CN108987336B - 用于形成低温半导体层及相关半导体器件结构的方法 - Google Patents

用于形成低温半导体层及相关半导体器件结构的方法 Download PDF

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CN108987336B
CN108987336B CN201810508072.5A CN201810508072A CN108987336B CN 108987336 B CN108987336 B CN 108987336B CN 201810508072 A CN201810508072 A CN 201810508072A CN 108987336 B CN108987336 B CN 108987336B
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P·雷伊塞宁
M·B·莫萨
P-F·许
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Abstract

公开了一种在低温下形成具有良好膜闭合的金属氮化物膜的方法。所述方法可以包括利用等离子体形成NH和NH2自由基以允许在低温下形成所述金属氮化物。所述方法还可以包括使蚀刻气体流动以产生具有均匀厚度的无定形膜。所述方法还可以包括使烷基肼流动以抑制所述金属氮化物膜的三维岛状生长。

Description

用于形成低温半导体层及相关半导体器件结构的方法
相关专利申请的交叉引用
本公开要求2017年6月2日提交并且标题为“METHODS FOR FORMING LOWTEMPERATURE SEMICONDUCTOR LAYERS AND RELATED SEMICONDUCTOR DEVICE STRUCTURES”的美国临时专利申请第62/514,585号的权益，该临时专利申请以引用方式并入本文。
技术领域
本公开总体上涉及用于在低温下形成半导体层的方法。具体而言，本公开例如涉及氮化物薄膜如氮化钛(TiN)薄膜的形成。这些氮化物膜由于膜闭合而以产生均匀膜的方式形成。
背景技术
氮化物膜已经用许多不同的方法形成。一些方法通过岛状生长导致形成膜。岛状生长可包括这样一个过程，其中多个单独的膜开始生长，在单独的膜生长之间的空白区域在随后的时间被填充。生长可像通过Volmer-Weber生长而建模的那样发生。
图1A-1D说明可能发生Volmer-Weber生长的现有技术方法。在图1A中，器件100包括衬底110和单层120。例如，衬底110可以包括氧化铪，而单层120可以包括氮化钛。单层120最初可以通过成核而形成并且可以在两个维度上横向生长。在衬底110上可以有多个不同的单层120。
在Volmer-Weber生长的下一个步骤中，可以存在在单层120上在第三个维度中生长的膜，从而形成尖峰生长体130，如图1B所示。由于尖峰生长体的表面能增加、表面化学封端和可用反应位点的密度，尖峰生长体130的形成可能是有利的。图1C示出了单层120已经转化成衬底110顶部上的尖峰生长体130的情形。
如图1D所示，Volmer-Weber生长可以继续，使得整个衬底110被尖峰生长体150覆盖，从而形成氮化钛的单层140。然而，试图让膜生长以完全填满空间可能会遇到困难。例如，在Volmer-Weber生长模型中，在最佳情况下，膜生长可能不会超过15-20埃。膜厚度小于20埃时，可能无法实现膜闭合。
因此，希望开发一种方法，其中可以通过闭合而形成膜，从而产生均匀的膜。该方法可应用于形成无定形膜或结晶膜。
附图说明
尽管本说明书以具体地指出并且明确地要求保护被视为本发明实施方案的内容的权利要求书结束，但是当结合附图阅读时，可以从本公开实施方案的某些实例的描述中更容易地确定本公开实施方案的优势，在附图中：
图1A、图1B、图1C和图1D示出了根据Volmer-Weber生长的现有技术的膜生长过程；
图2、图3和图4示出了根据本发明实施方案的用于形成膜的方法；以及
图5、图6和图7示出了根据本发明实施方案的用于形成膜的方法。
应了解，图中的元件仅为简单和清晰起见而进行说明，并且不一定按比例绘制。例如，图中的一些元件的尺寸可能相对于其他元件放大，以有助于改善对本公开所说明实施方案的理解。
具体实施方式
尽管下文公开某些实施方案和实例，但所属领域的技术人员应理解，本发明延伸超出了所具体公开的实施方案和/或本发明的用途以及显而易见的修改和其等效物。因此，预期本发明所公开的范围不应受下文所描述具体公开实施方案的限制。
如本文中所使用，术语“衬底”可以指可以使用或上面可以形成有器件、电路或膜的任何一种或多种底层材料。
本公开的实施方案可以包括用于在低温下形成金属氮化物膜的方法。所形成的膜可以是具有高度均匀性的无定形膜或结晶膜。所形成的膜可以是连续的无定形膜。膜可以形成在反应室内的衬底上。本发明的一个目的是形成无定形膜，形成方式使得可以避免类似于图1A-1D中所示的三维尖峰生长或岛状生长。本公开的实施方案可以包括在亚纳米级膜中实现超薄膜的良好膜闭合。在生产亚纳米闭合的TiN膜和pMOS多Vt调谐应用中，可以实现良好的膜闭合。
在本发明的一个实施方案中，在图2中公开了形成金属氮化物膜的方法。通过该方法形成的膜可以包括氮化钛(TiN)、氮化钨(WN)、氮化铪(HfN)、氮化铌(NbN)、氮化锆(ZrN)、氮化钽(TaN)和三元膜，例如钛氮化钽(TiTaN)。该方法可以包括金属氮化物子循环200和另外的处理子循环250。该方法还可以包括金属氮化物子循环200的重复循环300、可选的处理子循环250的重复循环310或整个方法的重复循环320。
图3示出了金属氮化物子循环200。金属氮化物子循环200可以包括金属卤素前体步骤210、惰性气体吹扫220、含氮等离子体前体步骤230和惰性气体吹扫240。金属卤素前体步骤210可以包括使例如以下金属卤素前体流动或脉冲到衬底上：例如氯化钛(TiClx)、溴化钛(TiBrx)、氟化钛(TiFx)、碘化钛(TiIx)、氯化钨(WClx)、溴化钨(WBrx)、氟化钨(WFx)、碘化钨(WIx)、氯化铌(NbClx)、溴化铌(NbBrx)、氟化铌(NbFx)、氯化钽(TaClx)、溴化钽(TaBrx)、氟化钽(TaFx)、氯化铪(HfClx)、溴化铪(HfBrx)、氯化锆(ZrClx)或溴化锆(ZrBrx)。惰性气体吹扫220和惰性气体吹扫240可以是可选的，或者可以包括使惰性气体例如氩气、氦气、氪气或氮气流动或脉冲。
金属氮化物子循环200还可以包括含氮等离子体前体步骤230。在该步骤中，当使氮气(N2)、氢气(H2)、氨气(NH3)、肼(N2H4)或叔丁基肼(C4H9N2H3)流动或脉冲到衬底上时，可以使用等离子体来形成NH或NH2自由基。自由基可以远程或原位形成。所形成的自由基是高度反应性的并且允许在低温下在衬底上形成金属氮化物。反应室的温度可低于300℃、低于250℃或低于200℃。反应室的压力可以在0.1与10托之间、或在1与5托之间、或在1与3托之间。
另外的处理子循环250可以是可选的并且可以包括可选的膜退火步骤260或可选的膜刻蚀步骤270，如图4所示。可选的膜退火步骤260可以导致膜致密化和潜在的结晶。可选的膜退火步骤260可以导致光滑的膜、结构的致密化和杂质的去除，从而产生更薄的膜。
可选的膜蚀刻步骤270可以包括热原子层蚀刻步骤。可选的膜蚀刻步骤270可以用于使用肼或肼衍生物形成的那些金属氮化物膜。在蚀刻步骤270期间，可以使蚀刻气体流动，包括：氯化钼(MoCl5)、氯化铌(NbCl5)、氯化钨(WCl5)、氟化铌(NbF5)、氯化钽(TaCl5)或氟化钽(TaF5)。蚀刻气体可以具有在超过一百个循环后完全蚀刻厚金属氮化物层的能力。
在可选的膜蚀刻步骤270期间反应室的温度可以低于500℃、低于450℃或低于400℃。在可选的膜蚀刻步骤270期间反应室的压力可以在0.1与10托之间、或在1与5托之间、或在1与3托之间。
由图2-4所示的方法产生的膜可具有膜闭合良好的无定形质量。例如，可以形成小于15埃的闭合的TiN膜。该方法的实施方案还可以应用于形成小于10埃的闭合的结晶膜。
在本发明的一个实施方案中，在图5中公开和示出了用于在衬底上形成金属氮化物膜的方法。该方法可以包括岛形成步骤400、烷基封端步骤410和金属氮化物形成步骤420。该方法中的每个步骤可以使用原子层沉积(ALD)技术和方法来形成。
类似于图1A中所示的情形，岛形成步骤400可导致在衬底上的多个不同位置处的金属氮化物膜的成核生长。随着岛的形成，岛上可存在反应位点以及衬底上可存在反应位点(例如-OH封端位点)。岛形成步骤400可以包括例如金属卤素前体和氮前体例如氯化钛和氨的流动。烷基封端步骤410(如图6所示)可用于使岛上的反应位点封端。
烷基封端步骤410可以包括金属卤素前体步骤500、惰性气体吹扫步骤510、烷基肼前体步骤520和惰性气体吹扫步骤530。金属卤素前体步骤500可以包括使例如以下金属卤素前体流动或脉冲到衬底上：例如氯化钛(TiClx)、溴化钛(TiBrx)、氟化钛(TiFx)、碘化钛(TiIx)、氯化钨(WClx)、溴化钨(WBrx)、氟化钨(WFx)、碘化钨(WIx)、氯化铌(NbClx)、溴化铌(NbBrx)、氟化铌(NbFx)、氯化钽(TaClx)、溴化钽(TaBrx)、氟化钽(TaFx)、氯化铪(HfClx)、溴化铪(HfBrx)、氯化锆(ZrClx)或溴化锆(ZrBrx)。惰性气体吹扫510和惰性气体吹扫530可以是可选的，或者可以包括使惰性气体例如氩气、氦气、氪气或氮气流动或脉冲。
烷基肼前体步骤520可以包括使烷基肼气体例如具有–CH3或–CH2-CH3封端的烷基肼气体流动或脉冲。烷基肼气体的实例包括：例如乙基肼(CH3CH2N2H3)、二乙基肼(C4H12N2)、叔丁基肼(C4H9N2H3)、甲基肼(CH3NHNH2)或二甲基肼((CH3)2N2H2)。作为烷基封端步骤410的结果，可以关闭岛状生长体上的反应位点以免进一步反应(因此，防止岛上的任何三维向上生长)，但是在衬底上仍然可以存在可用的反应位点。例如，使用烷基肼前体可以允许金属卤化物与反应位点(包含-OH基团)反应，而不是在岛上的反应位点上新形成的甲基和乙基末端。这种情形可减少向上的三维生长并促进横向的二维生长。
然后可以使用金属氮化物形成步骤420来填充岛之间的间隙。如图7所示，金属氮化物形成步骤420可以包括金属卤素前体步骤550、惰性气体吹扫560、含氮等离子体前体步骤570和惰性气体吹扫580。金属卤素前体步骤550可以包括使例如以下金属卤素前体流动或脉冲到衬底上：例如氯化钛(TiClx)、溴化钛(TiBrx)、氟化钛(TiFx)、碘化钛(TiIx)、氯化钨(WClx)、溴化钨(WBrx)、氟化钨(WFx)、碘化钨(WIx)、氯化铌(NbClx)、溴化铌(NbBrx)、氟化铌(NbFx)、氯化钽(TaClx)、溴化钽(TaBrx)、氟化钽(TaFx)、氯化铪(HfClx)、溴化铪(HfBrx)、氯化锆(ZrClx)或溴化锆(ZrBrx)。惰性气体吹扫560和惰性气体吹扫580可以是可选的，或者可以包括使惰性气体例如氩气、氦气、氪气或氮气流动或脉冲。
金属氮化物形成步骤420还可以包括含氮等离子体前体步骤570。在该步骤中，当使氮气(N2)、氢气(H2)、氨气(NH3)或肼(N2H4)流动或脉冲到衬底上时，可使用等离子体来形成NH或NH2自由基。自由基可以远程或原位形成。所形成的自由基是高反应性的并且允许在低温下在衬底上形成金属氯化物。反应室的温度可低于300℃、低于250℃或低于200℃。反应室的压力可以在0.1与10托之间、或在1与5托之间、或在1与3托之间。
由图5-7所示的方法产生的膜可具有膜闭合良好的无定形质量。例如，可以形成小于15埃的闭合的TiN膜。该方法的实施方案还可以应用于形成小于10埃的闭合的结晶膜。
在本发明的至少一个实施方案中，上述方法可以用于形成亚纳米闭合的TiN膜。通过在烷基肼前体步骤520期间使用叔丁基肼而不是在氮等离子体步骤570中使用氨，可以实现更大的覆盖率。另外，通过在比氨低得多的温度下使用叔丁基肼可以实现更大的覆盖率。例如，在250与325℃之间的温度下流动叔丁基肼可导致比在100至200℃以上的温度下的氨更高的钛覆盖率。
根据本发明的至少一个实施方案，可以为PMOS多Vt调谐应用生长TiN。这可以通过形成包含至少氧化铪、氮化钛、碳化钛和氮化钛的叠层来实现。可以使用叔丁基肼形成氮化钛膜，导致用50-100mV范围内的电压进行调谐，这可以通过沉积具有5-10埃范围内的厚度的氮化钛膜来实现。
上文所描述的本公开的实例实施方案不限制本发明的范围，这是因为这些实施方案仅仅是本发明实施方案的实例，本发明由所附权利要求书及其法定等效物界定。任何等效实施方案都旨在落在本发明的范围内。实际上，除本文中所展示和描述的例如所描述元件的替代适用组合等内容以外，对于所属领域的技术人员来说，本公开的各种修改将从描述中变得显而易见。此类修改和实施方案也旨在落在所附权利要求书的范围内。

Claims (16)

1.一种形成金属氮化物膜的方法，包括：
执行用于终止一系列分离的岛上的反应位点反应的能力的烷基封端步骤，其中所述烷基封端步骤包括：
使金属卤素前体流动；
使惰性气体流动；
使烷基肼前体流动，所述烷基肼前体与所述金属卤素前体反应以封闭所述一系列分离的岛中的反应位点；以及
使所述惰性气体流动；以及
执行金属氮化物子循环，其中所述金属氮化物子循环包括：
使金属卤素前体在反应室中的衬底上流动；
使惰性气体在所述衬底上流动以去除过量的所述金属卤素前体；
使氮前体在所述衬底上流动，所述金属卤素前体与所述氮前体反应形成金属氮化物膜；以及
使惰性气体在所述衬底上流动以去除过量的所述金属卤素前体和所述氮前体；
其中所述反应室的温度低于300℃、低于250℃或低于200℃。
2.根据权利要求1所述的方法，还包括处理子循环，所述处理子循环包括：
退火所述金属氮化物膜；以及
蚀刻所述金属氮化物膜。
3.根据权利要求1所述的方法，其中所述金属卤素前体为以下至少一种：氯化钛(TiClx)、溴化钛(TiBrx)、氟化钛(TiFx)、碘化钛(TiIx)、氯化钨(WClx)、溴化钨(WBrx)、氟化钨(WFx)、碘化钨(WIx)、氯化铌(NbClx)、溴化铌(NbBrx)、氟化铌(NbFx)、氯化钽(TaClx)、溴化钽(TaBrx)、氟化钽(TaFx)、氯化铪(HfClx)、溴化铪(HfBrx)、氯化锆(ZrClx)或溴化锆(ZrBrx)。
4.根据权利要求1所述的方法，其中所述氮前体为以下至少一种：烷基肼前体或含氮等离子体前体。
5.根据权利要求4所述的方法，其中所述烷基肼前体为以下至少一种：乙基肼(CH3CH2N2H3)、二乙基肼(C4H12N2)、叔丁基肼(C4H9N2H3)、甲基肼(CH3NHNH2)或二甲基肼((CH3)2N2H2)。
6.根据权利要求4所述的方法，其中所述含氮等离子体前体为以下至少一种：氮气(N2)、氢气(H2)、氨气(NH3)或肼(N2H4)。
7.根据权利要求1所述的方法，其中所述金属氮化物膜形成均匀厚度的连续无定形膜。
8.根据权利要求2所述的方法，其中在蚀刻所述金属氮化物膜期间，所述反应室的温度低于500℃、低于450℃或低于400℃。
9.根据权利要求2所述的方法，其中在蚀刻所述金属氮化物膜期间，所述反应室的压力在0.1与10托之间、在1与5托之间或在1与3托之间。
10.根据权利要求1所述的方法，其中所述惰性气体包括以下至少一种：氩气、氦气、氪气或氮气。
11.一种半导体器件，其中所述半导体器件由权利要求1所述的方法形成。
12.一种形成金属氮化物膜的方法，包括：
作为岛形成步骤在衬底上形成多个金属氮化物生长体，所述岛形成步骤包括：
使金属卤素前体在反应室中的衬底上流动；
使惰性气体在所述衬底上流动以去除过量的所述金属卤素前体；
使氮前体在所述衬底上流动，所述金属卤素前体与所述氮前体反应形成金属氮化物膜；以及
使惰性气体在所述衬底上流动以去除过量的所述金属卤素前体和所述氮前体；
作为烷基封端步骤将所述衬底上的所述金属氮化物生长体上的反应性位点封端，所述烷基封端步骤包括：
使金属卤素前体在反应室中的衬底上流动；
使惰性气体在所述衬底上流动以去除过量的所述金属卤素前体；
使烷基肼前体在所述衬底上流动，所述金属卤素前体与所述烷基肼前体反应；以及
使惰性气体在所述衬底上流动以去除过量的所述金属卤素前体和所述烷基肼前体；以及
作为金属氮化物形成步骤在所述衬底上形成金属氮化物膜，所述金属氮化物形成步骤包括：
使金属卤素前体在反应室中的衬底上流动；
使惰性气体在所述衬底上流动以去除过量的所述金属卤素前体；
使含氮等离子体前体在所述衬底上流动，所述金属卤素前体与所述含氮等离子体前体反应以形成金属氮化物膜；以及
使惰性气体在所述衬底上流动以去除过量的所述金属卤素前体和所述含氮等离子体前体；
其中所述反应室的温度低于300℃、低于250℃或低于200℃。
13.根据权利要求12所述的方法，其中所述金属卤素前体为以下至少一种：氯化钛(TiClx)、溴化钛(TiBrx)、氟化钛(TiFx)、碘化钛(TiIx)、氯化钨(WClx)、溴化钨(WBrx)、氟化钨(WFx)、碘化钨(WIx)、氯化铌(NbClx)、溴化铌(NbBrx)、氟化铌(NbFx)、氯化钽(TaClx)、溴化钽(TaBrx)、氟化钽(TaFx)、氯化铪(HfClx)、溴化铪(HfBrx)、氯化锆(ZrClx)或溴化锆(ZrBrx)。
14.根据权利要求12所述的方法，其中所述烷基肼前体为以下至少一种：乙基肼(CH3CH2N2H3)、二乙基肼(C4H12N2)、叔丁基肼(C4H9N2H3)、甲基肼(CH3NHNH2)或二甲基肼((CH3)2N2H2)。
15.根据权利要求12所述的方法，其中所述含氮等离子体前体为以下至少一种：氮气(N2)、氢气(H2)、氨气(NH3)或肼(N2H4)。
16.根据权利要求12所述的方法，其中所述惰性气体包括以下至少一种：氩气、氦气、氪气或氮气。
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