CN1926668B - 在高介电常数的介电材料上的硅的氮氧化物层的形成 - Google Patents

在高介电常数的介电材料上的硅的氮氧化物层的形成 Download PDF

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CN1926668B
CN1926668B CN2005800061381A CN200580006138A CN1926668B CN 1926668 B CN1926668 B CN 1926668B CN 2005800061381 A CN2005800061381 A CN 2005800061381A CN 200580006138 A CN200580006138 A CN 200580006138A CN 1926668 B CN1926668 B CN 1926668B
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gas
silicon
layer
substrate
sih
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CN1926668A (zh
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普拉文·K·纳沃卡
格雷格·东
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Applied Materials Inc
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Abstract

本发明的实施例提供了在设置在衬底上的介电层上沉积覆盖层的方法。在一实施例中，一种工艺包括暴露衬底在沉积工艺中以在其上形成介电层，在沉积工艺期间暴露该衬底于硅前驱物脉冲和氧化气体的顺序脉冲中以在该介电层上形成含硅的层，暴露该衬底于氮化工艺中以在其上形成覆盖层，暴露该衬底在退火工艺中预定的时间。该覆盖层可为约5或更薄的厚度。在一实例中，该氧化气体含有通过含有催化剂的水蒸汽产生器处理氢源气体和氧源气体生成的水蒸汽。在另一实例中，沉积、氮化和退火工艺在同一工艺腔室中进行。

Description

在高介电常数的介电材料上的硅的氮氧化物层的形成
背景技术
技术领域
本发明的实施方式主要涉及在衬底上沉积材料的方法，尤其涉及，在介电材料上沉积诸如硅氧化物或硅氮氧化物的覆盖层的方法。
在半导体工艺、平板显示工艺或其它电子器件工艺领域中，气相沉积工艺对在衬底上沉积材料已具有重要的地位。随着电子器件的几何结构不断变小和器件密度的不断增加，图形的尺寸和高宽比变得更加严格，例如，需要考虑0.07μm的图形尺寸和为10甚至更大的高宽比。相应地，以形成这些器件的材料的均匀沉积变得越来越重要。
虽然传统的化学气相沉积(CVD)已表明成功地用在低至0.15μm几何结构和高宽比的器件中，但更严格的器件几何结构需要另外的沉积技术。一种受到广泛关注的技术是原子层沉积(ALD)。在ALD工艺中，反应气体依次进入含有衬底的工艺腔室。一般地，第一反应物脉冲进入该工艺腔室并被吸收在衬底表面。第二反应物脉冲进入该工艺腔室并和第一反应物反应形成沉积材料。通常在输送每种反应气体之间进行冲洗步骤。该冲洗步骤可以是用载送气体的连续冲洗或在该反应气体输送之间的脉冲冲洗。
对小器件组件产生干扰的问题是从一材料层到另一材料层中存在元素的扩散。因为掺杂物(例如硼)容易扩散，所以由元素扩散引起的污染在与掺杂的多晶硅靠近的材料层中非常明显。为了限制掺杂物扩散，已采用氮化工艺以使高介电常数的介电材料诸如硅酸铪密化。密化工艺使氮进入介电材料与之结合并形成Si-N键和Hf-N键。虽然Si-N键为必要的，但Hf-N键因为它们的金属性特点将使漏电增加是不需要的。此外，由于多晶硅和许多高介电常数材料之间的相互作用通常具有错误的功函数阈值偏移，工业上已在努力引入适合用在衬底上的高介电常数材料。
另外，硅氮化物材料已用作在介电/栅介面处的有效的硼阻挡层。然而，硅氮化物材料由于本身固定的电荷可能具有不良的器件特性。理想的阻挡层应当形成介电/栅介面并通过阻挡掺杂物扩散至多晶硅层而改善多晶硅中载流子的迁移率。
在现有技术中，ALD工艺已用于在衬底上沉积薄的硅氧化物层。采用ALD工艺沉积、等离子体处理并接着进行退火的硅氧化物层已用作覆盖层。然而，硅氧化物层通常采用ALD工艺沉积，该ALD工艺用水或氧气交替Cl2SiH2脉冲。由于氯化硅烷前驱物的因素，可能导致该硅氧化物被卤素杂质污染。如果被卤素污染的硅氧化物层用作掺杂剂阻挡层，氯可能扩散进入多晶硅层，将对载流子的迁移率带来不利影响。
因此，需要一种沉积工艺用阻挡层诸如硅氧化物或硅氮化物覆盖介电材料。该阻挡层应当不会被卤素污染并在降低掺杂剂扩散的同时尽可能薄，以及该阻挡层和该介电层应当在化学上相容。
发明内容
在一实施例中，提供了一种在设置在衬底上的介电层上沉积覆盖层的方法，该方法包括暴露衬底在沉积工艺中以在其上形成介电层以及在沉积工艺期间暴露该衬底在硅前驱物和氧化气体的顺序脉冲中以在该介电层上形成含硅层。这种方法还包括暴露该衬底在氮化工艺中以在其上形成覆盖层以及可选地暴露该衬底在退火工艺中一段预定的时间。该覆盖层可为约的厚度或者更薄。在一实例中，该氧化气体包含由含有催化剂的水蒸汽产生器产生的氢源气体和氧源气体形成的水蒸汽。该介电层可含有HfO2、HfSiO4、HfSixOyNz、HFAlxOyNz、Al3O2、HfO2/Al3O2积层、LaAlOx、LaOx及其衍生物或它们的组合。优选地，在氮化工艺期间该覆盖层暴露于含氮的等离子体中。在另一实施例中，沉积、氮化和退火工艺在同一工艺腔室中进行。
在另一实施例中，提供一种在工艺腔室中在介电层上沉积覆盖层的方法，该方法包括在衬底上沉积介电层，并在ALD工艺期间暴露该介电层于硅前驱物和氧气的顺序脉冲中以在介电层上沉积含硅层，接着暴露含硅层于氮化工艺中以形成覆盖层。这种方法还提供暴露该衬底于退火工艺中以及接着在该覆盖层上沉积多晶硅层。
在另一实施例中，提供一种采用原子层沉积工艺在介电层上沉积含硅覆盖层的方法，该方法包括在工艺腔室内设置含有介电层的衬底，暴露该衬底于硅前驱物中，用冲洗气体冲洗该工艺腔室，暴露该衬底于含有水蒸汽的氧化气体中。该水蒸汽通过含有催化剂的水蒸汽产生器由氢源气体和氧源气体形成并用冲洗气体冲洗该工艺腔室。
在另一实施例中，提供一种在工艺腔室中在介电层上沉积覆盖层的方法，该方法包括在第一ALD工艺循环期间在衬底上沉积金属硅酸盐材料，该工艺循环包括依次地引入金属前驱物脉冲、第一氧化气体脉冲、硅前驱物脉冲和第二氧化气体脉冲。这种方法还提供通过停止金属前驱物脉冲和第一氧化气体脉冲改变第一ALD工艺循环以形成第二ALD工艺循环以及在第二ALD工艺循环期间，在该金属硅酸盐材料上沉积硅氧化物层，其中该第二ALD工艺循环包括依次通入硅前驱物脉冲和第二氧化气体脉冲。该氧化气体含有通过从水蒸汽产生器通入氢源气体和氧源气体形成的水蒸汽。在一实施例中，该工艺包括铪前驱物硅酸铪材料。在其它实施例中，该金属硅酸盐材料可包含铝、氮或镧。任选地包含掺杂剂(例如硼、磷或砷)的多晶硅层可沉积在硅的氮氧化物层上。
在又一实施例中，提供了一种用于在介电层上沉积覆盖层的方法，包括：在衬底上沉积介电层，其中所述介电层是高介电常数层；通过原子层沉积工艺在介电层上沉积含硅的层的步骤，该步骤包括向工艺腔室中交替脉冲硅前驱物和氧化气体，其中氧化气体含有通过含氢气体和含氧气体流过催化水蒸汽产生器所形成的水；暴露该含硅层在氮化工艺中；以及暴露所述衬底在退火工艺。
在又一实施例中，提供了一种用于通过原子层沉积工艺在介电层上沉积含硅覆盖层的方法，包括：在原子层沉积工艺腔室内提供其上形成有介电层的衬底，其中所述介电层是含铪氧化物层，该含铪氧化物层通过包括交替脉冲铪前驱物和一种氧化气体的步骤的第一原子层沉积工艺形成；将硅前驱物流入所述原子层沉积工艺腔室中以执行第二原子层沉积工艺；用冲洗气体冲洗所述工艺腔室；将所述氧化气体流入所述工艺腔室中以形成含硅覆盖层，所述氧化气体包含通过含氢气体和含氧气体流过催化水蒸汽产生器形成的水蒸汽；以及使用冲洗气体冲洗所述工艺腔室。
在又一实施例中，提供了一种用于在工艺腔室内在衬底表面上沉积含硅层的方法，包括：暴露其上沉积有介电层的衬底于硅前驱物和氧化气体中从而在其上形成硅氧化物层，其中所述介电层是含铪层，所述氧化气体含有通过含氢气体和含氧气体流过水蒸汽产生器所形成的水蒸汽；以及暴露硅氧化物层于氮化工艺中。
附图说明
因此为了更详细地理解本发明的以上所述特征，将参照附图中示出的实施例对以上简要描述的本发明进行更具体的描述。然而，应该注意，附图中只示出了本发明典型的实施例，因此不能认为是对本发明范围的限定，本发明可以允许其他等效的实施例。
图1示出了根据本文所述的一实施例在介电层上形成覆盖层工艺的工序图；
图2A-2F示出了根据本文所述的另一实施例在衬底表面上沉积积层的工艺工序图；
图3示出了根据本文所述的一实施例用于硅前驱物和氧化气体的ALD脉冲工序图；以及
图4示出了可用于实施本文所述的ALD工艺的工艺腔室的示意性截面图。
具体实施方式
本发明的实施例提供一种用于多种应用中的介电材料的制备方法，尤其是用于晶体管和电容器制造中的高介电常数的介电材料的制备方法。一些工艺使用原子层沉积(ALD)技术以控制沉积的介电材料的元素组成。实施例提供一种用作在高介电常数材料上覆盖层的含硅层(例如硅氧化物)的制备方法。在一实例中，该工艺包括产生含水蒸汽的氧化气体的水蒸汽产生器。在ALD工艺期间对硅前驱物和氧化气体依次脉冲以沉积含硅材料。该ALD工艺利用水蒸汽洁净地并有效地形成含硅层，从而显著增加产量。其它方面，在氮化工艺期间(例如去耦等离子体氮化(DPN))，含硅层暴露在氮气等离子体中，并接着暴露于退火工艺中。
在图1中，描述了一示例性工艺工序100用于形成覆盖的介电薄膜，诸如在高介电常数的栅介电材料上的硅氧化物层。图2A-2F相应于工艺工序100以描述半导体器件组件，诸如晶体管的组装。在步骤102中，采用传统的沉积技术诸如ALD、化学气相沉积(CVD)、物理气相沉积(PVD)、热技术或其组合，如在图2A-2B中所示将介电层210沉积在衬底200上。在优选的实施例中，介电层210可通过ALD工艺和ALD设备进行沉积，诸如在于2004年5月12日递交的受让给Applied Materials Inc的待审的美国临时专利申请第60/570,173号，发明名称为“Atomic Layer Deposition of Hafnium-containingHigh-K materials”中描述的该ALD工艺和ALD设备，在此引入其全部内容作为参考。介电层210通常以从约到约
Figure GA20186248200580006138101D00052
范围内的厚度沉积，优选地从约
Figure GA20186248200580006138101D00053
到约
Figure GA20186248200580006138101D00054
并更优选地从约到约例如
Figure GA20186248200580006138101D00057
在沉积介电层210之前，为了用多种功能基团限定衬底表面，衬底200可暴露于预处理工艺中。在开始如本文所述的沉积工艺之前有益的功能基团包括羟基(OH)、烷氧基(OR，其中R＝Me、Et、Pr或Bu)、卤氧基(OX，其中X＝F、Cl、Br或I)、卤化物(F、Cl、Br、或I)、氧气残留物、氨基物(NH或NH2)和酰胺基物(NR或NR2，其中R＝H、Me、Et、Pr或Bu)。该预处理工艺可暴露该衬底于反应物中，诸如NH3、B2H6、SiH4、SiH6、H2O、HF、HCl、O2、O3、H2O、H2O2、H2、原子-H、原子-N、原子-O、乙醇或胺。该功能基团可提供用于将进入的化学前驱物吸附于衬底表面上的基座。该预处理工艺可暴露该衬底表面于该反应物中从约5秒到约2分钟的时间范围，优选地从约10秒到约30秒。在一实例中，在开始ALD工艺之前，该衬底表面暴露于由WVG系统产生的水蒸汽中约15秒。
介电层210沉积在该衬底表面并可能具有同质的、异质的、分层的和/或积层的层叠或叠层的多种组成。介电层210通常为高介电常数材料并可能包括铪、锆、钛、钽、镧、铝、硅、氧和/或氮的组合。介电层210可能的组成包括含铪的材料，诸如铪氧化物(HfOx或HfO2)、硅酸铪(HfSixOy或HfSiO4)、铪硅氮氧化物(HfSixOyNz)、铪氮氧化物(HfOxNy)、铪铝氧化物(HfAlxOy)、铪铝硅氧化物(HfAlxSiyOz)、铪铝硅氮氧化物(HfAlwSixOyNz)、铪镧氧化物(HfLaxOy)；含锆的材料，诸如锆氧化物(ZrOx或ZrO2)、锆硅氧化物(ZrSixOy或ZrSiO4)、锆硅氮氧化物(ZrSixOyNz)、锆氮氧化物(ZrOxNy)、锆铝氧化物(ZrAlxOy)、锆铝硅氧化物(ZrAlxSiyOz)、锆铝硅氮氧化物(ZrAlwSixOyNz)、锆镧氧化物(ZrLaxOy)；其它含铝的材料或含镧的材料，诸如铝氧化物(Al2O3或AlOx)、铝氮化物(AlOxNy)、铝硅氧化物(AlSixOy)、铝硅氮氧化物(AlSixOyNz)、镧铝氧化物(LaAlxOy)、镧氧化物(LaOx或La2O3)，及其衍生物或它们的组合。适用于介电层210的其它介电材料可包括钛氧化物(TiOx或TiO2)、钛氮氧化物(TiOxNy)、钽氧化物(TaOx或Ta2O5)和钽氮氧化物(TaOxNy)。适用于介电层210的介电材料的层叠薄膜包括HfO2/Al2O3、HfO2/SiO2、La2O3/Al2O3和HfO2/SiO2/Al2O3。
在步骤104中，如图2C所示，硅氧化物层220采用ALD工艺沉积在介电层210上。硅氧化物层220可包括二氧化硅(SiO2)或其它硅氧化物(SiOx)，诸如较少的氧化组成。一般地，硅氧化物层220沉积为从约到约
Figure GA20186248200580006138101D00062
之间的厚度，优选地从约
Figure GA20186248200580006138101D00063
到约
Figure GA20186248200580006138101D00064
和更优选地从约
Figure GA20186248200580006138101D00065
到约
Figure GA20186248200580006138101D00066
例如，约
Figure GA20186248200580006138101D00067
在许多实施例中，硅氧化物层220具有约为
Figure GA20186248200580006138101D00068
或更薄的厚度。
与公开的用于在沉积介电层210之前对衬底200的预处理相似，在沉积硅氧化物220之前，介电层210可暴露于预处理工艺中。将该衬底装入工艺腔室中，该工艺腔室可实施循环的沉积并且通过设置预定温度、压力和载送气体的速率调节工艺条件。在一实施例中，用于沉积硅氧化物层220和用于沉积介电层210的工艺腔室为同一个工艺腔室。在另一实施例中，第一工艺腔室用于沉积介电层210，而第二工艺腔室用于沉积硅氧化物层220。该第一工艺腔室和第二工艺腔室可在不同的集簇设备上，但是优选地在同一集簇设备上。
图3描述了根据本发明的实施例，ALD工艺300形成氧化层220。在步骤302中，在该衬底表面上的介电层210暴露于硅前驱物脉冲中，该硅前驱物脉冲通入该工艺腔室中的时间为从约0.1秒到约5秒。然后在步骤304中冲洗气体的脉冲通入该腔室中以冲洗或者除去任何残余的硅前驱物或副产品。在步骤306中，氧化气体的脉冲通入该工艺腔室中。该氧化气体可包括多个媒介物，诸如水蒸汽、氧气。然后在步骤308中冲洗气体脉冲通入该工艺腔室中以冲洗或除去任何残留的氧化气体或副产品。适用的载送气体或冲洗气体可包括氦、氩、氮、氢形成的气体、氧气或及其组合。
在每个沉积循环之后，形成的硅氧化物层220具有特定的厚度。一般地，约8个ALD工艺循环完成可形成约为厚度的硅氧化物层220。根据具体的器件需求，随后的沉积循环可能为必要的以在步骤310中沉积具有预定厚度的硅氧化物层220。在步骤312中，一旦获得了硅氧化物层220的预定厚度，ALD工艺300将终止。
循环的沉积工艺或ALD工艺通常发生在工艺腔室中在压力范围从约1Torr到约100Torr下，优选地从约1Torr到约20Torr，例如，约10Torr。该衬底可加热至温度从约70℃到约1,000℃之间，优选地从约100℃到约450℃，和更优选地从约200℃到约400℃。
在步骤302中，该硅前驱物以约5标准立方厘米每分(sccm)到约200sccm范围的流速通入该工艺腔室。该硅前驱物通常用载送气体诸如氮气，以从约50sccm到约1000sccm范围的总流速通入。该硅前驱物根据具体的工艺和所需的硅氧化物层220以速率从约0.1秒到约10秒的范围脉冲进入该工艺腔室。在具有长脉冲的实施例中，该硅前驱物以速率从约1秒到约5秒的范围进行脉冲，例如约3秒。在具有短脉冲的实施例中，该硅前驱物以速率从约0.1秒到约1秒进行脉冲，例如约0.5秒。在一实施例中，该硅前驱物优选地为四(二甲基胺基)硅烷<(Me2N)4Si或TDMAS>或三(二甲基胺基)硅烷<(Me2N)3SiH或Tris-TDMAS>。
在步骤306中，氧化气体以从约20sccm到约1,000sccm范围的速通入该工艺腔室率，优选地从约50sccm到约200sccm。该氧化气体根据具体的工艺以速率从约0.1秒到约10秒的范围脉冲进入该工艺腔室。在具有长脉冲的实施例中，该氧化气体以速率从约1秒到约5秒的范围进行脉冲，例如1.7秒。在具有短脉冲的实施例中，该氧化气体以速率从约0.1秒到约3秒的范围进行脉冲，例如约0.5秒。
该氧化气体可由与该工艺腔室流动连接的水蒸汽生成(WVG)系统产生。该WVG系统通过氧源气体(例如O2)和氢源气体(例如H2)的催化反应生成超高纯度的水蒸汽。氢气和氧气分别以速率从约20sccm到200sccm的范围通入该WVG系统。通常，氧气流动要快于氢气流动以具有过量的氧气。例如，氢气的流速约为100sccm，而氧气的流速约为120sccm。因此，从WVG系统流出来的水蒸汽富含氧气。在一实例中，氢气的流速约为100sccm而氧气的流速约为120sccm，以产生含有流速约为100sccm的水蒸汽和流速约为70sccm的氧气的氧化气体。可以为每个独立的工艺实验性确定优选的氢气/氧气浓度以调节含有水蒸汽和氧气或氢气的氧化气体的向外流动。在另一实例中，氢气的流速约为50sccm而氧气的流速约为60sccm。
该WVG系统具有成排催化剂的反应器或催化剂盒，其中水蒸汽通过化学反应产生，不同于火法产生器由于点火产生水蒸汽。该催化剂可包括金属或合金，诸如钯、铂、镍及其组合或合金。本发明中对于ALD工艺来说超高纯度的水为理想的。在一实施例中，为了防止未发生反应的氢气向下流动，允许向WVG通入约5秒氧气。接着，允许氢气进入该反应器约5秒。氢气和氧气之间的催化反应是瞬时的，因此在氢气和氧气达到反应器后立即生成水蒸汽。调整氢气和氧气的流动允许该浓度精确地控制在从1％到100％的任意一点，也就是说，该氧化气体可包含水蒸汽、氢气、氧气及其组合。在一实例中，该氧化气体含有水蒸汽和氧气。在另一实例中，该氧化气体含有水蒸汽和氢气。类似地，通过使用同样的气流控制方法，也可调节水蒸汽的总量，每次得到精确和可重复的流动。在优选的实施例中，水蒸汽通常通过向该WVG系统中通入氧气和氢气生成。
适于生成含有水蒸汽的氧化气体的氧源气体可包括氧气(O2)、氧原子(O)、臭氧(O3)、一氧化二氮(N2O)、一氧化氮(NO)、二氧化氮(NO2)、五氧化二氮(N2O5)、过氧化氢(H2O2)及其衍生物或它们的组合。适于生成含有水蒸汽的氧化气体的氢源气体可包括氢气(H2)、氢原子(H)、合成气体(N2/H2)、氨气(NH3)、烃(CH4)、乙醇(例如CH3OH)及其衍生物和它们的组合。载送气体可和该氧源气体或氢源气体中任意之一一同流入，并可包括N2、He、Ar及其组合。优选地，该氧源气体为氧气或一氧化二氮，该氢源气体为氢气或合成气体，诸如氮气中5vol％的氢气。适用的WVG系统可从诸如由位于California，Santa Clara，的Fujikin ofAmerica，Inc生产的WVG，和由位于Menlo Park，California的Ultra Clean Technology公司生产的CSGS(Catalyst Steam Generator System)购买得到。
在步骤304和308中，优选地为氩气或氮气的冲洗气体或载送气体的脉冲通常以约2标准升每分(slm)到约22slm的流速通入，优选地约10slm。根据具体的工艺，该冲洗气体或载送气体以从约0.1秒到约10秒的范围的流速通入该工艺腔室。在长时间的实施例中，该冲洗气体或载送气体以速率从约为1秒到5秒的范围进行脉冲，例如约1.7秒。在短时间的实施例中，冲洗气体或载送气体以从约0.1秒到约3秒的速率进行脉冲，例如约0.5秒。每个工艺循环维持约2秒。各工艺周期(从步骤302至308)持续范围为从约0.01约至20秒的时间周期。例如，在长周期实施例中，处理周期持续约10秒，而在短周期中，处理周期持续约2秒。具体的压力和时间通过常规的实验获得。在一实例中，为了维持相似的产量，300mm直径的晶片需要的流速为200mm直径的晶片所需的2倍。
在一实施例中，在ALD工艺期间，氢气气体应用为载送气体、冲洗和/或反应气体以减少来自沉积的材料的卤素污染。含有卤素原子的前驱物(例如Cl2SiH2、SiCl4或Si2Cl6)可容易污染沉积的材料。氢气为还原剂并将生成卤化氢(例如HCl)作为挥发性的和可除去的副产品。因此，当氢气与前驱物化合物(例如硅或氧气前驱物)结合时，氢气可用作载送气体或反应气体并可包括另一载送气体(例如Ar或N2)。在一实例中，在约从100℃到约500℃的温度范围水/氢气混合物用于在本文所述的ALD工艺期间降低卤素浓度和增加沉积的硅氧化物层的氧气浓度。
多种硅前驱物落入本发明的范围内。一个重要的前驱物特点在于要有合适的气压。前驱物在周围温度和压力下可能具有气态、液态或固态。然而，在腔室内使用挥发性的前驱物。示例性的硅前驱物包括硅烷、烷基硅烷、烷基氨基硅烷、硅烷醇、烷氧基硅烷，例如，硅前驱物包括(Me2N)4Si、(Me2N)3SiH、(Me2-N)2SiH2、(Me2N)SiH3、(Et2N)4Si、(Et2N)3SiH、(MeEtN)4Si、(MeEtN)3SiH、Si(NCO)4、MeSi(NCO)3、SiH4、Si2H6、SiCl4、Si2Cl6、MeSiCl3、HSiCl3、Me2SiCl2、H2SiCl2、MeSiH3、Me2SiH2、EtSiH3、Et2SiH2、MeSi(OH)3、MeSi(OH)2、(EtO)4Si及其衍生物或者它们的组合。其它适于作为硅前驱物的烷氧基硅烷可由化学通式(RO)4-nSiLn表示，其中n＝0-3，R＝甲基、乙基、丙基或丁基以及L＝H、OH、F、Cl、Br或I或及其组合物。适于作为硅前驱物的其它烷基硅烷化合物包括R4-nSiHn，其中R分别地为甲基、乙基、丙基、丁基或其它烷基以及n＝0-3。适于作为硅前驱物的其它烷基氨基硅烷化合物包括(RR’N)4-nSiHn，其中R或R’分别为氢、甲基、乙基、丙基或丁基以及n＝0-3。此外，本发明的一些实施例中更高硅烷用作硅前驱物。在2003年10月17日递交的普通转让的公开号为10/688,797的美国专利申请，公开号为US 20040224089，发明名称为“Silicon-containing Layer Deposition with Silicon Compounds”中公开了更高硅烷，在此引入其全部内容作为参考描述硅前驱物。在ALD工艺期间使用的优选的硅前驱物在此包括(Me2N)3SiH、(Et2N)3SiH、(Me2N)4Si、(Et2N)4Si和(MeEtN)4Si。
在本发明另一的实施例中，通过停止在步骤102中使用特定反应物流入，诸如金属前驱物，同时继续通入其它反应物，诸如硅前驱物和/或氧化气体，在同一ALD腔室中实施步骤102和104。在一实施例中，介电层210包含硅酸铪并且该层通过ALD工艺沉积，该ALD工艺包括依次脉冲HfCl4、水蒸汽、TDMAS和水蒸汽，在ALD循环期间每个前驱物通过冲洗分开。介电层210通过重复ALD循环形成直到该薄膜具有约为
Figure GA20186248200580006138101D00101
的厚度(步骤102)。在不停止ALD工艺情况下，该ALD循环通过停止HfCl4半反应和多个水蒸汽半反应中之一并继续TDMAS半反应和其它水蒸汽半反应。该ALD工艺(步骤104)通过依次脉冲TDMAS和水蒸汽进行，同时每个前驱物由冲洗循环分开。在ALD工艺约8个循环后，在含有硅酸铪的介电层210上形成厚度约为
Figure GA20186248200580006138101D00102
的硅氧化物层220。
在步骤106期间，该衬底可移送至去耦等离子体氮化(DPN)腔室中，诸如CENTURATM DPN腔室，可从位于Santa Clara，California的Applied MaterialsInc购买。在一实施例中，该DPN腔室在同一集簇设备上作为ALD腔室用于沉积介电层210和/或该ALD腔室用于沉积硅氧化物层220。因此，该衬底可暴露于氮化工艺中而不被暴露于周围环境中。硅氧化物层220暴露于氮化工艺中以物理上使氮原子进入硅氧化物材料结合形成含氮的硅氧化物层230，如图2D中所示。含氮的硅氧化物层230的氮浓度可在从约5原子百分率(at％)到约40at％的范围，优选地从约10at％到约25at％。
优选地，该氮化工艺暴露硅氧化物层于氮等离子体中，诸如DPN工艺。在DPN工艺期间，硅氧化物层220用通过一起流入的N2和惰性气体等离子体形成的原子-N碰撞。除N2，其它含氮气体也可用于形成氮等离子体，诸如NH3、肼(例如N2H4或MeN2H3)、胺(例如Me3N、Me2NH或MeNH2)、苯胺(例如C6H5NH2)和叠氮化物(例如MeN3或Me3SiN3)。可用在DPN工艺中的其它惰性气体包括氦气、氖气或氙气。该氮化工艺进行的时间周期从约10秒到约120秒范围，优选地从约15秒到约60秒，例如，约30秒。此外，该氮化工艺在等离子体功率设置在约900瓦到约2700瓦的和压力在约10mTorr到约100mTorr下进行。氮气流速从约0.1slm到约1.0slm，同时惰性气体流速从约0.1slm到约1.0slm。在优选的实施例中，该氮化工艺为DPN工艺并包括由一起流入的Ar和N2形成的等离子体。
在另一实施例中，代替移送衬底进入DPN腔室，氮化工艺可包括在每个ALD半反应期间在ALD循环完成时和/或硅氧化物层220沉积完成时暴露硅氧化物层220于氮等离子体中。例如，氮化远程等离子体暴露于硅氧化物层220上以直接在ALD工艺腔室中形成含氮的硅氧化物层230。基本的氮化物也可能通过加热或热线生成并用在氮化工艺期间。考虑采用其它氮化工艺形成含氮的硅氧化物层230，该氮化工艺包括在含氮环境中对衬底退火处理，和/或在形成含氮的硅氧化物层230同时在ALD循环中在附加的半反应中包含氮气前驱物。例如，在ALD循环期间以形成硅氧化物的附加半反应可包含后紧接着冲洗气体的脉冲的NH3的脉冲。
衬底接着移送至退火腔室，诸如从位于Santa Clara，California的AppliedMaterials Inc.购买的CENTURATM RADIANCETM RTP腔室。该退火腔室可在同一集簇设备上作为沉积腔室和/或氮化腔室。因此，该衬底可在不暴露于周围环境下进行退火。图1，步骤108，该衬底进行退火处理使含氮的硅氧化物层230变为覆盖层240，诸如硅氮氧化物(SiCxNy)，如图2E中所示。该衬底加热至温度从约600℃到约1200℃范围内，优选地从约800℃到约1,100℃，维持时间周期为从约1秒到约120秒范围内，优选地从约30秒到约90秒，例如，在约1,000℃维持约60秒。一般地，该退火腔室气体含有至少一种退火气体，诸如O2、N2、NH3、N2H4、NO、N2O或其组合。该退火腔室维持在压力从约5Torr到约100Torr的范围流入，例如在约15Torr。含氮的硅氧化物层230中的氮原子化学结合进入覆盖层240。
一旦覆盖层240形成，如图2F中所示，可在其上沉积另外的材料，诸如多晶硅层250。多晶硅层250可通过CVD、原子层外延(ALE)、热分解方法或者现有技术中熟知的类似技术沉积。多晶硅层250通常包含掺杂剂，诸如硼、磷或砷。覆盖层240在介电层210和多晶硅层250之间的介面245处保持为掺杂剂阻挡层，因此载流子的迁移率在硼掺杂的多晶硅层250中增加。
硬件
图4示出了一实施例的工艺腔室380的示意截面图，该工艺腔室包括适用于诸如原子层沉积或快速化学气相沉积的循环沉积的气体输送装置430。在共同转让的公开号为第20030121608号的美国专利中公开了工艺腔室380的具体描述，在此引入其全部内容作为参考。在2004年5月12日递交的受让给AppliedMaterials，Inc.的在审美国临时专利申请第60/570/173号，发明名称为“AtomicLayer Deposition of Hafnium-containing High-K Materials”中描述了用于循环沉积的几个另外腔室，在此引入其全部内容作为参考。用在此处的术语原子层沉积(ALD)和快速化学气相沉积指依次引入反应物以在衬底表面上沉积薄层。可重复该依次引入的反应物以沉积多个薄层从而形成所需厚度的均匀层。该工艺腔室380也可适用于其它沉积技术。
该工艺腔室380包含具有侧壁384和底部386的腔室主体382。该工艺腔室380内的缝隙阀门388为从该工艺腔室380输送和取回衬底390的自动机械(未示出)提供了通道，该衬底诸如具有直径为200mm或320mm的半导体晶片或玻璃衬底。
衬底支架392在该工艺腔室380内将衬底390支撑在衬底的接收面391上。该衬底支架392安装在升降电动机414上以提升和降低该衬底支架392以及设置在其上衬底90。与升降电动机418相连的升降台416安装在该工艺腔室380中并提升和降低通过衬底支架392可移动地设置的杆420。该杆420在该衬底支架392的表面上提升和降低该衬底392。该衬底支架392可包括用于在处理该衬底390时将该衬底390固定在该衬底支架392上的真空卡盘、静电卡盘或压紧环。
该衬底支架392可加热以增加设置在其上的衬底390的温度。例如，该衬底支架392可利用诸如电阻加热器的嵌入式加热元件加热，或可利用诸如设置在该衬底支架392上方的加热灯的辐射热加热。冲洗环422可设置在该衬底支架392上以限定冲洗通道424，该通道424提供冲洗气体至该衬底390的外围部分以避免在其上的沉积。
气体输送装置430设置在该腔室体382的上部分以提供气体诸如工艺气体和/或冲洗气体进入该工艺腔室380。真空系统478与泵通道479相连用来从该工艺腔室380排出任意所需的气体并有助于在该工艺腔室380的泵区内维持所需的压力或所需的压力范围。
在一实施例中，如图4所示的该腔室允许该工艺气体和/或冲洗气体经由该气体输送装置430以参照该衬底390的平面的法线方向(也就是90°)进入该工艺腔室380。因此，该衬底390的表面对称地暴露于气体中，因此允许在衬底上形成均匀的薄膜。该工艺气体包括在一个脉冲期间的硅前驱物(例如TDMAS)和包括在另一个脉冲中的氧化气体(例如水蒸汽)。
在一实施例中，该气体输送装置430包含腔室盖432。该腔室盖432包括从该腔室盖432的中心部分延伸出的扩张式通道434和从扩张式通道434延伸至该腔室盖432外围部分的底部表面460。该底部表面460的尺寸和形状基本上覆盖设置在该衬底支架392上的衬底390。该腔室盖432可具有在腔室盖432的外围部分并靠近该衬底390的外周的阻塞462。该盖部分472包括扩张式通道434的一部分和气体入口436A、436B。扩张式通道434具有气体入口436A、436B以提供气体从两个相似的阀门442A、442B流入。从该阀门442A、442B流入的该气体可一起和/或独立地提供。
在一结构中，阀门442A和阀门442B连接以分离反应气体源但是优选地与同一冲洗气体源连接。例如，阀门442A与反应气体源48连接而阀门442B与反应气体源439连接，并且两个阀门442A、442B都与冲洗气体源440连接。每个阀门442A、442B包括具有阀门座组件444A、444B的输送管443A、443B以及包括具有与阀门452A、452B流动连接阀门座组件446A、446B的的冲洗管445A、445B。该输送管443A、443B与该反应气体源438、439相连并与扩张式通道434的该气体入口436A、436B相通。在一实施例中，附加的反应气体源(例如WVG系统输出)、输送管、气体入口和阀门可加在该气体输送装置430(未示出)中。输送管443A、443B的阀门座组件444A、444B控制从反应气体源438、439至扩张式通道434的反应气体流。该冲洗管445A、445B与该冲洗气体源440相连并与输送管443A、443B在该输送管443A、443B的该阀门座组件444A、444B的下游相交。该冲洗管4745A、445B的阀门组件446A、446B控制从该冲洗气体源440至输送管443A、443B的冲洗气体流。如果载送气体用于输送该反应气体源438、439的反应气体，优选地该同一气体用作载送气体和冲洗气体(例如氮气用作载送气体和冲洗气体)。在一实施例中，反应气体源438包含TDMAS或Tris-DMAS而气体源439包含来自WVG系统的含有水蒸汽的氧化气体。气体源439可与WVG系统流动相连或者气体源439可为WVG系统。
每个阀门座组件444A、444B、446A、446B可包含膜片和阀门座。该膜片可因受承载而打开或关闭并可分别地因受到控制而关闭或打开。该膜片可气动控制或可电动控制。气动控制阀门的实例包括可从Fujiken和Veriflow购买的气动控制阀门。电动控制阀门的实例包括可从Fujiken购买的电动控制阀门。可编程的逻辑控制器448A、448B可与阀门442A、442B连接用来控制阀门442A、442B的阀门座组件444A、444B、446A、446B的膜片的动作。气动控制阀门可以提供时间低至约0.02秒的气体脉冲。电动控制阀门可以时间周期低至约0.005秒的气体脉冲。电动控制阀门通常需要使用连接在该阀门和该可编程的逻辑控制器之间的驱动器。
每个阀门442A、442B可为零死容积阀门以当阀门的阀门座组件444A、444B为关闭时能使来自输送管443A、443B的反应气体的冲洗。例如冲洗管445A、445B可设置在靠近输送管443A、443B的阀门座组件444A、444B处。当该阀门座组件444A、444B关闭时，该冲洗管445A、445B可提供冲洗气体以冲洗该输送管443A、443B。在所示的实施例中，该冲洗管445A、445B设置为与该输送管443A、443B的阀门座组件444A、444B稍微分开从而当阀门座组件444A、444B打开时冲洗气体不会直接输送进入该阀门座组件444A、444B。这里所用的零死容积阀门定义为具有可忽略的死容积(也就是说，不是必须为零死容积)的阀门。
每个阀门442A、442B可适合提供反应气体438、439和冲洗气体440的组合气体流和/或独立气体流，通过阀门442A提供的反应气体438和冲洗气体440的组合气体流的一实例包含从冲洗气体源440通过冲洗管445A的冲洗气体的连续流和从反应气体源438通过输送管443A的反应气体脉冲。该冲洗气体的连续流可通过使该冲洗管445A的阀门座组件446A的膜片保持为打开提供。来自该反应气体源438的反应气体脉冲可通过该打开和关闭输送管443A的阀门座组件444A的的膜片提供。参照阀门442A，通过阀门442A提供的该反应气体438和冲洗气体440的独立气体流的一实例包含从该冲洗气体源440通过冲洗管445A的冲洗气体脉冲和从该反应气体源438通过输送管443A的反应气体脉冲。该冲洗气体脉冲可通过打开和关闭该打开的冲洗管445A的阀门座组件446A的膜片提供。来自该反应气体源438的该反应气体脉冲可通过打开和关闭该输送管443A的膜片阀门座444A提供。
该阀门442A、442B的输送管443A、443B通过气体导管450A、450B与气体入口436A、436B连接。该气体导管450A、450B可和该阀门442A、442B集成在一起或者分立开。一方面，该阀门442A、442B在靠近扩张式管道434处连接以减少该阀门442A、442B和该气体入口436A、436B之间的输送管443A、443B和气体导管450A、450B的不必要的容积。
图4中，扩张式管道434包括具有内径从扩张式管道434的上部分437到下部分435增加的管道，该管道靠近该腔室盖432的底表面460。在一具体的实施例中，用于腔室适合处理200mm直径衬底的该扩张式管道434的内径在该扩张式管道的上部分437处为在约0.2英寸(0.51cm)到约1.0英寸(2.54cm)之间，优选地在约0.3英寸(0.76cm)到约0.9英寸(2.29cm)之间和更优选地在约0.3英寸(0.76cm)和约0.5英寸(1.27cm)之间，以及在该扩张式管道434的下部分435处为在约0.5英寸(1.27cm)和约3.0英寸(7.62cm)之间，优选地在约0.75英寸(1.91cm)到约2.5英寸(6.35cm)和更优选地在约1.1英寸(2.79cm)到约2.0英寸(5.08cm)之间。
在另一具体的实施例中，用于适合处理300mm直径衬底的腔室的该扩张式管道434的内径在该扩张式管道434的上部分437处为在约0.2英寸(0.51cm)到约1.0英寸(2.54cm)之间，优选地在约0.3英寸(0.76cm)到约0.9英寸(2.29cm)之间和更优选地在约0.3英寸(0.76cm)和约0.5英寸(1.27cm)之间，以及在用于300mm衬底的该扩张式管道434的下部分435处为在约0.5英寸(1.27cm)和约3.0英寸(7.62cm)之间，优选地在约0.75英寸(1.91cm)到约2.5英寸(6.35cm)和更优选地在约1.2英寸(3.05cm)到约2.2英寸(5.59cm)之间。一般地，上述尺寸应用于适于提供总气流在约500sccm和约3,000sccm之间的扩张式管道。
在其它具体实施例中，可改变该尺寸以适合某种气流通过。一般地，较大的气流将需要较大直径的扩张式管道。在一实施例中，该扩张式管道434可为截锥形的形状(包括类似于截锥形的形状)。不管气体朝着该扩张式管道434的壁或者直接向下朝着该衬底提供，由于该气体的膨胀，该气流的速率将随着该气流经由扩张式管道434降低。该气流速率的减小有助于降低该气流将吹走吸附在该衬底390表面上的反应物的可能性。
不希望束缚于理论，普遍认为该扩张式管道的从该扩张式管道的上部分437到下部分435逐渐降低的直径允许经由该扩张式管道434较少的气体绝热膨胀，这有助于控制该气体的温度。例如，从该气体入口436A、436B输送进入该扩张式管道434的气体的突然绝热膨胀可导致该气体温度的下降，这将引起该前驱物气体的凝结和微粒的形成。在另一方面，普遍认为根据本发明实施例的逐渐扩张式管道434将提供气体的较少绝热膨胀。因此，更多的热量可传输至或自该气体，因此，通过控制该气体的周围环境温度(也就是说，控制该腔室盖432的温度)，可更容易地控制该气体的温度。该逐渐扩张式管道可包括一个或多个锥形内表面，诸如锥形平面、凹面、凸面或其组合或可包括一个或多个锥形内表面的截面(也就是说，一部分锥形和一部分非锥形)。
在一实施例中，该气体入口436A、436B位于靠近该扩张式管道434的上部437的位置。在其它实施例中，一个或多个气体入口可位于该上部分437和下部分435之间沿着该扩张式管道434的长度的位置。
图4中，控制单元480，诸如程序化的个人计算机，工作站计算机等可与该工艺腔室380连接控制工艺条件。例如，在衬底处理工序的不同阶段期间，该控制单元480可设置为控制从气体源438、439、440通过该阀门442A、442B的各种气体和冲洗气体流。直观地，该控制单元480包括中央处理单元(CPU)482、支持电路484和含有相关控制软件483的存储器486。
该控制单元480可以是能够在用于控制各种腔室和子处理器的工业装置中使用的通用计算机处理器的任意形式中之一。该CPU482可使用任意适合的存储器486，诸如随机存取存储器、只读存取器、软盘驱动器、光盘驱动器、硬盘或任意其它形式的本地的或远程的数字存储器。各种支持电路可与该CPU482连接用于支持该工艺腔室380。该控制单元480可与位于靠近单独的腔室元件的另一控制器连接，诸如阀门442A、442B的可编程逻辑控制器448A、448B的位置。该控制单元480和该工艺腔室380中各种其它元件之间的双向通讯通过称为信号总线488的集中的大量信号电缆处理，图4中示出了一些信号线。除控制来自气体源438、439、440(例如WVG系统)的工艺气体和冲洗气体和阀门442A、442B的可编程的逻辑控制器448A、448B，该控制单元480可设置为负责用于晶片处理的其它活动的自动控制，诸如晶片传送、温度控制、腔室抽空和其它活动，其中一些在本文其它部分描述。
用在此处的“衬底表面”，称为在其上可实施工艺的衬底上形成的任何衬底或材料表面。例如，其上可实施工艺的衬底表面根据应用包括材料，诸如硅、硅氧化物、应变硅、绝缘体上硅(SOI)、碳掺杂硅氧化物、硅的氮化物、掺杂硅、锗、镓、砷、玻璃、蓝宝石，以及任意其它材料诸如金属、金属氮化物、金属合金和其它导电材料。衬底表面的阻挡层、金属或金属氮化物包括钛、钛的氮化物、钨的氮化物、钽和钽的氮化。衬底可具有多种尺寸，诸如200mm或300mm直径晶片，以及矩形或正方形平面。本文描述的实施例工艺在许多衬底和表面上沉积含硅层，尤其地，高介电常数的介电材料。其上有利于实施本发明实施例的衬底包括，但不限于半导体晶片，诸如晶体硅(例如Si<100>或Si<111>)、硅氧化物、应变硅、硅锗、掺杂或未掺杂的多晶硅、掺杂或未掺杂的硅片和构图的或未构图的晶片。衬底可暴露于与处理的工艺中以抛光、蚀刻、还原、氧化、羟化、退火和/或烘干该衬底表面。
此处使用的“原子层沉积”或“循环沉积”为依次引入两个或更多反应性化合物以在衬底表面沉积一层材料。该两个、三个或更多反应性化合物可交替地进入工艺腔室的反应区。通常地，每个反应性化合物通过时间延迟分开以允许每个化合物在衬底表面吸附和/或反应。一方面，第一前驱物或化合物A脉冲进入该反应区随后为第一时间延迟。接着，第二前驱物或化合物B脉冲进入该反应区紧接着第二延迟。在每个时间延迟期间冲洗气体诸如氮气进入该工艺腔室中冲洗该反应区或从该反应区除去任何残留的反应性化合物或副产品。另外，该冲洗气体可在整个沉积工艺期间连续地流动从而在反应性化合物脉冲之间的时间延迟期间只有冲洗气体流。该反应性化合物为交替地脉冲直到在衬底表面上形成所需的薄膜或薄膜厚度。在任一情况中，该ALD工艺中脉冲化合物A、冲洗气体、脉冲化合物B和冲洗气体为一个循环。一个循环可用化合物A或化合物B中任意之一开始并继续该循环的每个指令直到得到所需厚度的薄膜。在另一实施例中，包含化合物A的第一前驱物、包含化合物B的第二前驱物和包含化合物C的第三前驱物分别地脉冲进入该工艺腔室中。另外，第一前驱物的脉冲在时间上可与第二前驱物的脉冲重迭，而第三前驱物的脉冲在时间上不与第一和第二前驱物任意之一的脉冲重迭。
在此使用“脉冲”意在表示具体化合物的量是间接地或非连续地进入工艺腔室的反应区中。在每个脉冲内具体化合物的量可根据脉冲的持续时间而随着时间改变。每个脉冲的时持续间根据多个因素是可变的，诸如，使用的该工艺腔室的体积容量、连接至其的真空系统和该具体化合物本身的挥发性/反应性。在此使用的“半反应”表示前驱物脉冲步骤后紧接着冲洗步骤。
实施例
该ALD工艺维持在从约70℃到约1,000℃的温度，优选地从约100℃到约400℃，例如约250℃。该ALD工艺在工艺腔室中进行，气压范围在从约0.1Torr到约100Torr，优选地从约1Torr到约10Torr。载送气体(例如N2或Ar)的流速在约2slm到约22slm，优选地约10slm。
实施例1-A含硅的覆盖层形成在高介电常数的栅介质上。最初地，衬底放置在ALD腔室中并且该衬底表面暴露于预处理的水蒸汽中以形成羟基基团。通过实施利用铪前驱物(TDEAH)、硅前驱物(TDMAS)和由水蒸汽产生器(WVG)系统产生的原位水蒸汽的ALD工序在基板表面上沉积硅酸铪，其中该WVG系统可从位于California，Santa Clara的Fujikin ofAmerica，Inc购买。该ALD循环包括依次脉冲TDEAH、水蒸汽、TDMAS和水蒸汽，同时每个前驱物通过氮气冲洗分开。通过重复该循环直到该薄膜的厚度约
Figure GA20186248200580006138101D00181
形成该硅酸铪层。
接着，在同一ALD腔室中在该硅酸铪层上形成该含硅的覆盖层。硅氧化物通过依次脉冲具有由WVG系统形成的原位水蒸汽的脉冲硅前驱物(TDMAS)随着ALD工艺生长。载送气体，诸如氮气以约2slm的流率导入ALD工艺腔室中。该TDMAS定量进入该载送气体并脉冲进入该腔室约1秒。氮气冲洗气体脉冲进入该腔室约1.5秒以除去任何非结合的TDMAS。氢气和氧气分别以100sccm和约80sccm的流速由WVG系统提供。从WVG系统出来的该原位水蒸汽具有约100sccm的水和约30sccm的氧气。该原位水蒸汽脉冲进入该腔室为1.7秒。该氮气的冲洗气体脉冲进入该腔室为1.5秒以除去任何非结合的或未反应的反应物。该ALD循环重复8次以产生约
Figure GA20186248200580006138101D00182
厚度的硅氧化物层。
该衬底移送至去耦等离子体氮化(DPN)腔室，诸如可从位于California，Santa Clara的Applied Materials，Inc购买的CENTURATM DPN腔室。该衬底表面通过共流入N2和氩等离子体暴露氮化工艺中。该氮化工艺进行约30秒使氮原子进入硅氧化物层结合。该衬底接着移送至退火腔室，诸如可从位于California，Santa Clara的Applied Materials，Inc购买的CENTURATMRADIANCETM RTP腔室并暴露于退火工艺中。该衬底在压力维持在约15Torr的O2环境中，保持温度约为1,000℃约1分钟。这种结合的氮原子与硅氧化物结合形成键以生成硅的氮氧化物。
实例2-A含硅的覆盖层形成在高介电常数的栅介质上。最初地，衬底放置在与安装有远程等离子体产生器的ALD腔室中，该衬底表面暴露于预处理的水蒸汽中以形成羟基基团。通过执行利用铪前驱物(HfCl4)、硅前驱物(Tris-DMAS)和由WVG系统产生的原位水蒸汽的ALD工艺在该衬底表面上沉积硅酸铪层。该ALD循环包括依次地脉冲HfCl4、水蒸汽、Tri-DMAS和水蒸汽，同时每个前驱物通过氩气冲洗分开。通过重复该循环直到该薄膜具有约为的厚度形成该硅酸铪层，接着，改变该ALD循环。该铪前驱物脉冲和其中一个水蒸汽脉冲停止。因此，形成硅氧化物而不是硅酸铪的该ALD循环，包括继续依次脉冲Tris-DMAS和由WVG系统形成的水蒸汽。载送气体，诸如氩气，以约2slm的流速导向进入该ALD工艺腔室。该Tris-DMAS定量进入该载送气体中并脉冲进入该腔室约1秒。氩气的冲洗气体脉冲进入该腔室1.5秒以除去任何非结合的Tris-DMAS。氢气和氩气分别以100sccm和80sccm的流速供给WVG系统。从WVG系统排出的该原位水蒸汽具有约100sccm的水蒸汽和约30sccm的氧气。该原位水蒸汽脉冲进入该腔室1.7秒。该氩气脉冲进入该腔室1.5秒以除去任何非结合的或未反应的反应物。该ALD循环重复8次以生成约厚度的硅氧化物层。
该衬底保持在安装由远程等离子体产生器的同一ALD腔室中。该衬底表面暴露于远程等离子体氮化工艺约30秒使氮原子进入硅氧化物层内与之结合。该衬底接着移送到另一退火腔室，诸如可从位于California，Santa Clara的Applied Materials，Inc购买的CENTURATM RADIANCETM RTP腔室并暴露于退火工艺中。该衬底在压力维持在约15Torr的O2环境中，保持温度约为1,000℃约1分钟。这种结合的氮原子与硅氧化物形成键以生成硅的氮氧化物。
虽然上文提到了本发明的实施例，但是在不脱离本发明的基本范围以及以下权利要求所确定的范围的情况下，可以设计出本发明的其它和另外的实施例。

Claims (59)

1.一种用于在介电层上沉积覆盖层的方法，包括：
通过包括向衬底表面交替地脉冲金属前驱物和一种氧化气体的步骤的第一原子层沉积工艺在衬底上沉积介电层，其中所述介电层是高介电常数层；
通过第二原子层沉积工艺在介电层上沉积含硅层的步骤，该步骤包括向工艺腔室中交替脉冲硅前驱物和所述氧化气体，其中所述氧化气体含有通过含氢气体和含氧气体流过催化水蒸汽产生器所形成的水蒸汽；
暴露该含硅层在氮化工艺中；以及
暴露所述衬底在退火工艺。
2.根据权利要求1所述的方法，其特征在于，所述氮化工艺包含氮等离子体。
3.根据权利要求2所述的方法，其特征在于，所述退火工艺在从600℃到1200℃的温度范围内执行，执行时间周期在从1秒到120秒的范围内。
4.根据权利要求3所述的方法，其特征在于，所述覆盖层厚度为
Figure FA20186248200580006138101C00011
或者更少。
5.根据权利要求3所述的方法，其特征在于，在所述覆盖层上沉积多晶硅层。
6.根据权利要求5所述的方法，其特征在于，所述多晶硅层含有选自由硼、磷、砷和其组合所组成的群组中的掺杂剂。
7.根据权利要求6所述的方法，其特征在于，所述介电层含有选自由HfO2、HfSiO4、HfSixOyNz、HfAlxOyNz、Al2O3、HfO2/Al2O3积层、LaAlOx、LaOx及其衍生物和它们的组合所组成的群组中的材料。
8.根据权利要求1所述的方法，其特征在于，在同一工艺腔室内执行所述沉积介电层的步骤、沉积含硅层的步骤和氮化工艺。
9.根据权利要求1所述的方法，其特征在于，所述氧化气体含有通过将含氢气体和含氧气体流过水蒸汽产生器所形成的水蒸汽。
10.根据权利要求9所述的方法，其特征在于，所述水蒸汽产生器含有催化剂。
11.根据权利要求10所述的方法，其特征在于，所述含氧气体含有选自由O2、N2O、NO2、N2O5及其衍生物和它们的组合所组成的群组中的至少一种气体。
12.根据权利要求11所述的方法，其特征在于，所述含氢气体包括在载送气体中氢气的体积百分比含量为5％或者更少的合成气体。
13.根据权利要求11所述的方法，其特征在于，所述硅前驱物选自由(Me2N)4Si、(Me2N)3SiH、(Et2N)4Si、(Et2N)3SiH、(MeEtN)4Si、(MeEtN)3SiH、SiH4、SiCl4、H2SiCl2、Si2H6、Si2Cl6及其衍生物和它们的组合所组成的群组。
14.一种用于通过原子层沉积工艺在介电层上沉积含硅覆盖层的方法，包括：
在原子层沉积工艺腔室内提供其上形成有介电层的衬底，其中所述介电层是含铪氧化物层，该含铪氧化物层通过包括交替脉冲铪前驱物和一种氧化气体的步骤的第一原子层沉积工艺形成；
将硅前驱物流入所述原子层沉积工艺腔室中以执行第二原子层沉积工艺；
用冲洗气体冲洗所述工艺腔室；
将所述氧化气体流入所述工艺腔室中以形成含硅覆盖层，该氧化气体包含通过含氢气体和含氧气体流过催化水蒸汽产生器形成的水蒸汽；以及
使用冲洗气体冲洗所述工艺腔室。
15.根据权利要求14所述的方法，其特征在于，所述含氧气体含有选自由O2、N2O、NO2、N2O5及其衍生物和它们的组合所组成的群组中的至少一种气体。
16.根据权利要求15所述的方法，其特征在于，所述含氢气体含有在载送气体中氢气的体积百分比含量为5％或者更少的合成气体。
17.根据权利要求15所述的方法，其特征在于，所述含硅层暴露于氮化工艺中以在其上形成含氮硅层。
18.根据权利要求17所述的方法，其特征在于，在所述氮化工艺以后暴露所述衬底于温度范围在从600℃到1200℃退火工艺中1秒到120秒。
19.根据权利要求18所述的方法，其特征在于，在同一工艺腔室内执行所述沉积、氮化和退火工艺。
20.根据权利要求15所述的方法，其特征在于，所述硅前驱物选自由(Me2N)4Si、(Me2N)3SiH、(Et2N)4Si、(Et2N)3SiH、(MeEtN)4Si、(MeEtN)3SiH、SiH4、SiCl4、H2SiCl2、Si2H6、Si2Cl6及其衍生物和它们的组合所组成的群组。
21.根据权利要求20所述的方法，其特征在于，所述含硅覆盖层厚度为或者更少。
22.根据权利要求20所述的方法，其特征在于，在所述含硅覆盖层上沉积多晶硅层。
23.根据权利要求22所述的方法，其特征在于，所述多晶硅层含有选自由硼、磷、砷和它们的组合所组成的群组中的掺杂剂。
24.根据权利要求23所述的方法，其特征在于，所述介电层含有选自由铪氧化物、硅酸铪、铪硅氮氧化物、铪铝氮氧化物、以及HfO2/Al2O3的积层、及其衍生物和它们的组合所组成的群组中的材料。
25.一种用于在工艺腔室内在衬底表面上沉积含硅层的方法，包括：
在第二原子层沉积工艺期间，暴露其上设置有通过包括交替地脉冲铪前驱物和一种氧化气体的步骤的第一原子层沉积工艺所形成的含铪介电层的衬底于硅前驱物和所述氧化气体中从而在其上形成硅氧化物层，所述氧化气体含有通过含氢气体和含氧气体流过水蒸汽产生器所形成的水蒸汽；以及
暴露硅氧化物层于氮化工艺中。
26.根据权利要求25所述的方法，其特征在于，所述含氧气体包含选自由O2、N2O、NO2、N2O5及它们组合所组成的群组中的至少一种气体。
27.根据权利要求26所述的方法，其特征在于，所述含氢气体含有在载送气体中氢气的体积百分比含量为5％或者更少的合成气体。
28.根据权利要求27所述的方法，其特征在于，所述水蒸汽产生器含有催化剂。
29.根据权利要求25所述的方法，其特征在于，所述氮化工艺包含氮等离子体。
30.根据权利要求29所述的方法，其特征在于，在所述氮化工艺之后，所述衬底在600℃到1200℃的温度范围内退火1秒到120秒。
31.根据权利要求29所述的方法，其特征在于，所述硅前驱物选自由(Me2N)4Si、(Me2N)3SiH、(Et2N)4Si、(Et2N)3SiH、(MeEtN)4Si、(MeEtN)3SiH、SiH4、SiCl4、H2SiCl2、Si2H6、Si2Cl6及其衍生物和它们的组合所组成的群组。
32.根据权利要求31所述的方法，其特征在于，在所述含硅层上沉积多晶硅层。
33.根据权利要求32所述的方法，其特征在于，所述多晶硅层含有选自由硼、磷、砷和它们的组合所组成的群组中的掺杂剂。
34.根据权利要求31所述的方法，其特征在于，所述硅氧化物层厚度约为或者更少。
35.根据权利要求34所述的方法，其特征在于，所述介电层含有选自由铪氧化物、硅酸铪、铪硅氮氧化物、铪铝氮氧化物、以及HfO2/Al2O3的积层、及其衍生物和它们的组合所组成的群组中的材料。
36.一种用于在工艺腔室内在衬底上沉积含硅材料的方法，包括：
在第一原子层沉积工艺期间在衬底上沉积金属硅酸盐材料，包括：
暴露所述衬底于金属前驱物；
暴露所述衬底于氧化气体中，其中所述氧化气体含有通过氢源气体和氧源气体流过水蒸汽产生器所形成的水蒸汽；
暴露所述衬底于硅前驱物中；以及
暴露所述衬底于所述氧化气体中；以及
在第二原子层沉积工艺期间在所述金属硅酸盐材料上沉积硅氧化物层，包括：
暴露所述衬底于所述硅前驱物；以及
暴露所述衬底于所述氧化气体中。
37.根据权利要求36所述的方法，其特征在于，所述氧源气体含有选自由O2、N2O、NO2、N2O5及它们组合所组成的群组中的至少一种气体。
38.根据权利要求37所述的方法，其特征在于，所述氢源气体含有在载送气体中氢气的体积百分比含量为5％或者更少的合成气体。
39.根据权利要求37所述的方法，其特征在于，所述水蒸汽产生器包含催化剂。
40.根据权利要求36所述的方法，其特征在于，暴露所述硅氧化物层于氮化工艺中以在其上形成硅的氮氧化物层。
41.根据权利要求40所述的方法，其特征在于，在氮化工艺之后所述衬底在从600℃到1200℃的温度范围退火1秒到120秒。
42.根据权利要求41所述的方法，其特征在于，所述硅前驱物选自由(Me2N)4Si、(Me2N)3SiH、(Et2N)4Si、(Et2N)3SiH、(MeEtN)4Si、(MeEtN)3SiH、SiH4、SiCl4、H2SiCl2、Si2H6、Si2Cl6及其衍生物和其组合所组成的群组。
43.根据权利要求42所述的方法，其特征在于，在所述硅的氮氧化物层上沉积多晶硅层。
44.根据权利要求43所述的方法，其特征在于，所述多晶硅层含有选自由硼、磷、砷和其组合所组成的群组中的掺杂剂。
45.根据权利要求40所述的方法，其特征在于，所述硅的氮氧化层厚度为
Figure FA20186248200580006138101C00051
或者更少。
46.根据权利要求45所述的方法，其特征在于，所述金属硅酸盐材料含有铪并且所述金属前驱物为铪前驱物。
47.根据权利要求46所述的方法，其特征在于，所述金属硅酸盐材料还含有选自由铝、氮、镧及其组合所组成的群组中的元素。
48.一种在工艺腔室中用于在衬底上沉积含硅材料的方法，包括：
在第一原子层沉积工艺循环期间在衬底上沉积金属硅酸盐材料，该第一原子层沉积工艺循环包括顺序导入金属前驱物脉冲、第一氧化气体脉冲、硅前驱物脉冲和第二氧化气体脉冲，其中所述氧化气体含有通过氢源气体和氧源气体流过水蒸汽产生器所形成的水蒸汽；
通过停止所述金属前驱物脉冲和第一氧化气体脉冲改变所述第一原子层沉积工艺循环以形成第二原子层沉积工艺循环；以及
在所述第二原子层沉积工艺循环期间在所述金属硅酸盐材料上沉积硅氧化物层，所述第二原子层沉积工艺循环包括顺序导入所述硅前驱物脉冲和所述第二氧化气体脉冲。
49.根据权利要求48所述的方法，其特征在于，所述氧源气体含有选自由O2、N2O、NO2、N2O5及其组合所组成的群组中的至少一种气体。
50.根据权利要求49所述的方法，其特征在于，所述氢源气体含有在载送气体中氢气的体积百分比含量为5％或者更少的合成气体。
51.根据权利要求49所述的方法，其特征在于，所述水蒸汽产生器包含催化剂。
52.根据权利要求48所述的方法，其特征在于，暴露所述硅氧化物层于氮化工艺中以在其上形成硅的氮氧化物层。
53.根据权利要求52所述的方法，其特征在于，在所述氮化工艺之后，所述衬底在600℃到1200℃的温度范围内退火1秒到120秒。
54.根据权利要求53所述的方法，其特征在于，所述硅前驱物选自由(Me2N)4Si、(Me2N)3SiH、(Et2N)4Si、(Et2N)3SiH、(MeEtN)4Si、(MeEtN)3SiH、SiH4、SiCl4、H2SiCl2、Si2H6、Si2Cl6及其衍生物和其组合所组成的群组。
55.根据权利要求54所述的方法，其特征在于，在所述硅的氮氧化物层上沉积多晶硅层。
56.根据权利要求55所述的方法，其特征在于，所述多晶硅层含有选自由硼、磷、砷和其组合所组成的群组中的掺杂剂。
57.根据权利要求52所述的方法，其特征在于，所述硅的氮氧化物层厚度为
Figure FA20186248200580006138101C00061
或者更少。
58.根据权利要求57所述的方法，其特征在于，所述金属硅酸盐材料含有铪并且所述金属前驱物为铪前驱物。
59.根据权利要求58所述的方法，其特征在于，所述金属硅酸盐材料进一步含有选自由铝、氮、镧及其组合所组成的群组中的元素。
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