CN100366792C - 薄膜形成方法及薄膜形成装置 - Google Patents

薄膜形成方法及薄膜形成装置 Download PDF

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CN100366792C
CN100366792C CNB018203493A CN01820349A CN100366792C CN 100366792 C CN100366792 C CN 100366792C CN B018203493 A CNB018203493 A CN B018203493A CN 01820349 A CN01820349 A CN 01820349A CN 100366792 C CN100366792 C CN 100366792C
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山﨑英亮
河野有美子
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Abstract

本发明涉及一种采用ALD法的薄膜形成方法及薄膜形成装置，通过ALD法将多种原料气体逐类、并经多次供应，进行成膜，在此工序之前，实施同时提供多种原料气体中的至少两种的前置处理，从而使得成膜中的潜伏期缩短并提高产率。

Description

薄膜形成方法及薄膜形成装置
技术领域
本发明涉及薄膜形成方法及薄膜形成装置，本发明尤其涉及通过交替供应原料气体来形成膜的薄膜形成方法及薄膜形成装置。
背景技术
近年，伴随半导体集成电路的微细化、高集成化，要求在基片(例如半导体基片)上形成的绝缘膜及金属布线膜等，能够达到薄膜化，并且具有很好地覆盖复杂形状的、对晶片整体来说宏观均匀、同时在微观上达到纳米级平滑的效果。但是，传统的化学气相淀积法(CVD法)不能完全满足所述全部要求。另一方面，ALD(Atomic LayerDeposition)法作为能够满足这些要求的成膜方法，备受关注。该ALD法是，在成膜时，通过对原料气体逐类地进行交替供应，使得原料气体吸附在反应表面，进而形成原子层、分子层级的膜，重复这些工序就得到规定厚度的薄膜。
具体地说，向基片上供应第一原料气体，并在基片上形成其吸附层。之后，向基片供应第二原料气体并使之反应。根据该方法，因为第一原料气体在基片上吸附后与第二原料气体反应，所以可以使成膜温度低温化。
并且，对于在孔上的成膜，也能够避免传统的CVD法无法解决的问题，即原料气体在孔的上部反应而被浪费，从而导致覆盖能力低下。
还有，吸附层的厚度一般为原子、分子的单层，或者最多也就是2、3层，并且具有一种自调节性，根据其温度和压力，即使供应多于形成吸附层所需量的原料气体，也能将多余部分排出，因此有利于控制超薄膜的厚度。而且，因为以原子层、分子层级进行一次成膜，所以易进行完全反应，膜中很难残留杂物，比较理想。
但是，与如上所述的ALD法可以得到良好的膜特性相反，一次成膜是以原子层、分子层级进行的，因此，由此而来的总成膜时间变得较长。
尤其是，因为存在最初的几个周期并不进行实质性成膜的潜伏期(培养期incubation time)，从而导致产率(throughput)严重低下。
发明内容
本发明的总的目的是提供一种解决上述问题的、经过改进的薄膜形成方法及薄膜形成装置。
本发明的更具体目的是，提供一种缩短ALD法的潜伏期并且产率高的薄膜形成方法及薄膜形成装置。
为了达到所述目的，本发明是一种在基片上反应多种原料气体，从而在该基片上形成薄膜的薄膜形成方法，其特征在于，具有：
同时提供所述多种原料气体中的至少两种的工序；以及
在实施该工序后，通过将所述多种原料气体逐类、依次经多次供应，从而形成薄膜的工序。
这样，在通过ALD法将多种原料气体逐类、依次经多次供应的成膜之前，实施同时提供多种原料气体中的至少两种的前置处理，  从而，使潜伏期缩短并提高产率。
此外，在所述说明中，将多种原料气体逐类、依次经多次供应时，在相互起反应的两种原料气体的供应过程的间歇，最好进行真空排气或用第三种气体进行替换。由此，在供应相互起反应的两种原料气体的间歇，可以避免不必要反应的发生。
还有，在所述发明中，所述原料气体最好是WF6气体、NH3气体、SiH4气体。由此，在基片上形成WNx薄膜。
还有，在所述发明中，同时提供所述多种原料气体中的至少两种的时间下限为0.1秒，而其上限最好是根据该气体的组成，形成厚度为2.0nm的膜时所用的时间。通过这样的设定，可以有效缩短潜伏期。
附图的简要说明
参照附图阅读以下的详细说明，就会进一步了解本发明的其他目的、特征以及优点。
图1是通过现有的ALD法进行成膜的流程图。
图2是分别实施现有的ALD法和根据本发明的超薄膜形成方法时，原料气体供应周期数和成膜厚度的关系图表。
图3是用于实施本发明中超薄膜形成方法的真空处理装置的简单结构图。
图4是本发明一个实施例的W2N薄膜形成方法的实施流程图。
图5是实施本发明一个实施例的薄膜形成方法时的，晶片温度与一个周期的成膜厚度的关系图表。
图6是实施本发明一个实施例的薄膜形成方法时的，WF6气体或NH3气体的供应量与每一个周期的成膜厚度的关系示意图。
图7是本发明一个实施例的薄膜形成方法的实施流程图。
图8是用于实施本发明中一个实施例的薄膜形成方法的真空处理装置的简单结构图。
图9是本发明一个实施例的TiN薄膜形成方法的实施流程图。
本发明的最佳实施方式
以下，参照附图说明本发明的实施例。
图3是用于实施本发明中一个实施例的薄膜形成装置(以下称为真空处理装置)的简单结构图。
在说明薄膜形成方法之前，先说明一下用于薄膜形成的真空处理装置。
所述真空处理装置由气体供应源10A～10C、喷头20、喷头加热器21、容器30、容器加热器31、基座32、支撑部件33、排气管40、阀41、真空泵42及电源50等构成。
气体供应源10A～10C经过设在喷头20的气体流入口22～24、及导入通路25、26等，向容器30内供应气体。即，气体供应源10A～10C分别供应气体，使得这些气体对容器30内的半导体晶片W进行设定的成膜处理。具体地说，气体供应10A供应作为原料气体的WF6气体，气体供应10B供应作为原料气体的NH3气体，气体供应10C供应作为原料气体的SiH4(硅烷)气体。
喷头20设置在贯通容器30的上壁中央部分的位置。本实施例所示的喷头20由组装成一体的、上下3层的块体20A、20B、20C构成。设置在该喷头20中的气体流路25(由25A、25B、25C组成)，从气体供应10A经过图中未示出的质量流控制器(mass flow controller)等，按设定的流量供应WF6气体。
而且，设置在喷头20中的气体流路26(由26A、26B、26C组成)，从气体供应10B、10C经过图中未示出的质量流控制器等，按设定的流量供应NH3气体及SiH4气体。此时，各气体流路25、26被设计成能够均匀地向容器30内供应各种气体的结构。
此时，将供应WF6气体的气体流路25和供应NH3气体、SiH4气体的气体流路26分开，其理由是为了抑制WF6气体与NH3气体或与SiH4气体在喷头20内发生反应。还有，当有必要抑制NH3气体与SiH4气体的反应时，也可以采用进一步分割气体流路26的结构。
还有，虽然图中没有示出，喷头20中还设有供应惰性气体的气体流入口或流路，其中，所述惰性气体是稀释前置处理及成膜中所用气体的Ar或N2等，而该气体流入口经过质量流控制器等连接在惰性气体的气体供应源上。
喷头加热器21设置在喷头20的上面，控制喷头20的温度，从而，对通过喷头20内部的气体进行加热及防止NH4F等低汽压反应副生成物向喷头20的附着。并且，容器30是用于对半导体晶片W进行规定处理的处理室。
基座32由支撑部件33固定在容器30内，用于装载通过图中没有示出的搬运机构搬运来的、作为处理对象的半导体晶片W。而且，基座32内部备有，将半导体晶片W导向基座32中央侧的导向环(guidering)34和用于控制半导体晶片W的温度的台式加热器35。台式加热器35由设置在容器30外的电源50供电。
排气管40设置在容器30底部，经过调节排气流量的阀41连接在真空泵42上。真空泵42通过排气管41将气体从容器30内排出，可以使容器30内部达到真空度或维持在规定的压力上，其中，所述达到真空度由真空泵42的排气能力、容器30、排气管40和阀41的通过能力(conductance)决定。
接下来，就本发明人使用上述真空处理装置实施的薄膜处理方法进行说明。本发明人就通过ALD法的成膜方法，按照如图1所示的流程图进行了成膜，并特别研究了成膜初期的状态。以下，就图1所示的薄膜形成处理的每个处理进行说明。
(步骤100)将半导体晶片W搬入容器30内，并装载在预先加热到规定温度如450度的基座32上。
(步骤110)向喷头20供应Ar或N2等惰性气体的同时，对容器30进行排气，使得其内压保持在如400Pa，同时通过基座32的传热对半导体晶片进行加热。
(步骤120)停止气体的供应，对容器30进行真空排气，使其内气压达到如20Pa以下。
(步骤130)向喷头20供应混合了若干Ar、N2的 WF6气体，同时，对容器30进行排气，使得其内部保持在规定的压力上，例如供应WF6气体，使其为，分压×时间＝470Pa.sec。
(步骤140)停止气体的供应，对容器30进行真空排气，使其内气压达到如20Pa以下。
(步骤150)向喷头20供应混合了若干Ar、N2的NH3气体的同时，对容器30进行排气，使得其内部保持在规定的压力上，例如向晶片上较均匀地供应NH3气体，使其气压×时间达到470Pa.sec。
(步骤160)停止气体的供应，对容器30进行真空排气，使其内气压达到如20Pa以下。
(步骤170)按规定的次数重复(步骤130)到(步骤160)。
对经过所述处理形成的薄膜进行研究的结果可知，用ALD法形成氮化钨膜(W2N膜)时，如图2中点划线B所示，在成膜初期10个周期内没有进行实质性的成膜，即存在相当于10个周期的潜伏期T。
这里，为了减小所述潜伏期T，本发明人就前置处理进行了反复研究发现，通过同时提供多种原料气体中的至少两种的前置处理，如图2的实线A所示，所述潜伏期T成为0，从而可以从最初的第1个周期开始进行成膜。
图4是根据本发明改进的薄膜形成方法的实施流程图。本发明的特征在于，在步骤110与步骤120之间，作为步骤115，实施了同时提供多种原料气体中的至少两种的前置处理。以下，就图4中所示的薄膜形成装置的各个处理进行说明。还有，在图4中，与先前说明的图1所示的处理相同的处理，也采用同样的步骤号表示。
(步骤100)将半导体晶片W搬入容器30内，并装载在预先加热到规定温度如450度的基座32上。
(步骤110)向喷头20供应Ar或N2等惰性气体，同时，对容器30进行排气，使得其内压保持在如400Pa，并通过基座32的传热对半导体晶片进行加热。
(步骤115)进行一种前置处理，即，将混合了若干Ar、N2并将分压调整到如下量的WF6气体和NH3气体同时提供7.5sec。该处理时间相当于用所述流量构成形成厚度为1nm的W2N膜时所用的时间。而且，此时的WF6气体的分压为0.2Pa，NH3气体的分压为102Pa。
(步骤120)停止气体的供应，对容器30进行真空排气，使其内气压达到如20Pa以下。
(步骤1 30)向喷头20供应混合了若干Ar、N2的 WF6气体，同时，对容器30进行排气，使得其内部保持在规定的压力上，例如供应WF6气体，使其为，分压×时间＝470Pa.sec。
(步骤140)停止气体的供应，对容器30进行真空排气，使其内气压达到如20Pa以下。
(步骤150)向喷头20供应混合了若干Ar、N2的NH3气体的同时，对容器30进行排气，使得其内部保持在规定的压力上，例如向晶片上较均匀地供应NH3气体，使其气压×时间达到470Pa.sec。
(步骤160)停止气体的供应，对容器30进行真空排气，使其内气压达到如20Pa以下。
(步骤170)按规定的次数重复(步骤130)到(步骤160)。
这里，对图1所示的流程图对应的薄膜形成方法与图4所示的流程图对应的薄膜形成方法比较并进行说明。
不按照图4所示的、与本发明相关的薄膜形成方法，而按照图1所示的流程图进行成膜，并从(步骤130)到(步骤170)重复30个周期时，在最初的10个周期没有形成膜，此后，在20个周期中以每周期0.64nm的速度形成膜，因此作为膜的总厚度达到了12.8nm。
另一方面，根据本发明，按照图4的流程图进行成膜，并从(步骤130)到(步骤170)同样地重复30个周期时，因为从最初的第1个周期开始形成膜，所以，膜的总厚度达到了20.1nm，进而改善了产率。
这里，所述实施例所示的是，通过ALD法形成W2N膜时，在供应WF6气体和NH3气体的间歇进行真空排气的例子。然而，本发明并不局限于该例，也可以用规定的气体代替真空排气来将WF6气体或NH3气体挤出，即进行所谓的净化处理。具体地说，停止WF6气体或NH3气体的供应后，例如供应500sccm以上大流量的Ar、N2等惰性气体或H2气体，从而挤出容器30内的WF6气体或NH3气体。
这里，采用H2气体作为净化气体尤其对不希望W2N膜被氧化的情况很有效。并且，将真空排气、净化、真空排气作为一组应用时，虽然会延长总成膜时间，但因为增强除去残留的WF6气体或NH3气体的效果，所以比较好。
还有，所述实施例所示的是，作为用ALD法形成W2N膜的条件，即，将晶片温度设为370℃、将WF6气体和NH3气体的每周期供应量都设为470Pa.sec，其结果，每周期所形成的W2N膜的量大约在0.6到0.7nm的例子。然而，本发明人就所述W2N膜的形成方法进行反复研究的结果，发现了以下如图5、6所示的关系。
图5表示的是每一个周期的成膜厚度和晶片温度的关系。如图中所示，晶片温度在300℃～450℃的范围时，每个周期的成膜厚度不依赖于晶片温度而保持一定。然而，当晶片温度超过450℃后，每个周期的成膜厚度发生减小的现象。每个周期的成膜厚度不依赖于晶片温度而保持一定的所述区域，表示其反应是以原料的吸附作为决定速度的过程。因而，以其良好的控制能力、优良的覆盖性，比较适合作为获得W2N膜的区域。
并且，图6是在晶片温度370℃的环境下进行实验所得到的，表示每个周期的成膜厚度与WF6气体或NH3气体的供应量关系的例子。如图所示可知，当气体供应量在200Pa.sec以上时，每个周期的成膜厚度达到饱和。该区域表示的反应进行是以原料的吸附作为决定速度的过程。因而，以其良好的控制能力、优良的覆盖性，比较适合作为获得W2N膜的区域。
还有，所述实施例中，同时提供多种原料气体中的至少两种以上的前置处理(即，图4中的步骤115那样的处理)的时间为7.5sec。然而，该处理时间并不局限于此。
在图4的步骤115进行的所谓前置处理，具有重整(改質)对象表面(晶片表面)，从而使在此后用ALD法进行成膜时，容易吸附原料气体的效果。即，不管是多短的时间，只要由同时提供多种原料气体中的至少两种以上而成的混合体到达对象表面，就会有重整对象表面的效果，因而，将混合体到达对象表面所需要的时间作为处理时间的下限，为0.1sec以上。
另一方面，如果前置处理的时间超过相当于成膜2.0nm所需的时间，就会因为所述前置处理，在对象表面(晶片表面)形成膜。因此，通过ALD法所形成的膜，会在前置处理时形成的膜上形成。
在所述前置处理时形成的膜，因为是通过同时提供多种原料气体中的至少两种而形成的膜，所以与通过ALD法所形成的膜相比，其覆盖性、平滑性、纯度都比较差。从而，在所述前置处理时形成的膜影响在其上部通过ALD法所形成的膜，使得通过ALD法所形成的膜的覆盖性、平滑性、纯度等特性恶化。因此，不希望前置处理时间超过相当于形成厚度为2.0nm的膜的时间。
针对这种情况，当前置处理时间在相当于形成厚度为0.1nm～2.0nm的膜的时间范围内时，既可以促进基于ALD法的原料气体的吸附，同时也不影响通过ALD法所形成膜的膜质，因而，比较理想。
而且，2.0nm以下的膜非常薄，有时，甚至用如SEM(扫描式电子显微镜)等装置也无法检测到。但是，能够实现前置处理所带来的效果的膜的厚度，可以通过所述前置处理的实施时间来控制。从而，不需要直接测定通过前置处理所形成膜的厚度，而只是通过管理前置处理实施时间的简单处理，就可以达到上述规定的效果。
还有，在上述实施例中，对于用ALD法的成膜，说明了交替供应WF6气体和NH3气体来生成W2N膜的例子，但本发明并不局限于此，如图7所示的流程图，也可以将WF6气体、NH3气体、SiH4气体按该顺序反复供应。
此时，WF6气体和SiH4气体的供应次序相邻时，形成W或WSix等，因而，会形成W2N膜中含这些成分的混合膜(WNX)。因为W或WSix的电阻率比W2N低，所以可以通过改变各种气体的供应量或改变供应顺序来控制WNX膜中W或WSix的量。据此，可以获得低于W2N单膜的电阻率或是使膜中含有Si，进而，可以形成任意特性的薄膜。例如，当按WF6、SiH4、NH3、WF6、SiH4的顺序重复供应时，WNx中的W2N比率降低，W和WSix的比率增加，从而可以获得电阻率低的WNx膜。
此外，所述的实施例，采用图3所示的真空处理装置，当同时提供多种原料气体中的至少两种的前置处理时，以及其后将多种原料气体逐类多次供应而形成薄膜时(ALD法成膜时)，都通过喷头20来实施各种气体的供应。
但本发明并不局限于此，如图8(对于与图3结构相同的结构，用同一符号标注)所示，也可以具有，在前置处理时通过喷头20供应气体，但是在通过ALD法形成膜时，不经喷头20，而是从侧面将各种气体导入容器30内的结构。
具体结构是，将连接在气体供应源10A～10C的气体供应管道分成管道44A～46A和管道44B～46B，并将管道44A～46A接到喷头20，将管道44B～46B接到设置在容器30侧面的喷嘴47～49上。并且，通过在管道44A～46A上设置阀装置44C～46C，在管道44B～46B上设置阀装置44D～46D，来控制流过管道44A～46A及管道44B～46B内的气体流量。
在前置处理中，因为同时提供多种原料气体中的至少两种，所以需要喷头20使得能够向晶片表面均匀供应。因此，在前置处理时，关闭阀装置44D～46D的同时，打开阀装置44C～46C，并通过输送，向容器内供应原料气体。另一方面，用ALD法成膜时，关闭阀装置44C～46C的同时，打开阀装置44D～46D，从容器30的侧面供应原料气体。
用ALD法成膜时，因为原料气体的吸附过程决定成膜速度，所以气体的供应即使具有喷嘴47～49这样的结构也不成问题。从气体的替换观点看，与通过能力小的喷头20相比，使用结构简单的喷嘴47～49更为有利、合适。
并且，在上述实施例中，对于通过ALD法的成膜，主要说明了交替供应WF6气体和NH3气体来形成W2N膜的例子，以及交替供应WF6气体、NH3气体、SiH4气体来形成WNx膜的例子，但本发明并不局限于此，当然也适用于其它的金属膜或绝缘膜的成膜。
以下，根据图9说明，通过交替供应TiCl4气体和NH3气体形成TiN膜的例子。
(步骤300)将半导体晶片W搬入容器30内，并装载在预先加热到规定温度如450℃的基座32上。
(步骤310)向喷头20供应Ar或N2等惰性气体的同时，对容器30进行排气，使得其内压保持在如400Pa，同时通过基座32的传热对半导体晶片进行加热。
(步骤315)进行一种前置处理，即，将混合了若干Ar、N2并将分压调整到如下量的TiCl4气体和NH3气体同时提供10sec。该处理时间相当于用该流量结构形成厚度为2nm的TiN膜时所用的时间。
TiCl4分压＝23Pa，NH3分压＝301Pa
(步骤320)停止气体的供应，对容器30进行真空排气，使其内气压达到如20Pa以下。
(步骤330)向喷头20供应混合了若干Ar、N2的TiCl4气体，同时对容器30进行排气，使得其内部保持在规定的压力上，例如供应TiCl4，使其为，分压×时间＝260Pa.sec。
(步骤340)停止气体的供应，对容器30进行真空排气，使其内气压达到如20Pa以下。
(步骤350)向喷头20供应混合了若干Ar、N2的NH3气体的同时，对容器30进行排气，使得其内部保持在规定的压力上，例如向晶片上较均匀地供应NH3气体，使其达到665Pa.sec。
(步骤360)停止气体的供应，对容器30进行真空排气，使其内气压达到如20Pa以下。
(步骤370)按规定的次数重复(步骤330)到(步骤360)，如进行100个周期时，获得总厚度14nm。
此外，不按照所述实施例，没有进行步骤315的情况下，在(步骤370)重复(步骤330)到(步骤360)时，在最初的8个周期没有发现膜的形成，且在100个周期后获得了总厚度为12.8nm的膜。
以上，所述实施例所表示的是，通过ALD法形成TiN膜时，在供应TiCl4气体和NH3气体之间进行真空排气的例子，然而，它并不局限于此例，相反地，也可以在停止TiCl4气体或NH3气体的供应后，例如供应500sccm以上大流量的Ar、N2等惰性气体或H2，从而挤出容器30内的TiCl4气体或NH3气体。这里，H2尤其对不希望使TiN膜被氧化的情况是有效的。并且，将真空排气、净化、真空排气作为一组应用时，虽然会延长总成膜时间，但因为提高了除去残留的TiCl4气体或NH3气体的效果，所以较好。
如上述本实施例，在通过交替供应原料气体进行成膜的成膜方法(ALD法)的实施之前，通过实施同时提供多种原料气体中的至少两种的前置处理，能够缩短通过交替供应原料气体进行成膜的薄膜形成处理的潜伏期，进而可以进行高产率的薄膜形成。
本发明并不局限于具体公开的实施例，在不脱离本发明权利范围的条件下，可以采用各种变形例或实施例。

Claims (10)

1.一种薄膜形成方法，在基片上反应多种原料气体，从而在该基片上形成薄膜，其特征在于，具有：
同时提供所述多种原料气体中的至少两种的工序；以及
在实施该工序后，通过将所述多种原料气体逐类、依次经多次供应，从而形成膜的工序。
2.如权利要求1所述的薄膜形成方法，其特征在于，
将所述多种原料气体逐类、依次经多次供应时，在相互起反应的两种原料气体的供应过程间歇，进行真空排气或用第三种气体进行替换。
3.如权利要求1所述的薄膜形成方法，其特征在于，
所述原料气体是WF6气体、NH3气体、SiH4气体。
4.如权利要求2所述的薄膜形成方法，其特征在于，
所述原料气体是WF6气体、NH3气体、SiH4气体。
5.如权利要求3所述的薄膜形成方法，其特征在于，
同时提供所述多种原料气体中的至少两种的时间下限为0.1秒，而其上限为根据所述气体的组成，形成厚度为2.0nm的膜时所用的时间。
6.如权利要求4所述的薄膜形成方法，其特征在于，
同时提供所述多种原料气体中的至少两种的时间下限为0.1秒，而其上限为根据所述气体的组成，形成厚度为2.0nm的膜时所用的时间。
7.如权利要求1所述的薄膜形成方法，其特征在于，
所述原料气体是WF6气体和NH3气体。
8.如权利要求1所述的薄膜形成方法，其特征在于，
所述原料气体是TiCl4气体和NH3气体。
9.如权利要求1所述的薄膜形成方法，其特征在于，
在所述同时供应的工序中，同时供应所述多种原料气体中的含有所述薄膜的成分的彼此可反应的两种原料气体。
10.如权利要求9所述的薄膜形成方法，其特征在于，
在所述逐类、依次经多次供应的工序中，供应在所述同时供应的工序中供应的所述两种原料气体。
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