CN111910175A - 用于重整非晶碳聚合物膜的方法 - Google Patents

用于重整非晶碳聚合物膜的方法 Download PDF

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CN111910175A
CN111910175A CN202010348121.0A CN202010348121A CN111910175A CN 111910175 A CN111910175 A CN 111910175A CN 202010348121 A CN202010348121 A CN 202010348121A CN 111910175 A CN111910175 A CN 111910175A
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amorphous carbon
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carbon polymer
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CN111910175B (zh
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T.J.V.布兰夸特
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Abstract

一种用于重整非晶碳膜的方法，作为其沉积工艺的一部分，所述方法包括以下工艺：(i)在反应空间中将非晶碳膜沉积在衬底上，直到非晶碳膜的厚度达到预定厚度，然后停止沉积工艺；并且(ii)在基本上不含氢、氧和氮的气氛中，将非晶碳膜暴露于Ar和/或He等离子体。

Description

用于重整非晶碳聚合物膜的方法
技术领域
本发明总体上涉及用于重整非晶碳聚合物膜(特别关于热稳定性)的方法。
背景技术
在制造集成电路(例如用于浅沟槽隔离、金属间电介质层、钝化层等的那些)的方法中，通常需要用绝缘材料填充沟槽(通常具有一或更高纵横比的任何凹部)。然而，随着大规模集成(LSI)装置的布线间距的小型化，由于现有沉积工艺的限制，高纵横比空间(例如，AR≥3)的无空隙填充变得越来越困难。
进一步地，为了使沉积膜致密，修复来自离子轰击的损害和/或改善化学/物理特性，经常执行沉积膜的退火。在本公开内容中，“退火”指应用于具有已经形成的膜基质的膜的过程，在所述过程中，将膜/层处理以改变为其稳定形式，例如，将端基改变成更稳定的基团(例如，去除含氢的末端)，其与“固化”不同，所述“固化”是应用于层以形成膜基质的过程。
尽管非晶碳聚合物膜可用于间隙填充技术和/或如例如硬掩模中的图案化中，但常规的非晶碳聚合物通常具有高热收缩率。当发生显著收缩时，非晶碳聚合物膜很可能从接触表面脱离和/或经历其特性的劣化。
鉴于常规的间隙填充技术和/或图案化技术，本发明的一个实施例(然而，并不限于此)提供了形成具有高热稳定性的非晶碳聚合物膜的方法。
对相关领域中涉及的问题和解决方案的任何讨论已仅出于为本发明提供背景的目的而包括在本公开内容中，并且不应该视为承认讨论中的任何或全部在制备本发明时是已知的。
当通过使用等离子体辅助方法形成非晶碳聚合物膜时，所得的非晶碳聚合物膜由氢化的非晶碳聚合物构成。在本公开内容中，氢化的非晶碳聚合物可以简称为非晶碳聚合物，其也可以被称为“aC:H”或简称为缩写“aC”。进一步地，在本公开内容中，除非另有说明，否则SiC、SiCO、SiCN、SiCON等等是以非化学计量的方式指示膜类型(简单地由主要构成元素指示)的缩写。
发明内容
在一些实施例中，一种用于重整非晶碳聚合物膜的方法，作为其沉积工艺的一部分，所述方法包括以下工艺：(i)在反应空间中将非晶碳聚合物膜沉积在衬底上，直到非晶碳聚合物膜的厚度达到预定厚度，然后停止沉积工艺；并且(ii)在基本上不含氢、氧和氮的气氛中，将非晶碳聚合物膜暴露于Ar和/或He等离子体。相应地，可以显著改善非晶碳聚合物膜的热稳定性。“基本上不含氢、氧和氮的气氛”指不将含有氢、氧或氮的气体进料到反应空间，在所述反应空间中，可能含有氢、氧和/或氮的残留气体和/或从膜中释放的气体可以作为杂质或非物质组分存在。在一些实施例中，在工艺(ii)中，仅将处于非激发态的Ar和/或He气体进料到反应空间，并且通过施加到在反应空间中提供的电极(例如，电容耦合的扁平电极)的RF功率来激发，或仅将处于激发态的Ar和/或He气体进料到反应空间。
在一些实施例中，在工艺(i)中每1nm至15nm的膜生长之后，周期性地进行方法(ii)。
出于概述本发明的各方面和所实现的优于相关技术的优势的目的，在本公开中描述本发明的某些目的和优势。当然，应理解，未必所有这些目标或优点都可以根据本发明的任何特定实施例来实现。因此，举例来说，本领域技术人员将认识到，本发明可以按照实现或优化如本文所传授的一个优点或一组优点的方式实施或进行，而不必实现如本文中可能传授或表明的其它目标或优点。
本发明的另外方面、特征和优势将从之后的详细描述变得显而易见。
附图说明
现将参照优选实施方案的附图来描述本发明的这些和其他特征，这些优选实施方案意图说明而非限制本发明。各图出于说明性目的而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中的用于沉积电介质膜的PEALD(等离子体增强原子层沉积)设备的示意图。
图1B示意了可用于本发明的一个实施方案中的使用流通系统(FPS)的前体供给系统的示意图。
图2是显示了在不同条件下退火后，没有等离子体处理(“STD”)、具有Ar等离子体处理(“Ar”)、以及具有He等离子体处理(“He”)的非晶碳聚合物膜的收缩的图，其中“Ar”和“He”代表本发明的实施例。
图3显示了没有等离子体处理(“STD”)、具有Ar等离子体处理(“Ar”)、以及具有He等离子体处理(“He”)的非晶碳聚合物膜的傅立叶变换红外(FTIR)光谱，其中“Ar”和“He”代表本发明的实施例。
图4显示了根据本发明的一个实施例，经受具有He等离子体处理的间隙填充工艺的沟槽的横截面视图的STEM照片，其中箭头显示了指示He等离子体处理的略微更暗的界面。
图5是示出了根据本发明的一个实施例的膜形成工艺顺序的图表，其中以灰色的单元格表示开启状态，而以白色的单元格表示断开状态，并且每栏的宽度列不代表每个过程的持续时间。
具体实施方式
在本公开中，取决于上下文，“气体”可包含汽化固体和/或液体，且可由单一气体或气体混合物构成。同样，取决于上下文，冠词“一”是指一个物种或包括多个物种的属。在本公开中，通过喷头引入反应室中的工艺气体可包括无硅烃前体和添加剂气体、基本上由其组成或由其组成。添加剂气体可以包括等离子体生成气体，用于在将RF功率施加于添加剂气体时，激发前体以形成非晶碳聚合物。添加剂气体可为惰性气体，其可作为载气和/或稀释气体进料到反应室。添加剂气体可不含用于氧化或氮化前体的反应气体。或者，添加剂气体可含有用于氧化或氮化前体的反应气体，程度为不干扰等离子体聚合形成基于非晶碳的聚合物。此外，在一些实施例中，添加剂气体仅含有等离子体生成气体(例如，稀有气体)。前体和添加剂气体可以混合气体引入到反应空间或分别引入到反应空间。可利用载气如稀有气体引入前体。除工艺气体外的气体，即在不穿过喷头的情况下引入的气体，可用于例如密封反应空间，这包括如稀有气体的密封气体。在一些实施例中，术语“前体”一般指参与产生另一种化合物的化学反应的化合物，并且特别指构成膜基质或膜主要骨架的化合物，而术语“反应物”指除前体外的化合物，其活化前体、修饰前体或催化前体的反应，其中所述反应物可以为膜基质提供元素(例如O、C、N)，并且当处于激发态时，变成膜基质的一部分。术语“等离子体生成气体”指除前体和反应物外的化合物，当暴露于电磁能时，所述化合物生成等离子体，其中所述等离子体生成气体可能不为膜基质提供元素(例如O、C、N)，所述元素变成膜基质的一部分。术语“重整气体”指这样的气体，当处于激发态时，该气体通常在不进一步生长膜的情况下(没有任何前体)重整已经沉积的膜。在一些实施例中，“重整气体”是等离子体生成气体。
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基本上无小孔的覆盖整个目标或相关表面的层，或仅仅是指覆盖目标或相关表面的层。在一些实施例中，“层”是指在表面上形成的具有某一厚度的结构，或膜或非膜结构的同义词。膜或层可由具有某些特征的离散单个膜或层构成或由多个膜或层构成，并且相邻膜或层之间的边界可以透明或可以不透明，并且可基于物理、化学和/或任何其它特征、形成工艺或序列和/或相邻膜或层的功能或目的而建立。此外，在本公开中，由于可工作范围可基于常规工作而确定，因此变量的任何两个数字可构成变量的可工作范围，且所指示的任何范围可包括或排除端点。另外，所指示的变量的任何值(不论其是否用“约”指示)可指精确值或近似值并且包含等同物，并且在一些实施例中，可指平均值、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”独立地指“典型地或广泛地包括”、“包括”、“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。
在本公开内容中，在一些实施例中，“连续地”指不中断真空，不中断为时间线，无任何材料插入步骤，不改变处理条件，其后立即，作为下一步骤，或在除两个结构外的两个结构之间不插入离散物理或化学结构。
在本公开内容中，“凹部或台阶”指具有在衬底上形成的顶表面、侧壁和底表面的任何结构，其可以在高度方向上连续地串联布置或者可以是单个凹部或台阶，并且可以构成沟槽、通孔或其它凹部。在本公开内容中，在相邻的突出结构和任何其它凹部图案之间的凹部被称为“沟槽”。即，沟槽为包含孔/通孔的任何凹部图案，且其在一些实施例中具有约20nm到约100nm(通常为约30nm到约50nm)的宽度(其中当沟槽具有与宽度基本上相同的长度时，其被称作孔/通孔，且其直径为约20nm到约100nm)、约30nm到约100nm(通常约40nm到约60nm)的深度以及约2到约10(通常约2到约5)的纵横比。沟槽的适当尺寸可取决于工艺条件、膜组成、既定应用等而变化。
在一些实施例中，一种用于重整非晶碳聚合物膜的方法，作为其沉积工艺的一部分，所述方法包括两个工艺：(i)在反应空间中将非晶碳聚合物膜沉积在衬底上，直到非晶碳聚合物膜的厚度达到预定厚度，然后停止沉积工艺；并且(ii)在基本上不含氢、氧和氮的气氛中，将非晶碳聚合物膜暴露于Ar和/或He等离子体。
在一些实施例中，非晶碳聚合物膜是可流动的膜，并且在其它实施例中，非晶碳聚合物膜是不可流动的膜。
可流动膜的沉积是本领域已知的；然而，常规的可流动膜的沉积使用化学气相沉积(CVD)伴随RF功率的持续施加，因为脉冲等离子体辅助沉积(例如PEALD)众所周知用于沉积保形膜，所述保形膜是具有与可流动膜的那些完全相反的特征的膜。在一些实施例中，可流动膜是由非晶碳聚合物构成的无硅含碳膜，并且尽管任何合适的一种或多种烃前体都可以是候选物，但在一些实施例中，前体包括在25℃下具有1,000Pa或更高的蒸气压的不饱和或环状烃。在一些实施例中，前体是选自以下的至少一种：C2-C8炔烃(CnH2n-2)、C2-C8烯烃(CnH2n)、C2-C8二烯(CnHn+2)、C3-C8环烯烃、C3-C8轮烯(CnHn)、C3-C8环烷烃和前述的取代烃。在一些实施例中，前体为乙烯、乙炔、丙烯、丁二烯、戊烯、环戊烯、苯、苯乙烯、甲苯、环己烯和/或环己烷。
在一些实施例中，作为用于沉积可流动膜的间隙填充技术，可以使用美国专利申请号16/026,711中公开的方法，其在其中不需要氮、氧或氢等离子体的条件下，通过使用烃前体的等离子体辅助沉积来提供完全的间隙填充，而基本上不形成空隙，所述美国专利申请的公开内容以引用的方式整体并入本文。
通过改变沉积条件或工艺参数，可以形成不可流动的膜。例如，此类参数包括但不限于前体的分压、沉积温度、沉积压力等。例如，通过增加沉积温度、降低沉积压力和/或降低前体比率(前体流量与载气/稀释气体流量的比率)，膜的流动性变低。在一些实施例中，工艺(i)(沉积工艺)通过等离子体增强的原子层沉积(PEALD)或其它循环的等离子体辅助沉积(例如，循环PECVD)来进行。作为等离子体，可以使用电容耦合等离子体、电感耦合等离子体、远程等离子体、由RF功率生成的等离子体、由微波生成的等离子体等。
在一些实施例中，当工艺(i)(沉积工艺)中的沉积膜的厚度达到单层厚度或更大，但为15nm或更小，优选10nm或更小，更优选5nm或更小时，沉积工艺停止，随后为工艺(ii)(重整工艺)。随着膜厚度在工艺(ii)之前(在先前的工艺(ii)之后，如果存在的话)增加，总体重整效果降低。如果膜厚度大于通过处理的重整效果可以获得的最大深度，则在深度/厚度方向上的膜质量/特性变得不均匀。如果膜厚度足够小用于接收通过处理的重整效果，则在深度/厚度方向上的膜质量/特性变得均匀，从而在经受在例如200℃至400℃下的后续退火或其它高热预算工艺时，均匀地抑制膜的收缩。
在一些实施例中，将工艺(i)和(ii)重复多次，直到非晶硅膜的厚度达到所需的最终厚度。
在一些实施例中，工艺(ii)中的气氛在工艺(i)中使用的反应空间中，其中工艺(i)和工艺(ii)可以连续地执行。可替代地，在其它实施例中，工艺(ii)中的气氛在与工艺(i)中使用的反应空间不同的另一个反应空间中。
在一些实施例中，工艺(ii)包括：将Ar和/或He进料到气氛中，而不进料氢、氧和氮；并且以生成Ar和/或He等离子体的方式将电磁能施加到气氛中。作为等离子体，尽管通常可以使用电容耦合等离子体，但也可以使用电感耦合等离子体、远程等离子体、由RF功率生成的等离子体、由微波生成的等离子体等。在一些实施例中，He等离子体是最有效的。Ar和/或He等离子体可以减少来自非晶碳聚合物膜的热不稳定的氢相关级分，例如甲基和/或亚甲基级分(例如，通过进一步促进聚合，而不是通过分开级分)，从而增加了膜的热稳定性。
在一些实施例中，RF功率在0.06W/cm2至0.96W/cm2/衬底的单位面积的范围内，并且工艺(ii)的持续时间在2秒至300秒的范围内，使得等离子体处理可以有效地重整非晶碳聚合物膜。
在一些实施例中，等离子体处理(重整工艺)可以在下文描述的条件下进行。
作为用于等离子体处理的重整气体，使用Ar和/或He气体作为主要气体。在进行重整工艺用于最有效处理的同时，基本上没有前体或反应物进料到反应空间；然而，反应空间的气氛可能被杂质或非故意组分例如留在气氛中的残留气体污染，即使在吹扫和/或由于等离子体处理而从膜中释放的气体之后。只要该气氛基本不含氢、氧和氮，在反应空间的气氛中可以存在除Ar或He外的气体。这些元素通常干扰通过Ar和/或He等离子体处理的重整反应。例如，如果在重整工艺期间将H2添加到反应空间中，则非晶碳聚合物膜可能灰化。通过基本上仅使用Ar和/或He，可以极大地改善非晶碳聚合物膜的热稳定性。在一些实施例中，在重整工艺期间，反应空间中的Ar/He气体体积比在1/0至0/1的范围内。
关于重整温度，当处理通常以循环方式原位进行时，优选地，该温度与可流动的沉积相容(例如，<125℃)。当处理在不同的室中或在不可流动的膜上外来施加时，不存在对温度施加的限制(例如，<800℃)。
关于用于重整工艺的RF功率，在一些实施例中，将50-800W，优选200-600W的RF功率施加到电极，如对于300-mm晶片测量的(使用300-mm晶片的单位面积计算的RF功率(W/cm2)，对于不同尺寸的晶片可以计算RF功率)。
关于重整工艺的持续时间，在一些实施例中，等离子体处理(施加RF功率的时期)持续2-300秒，优选10-30秒。
在一些实施例中，衬底具有在其表面上的图案化的凹部或台阶，非晶碳聚合物膜沉积在所述表面上，尽管重整工艺也适用于沉积在平坦表面上作为毯式碳聚合物膜的非晶碳聚合物膜。
实施例关于作为示例且没有任何限制的附图进行说明。
图5是示出了根据本发明的一个实施例的膜形成工艺顺序的图表，其中以灰色的单元格表示开启状态，而以白色的单元格表示断开状态，并且每栏的宽度列不代表每个过程的持续时间。通过这种该重整技术，可以显著改善非晶碳聚合物膜的热稳定性，并且还可以显著降低膜的干蚀刻速率。
这个过程顺序包括沉积工艺(“进料”→“吹扫”→“RF脉冲-1”(等离子体聚合)→“吹扫”)，以及等离子体处理工艺(“稳定”→“RF脉冲-2”(等离子重整)→“吹扫”)。等离子体聚合工艺包括使用无Si和金属、含有C的前体和等离子体生成气体，通过PEALD将非晶碳聚合物膜沉积在衬底上的台阶表面上，所述等离子体生成气体通过在两个电极之间施加射频功率(RF)生成等离子体，衬底平行地放置在所述两个电极之间，其中在PEALD的每个单层沉积循环中施加RF功率，其中所述等离子体生成气体和载气连续流动，并且还在“进料”后的“吹扫”期间以及在“RF脉冲-1”后的“吹扫”期间充当吹扫气体。
沉积工艺是PEALD工艺，在起始等离子体处理工艺前，对于其形成单层的一个循环可以重复q次，直到获得所需厚度的非晶碳聚合物膜，其中q是1至50(优选3至35)的整数，取决于膜的预期用途等，以便在起始等离子处理工艺前，沉积具有1nm至15nm(优选5nm至10nm)厚度的非晶碳聚合物膜。
接下来，等离子体处理工艺开始，其包括将重整气体(Ar和/或He)进料到反应空间(“稳定”)，所述反应空间通过RF功率(RF)激发，以生成等离子体且重整非晶碳聚合物膜，而无需进一步沉积聚合物膜(“RF脉冲-2”)，随后为吹扫(“吹扫”)，其中在等离子体处理工艺自始至终，将重整气体连续地进料到反应空间。例如，在100Pa至600Pa(优选200Pa至400Pa)的压力下，所述压力低于(例如，小于一半)用于等离子体聚合的那种，用于等离子体重整的RF功率在50W至1000W(优选150W至500W)的范围内，其等于或高于用于等离子体聚合的那种。通常，通过等离子处理，膜的厚度可以基本上不变或可以略微降低(例如，大于0％，小于10％，更通常小于5％)。
在一些实施例中，在整个工艺自始至终，载气例如以0sccm至2000sccm(优选100sccm至500sccm)的范围连续地进料到反应空间。另外，工艺的温度可以在-50℃至175℃(优选35℃至150℃)的范围内。
沉积工艺中的等离子体生成气体和等离子体处理工艺中的重整气体可以相同或不同，例如，两者均可以为Ar和/或He。
进一步地，需要时，沉积工艺和等离子体处理工艺重复p次，直到获得具有所需厚度的非晶碳聚合物膜，其中p是1至120(优选3至24)的整数，取决于膜的预期用途等，以便沉积具有5nm至1000nm(优选20nm至200nm)厚度的最终非晶碳聚合物膜。
载气的连续流动可以使用流通系统(FPS)来实现，其中载气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进行切换，其中当预期仅将载气进料到反应室时，关闭绕道管线，而当预期将载气和前体气体两者进料到反应室时，关闭主管线，并且载气流过绕道管线且连同前体气体一起从瓶中流出。通过这种方式，载气可以连续流入反应室中，并且可以通过在主管线与绕道管线之间切换而运载呈脉冲形式的前体气体。图1B示出了根据本发明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的(a)中所示，当将前体进料到反应室(未显示)时，首先，载气，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中。载气从瓶20中流出，同时运载量对应于瓶20内部的蒸气压的前体气体，并且流过具有阀f和e的气体管线，并且接着与前体一起进料到反应室。在上文中，阀a和d是关闭的。当仅将载气(稀有气体)进料到反应室时，如图1B的(b)中所示，载气流过具有阀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。
工艺循环可使用任何合适的设备，包括例如图1A中示意的设备来执行。图1A是PEALD设备的示意图，所述设备宜与被编程以进行下文所描述的工序的控制装置结合，可用于本发明的一些实施例中。在这个图中，通过提供一对并联并且在反应室3的内部11(反应区)中彼此面对面的导电平板电极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。在下部平台2(下部电极)中提供温度调节器，并且使其上所放置的衬底1的温度在给定温度下保持恒定。上部电极4也充当喷淋板，并且反应气体和/或稀释气体(如果存在的话)以及前体气体分别通过气体管线21和气体管线22以及通过喷淋板4引入反应室3中。此外，在反应室3中，提供具有排气管线7的环形管道13，通过所述管道排出反应室3的内部11中的气体。另外，安置在反应室3下方的传送室5具备密封气体管线24以将密封气体通过传送室5的内部16(传送区)引入到反应室3的内部11中，其中提供用于分隔反应区和传送区的隔离板14(此图省略闸阀，晶片通过闸阀传入传送室5或从所述传送室传出)。转移室还具备排气管线6。在一些实施方案中，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他含氧气氛。
在一些实施例中，在图1A中所描绘的设备中，图1B中示出的切换非活性气体的流动与前体气体的流动的系统(较早描述)，可以用于引入以脉冲形式的前体气体，而基本上不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(用于加工彼此靠近设置的晶片的两个部分或隔室)，其中反应物气体和稀有气体可以通过共享管线供给，而前体气体通过非共享管线供给。
具有填充能力的膜可以应用于各种半导体装置，包括但不限于3D交叉点存储装置中的单元隔离、自对准通孔、伪栅极(替换当前的多晶Si)、反向色调图案化、PC RAM隔离、切割硬掩模和DRAM存储节点接触(SNC)隔离。
实例
在其中未指定条件和/或结构的下述实例中，鉴于本公开内容，本领域的技术人员可以容易地作为例行实验提供此类条件和/或结构。熟练的技术人员应了解，实例中所用的设备包含(多个)控制器(未示出)，其被编程或以其它方式配置成使得能够进行本文其它地方所描述的沉积和反应器清洁工艺。如技术人员应了解的，(多个)控制器与各种电源、加热系统、泵、机器人装置和反应器的气体流量控制器或阀连通。
实例1
通过在美国专利申请号16/026,711中定义的类PEALD工艺，将非晶碳聚合物膜沉积在Si衬底(具有300mm的直径和0.7mm的厚度)上，其每个沉积循环使用图1A中所示的设备和图1B中所示的气体供给系统(FPS)，在下表1中所示的条件下，如图5中所示的沉积工艺进行。由于如图5中所示的重整工艺在类PEALD工艺的每12个循环(q＝12)后进行，所以在下表2中所示的条件下，该工艺在与沉积工艺相同的反应室中进行。将上述组合循环重复24次(p＝24)。膜的总(最终)厚度为大致100nm。
表1(数值为近似值)
Figure BDA0002470906290000111
表2(数值为近似值)
Figure BDA0002470906290000112
在重整工艺中，每当膜厚度增加约5nm增量(沉积循环与重整循环的比率为12)时，将非晶碳聚合物膜暴露于Ar等离子体(“Ar”)或He等离子体(“He”)。作为比较实例，未在“STD”中进行重整工艺，即，沉积非晶碳聚合物膜而无重整工艺。每种所得的非晶碳聚合物膜(三种“STD”膜、一种“Ar”膜和两种“He”膜)在下表3中所示的条件之一下进行退火，以便评估每种膜的热稳定性(在退火后的膜收缩)。
表3(数值为近似值)
Figure BDA0002470906290000121
结果显示于图2中。图2是显示了在退火后，没有等离子体处理(“STD”)、具有Ar等离子体处理(“Ar”)、以及具有He等离子体处理(“He”)的非晶碳膜的收缩的图。如图2中所示，与没有等离子体循环处理形成的非晶碳聚合物膜相比，使用Ar或He等离子体循环处理形成的非晶碳聚合物膜显示在各种退火条件下令人惊讶的低收缩，指示高热稳定性。
图3显示了(在经受退火之前)没有等离子体处理(“STD”)、具有Ar等离子体处理(“Ar”)、以及具有He等离子体处理(“He”)的非晶碳膜的傅立叶变换红外(FTIR)光谱。如图3中所示，与没有等离子体循环处理形成的非晶碳聚合物膜相比，使用Ar或He等离子体循环处理形成的非晶碳聚合物膜显示H相关峰的显著降低，其中Ar或He等离子体循环处理减少了热不稳定的甲基和亚甲基级分。
实例2
以与实例1中相同的方式形成非晶碳聚合物膜(“STD”、“Ar”和“He”)，并且评估所得的非晶碳聚合物膜的特性。结果显示于下表4中。
表4(数值为近似值)
Figure BDA0002470906290000131
如表4中所示，具有He等离子体处理的非晶碳聚合物膜(“He膜”)的热收缩率显著低于没有等离子体处理的非晶碳聚合物膜(“STD膜”)的那种，其中He膜的热收缩率基本上为零，指示He膜的热稳定性极佳。除图3的FTIR中所示的结果之外，考虑到表4中的数据显示He等离子体处理影响膜的特性，其方式为He膜的RI高于STD膜的RI，He膜的水接触角低于STD膜的水接触角，与STD膜的应力相比，He膜的应力是高度压缩的，并且He膜的C含量高于STD膜的C含量，而H膜的H含量低于STD-膜的H含量，He等离子体处理很可能已促进了膜基质的进一步聚合，从而减少了来自非晶碳聚合物膜的热不稳定的氢相关级分，例如甲基和/或亚甲基级分，并且减少了在表面处的氢键。应当注意，在每种膜中都检测到氧原子，并且这可能是因为在衬底从反应室中取出后，膜暴露于空气中。
有趣的是，根据图3的FTIR中的数据和表4中所示的数据，如以类似于He等离子体处理的方式分析的，在Ar等离子体处理中，聚合看起来比He等离子体处理中进展更少，其中聚合进展到一定程度，减少了膜基质中的氢键，而在表面上的氢键增加(在表面上的更多氢化)。因此，尽管Ar膜的组成看起来与STD膜的组成基本上相同，但与氢相关的膜的化学结构视为不同的，其中Ar膜比STD膜更热稳定，但比He膜更热不稳定。在一些实施例中，Ar膜和He膜是氢化的非晶碳聚合物，其组成由大于50％的碳原子和大于35％但小于50％的氢原子构成(如使用例如卢瑟福背散射光谱法(RBS)测量的)，其中热收缩率小于10％(优选小于5％)，如在置于作为参考/标准条件的N2的气氛中、在400Pa的压力下、在300℃的温度下30分钟时测量的。
实例3
将非晶碳聚合物膜沉积在具有SiO衬里的Si衬底(具有300mm的直径和0.7mm的厚度)上，所述SiO衬里含有具有大约90nm深度(纵横比为大约1.8)、与大约50nm开口的窄/深沟槽，以及具有大约90nm深度、与大约5nm至10nm开口的窄/浅沟槽，其方式与实例1中用He的重整相同，除了He等离子体处理在大约每10nm后进行(24个沉积循环)之外，如在平面表面上测量的(如毯式沉积)。
图4显示了经受具有He等离子体处理的间隙填充工艺(自下而上沉积)的沟槽的横截面视图的STEM照片，其中箭头显示了指示He等离子体处理的略微更暗的界面。尽管较暗的界面指示He等离子体处理，但它们并不代表通过He等离子体处理而重整的层，即重整效果渗透超出界面并到达层在相邻界面之间的较深部分。在本实例中，使用SiO衬里，以便减少结构的CD，且SiO衬里是唯一保形的层。如通过箭头所示，虽然如在平面表面上测量的，每大约10nm循环进行He等离子体处理，但在沟槽中观察到非晶碳聚合物的粘稠液体状行为，其中相邻界面之间的距离在沟槽中显著大于在沟槽上方。有趣的是，随着膜生长进展，相邻界面之间的距离从底部开始逐渐增加，并且在深度中在沟槽的中间变得最大，然后朝向沟槽的顶部逐渐降低，指示非晶碳聚合物表现如粘性液体。进一步地，膜在窄沟槽中比在更宽的沟槽中更快速填充，指示体积增长。由于He等离子体处理形成了充当沉积标记物的较暗界面，因此在STEM照片中可以容易地观察到上述行为。通常，例如，等离子体重整效果达到约10nm的深度，并且因此，在其中相邻界面之间的距离大于10nm的沟槽内部，等离子体重整效果可以视为不足的；然而，看起来暂时沉积在沟槽的顶部和侧壁上，且暴露于Ar/He等离子体的膜部分向下移动以填充沟槽，并且因此，预期每个非晶碳聚合物层可能是相对均匀的，即使它们的厚度在沟槽内部超过10nm(与沟槽的侧壁和顶部相邻的界面不如远离侧壁和顶部的界面清晰)。
本领域的技术人员应理解，可以进行众多和各种修改，而不脱离本发明的精神。因此，应清楚地理解，本发明的形式仅是示意性的，而非意在限制本发明的范围。

Claims (9)

1.一种用于重整非晶碳膜的方法，作为其沉积工艺的一部分，所述方法包括以下工艺：
(i)在反应空间中将非晶碳膜沉积在衬底上，直到所述非晶碳膜的厚度达到预定厚度，然后停止沉积工艺；和
(ii)在基本上不含氢、氧和氮的气氛中，将所述非晶碳膜暴露于Ar和/或He等离子体。
2.根据权利要求1所述的方法，其中工艺(i)和(ii)重复多次，直到所述非晶硅膜的厚度达到所需的最终厚度。
3.根据权利要求1所述的方法，其中所述工艺(i)中的预定厚度是单层厚度或更大，但为10nm或更小。
4.根据权利要求1所述的方法，其中所述工艺(ii)中的气氛在工艺(i)中使用的反应空间中。
5.根据权利要求1所述的方法，其中所述工艺(ii)中的气氛在与工艺(i)中使用的反应空间不同的另一个反应空间中。
6.根据权利要求1所述的方法，其中工艺(ii)包括：
将Ar和/或He进料到气氛中，但不进料氢、氧和氮；以及
以生成所述Ar和/或He等离子体的方式，将RF功率施加到所述气氛中。
7.根据权利要求6所述的方法，其中RF功率在每单位面积衬底0.06W/cm2至0.96W/cm2的范围内，并且工艺(ii)的持续时间在2秒至300秒的范围内。
8.根据权利要求1所述的方法，其中工艺(i)通过等离子体增强的原子层沉积(PEALD)来进行。
9.根据权利要求1所述的方法，其中所述衬底具有在其表面上的图案化的凹部或台阶，所述非晶碳膜沉积在所述表面上。
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