饱和后与前体暴露无关，并且由此每一循环对前体的供应使得反应性表面位点是饱和的。将增加反应物和前体的反应性的催化剂以脉冲形式供应到反应室(“馈送2”)，其贯穿沉积循环连续流动，同时在不馈送前体的情况下将反应物和惰性气体连续馈送到反应室，从而形成单层。由于反应物的反应性较低，因此反应物可以贯穿循环连续流动，并且通过以脉冲形式供应催化剂，可以活化沉积反应。对于热ALD，连续的反应物流动不是已知的，并且可以将压力波动降到最低或基本上抑制，并且增加能控性。
如上文相关于图2的顺序所提及，在每个阶段供应过量的前体以使敏感的结构表面饱和。在一些实施例中，可以减少一种或多种前体的脉冲时间，使得不实现完全饱和并且少于一单层吸附于衬底表面上。在“馈送1”后，净化反应室(“净化1”)，其中不将前体馈送到反应室，同时在不供应催化剂的情况下将惰性气体和反应气体连续馈送到反应空间，从而从衬底的表面去除非化学吸附前体和过量气体。在“馈送2”后，净化反应室(“净化2”)，其中在不馈送前体并且不供应催化剂到反应室的情况下，将惰性气体和反应气体连续馈送到反应空间，从而从衬底的表面去除副产物和过量气体。由于反应气体连续流动，并且也由于进入反应空间的惰性气体作为恒定流(前体和催化剂分别间歇地或以脉冲形式注射于其中)连续流动，因此可以有效地进行净化以从层表面快速去除过量气体和副产物，从而有效地继续多个热ALD循环直到获得所期望的层厚度。
图6显示根据本发明的另一个实施例的与一个循环的PEALD的示意性过程顺序组合的一个循环的热ALD的示意性过程顺序，其中灰色单元表示开启状态而白色单元表示断开状态，并且每栏的宽度不表示每一过程的持续时间。在一个循环的热ALD和PEALD的这种连续的组合过程顺序中，热ALD包含“馈送1”、“净化1”、“馈送2”和“净化2”，这基本上分别对应于图5中所说明的那些。在重复以上循环m次(m是1到3000、优选1到1000的整数)后，开始PEALD，其包含“馈送3”、“净化3”、“RF”和“净化4”，这基本上分别对应于图4中所说明的“馈送”、“净化1”、“RF”和“净化2”。以上循环可以重复n次(n是1到1000、优选1到150的整数)。n/m的比可以在0.1到3、优选0.2到2的范围内。以这种顺序，可以将压力波动降到最低或基本上抑制，并且增加能控性。
举例来说，过程循环可以使用任何合适的设备包括图1A中所说明的设备来进行。图1A是可用于本发明的一些实施例的用于热ALD和等离子体增强ALD(PEALD)沉积氧化物膜的ALD(原子层沉积)设备的示意性图示，期望将其与被编程以进行下文所描述的顺序的控制器结合。在这个图中，通过提供一对并联的并且在反应室3的内部11(反应区)中彼此面对面的导电(电容耦合)平板电极4、2，将HRF功率(13.56MHz或27MHz)25施加到一侧，并且使另一侧12电接地，在电极之间激发等离子体。温度调节器提供于下部阶段(下部电极2)中，并且放置于其上的衬底1的温度在指定温度下保持恒定。上部电极4同样充当喷淋板，并且前驱气体和反应气体(和稀有气体)分别通过气体管线21和气体管线22引入反应室3中，并且针对PEALD通过喷淋板。另外，在反应室3中，提供具有排气管线7的环形管道13，通过其反应室3的内部11中的气体被排出。另外，在反应室3下方设置的转移腔室5具备密封气体管线24以将密封气体经由转移腔室5的内部16(转移区)引入反应室3的内部11中，在转移腔室中提供用于隔离反应区和转移区的隔离板14(从这个图中省略闸阀，通过其晶片转移于传递腔室5中或从传递腔室转移)。转移腔室还具备排气管线6。在一些实施例中，在同一反应空间中进行多元素膜的沉积和表面处理，使得所有步骤可以连续进行而不将衬底暴露于空气或其它含氧气氛。
在一些实施例中，对于通过热ALD沉积的第一氧化物膜，使用与用于通过PEALD沉积的第二氧化物膜的前体和反应物不同的前体和反应物，但第一氧化物膜和第二氧化物膜构成单一连续的氧化物膜(具有单一膜类型)。在热ALD中，前体和反应物在接触时倾向于彼此反应，并且因此在一些实施例中，使用与供应用于PEALD的反应物的端口不同的端口将反应物供应到反应室。在图1A中所说明的设备中，通过将反应物通过反应室3内部所提供的喷淋板的上游的气体管线27引入到歧管管道23，和/或通过将反应物通过喷淋板中所提供的气体端口18引入在喷淋板处，和/或通过将反应物通过反应室3的侧壁中所提供的气体端口17(密闭地穿透环形管道13)引入在喷淋板与上面放置衬底1的基座2之间，可以将用于热ALD的反应物供应到反应室。对于热ALD，当使用不同的前体时，将前体通过气体管线26供应到歧管管道23。在一些实施例中，远程等离子体单元可以用于通过将激发气体供应到歧管管道23来激发气体。
在一些实施例中，在图1A中所描绘的设备中，图1B中所说明的切换非活性气体的流量与前驱气体的流量的系统(在前面描述)可以用于引入呈脉冲形式的前驱气体而不基本上使反应室的压力波动。
在一些实施例中，可以使用双室反应器(用于加工彼此密切设置的晶片的两个部分或隔室)，其中反应气体和稀有气体可以通过共享管线供应而前驱气体通过未共享管线供应。
所属领域的技术人员将了解，设备包括一个或多个被编程或以其它方式被配置成使得进行沉积和本文中其它地方所描述的反应器清洗工艺的控制器(未显示)。如所属领域的技术人员将了解，控制器连通有各种电源、加热系统、泵、机器人技术和反应器的气体流量控制器或阀。
图7是可用于本发明的另一个实施例的用于热ALD和等离子体增强ALD(PEALD)沉积氧化物膜的的ALD设备的示意性图示。在这个设备中，气体管线31、32、33和34对应于图1A中所说明的设备的气体管线21、22、26和27；RF源51对应于图1A中的RF源25；歧管管道41对应于图1A中的歧管管道23；喷头44对应于图1A中的喷淋板；反应室52对应于图1A中的反应室3；排气管线45对应于图1A中的排气管线6；并且基座43对应于图1A中的基座2。图1A中所指示的任何结构可以在图7中所说明的设备中提供。闸阀42是远程等离子体单元的闸阀。在这个设备中，可以将催化剂供应到反应室52。由于催化剂与前体具有反应性，因此在一些实施例中，直接将催化剂供应到反应室52而不使其与喷头44上游的前体混合。举例来说，通过在如图7中所说明的喷头44中提供具有其它孔37的另一个气体通道，其与如图1A中所说明的用于前体的具有孔的气体通道分隔开，可以将催化剂通过气体管线35供应到喷头44中的具有孔37的气体通道，使得可以在不与前体接触的情况下将催化剂馈送到反应室，直到催化剂进入反应室52的内部(但图7显示具有孔37的通道仅分布在喷头的外周边的附近，孔37可以贯穿喷头的整个表面均匀分布)。或者或另外，可以将催化剂通过反应室52的侧壁中所提供的气体端口36馈送到反应室52。
在一些实施例中，热ALD循环和PEALD循环可以在显示于下表1中的条件下如图3中所说明连续进行。
表1(数值是近似的)
Figure GDA0003228913400000141
Figure GDA0003228913400000151
针对300mm晶片的上文所指示的RF功率可以转化成W/cm2(每单位面积晶片的瓦数)，其可以适用于具有不同直径如200mm或450mm的晶片。
通常，第一氧化物膜的厚度在约1nm到约7nm的范围内，而第二氧化物膜的厚度在约5nm到约30nm的范围内，其中第二氧化物膜的厚度大于第一氧化物膜的厚度(在认为适当时可以根据膜的应用和目的等选择所期望的膜厚度)。组合的氧化物膜可以通过将其沉积于碳膜(例如，非晶碳)上用于双图案化或可以通过将其沉积于模板(例如，硅衬底)上而用作层间电介质膜。
在一些实施例中，热ALD循环和PEALD循环可以在显示于下表2中的条件下如图6中所说明连续进行。
表2(数值是近似的)
Figure GDA0003228913400000161
第一氧化物膜和第二氧化物膜可以具有显示于下表3中的特性。
表3(数值是近似的)
Figure GDA0003228913400000171
在上文中，第一氧化物膜的WER低于第二氧化物膜的WER，并且第一氧化物膜的膜密度也低于第二氧化物膜的膜密度。
进一步参考下文的工作实例来阐述本发明。然而，所述实例并不打算限制本发明。在不指定条件和/或结构的实例中，鉴于本公开，所属领域的技术人员可以按照常规实验容易地提供这类条件和/或结构。同样，在一些实施例中，可以将具体实例中所应用的数值修改至少±50％的范围，并且数值是近似的。
实例
实例1到5
通过热ALD和PEALD的组合工艺，使用图3或4中所说明的顺序，在形成于硅衬底(具有300mm的直径和0.7mm的厚度)上的非晶碳膜(具有100nm的厚度)上形成氧化硅膜，其具有纵横比是1的宽沟槽(开口宽度是100nm)和纵横比是3.5的窄沟槽(开口宽度是30nm)，所述顺序的一个循环在显示于下表4(过程循环)中的常见条件下，使用图1A中所说明的ALD设备和图1B中所说明的气体供应系统(FPS)进行，而特定条件和顺序指示于表5中。将第一反应物通过图1A中所说明的歧管管道馈送到反应室。
表4(数值是近似的)
Figure GDA0003228913400000181
表5(数值是近似的)
Figure GDA0003228913400000191
在表5中，具有“*”的实例编号指示比较实例。评估所获得的每个膜。表6显示评估结果。
表6(数值是近似的)
Figure GDA0003228913400000192
在表6中，“碳膜收缩率”表示在氧化物膜沉积后减小的碳膜的厚度与在氧化物膜沉积前碳膜的厚度的比的百分比；“侧壁覆盖率”表示窄沟槽的侧壁处氧化物膜的厚度与衬底的顶部表面处氧化物膜的厚度的比的百分比；“图案负载率”表示窄沟槽的侧壁处氧化物膜的厚度与宽沟槽的侧壁处氧化物膜的厚度的比的百分比；“热ALD GPC”表示生长速率/循环。
如表6中所显示，当氧化硅膜通过PEALD完全沉积时，下伏碳膜受损并且显示显著的膜收缩率(实例1)，然而当氧化硅膜通过热ALD首先沉积为保护层，并且接着通过PEALD连续沉积为块体层时，下伏碳膜受损的程度非常小并且显示显著更低的膜收缩率(实例2-5)。此外，作为保护层，使用TICS的通过热ALD沉积的氧化硅膜(实例3和5)似乎比使用BDEAS的氧化硅膜(实例2和4)更好。另外，通过PEALD工艺沉积的氧化硅膜(实例1)和通过热ALD和PEALD的组合工艺沉积的氧化硅膜(实例2-5)的保形性并非显著不同(其均显示大于90％的保形性)。
实例6到11
除了在无碳膜的情况下将氧化物膜直接沉积于硅衬底上以外，以基本上类似于如实例1到5中所描述的方式在硅衬底上形成氧化硅膜，其中特定条件和顺序指示于表7中。
表7(数值是近似的)
Figure GDA0003228913400000201
在表7中，具有“*”的实例编号指示比较实例。评估所获得的每个膜。表8显示评估结果。
表8(数值是近似的)
Figure GDA0003228913400000211
在表8中，“氧化Si衬底的厚度”表示在氧化物膜沉积后基于观测的氧化硅衬底的厚度。
如表8中所显示，当氧化硅膜通过PEALD完全沉积时，下伏硅层受损并且氧化(实例6)，然而当氧化硅膜通过热ALD首先沉积为保护层，并且接着通过PEALD连续沉积为块体层时，下伏硅层受损和氧化的程度非常小(实例7-11)。此外，作为保护层，使用TICS的通过热ALD沉积的氧化硅膜(实例9)似乎比使用OMCTS的氧化硅膜(实例10和11)更好，并且具有5nm厚度的氧化硅膜(实例9)也比2nm的氧化硅膜(实例8)更好。与通过热ALD使用TICS沉积的氧化硅膜(实例9)相比，通过热ALD使用OMCTS沉积的氧化硅膜(实例10和11)显示显著更高的GPC(因为硅烷醇盐具有高反应性)。另外，通过PEALD工艺沉积的氧化硅膜(实例6)和通过热ALD和PEALD的组合工艺沉积的氧化硅膜(实例7-11)的保形性并非显著不同(其均显示大于90％)。
实例12到17
除了连续馈送第1反应物、使用图2、4、5或6中所说明的顺序添加催化剂以外，以基本上类似于实例1到5中的方式在非晶碳膜上形成氧化硅膜，所述顺序的一个循环在显示于下表9(过程循环)中的常见条件下进行，而特定条件和顺序指示于表10中。通过喷头经由图7中所说明的不同气体通道将催化剂馈送到反应室。
表9(数值是近似的)
Figure GDA0003228913400000221
表10(数值是近似的)
Figure GDA0003228913400000231
在表10中，具有“*”的实例编号指示比较实例。评估所获得的每个膜。表11显示评估结果。
表11(数值是近似的)
Figure GDA0003228913400000232
在表11中，术语对应于表6中所用的那些术语。在“热ALD GPC”中，圆括号中的数值显示通过PEALD的GPC。
如表11中所显示，当氧化硅膜通过PEALD完全沉积时，下伏碳膜受损并且显示显著的膜收缩率(实例12)，然而当氧化硅膜通过热ALD首先沉积为保护层，并且接着通过PEALD连续沉积为块体层时(实例15-17)，并且当氧化硅膜通过热ALD完全沉积时(实例13和14)，下伏碳膜受损的程度非常小并且显示显著更低的膜收缩率。此外，意外地，即使当通过PEALD沉积第二氧化硅膜，通过在沉积第二氧化硅膜之前将第一氧化硅膜通过热ALD以1nm到3nm的厚度沉积为保护膜时(实例15-17)，也完全避免了等离子体施加于底膜的不良影响(实例15-17中的碳膜收缩率基本上等于或小于实例13-14中的碳膜收缩率，其中仅进行热ALD)。相比于实例13(不使用催化剂)，也可以在实例4(表6)中观测到以上结果。此外，相比于当不添加催化剂并且以脉冲形式馈送反应物时所获得的GPC(实例13)，当在热ALD中在连续馈送反应物的同时以脉冲形式添加催化剂时，GPC显著增加(实例14到17)。同样，相比于具有1nm厚度的第一氧化硅膜(实例16)，当通过热ALD沉积的第一氧化硅膜的厚度是3nm时，基本上检测不到膜收缩率(实例15)。另外，通过PEALD工艺完全沉积的氧化硅膜(实例12)、通过热ALD工艺完全沉积的氧化硅膜(实例13和14)和通过热ALD和PEALD的组合工艺沉积的氧化硅膜(实例15-17)的保形性并非显著不同(其均显示大于90％的保形性)。
实例18到21
除了在无碳膜的情况下将氧化物膜直接沉积于硅衬底上以外，以基本上类似于如实例12到17中所描述的方式在硅衬底上形成氧化硅膜，其中特定条件和顺序指示于表12中。
表12(数值是近似的)
Figure GDA0003228913400000241
在表12中，具有“*”的实例编号指示比较实例。评估所获得的每个膜。表13显示评估结果。
表13(数值是近似的)
Figure GDA0003228913400000251
在表13中，术语对应于表8中所用的那些术语。在“热ALD GPC”中，圆括号中的数值显示通过PEALD的GPC。
如表13中所显示，当氧化硅膜通过PEALD完全沉积时，下伏硅层受损并且氧化(实例18)，然而当氧化硅膜通过热ALD首先沉积为保护层，并且接着通过PEALD连续沉积为块体层时，底层受损和氧化的程度非常小(实例19-21)。此外，相比于当不添加催化剂并且以脉冲形式馈送反应物时所获得的GPC(表8中的实例7)，当在热ALD中在连续馈送反应物的同时以脉冲形式添加催化剂时，GPC显著增加(实例21)。同样，相比于具有1nm厚度的第一氧化硅膜(实例20)，当通过热ALD沉积的第一氧化硅膜的厚度是3nm时，基本上检测不到下伏硅层的氧化(实例19)。另外，通过PEALD工艺完全沉积的氧化硅膜(实例18)和通过热ALD和PEALD的组合工艺沉积的氧化硅膜(实例19-21)的保形性并非显著不同(其均显示大于90％的保形性)。
鉴于前述，证实到通过热ALD和PEALD的组合连续工艺，根据本文明确、必然或本质上公开的实施例，可以基本上在不损坏底层(由等离子体引起)的情况下沉积高质量的氧化物膜。
所属领域的技术人员应理解，可以在不脱离本发明的精神的情况下进行大量和各种修改。因此，应明确理解，本发明的形式仅是说明性的，并且并不打算限制本发明的范围。

Claims (17)

1.一种用于通过热ALD和PEALD将氧化物膜沉积于衬底上的方法，其包含：
在反应室中提供衬底；
通过热ALD在所述反应室中将第一氧化物膜沉积于所述衬底上；和
在不中断真空的情况下，通过PEALD在所述反应室中将第二氧化物膜连续沉积于所述第一氧化物膜上。
2.根据权利要求1所述的方法，其中所述热ALD的循环包含将前体馈送到所述反应室，所述前体是至少一种选自由以下组成的群组的化合物的气体：异氰酸酯硅烷、无机硅烷和含硅烷醇盐。
3.根据权利要求1所述的方法，其中所述热ALD的循环包含将反应物馈送到所述反应室，所述反应物是至少一种选自由以下组成的群组的气体：H2O、醚、醇、H2与O2的混合物和H2O2。
4.根据权利要求1所述的方法，其中所述热ALD的循环包含通过将反应物引入到所述反应室内部所提供的喷头的上游的歧管管道，通过在所述喷头处引入所述反应物，和/或通过将所述反应物引入所述喷头与上面放置所述衬底的基座之间，来将所述反应物馈送到所述反应室。
5.根据权利要求1所述的方法，其中所述PEALD的循环包含使用连续流动到所述反应室的运载气体以脉冲形式馈送前体，和将反应物连续馈送到所述反应室。
6.根据权利要求5所述的方法，其中所述反应物是至少一种选自由以下组成的群组的气体：O2、CO2和N2O。
7.根据权利要求1所述的方法，其进一步包含在通过所述热ALD和所述PEALD进行所述沉积后清洗所述反应室。
8.根据权利要求7所述的方法，其中所述清洗使用清洗气体通过将所述清洗气体馈送在混合前体和反应物的位置的上游来进行。
9.根据权利要求8所述的方法，其中所述清洗气体通过所述反应室的上游的远程等离子体单元来激发或使用含氟气体原位激发。
10.根据权利要求1所述的方法，其中所述热ALD的循环包含将反应物馈送到所述反应室，所述反应物是连续通过所述循环的至少一种选自由以下组成的群组的气体：乙醇、H2O和O3。
11.根据权利要求1所述的方法，其中所述热ALD的循环包含将催化气体以脉冲形式馈送到所述反应室，所述催化气体是除前体和反应物以外的并且在所述循环中能够促进所述氧化物膜沉积的气体。
12.根据权利要求11所述的方法，其中所述催化气体是至少一种选自由以下组成的群组的化合物的气体：吡啶、烷基金属、吡啶基硅烷和硅氮烷。
13.根据权利要求1所述的方法，其中所述第一氧化物膜具有1到7nm的厚度，并且所述第二氧化物膜具有5到30nm的厚度，其中所述第二氧化物膜比所述第一氧化物膜更厚。
14.根据权利要求1所述的方法，其中在上面沉积有所述第一氧化物膜的所述衬底的表面由非晶碳构成。
15.根据权利要求1所述的方法，其中在上面沉积有所述第一氧化物膜的所述衬底的表面由硅构成。
16.根据权利要求1所述的方法，其中所述衬底具有图案化凹槽，并且所述第一氧化物膜和所述第二氧化物膜沉积于所述凹槽上。
17.根据权利要求2所述的方法，其中所述无机硅烷是氨基硅烷、硅烷胺或含硅烷氢氧化物。
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US20190368040A1 (en) 2018-06-01 2019-12-05 Asm Ip Holding B.V. Infiltration apparatus and methods of infiltrating an infiltrateable material
US11718913B2 (en) 2018-06-04 2023-08-08 Asm Ip Holding B.V. Gas distribution system and reactor system including same
TWI840362B (zh) 2018-06-04 2024-05-01 荷蘭商Ａｓｍ Ｉｐ私人控股有限公司 水氣降低的晶圓處置腔室

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