CN112376024A - 一种氧化物薄膜的制备方法 - Google Patents

一种氧化物薄膜的制备方法 Download PDF

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CN112376024A
CN112376024A CN202011157653.2A CN202011157653A CN112376024A CN 112376024 A CN112376024 A CN 112376024A CN 202011157653 A CN202011157653 A CN 202011157653A CN 112376024 A CN112376024 A CN 112376024A
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target
power
oxygen
mixed gas
argon
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CN112376024B (zh
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罗建恒
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Beijing Naura Microelectronics Equipment Co Ltd
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Beijing Naura Microelectronics Equipment Co Ltd
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Priority to CN202011157653.2A priority Critical patent/CN112376024B/zh
Publication of CN112376024A publication Critical patent/CN112376024A/zh
Priority to EP21885015.4A priority patent/EP4234756A1/en
Priority to PCT/CN2021/125198 priority patent/WO2022089288A1/zh
Priority to US18/250,541 priority patent/US20230399734A1/en
Priority to JP2023524557A priority patent/JP2023546468A/ja
Priority to KR1020237013507A priority patent/KR20230072489A/ko
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Abstract

本发明公开一种氧化物薄膜的制备方法，包括：将待沉积薄膜的晶圆放入反应腔室的基座上；向反应腔室内通入氩气和氧气的混合气体，对靶材施加直流功率和射频功率，使该混合气体形成等离子体，该等离子体轰击靶材，以在晶圆上形成氧化物薄膜；停止对靶材施加功率，向反应腔室内通入氩气、氧气和氮气的混合气体，对基座施加射频功率，使该混合气体形成等离子体，该等离子体轰击氧化物薄膜，以形成氮氧化物薄层；继续向反应腔室内通入氩气、氧气和氮气的混合气体，对靶材施加直流功率和射频功率，继续对基座施加射频功率，使该混合气体形成等离子体，该等离子体轰击靶材和氮氧化物薄层，以在氮氧化物薄层上形成氮氧化物薄膜。

Description

一种氧化物薄膜的制备方法
技术领域
本发明涉及半导体工艺领域，更具体地，涉及一种氧化物薄膜的制备方法。
背景技术
近年来，超大规模集成电路技术发展迅速，器件特征尺寸在不断缩小，器件密度不断增大，金属化互连所带来的RC迟滞已经成为阻碍超高密度集成电路效能及速度的关键因素。因此，减少RC互连延迟成是近年来半导体行业的主攻方向。在集成电路制造中，金属线通常嵌入在具有低介电常数的层间电介质(ILD)材料之中。在大马士革互连工艺中，蚀刻停止层通常沉积在单独的ILD层和金属线上，并且用于IC制造工艺的图案化制作，以保护位于这些层下面的材料在图案化期间不被蚀刻，同时蚀刻停止层通常不会被完全去除，并且作为较厚的ILD层之间的薄膜保留在最终制造的半导体器件中。
氧化铝因其良好的工艺兼容性逐渐被用作蚀刻停止层。通常采用CVD方法制备氧化铝薄膜，但是其薄膜杂质多、密度小且工艺成本高。与CVD工艺相比，脉冲磁控溅射技术制备的氧化铝薄膜因其良好的薄膜均匀性、杂质少、密度大等优势成为集成电路金属化制程中最常用的物理气相沉积方法(PVD)之一。然而传统PVD方法制备非导电氧化物薄膜时的工艺窗口小，局限性日益突出，如沉积速率低、蚀刻不均匀及频繁的电弧异常放电引起颗粒缺陷对后续工艺集成造成了很大的困难。因此，迫切需要寻找一种新薄膜的制备方法。
发明内容
本发明的目的是提出一种氧化物薄膜的制备方法，解决在工艺过程中沉积速率低、颗粒缺陷，表面粗糙度大，薄膜密度低的问题，所述制备方法包括：
步骤1：将待沉积薄膜的晶圆放入反应腔室的基座上；
步骤2：向所述反应腔室内通入氩气和氧气的混合气体，对靶材施加直流功率和射频功率，使该混合气体形成等离子体，该等离子体轰击所述靶材，以在所述晶圆上形成氧化物薄膜；
步骤3：停止对所述靶材施加功率，向所述反应腔室内通入氩气、氧气和氮气的混合气体，对所述基座施加射频功率，使该混合气体形成等离子体，该等离子体轰击所述氧化物薄膜，以形成氮氧化物薄层；
步骤4：继续向所述反应腔室内通入氩气、氧气和氮气的混合气体，对所述靶材施加直流功率和射频功率，继续对所述基座施加射频功率，使该混合气体形成等离子体，该等离子体轰击所述靶材和所述步骤3形成的所述氮氧化物薄层，以在所述氮氧化物薄层上形成氮氧化物薄膜。
可选方案中，所述步骤1中的工艺条件为：所述反应腔室的真空度小于5E-6Torr；所述基座的温度为250℃～350℃。
可选方案中，在所述步骤2中和/或所述步骤3中，氩气的流量小于500sccm，氧气的流量小于500sccm，其中氩气的流量大于氧气的流量。
可选方案中，在所述步骤2中，对所述靶材施加的直流功率小于10000W，对所述靶材施加的射频功率小于3000W，其中射频功率与直流功率的比值为2～4。
可选方案中，在所述步骤2中，对所述靶材施加的直流功率为100～200W，对所述靶材施加的射频功率为300～600W，其中射频功率与直流功率的比值为3。
可选方案中，在所述步骤4中，对所述靶材施加的直流功率小于10000W，对所述靶材施加的射频功率小于3000W，其中射频功率与直流功率的比值为2～7。
可选方案中，在所述步骤4中，对所述靶材施加的直流功率为3000～6000W，对所述靶材施加的射频功率为1000～2000W，其中射频功率与直流功率的比值为3～6。
可选方案中，在所述步骤3和/或所述步骤4中，氧气和氮气的流量之和大于氩气的流量。
可选方案中，在所述步骤3和/或所述步骤4中，对所述基座施加的射频功率小于500W。
可选方案中，所述靶材包括铝、钛、硅、铪或钽靶材，或者包括铝、钛、硅、铪或钽的化合物靶材。
本发明的有益效果在于：
在步骤2中，对靶材同时施加直流功率和射频功率，能够减少氧化物沉积过程中颗粒缺陷的产生。在步骤3中，通入氩气、氧气和氮气的混合气体，并对基座施加射频功率，可以原位生成氮氧化物薄层，还可以对氧化物薄膜表面进行一定的刻蚀，在减少氧化物薄膜表面缺陷的同时降低表面的粗糙度。在步骤4中，继续通入氩气、氧气和氮气的混合气体，同时对靶材施加直流功率和射频功率，并对基座施加射频功率，可以在晶圆表面沉积形成高密度，低粗糙度的薄膜，而高质量的表面可以抑制蚀刻层和金属之间形成过渡层，减少金属层的氧化。
本发明的方法具有其它的特性和优点，这些特性和优点从并入本文中的附图和随后的具体实施方式中将是显而易见的，或者将在并入本文中的附图和随后的具体实施方式中进行详细陈述，这些附图和具体实施方式共同用于解释本发明的特定原理。
附图说明
通过结合附图对本发明示例性实施例进行更详细的描述，本发明的上述以及其它目的、特征和优势将变得更加明显。
图1示出了根据本发明一实施例的氧化物薄膜的制备方法步骤流程图。
图2示出了根据本发明一实施例和现有技术制备的氧化物薄膜颗粒缺陷数量的对比图。
图3示出了根据本发明一实施例和现有技术制备的氧化物薄膜刻蚀均匀性的对比图。
具体实施方式
下面将更详细地描述本发明。虽然本发明提供了优选的实施例，然而应该理解，可以以各种形式实现本发明而不应被这里阐述的实施例所限制。相反，提供这些实施例是为了使本发明更加透彻和完整，并且能够将本发明的范围完整地传达给本领域的技术人员。
本发明一实施例提供了一种氧化物薄膜的制备方法，图1示出了根据本发明一实施例的半导体工艺中薄膜的制备方法步骤流程图。请参考图1，薄膜的制备方法包括：
步骤1：将待沉积薄膜的晶圆放入反应腔室的基座上；
步骤2：向反应腔室内通入氩气和氧气的混合气体，对靶材施加直流功率和射频功率，使该混合气体形成等离子体，该等离子体轰击靶材，以在晶圆上形成氧化物薄膜；
步骤3：停止对靶材施加功率，向反应腔室内通入氩气、氧气和氮气的混合气体，对基座施加射频功率，使该混合气体形成等离子体，该等离子体轰击上述氧化物薄膜，以形成氮氧化物薄层；
步骤4：继续向反应腔室内通入氩气、氧气和氮气的混合气体，对靶材施加直流功率和射频功率，继续对基座施加射频功率，使该混合气体形成等离子体，该等离子体轰击靶材和步骤3形成的氮氧化物薄层，以在氮氧化物薄层上形成氮氧化物薄膜。
为了便于理解本方案，首先对用于制备薄膜的设备进行简单的介绍。薄膜的制备在反应腔室中进行，反应腔室中设有基座，用于承载待沉积薄膜的晶圆，基座中带加热或冷却功能。反应腔室连接有真空系统，真空系统可对反应腔体进行抽气，使反应腔室达到较高的真空度，以满足工艺所需的真空条件。工艺所需的气体(如氩气、氧气等)通过流量计连接到反应腔室，工艺所需要的靶材被密封在反应腔室的上方区域(基座的上方)。上述靶材可以是纯金属也可以是金属化合物，也可以是硅或二氧化硅(当需要沉积硅的氧化物)。进行薄膜沉积时，电源会施加功率至靶材，使其相对于接地的反应腔室为负偏压，另外，高压使氩气、氧气电离放电而产生带正电的等离子体，带正电的等离子体被靶材吸引并轰击靶材。当等离子体的能量足够高时，会使靶材表面的原子逸出并沉积在晶圆上，以实现对晶圆表面的薄膜沉积。
本实施例以在晶圆表面沉积氧化铝和氮氧化铝的复合薄膜为例，对制备方法进行详细说明。
具体地，执行步骤1，根据沉积的薄膜不同，对反应腔室设定适合的工艺条件，将待沉积薄膜的晶圆放入反应腔室的基座上，将基座温度调至工艺所需的温度。在本实施例中，用于沉积氧化铝薄膜，设定的工艺条件为，反应腔室的真空度小于5E-6Torr；基座的温度为250℃～350℃，优选的，如300℃。
执行步骤2，向反应腔室内通入氩气和氧气的混合气体，对靶材施加直流功率和射频功率，使该混合气体形成等离子体，等离子体轰击靶材，以在晶圆上形成氧化物薄膜。在现有技术中，对靶材只施加脉冲直流功率，由于氧化铝薄膜是一种非导电氧化物，脉冲直流功率在一个周期内存在正电压和负电压两个阶段，在负电压段，电源工作于靶材的溅射，正电压段，引入电子中和靶面累积的正电荷。工艺过程中沉积速率低、蚀刻不均匀、频繁的电弧异常放电引起颗粒缺陷，表面粗糙度大，薄膜密度低，容易吸附空气中的水、氧、碳等杂质气体形成表面缺陷等对后续工艺集成造成了很大的困难。本实施例中，对靶材同时施加直流功率和射频功率，可以降低离子能量，避免对底层ILD薄膜造成损伤，形成高密度的氧化铝接触层薄膜。
执行步骤3，停止对靶材施加功率，向反应腔室内通入氩气、氧气和氮气的混合气体，对基座施加射频功率，使该混合气体形成等离子体，等离子体轰击氧化物薄膜进行表面处理。在本步骤中，对基座施加射频功率，可以原位形成氮氧化物薄层，即在氧化物薄膜的表面生成一层较薄的氮氧化物层，还可以对形成的氧化物薄膜表面进行一定的刻蚀，在减少技术氧化物薄膜表面缺陷的同时降低表面的粗糙度。
执行步骤4，继续向反应腔室内通入氩气、氧气和氮气的混合气体，对靶材施加直流功率和射频功率，继续对基座施加射频功率，使该混合气体形成等离子体，等离子体轰击靶材和步骤3形成的氮氧化物薄层(或者说氧化物薄膜)，以在氮氧化物薄层(或者说氧化物薄膜)上形成氮氧化物薄膜。在本步骤中，同时对靶材施加直流功率和射频功率，对基座施加射频功率，对薄膜进行刻蚀修复和沉积工艺同时进行，沉积的速率大于刻蚀的速率，以在晶圆表面沉积形成高密度，低粗糙度的薄膜，高质量的表面可以抑制蚀刻层和金属之间形成过渡层，减少金属层的氧化。
在本实施例中，在步骤2中，反应腔室的工艺压力维持在3～10mTorr，氩气的流量小于500sccm，优选实施例中，氩气的流量范围为50～200sccm；氧气的流量小于500sccm，优选实施例中，氧气的流量范围为20～100sccm。本实施例中，氩气的流量大于氧气的流量，即氩气与氧气的比例大于1。这和现有技术(氩气和氧气的比例小于0.5)有很大的不同，氧气比例过高不利于颗粒缺陷和蚀刻均匀性的控制。对靶材施加的直流功率小于10000W，优选实例中，直流功率范围为100～200W。对靶材施加的射频功率小于3000W，优选实例中，射频功率范围为300～600W。其中对靶材施加的射频功率与直流功率的比值为3左右，如2或3或4。合适的功率比例能够在增加铝和氧的原子高密度等离子体中的离化和碰撞(当沉积氧化铝薄膜时)，改变薄膜在衬底表面生长时的横向迁移，从而形成低损伤、高密度薄膜，不会对前层的低介电常数的层间介质层造成损伤改变材料的介电常数。
在本实施例中，在步骤3中，反应腔室的工艺压力维持在3～10mTorr，氩气的流量小于500sccm，优选实施例中，氩气的流量范围为50～200sccm；氧气的流量小于500sccm，优选实施例中，氧气的流量范围为20～100sccm。本实施例中，氧气和氮气的流量之和大于氩气的流量，即氧气和氮气的流量之和与氩气的流量的比值大于1。对基座施加的射频功率小于500W，优选实施例中，对基座施加的射频功率范围为50～100W。这种设置方式可以对薄膜表面进行一定的轰击，原位形成氮氧化物铝薄层，在减少表面缺陷的同时降低表面的粗糙度。
在本实施例中，在步骤4中，反应腔室的工艺压力维持在3～10mTorr，氩气的流量小于500sccm，优选实施例中，氩气的流量范围为50～200sccm；氧气的流量小于500sccm，优选实施例中，氧气的流量范围为20～100sccm。本实施例中，氧气和氮气的流量之和与氩气的流量的比值大于1。对靶材施加的直流功率小于10000W，优选实例中，直流功率范围为3000～6000W，对靶材施加的射频功率小于3000W，优选实例中，射频功率范围为1000～2000W，其中射频功率与直流功率的比值控制在2至7之间，优选的，在3～6之间，如3、5、6等。对基座施加的射频功率小于500W，优选实施例中，对基座施加的射频功率范围为50～200W。这些参数的比值设置，可以使表面沉积形成高密度，低粗糙度的氮氧化铝薄膜，高质量的表面可以抑制蚀刻层和金属之间形成过渡层，减少金属层的氧化。
图2示出了根据本发明一实施例和现有技术制备的氧化物薄膜颗粒缺陷数量的对比图。图3示出了根据本发明一实施例和现有技术制备的氧化物薄膜刻蚀均匀性的对比图。参考图2和图3，可以清楚的看到本技术方案颗粒缺陷明显减少，晶圆上膜内大于30纳米的颗粒数量在5颗以内，湿法蚀刻均匀性也得到了极大的改善，均匀性从12.49％降到2.24％。
以上描述以形成铝的氧化物和氮氧化物薄膜为例，应该理解本发明的方法还可以制备其他薄膜，如用于制备钛、硅、铪或钽的氧化物和氮氧化物的复合薄膜。
本发明降低了工艺过程中的氧气比例，在靶材上使用射频/直流共溅射，减少金属氧化物沉积过程中的颗粒缺陷的产生，同时工艺中沉积氮氧化物薄膜，抑制空气中的水、氧、碳在金属氧化物表面吸附产生颗粒缺陷。靶材上增加射频电源增加等离子体中氧的碰撞离化，改变氧原子的分布，改善氧化物薄膜湿法蚀刻均匀性问题。本发明增加了薄膜生长过程中离子能量和分布的控制方式，扩大了工艺窗口，提供了一种制备高密度氧化物薄膜的方法。
以上已经描述了本发明的各实施例，上述说明是示例性的，并非穷尽性的，并且也不限于所披露的各实施例。在不偏离所说明的各实施例的范围和精神的情况下，对于本技术领域的普通技术人员来说许多修改和变更都是显而易见的。

Claims (10)

1.一种氧化物薄膜的制备方法，其特征在于，所述方法包括：
步骤1：将待沉积薄膜的晶圆放入反应腔室的基座上；
步骤2：向所述反应腔室内通入氩气和氧气的混合气体，对靶材施加直流功率和射频功率，使该混合气体形成等离子体，该等离子体轰击所述靶材，以在所述晶圆上形成氧化物薄膜；
步骤3：停止对所述靶材施加功率，向所述反应腔室内通入氩气、氧气和氮气的混合气体，对所述基座施加射频功率，使该混合气体形成等离子体，该等离子体轰击所述氧化物薄膜，以形成氮氧化物薄层；
步骤4：继续向所述反应腔室内通入氩气、氧气和氮气的混合气体，对所述靶材施加直流功率和射频功率，继续对所述基座施加射频功率，使该混合气体形成等离子体，该等离子体轰击所述靶材和所述步骤3形成的所述氮氧化物薄层，以在所述氮氧化物薄层上形成氮氧化物薄膜。
2.根据权利要求1所述的方法，其特征在于，所述步骤1中的工艺条件为：所述反应腔室的真空度小于5E-6Torr；所述基座的温度为250℃～350℃。
3.根据权利要求1所述的方法，其特征在于，在所述步骤2中和/或所述步骤3中，氩气的流量小于500sccm，氧气的流量小于500sccm，其中氩气的流量大于氧气的流量。
4.根据权利要求1所述的方法，其特征在于，在所述步骤2中，对所述靶材施加的直流功率小于10000W，对所述靶材施加的射频功率小于3000W，其中射频功率与直流功率的比值为2～4。
5.根据权利要求4所述的方法，其特征在于，在所述步骤2中，对所述靶材施加的直流功率为100～200W，对所述靶材施加的射频功率为300～600W，其中射频功率与直流功率的比值为3。
6.根据权利要求1所述的方法，其特征在于，在所述步骤4中，对所述靶材施加的直流功率小于10000W，对所述靶材施加的射频功率小于3000W，其中射频功率与直流功率的比值为2～7。
7.根据权利要求1所述的方法，其特征在于，在所述步骤4中，对所述靶材施加的直流功率为3000～6000W，对所述靶材施加的射频功率为1000～2000W，其中射频功率与直流功率的比值为3～6。
8.根据权利要求1所述的方法，其特征在于，在所述步骤3和/或所述步骤4中，氧气和氮气的流量之和大于氩气的流量。
9.根据权利要求1所述的方法，其特征在于，在所述步骤3和/或所述步骤4中，对所述基座施加的射频功率小于500W。
10.根据权利要求1-9任一项所述的方法，其特征在于，所述靶材包括铝、钛、硅、铪或钽靶材，或者包括铝、钛、硅、铪或钽的化合物靶材。
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