CN105369215A - 含硅膜的等离子体增强周期化学气相沉积 - Google Patents

含硅膜的等离子体增强周期化学气相沉积 Download PDF

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CN105369215A
CN105369215A CN201510250443.0A CN201510250443A CN105369215A CN 105369215 A CN105369215 A CN 105369215A CN 201510250443 A CN201510250443 A CN 201510250443A CN 105369215 A CN105369215 A CN 105369215A
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source
silicon
substrate
film
ald
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H.思里丹达姆
萧满超
雷新建
T.R.加夫尼
E.J.小卡瓦克基
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Versum Materials US LLC
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Air Products and Chemicals Inc
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Abstract

本发明公开了由含有Si-H3的烷氨基硅烷，优选式(R1R2N)SiH3(其中R1和R2独立地选自C2-C10)以及氮源或氧源(优选氨或氧)进行等离子体增强周期化学气相沉积氮化硅、碳氮化硅、氧氮化硅、羧基氮化硅和掺碳的氧化硅的方法，使得膜与由热化学气相沉积获得的膜相比具有改进的特性，例如蚀刻速率、氢浓度和应力。

Description

含硅膜的等离子体增强周期化学气相沉积
本申请是申请日为2008年2月27日，申请号为200810088179.5，发明名称为“含硅膜的等离子体增强周期化学气相沉积”的发明专利申请的分案申请。
相关申请的相互引用
本申请要求于2007年2月27日提交的美国临时专利申请No.60/903,734的优先权。
发明背景
电子器件制造业已经把氮化硅、碳氮化硅和氧氮化硅的化学气相沉积(CVD)、周期化学气相沉积(CCVD)或原子层沉积(ALD)用于制造集成电路中。该工业应用的实例包括：US2003/0020111；US2005/0048204A1；US4720395；US7,166,516；Gumpher，J.，W.Bather，N.Mehta和D.Wedel.“CharacterizationofLow-TemperatureSiliconNitrideLPCVDfromBis(tertiary-butylamino)silaneandAmmonia.”JournalofTheElectrochemicalSociety151(5)；(2004)G353-G359；US2006/045986；US2005/152501；US2005/255714；US7,129,187；US2005/159017；US6,391,803；US5,976,991；US2003/0059535；US5,234,869；JP2006-301338；US2006/087893；US2003/26083；US2004/017383；US2006/0019032；US2003/36097；US2004/044958；US6,881,636；US6,963,101；US2001/0000476；和US2005/129862。如下所述，本发明提供在衬底上将含硅膜如氮化硅、碳氮化硅、氧氮化硅和掺碳的氧化硅的CVD或ALD的现有工业方法的改进。
发明概述
本发明是将含硅膜如氮化硅、碳氮化硅、氧氮化硅和掺碳的氧化硅沉积到衬底上的方法。
本发明的实施方式之一是将氮化硅、碳氮化硅、氧氮化硅和羧基氮化硅沉积到半导体衬底上的方法，包括：
a.在远距等离子体(remoteplasma)条件下使含氮源与加热的衬底相接触以在所述加热的衬底上吸收至少一部分含氮源，
b.清除任何未吸收的含氮源，
c.使所述加热的衬底与具有一个或多个Si-H3片段的含硅源接触以与所吸收的含氧源反应，其中所述含硅源含有选自以下组中的一个或多个H3Si-NR0 2(R0＝SiH3，R，R1或R2，定义如下)基团，该组包括一种或多种的：
其中，式中的R和R1代表具有2-10个碳原子的脂族基团，其中式A中的R和R1也可以是环状基团，且R2选自单键、(CH2)n、环或SiH2，和
d.清除未反应的含硅源。
本发明的另一实施方式是将氧氮化硅、羧基氮化硅和掺碳的氧化硅沉积到半导体衬底上的方法，包括：
a.在远距等离子体条件下使含氧源与加热的衬底相接触以在所述加热的衬底上吸收至少一部分含氧源，
b.清除任何未吸收的含氧源，
c.使所述加热的衬底与具有一个或多个Si-H3片段的含硅源接触以与所吸收的含氧源反应，其中所述含硅源含有选自以下组中的一个或多个H3Si-NR0 2(R0＝SiH3，R，R1或R2，定义如下)基团，该组包括一种或多种：
其中，式中的R和R1代表具有2-10个碳原子的脂族基团，其中式A中的R和R1也可以是环状基团，且R2选自单键、(CH2)n、环或SiH2，和
d.清除未反应的含硅源。
附图简述
图1是典型的用于氮化硅、碳氮化物、氧氮化硅和羧基氮化硅的等离子体增强周期化学气相沉积的流程图。
图2是在下述PEALD试验条件下DIPAS的沉积速率与脉冲时间图：等离子体功率为1.39kW的5sccm的NH3、10sccm的吹扫气体N2、衬底温度400℃、不锈钢容器中的DIPAS为40℃。
图3是典型的用于氧氮化硅和掺碳的氧化硅的等离子体增强周期化学气相沉积的流程图。
图4是实施例1所述的膜的FTIP光谱并在实施例2中进行讨论。
发明详述
本发明公开了由含有Si-H3的烷氨基硅烷，优选式(R1R2N)SiH3(其中R1和R2独立地选自C2-C10)以及氮源(优选氨)进行等离子体增强周期化学气相沉积氮化硅、碳氮化硅、氧氮化硅、羧基氮化硅和掺碳的氧化硅的方法，使得膜与由热化学气相沉积获得的膜相比具有改进的特性，例如蚀刻速率、氢浓度和应力。或者，该方法可按照原子层沉积(ALD)、等离子体辅助原子层沉积(PAALD)、化学气相沉积(CVD)、低压化学气相沉积(LPCVD)、等离子体增强化学气相沉积(PECVD)或旋转涂布沉积(Spinondeposition)(SOD)来进行。
等离子体增强周期化学气相沉积氮化硅、碳氮化硅、氧氮化硅和羧基氮化硅的典型周期示于图1中。
远距等离子体室是AdvancedEnergyIndustries公司制造的LitmasRPS。LitmasRPS是结合有固态RF功率输出系统的圆柱形感应等离子体源(石英室)。水冷线圈卷绕在室的周围，为室提供冷却并形成RF天线。频率操作范围在1.9MHz-3.2MHz。DC输出功率范围为100W-1500W。
ALD系统是CambridgeNanoTech公司制造的Savannah100。ALD反应器是阳极化铝且容纳有100mm的硅衬底。ALD反应器具有包埋的盘形加热部件，其从底部加热的衬底。也有包埋在反应器壁内的管式加热器。前体阀总管包封在加热器中，加热封套用于加热前体容器。在前体阀总管中的ALD阀是三通阀，可向ALD反应器中连续地供给10-100sccm的惰性气体。
氮化硅、碳氮化硅、氧氮化硅和羧基氮化硅的沉积方法描述如下。
在方法的第一步骤中，安装在沉积室上游约12英寸处的远距等离子体室内产生氨等离子体(ammoniaplasma)，并以预定体积流速、预定的时间供应到沉积室中。通常，通过开启远距等离子体头和ALD反应器之间的门阀(gatevalve)，经0.1-80秒的一段时间将氨等离子体供给到ALD室中以使氨自由基被充分的吸附，使得衬底表面饱和。沉积过程中，供给到远距等离子体室入口的氨的流速通常在1-100sccm范围内。等离子体室中的PF功率在100W-1500W之间变化。沉积温度是常规的，范围约200-600℃，对原子层沉积来说优选200-400℃，对周期化学气相沉积来说优选400-600℃。示例性的压力从50mtorr-100torr。此外，氨中其他的含氮源能够是氮、肼、单烷基肼、二烷基肼和其混合物。
在方法的第二步骤中，惰性气体如Ar、N2或He可用于从室中吹扫未反应的氨自由基。通常在周期沉积方法中，气体如Ar、N2或He以10-100sccm的流速供入到室中，从而清除留在室中的氨自由基和任何的副产品。
在方法的第三步骤中，有机氨基硅烷诸如二乙基氨基硅烷(DEAS)、二异丙基氨基硅烷(DIPAS)、二叔丁基氨基硅烷(DTBAS)、二仲丁基氨基烷基、二叔戊基氨基硅烷和其混合物以预定摩尔体积(例如1-100微摩尔)、以预定一段时间(优选约0.005-10秒)导入到室中。硅前体与吸附在衬底表面上的氨自由基反应导致氮化硅的形成。使用了常规的沉积温度200-500℃和压力50mtorr-100torr。
在方法的第四步骤中，用惰性气体如Ar、N2或He从室中吹扫未反应的有机氨基硅烷。通常在周期沉积方法中，气体如Ar、N2或He以10-100sccm的流速供入到室中，从而清除留在室中的有机氨基硅烷和任何的副产品。
上述的四个方法步骤包括典型的ALD过程周期。该ALD过程周期重复若干次直到获得所需的膜厚度。
图2显示了衬底温度为400℃时的典型ALD饱和曲线。
等离子体增强周期化学气相沉积氧氮化硅和掺碳的氧化硅的典型周期示于图3中。
在方法的第一步骤中，安装在沉积室上游约12英寸处的远距等离子体室内产生氧等离子体(oxygenplasma)，并以预定体积流速、预定的时间供应到沉积室中。通常，通过开启远距等离子体头和ALD反应器之间的门阀，经0.1-80秒的一段时间将氧等离子体供给到ALD室中以使含氧自由基被充分地吸附，使得衬底表面饱和。沉积过程中，供给到远距等离子体室入口的氧流速通常在1-100sccm范围内。等离子体室中的RF功率在100W-1500W之间变化。沉积温度是常规的，范围约200-600℃，对原子层沉积来说优选200-400℃，对周期化学气相沉积来说优选400-600℃。示例性的压力从50mtorr-100torr。除氧以外，其它含氧源可以是臭氧、一氧化二氮和它们的混合物。
在方法的第二步骤中，惰性气体如Ar、N2或He可用于从室中吹扫未反应的含氧自由基。通常在周期沉积方法中，气体如Ar、N2或He以10-100sccm的流速供入到室中，从而清除留在室中的含氧自由基和任何的副产品。
在方法的第三步骤中，有机氨基硅烷诸如二乙基氨基硅烷(DEAS)、二异丙基氨基硅烷(DIPAS)、二叔丁基氨基硅烷(DTBAS)、二仲丁基氨基烷基、二叔戊基氨基硅烷和其混合物以预定摩尔体积(例如1-100微摩尔)、以一段预定时间(优选约0.005-10秒)导入到室中。硅前体与吸附在衬底表面上的含氧自由基反应导致氧化硅的形成。使用了常规的沉积温度200-500℃和压力50mtorr-100torr。
在方法的第四步骤中，用惰性气体如Ar、N2或He从室中吹扫未反应的有机氨基硅烷。通常在周期沉积方法中，气体如Ar、N2或He以10-100sccm的流速供入到室中，从而清除留在室中的有机氨基硅烷和任何的副产品。
上述四个方法步骤包括ALD过程周期。该ALD过程周期重复若干次直到获得所需的膜厚度。
实施例1
在将ALD反应器抽到～40mT真空度以下并用10sccm的N2清洗后，在ALD反应器中导入所述硅前体和NH3。在温度400℃进行沉积。远距等离子体也可用于降低所需的沉积温度。在导入到反应器之前，将所述硅前体在加热套包封的水浴瓶(bubbler)中预热到40℃。结果总结在表1中。
由于在一次沉积期间仅使用极少量的化合物，所以来自水浴瓶的所述硅前体的流速(每单位时间量)在给定温度下被认为是恒定的。因此，加入ALD反应器中的所述硅前体的量与用于导入所述硅前体的脉冲时间成线性比例。
从表1中可以看出，即使在沉积温度和氮前体的数量保持相同时，形成氮化硅膜的速率随着加入到反应器中所述硅前体的量的变化而变化。
同样从表1中可以看出，当其他处理条件保持相同时，随着所述硅前体的脉冲时间(或量)从0.01秒增加到0.05秒，形成氮化硅膜的速率开始从0.156A/周期增加。然而，随后即使加入更多硅前体后，速率几乎保持不变。这表明使用Si前体形成的膜确实是ALD膜。
表1
温度(℃) NH3脉冲(秒) 硅前体脉冲时间(秒) 沉积速率(A/周期)
400 3 0.01 0.156
400 3 0.025 0.272
400 3 0.05 0.318
400 3 0.1 0.307
400 3 0.2 0.3
实施例2
使用FTIP对所沉积的ALD膜进行分析。膜的FTIP光谱示于图4中。从图4中可以看出，1046cm-1处存在有吸收峰，表明膜中存在氧化物。3371处的峰是N-H展宽(stretch)(有一些O-H)且在接近1130cm-1的肩部具有相应的摇摆(rock)。2218峰来自Si-H且其宽的形状表明是低应力的膜。813的峰接近Si-N。沉积膜的EDX分析也证实了膜中Si和N的存在。
上述列出的包括试验实施例的本发明的实施方式是对本发明所作的许多实施方式的示例。可以构想的是，可使用许多其他配置的方法并且方法中所用材料可选自除具体公开的那些以外的许多材料。简言之，本发明已经针对特别的实施方式进行了阐述，但本发明的整个保护范围应该由所附的权利要求加以确定。

Claims (14)

1.一种将氮化硅、碳氮化硅沉积到半导体衬底上的原子层沉积(ALD)方法，包括：
a.在远距等离子体条件下在200至400℃使含氮源与加热的衬底相接触以在所述加热的衬底上吸收至少一部分含氮源，
b.清除任何未被吸收的含氮源，
c.使所述加热的衬底与具有一个或多个Si-H3片段的含硅源接触以与所吸收的含氮源反应，其中所述含硅源选自二异丙基氨基硅烷（DIPAS）、二叔丁基氨基硅烷（DTBAS）、二仲丁基氨基硅烷、二叔戊基氨基硅烷和它们的混合物，和
d.清除未反应的含硅源。
2.权利要求1所述的ALD方法，其中，重复所述方法直到形成所需厚度的膜。
3.权利要求1所述的ALD方法，其中，所述含氮源选自氮、氨、肼、单烷基肼、二烷基肼和它们的混合物。
4.一种将氧氮化硅、羧基氮化硅和掺碳的氧化硅沉积到半导体衬底上的原子层沉积(ALD)方法，包括：
a.在远距等离子体条件下在200至400℃使含氧源与加热的衬底相接触以在所述加热的衬底上吸收至少一部分含氧源，
b.清除任何未被吸收的含氧源，
c.使所述加热的衬底与具有一个或多个Si-H3片段的含硅源接触以与所吸收的含氧源反应，其中所述含硅源选自二异丙基氨基硅烷（DIPAS）、二叔丁基氨基硅烷（DTBAS）、二仲丁基氨基硅烷、二叔戊基氨基硅烷和它们的混合物，和
d.清除未反应的含硅源。
5.权利要求4所述的ALD方法，其中，重复所述方法直到形成所需厚度的膜。
6.权利要求4所述的ALD方法，其中，所述含氧源选自氧、一氧化二氮、臭氧和它们的混合物。
7.包含二异丙基氨基硅烷的源用于在原子层沉积方法中在衬底上沉积含硅膜的用途，所述含硅膜选自氮化硅、碳氮化硅、氧氮化硅、氧化硅和掺碳的氧化硅。
8.权利要求7所述的用途，其中所述含硅膜包含氧化硅膜，且所述源进一步包含含氧源。
9.包含二仲丁基氨基硅烷的源用于在原子层沉积方法中在衬底上沉积含硅膜的用途，所述含硅膜选自氮化硅、碳氮化硅、氧氮化硅、氧化硅和掺碳的氧化硅。
10.权利要求9所述的用途，其中所述含硅膜包含氧化硅膜，且所述源进一步包含含氧源。
11.包含二叔戊基氨基硅烷的源用于在原子层沉积方法中在衬底上沉积含硅膜的用途，所述含硅膜选自氮化硅、碳氮化硅、氧氮化硅、氧化硅和掺碳的氧化硅。
12.权利要求11所述的用途，其中所述含硅膜包含氧化硅膜，且所述源进一步包含含氧源。
13.一种将氮化硅、碳氮化硅、氧氮化硅和羧基氮化硅沉积到半导体衬底上的方法，包括：
a.在远距等离子体条件下使含氮源与加热的衬底相接触以在所述加热的衬底上吸收至少一部分含氮源，
b.清除任何未被吸收的含氮源，
c.使所述加热的衬底与具有一个或多个Si-H3片段的含硅源接触以与所吸收的含氮源反应，其中所述含硅源具有选自以下组中的一个或多个H3Si-NR0 2(R0=SiH3，R、R1或R2定义如下)基团，该组包括一种或多种的：
其中，式中的R和R1代表具有2-10个碳原子的脂族基团，其中式A中的R和R1也可以是环状基团，且R2选自单键、(CH2)n、环或SiH2，和
d.清除未反应的含硅源。
14.一种将氧氮化硅、羧基氮化硅和掺碳的氧化硅沉积到半导体衬底上的方法，包括：
a.在远距等离子体条件下使含氧源与加热的衬底相接触以在所述加热的衬底上吸收至少一部分含氧源，
b.清除任何未被吸收的含氧源，
c.使所述加热的衬底与具有一个或多个Si-H3片段的含硅源接触以与所吸收的含氧源反应，其中所述含硅源含有选自以下组中的一个或多个H3Si-NR0 2(R0=SiH3，R、R1或R2定义如下)基团，该组包括一种或多种：
其中，式中的R和R1代表具有2-10个碳原子的脂族基团，其中式A中的R和R1也可以是环状基团，且R2选自单键、(CH2)n、环或SiH2，和
d.清除未反应的含硅源。
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