CN106165069B - 在铝等离子体装备部件上生成紧密的氧化铝钝化层 - Google Patents

在铝等离子体装备部件上生成紧密的氧化铝钝化层 Download PDF

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CN106165069B
CN106165069B CN201580016760.4A CN201580016760A CN106165069B CN 106165069 B CN106165069 B CN 106165069B CN 201580016760 A CN201580016760 A CN 201580016760A CN 106165069 B CN106165069 B CN 106165069B
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aluminum
hno
minute
plasma
drying
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CN106165069A (zh
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S·J·金
L·卡琳塔
Y·帕里克
A·卡达姆
P·S·古拉迪雅
B·塔库尔
D·卢博米尔斯基
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Applied Materials Inc
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Abstract

用于在铝部件上生成紧密的氧化铝钝化层的工艺包括以下步骤：在去离子水中冲洗部件达至少1分钟；干燥此部件达至少1分钟；以及在低于10℃的温度下，将此部件暴露于浓硝酸达1至30分钟。所述工艺也包括以下步骤：在去离子水中冲洗部件达至少1分钟；干燥此部件达至少1分钟；以及将此部件暴露于NH4OH达1秒至1分钟。所述工艺进一步包括以下步骤：在去离子水中冲洗部件达至少1分钟；以及干燥此部件达至少1分钟。用于等离子体处理系统的部件包括铝部件，所述铝部件涂覆有AlxOy膜，所述AlxOy膜具有4纳米至8纳米的厚度，并且所述AlxOy膜的表面粗糙度比不具有所述AlxOy薄膜的部件的表面粗糙度增加少于0.05微米。

Description

在铝等离子体装备部件上生成紧密的氧化铝钝化层
相关申请案的交叉引用
本申请案要求于2014年9月15日提交的美国非临时专利申请案案号14/486,105的优先权，此美国非临时专利申请案案号14/486,105则要求于2014年3月31日提交的美国临时专利申请案案号61/973,077的优先权权益。上述两申请案的完整内容通过引用结合在本文中用于所有目的。
技术领域
本公开属于半导体工艺工程领域。更特别地，公开了在铝等离子体装备部件上生成紧密的氧化铝钝化层以快速地稳定使用此等离子体装备部件的等离子体处理装备内的蚀刻速率的实施例。
背景技术
半导体处理经常利用等离子体处理来蚀刻或清洁半导体晶片。通过稳定且良好地受控的等离子体处理参数可促进可预测且可再现的晶片处理。对等离子体处理中所涉及的装备和/或材料的某些改变会临时地破坏等离子体处理的稳定性。例如，以下各项会破坏工艺稳定性：将在等离子体蚀刻环境中不稳定的材料引入等离子体腔室；在等离子体腔室中执行的多个等离子体工艺之间进行切换；使腔室暴露于与常见情况不同的气体或等离子体；和/或替换作为等离子体腔室的部件或在等离子体腔室中的部件。在此类情况下，最初，工艺会显著地改变，但会随着时间而稳定(例如，随着被引入的材料从工艺腔室中被逐渐清除，或随着工艺腔室内的表面涂层与等离子体工艺条件达成平衡。
发明内容
在实施例中，用于在铝部件上生成氧化铝钝化层的工艺包括以下步骤：在低于10℃的温度下，将铝部件暴露于具有至少30％浓度的硝酸(HNO3)达1分钟与30分钟之间的时间。
在实施例中，用于等离子体处理系统中的部件包括涂覆有AlxOy膜的铝部件，所述AlxOy膜具有4纳米至8纳米的厚度，并且所述AlxOy膜的表面粗糙度比不具有所述AlxOy膜的铝部件的表面粗糙度增加少于0.05微米。
在实施例中，用于在铝部件上生成紧密的氧化铝钝化层的工艺包括以下步骤：在去离子水中冲洗铝部件达至少1分钟；干燥此铝部件达至少1分钟；以及在低于10℃的温度下，将此铝部件暴露于浓度为至少30％的硝酸(HNO3)达1分钟与30分钟之间的时间。所述工艺也包括以下步骤：在去离子水中冲洗铝部件达至少一分钟；干燥此铝部件达至少1分钟；以及将此铝部件暴露于氢氧化铵(NH4OH)达1秒与1分钟之间的时间。所述工艺进一步包括以下步骤：在去离子水中冲洗铝部件达至少1分钟；以及干燥此铝部件达至少1分钟。
附加实施例和特征部分地在以下描述中陈述，并且部分地将在审查了本说明书后对本领域技术人员而言是显而易见的或可通过实践本发明来学习。可通过说明书中所描述的手段、组合和方法来实现并获得本发明的特征和优点。
附图说明
通过结合以下简要描述的附图来参照以下具体实施方式，可理解本公开，其中贯穿若干附图，使用同样的参考标号来指示类似的部件。应注意的是，为了使说明清楚，附图中的某些元件可能不是按比例绘制的。为了使说明清楚，在示出物件的多个实例的情况下，可能仅标示这些实例中的仅一些实例。
图1示意性地阐释根据实施例的等离子体处理系统的主要元件。
图2描述用于在铝等离子体装备部件上产生紧密的氧化铝钝化层的示例性工艺。
图3A和图3B是在类似倍率下的扫描电子显微镜(SEM)照片，两图分别显示在实施例中、在类似的工艺条件下、利用稀硝酸(HNO3)和浓硝酸(HNO3)来处理的Al表面。
图4A和图4B为在类似的倍率下的透射电子显微镜(TEM)照片，两图分别显示在实施例中、以先前已知的最佳方法清洁的铝表面的剖面切片，所述先前已知的最佳方法包括以稀HNO3以及在室温下以浓HNO3进行的处理。
图5A和图5B各自显示在实施例中、对于不同的温度和时间、以高浓(69％)的HNO3处理的铝表面的一系列SEM照片。
图6A至图6H示出完全相同的倍率下的SEM照片，各照片显示在多个实施例中、在室温(RT)或低温下、对于短时间或长时间、以浓HNO3或高浓HNO3处理的铝表面。
图7是示出在实施例中使用激光显微法测量的经处理和未处理的铝样本的表面粗糙度的结果的柱状图。
图8A和图8B是分别示出实施例中的以稀HNO3和浓HNO3处理的等离子体部件的工艺稳定性的结果的图表。
具体实施方式
图1示意性阐释根据实施例的等离子体处理系统100的主要元件。系统100被描绘为单晶片或半导体晶片等离子体处理系统，但是对本领域技术人员而言将显而易见的是，本文所述的技术和原理适用于任何类型的工件(例如，不一定是晶片或半导体的物件)的处理系统。处理系统100包括壳体110，所述壳体110可用于晶片接口115、用户接口120、工艺腔室130、控制器140以及一个或多个电源150。工艺腔室130包括一个或多个晶片台座135，晶片接口115可将工件50(例如，半导体晶片，但可以是其他类型的工件)置于所述晶片台座135上以进行处理。(多种)气体155可通过气室139和扩散板137而被引入工艺腔室130中，并且射频生成器(RF Gen)165供应功率以在工艺腔室130中点燃等离子体。晶片台座135的表面、工艺腔室130的壁和底面以及扩散板137都是可能显著地影响系统100的处理特性的表面。特别地，扩散板137可形成许多穿过此扩散板137的许多小孔，以便在工艺腔室130中均匀地分布气体和/或等离子体，并且这些孔的壁的表面化学效应可能是显著的。
以示例方式列出示出为系统100的部分的元件，并且这些元件不是详尽的。还可以包括许多其他可能的元件，但是为了使说明清楚没有示出它们，所述其他可能的元件诸如：压力和/或流量控制器；气体或等离子体歧管或分配装置；离子抑制板；电极、磁芯和/或其他电磁装置；机械、压力、温度、化学、光学和/或电子传感器；晶片或其他工件搬运机制；观察和/或其他存取端口(access port)等。为使说明清楚，也没有示出系统100内元件的内部连接和协同作用。除了RF生成器165和气体155之外，其他代表性设施(诸如，真空泵160和/或通用电功率170也可与系统100连接。如同系统100内所示的元件，显示为与系统100连接的设施使说明性的而非详尽的，其他类型的设施也可与系统100连接，但是为了使说明清楚而未示出，其他类型的设施诸如，加热或冷却流体、压缩空气、网络能力、废料处理系统等。类似地，虽然上述描述提及在工艺腔室130中点燃等离子体，但是下文讨论的原理可同等地适用于所谓“下游(downstream)”或“远程(remote)”等离子体系统，所述“下游”或“远程”等离子体系统在第一位置处产生等离子体，并且使等离子体和/或等离子体反应产物移动至第二位置以进行处理。
某些等离子体工艺对等离子体腔室中的表面条件是敏感的。在半导体工艺的状况下，对工艺稳定性和均匀度的需求随器件的几何形状缩减和晶片尺寸增加而加剧。新装备(或已替换任何腔室部件的设备)可能需要显著的停机时间以通过模拟处理来调整腔室，直到实现可接受的工艺稳定性，所述模拟工艺就是在不暴露实际工件的情况下执行典型的等离子体工艺。
对腔室表面调节非常敏感的一个等离子体工艺是以由三氟化氮(NF3)和氧化氮(N2O)气体形成的等离子体蚀刻薄氮化硅(Si3N4)层。等离子体腔室部件(诸如，图1的晶片台座135、腔室130的壁和底面以及扩散板137)可由铝制成，并且可涂覆有氧化铝薄层(一般以AlxOy表示，通常大约是Al2O3，但氧化铝化学计量上的变体被构想为并认为在本公开的范围内)。新的铝部件可被清洁，并且经受稀硝酸(HNO3)混合物处理以生成氧化铝层，这可以采取以下形式：将铝部件放置为接触浸泡在HNO3中的垫片。当HNO3用于任何类型的处理时，经常以其稀释的形式来利用，因为认为稀释形式处置起来更安全。
在本文的实施例中，可使用浓HNO3而非稀HNO3以在等离子体腔室部件上生成氧化铝层。本文中使用“高浓(highly concentrated)”HNO3代表具有60重量％至100重量％的浓度的HNO3，而本文使用“浓(concentrated)”HNO3(包含高浓HNO3)代表具有30重量％至100重量％的浓度的HNO3。虽然处置浓HNO3时须小心谨慎，但是本文中的实施例利用浓HNO3以在铝部件上提供相比由稀HNO3所提供的更致密且较少孔的AlxOy层，从而使在氮化物等离子体蚀刻环境中所需的调节时间最小化。人们也相信，将铝部件浸泡在浓HNO3而非使浸泡过HNO3的垫片接触此部件是有利的，这体现这样做在暴露的Al表面(包括在裂缝、孔洞等处的Al表面)上产生紧密、平滑且均匀的AlxOy层。也已发现浓HNO3比其他酸和/或氧化剂能提供更紧密且更平滑的氧化铝层，所述其他酸和/或氧化剂诸如，H2O2、HCl、HF、HNO3+HF、H2SO4、HCl+HNO3和NH4OH。
人们进一步相信，在低温下执行HNO3处理达相对短的时间量限制HNO3的离解(例如，4HNO3＝>2H2O+4NO2+O2)，从而进一步通过抑制H2O对原始铝表面的攻击来促进紧密(也即，致密的)且无孔的AlxOy层。当在合理的工艺时间内可实现的AlxOy层的厚度不改变太多(5至6纳米的AlxOy层)时，以浓HNO3处理的铝表面保持大致与其初始状条件一样平滑，而不是如以稀HNO3处理而观察到的较粗糙的铝表面。人们相信，使表面粗糙度最小化是铝部件所暴露的等离子体工艺的快速稳定的关键，因为表面粗糙化在AlxOy层中呈现出变异，所述变异与等离子体工艺相互作用直到变异被消除为止。例如，在表面凸起处或凹陷处的AlxOy中的初始局部薄点和/或空隙可能与等离子体相互作用，直至的AlxOy层达到至少数纳米厚度为止。人们相信，本文的实施例能够产生先前未在在铝部件上出现的表面光洁度(surface finish)，即，产生紧密的AlxOy膜，所述紧密AlxOy膜的净表面粗糙度比此膜所存在于的铝部件增加少于0.05微米。现在公开利用浓HNO3以生成紧密的AlxOy层的实施例、处理结果以及通过此工艺所生成的经钝化部件的示例以及经钝化部件的快速工艺稳定效果。
以浓HNO3进行处理以形成紧密的AlxOy层
图2描述用于在铝等离子体装备部件上产生紧密的氧化铝钝化层的示例性工艺200。工艺200可用于例如新的或已被处理而去除了先前涂层的铝部件。如下文进一步所述，工艺200的某些部分能以与示例性工艺200中显示的那些部分不同的方式来执行。
工艺200开始于以去离子(DI)水冲刷(flush)铝部件达5分钟(210)，随后，在干净的干燥空气(clean dry air，CDA)中干燥铝部件达5分钟(215)。当步骤210和215进行时，在任选的步骤220中，可将浓HNO3或高度浓HNO3浴冷却至低温(例如，低于10℃)。在一些实施例中，所述浴有利地为至少60％的HNO3，以将H2O对形成的AlxOy层的效应最小化。在某些实施例中，所述浴有利地冷却至低于5℃，以使AlxOy层的表面粗糙度最小化，然而在其他实施例中，HNO3浴也可处于室温下，以使对于冷却HNO3浴的装备和功率要求最小化。铝部件接着接受HNO3处理达1至30分钟(225)(有利地，约1至15分钟)，接着由另一DI水冲刷达1至30分钟(230)(有利地，约5分钟)，并且进行1至30分钟(有利地，约5分钟)的CDA干燥(235)。HNO3处理可生长约4至8纳米(典型地，约5至6纳米)的AlxOy，同时不会使铝部件的表面粗糙度比其原始粗糙度增加超过0.05微米。随后，铝部件被暴露于氢氧化铵(NH4OH)达1秒至1分钟(240)(有利地，约1至5秒)以中和任何剩余的HNO3。在暴露于NH4OH之后是最终的DI水冲刷达1至30分(245)(有利地，约5分钟)以及1至30分钟(有利地，约5分钟)的CDA干燥(250)。
工艺200的多种替代和重组对本领域技术人员是显而易见的，并且所有此类替代和重组均视为落入本公开的范围内。此类替代和重组的一些示例为：省略最初的去离子(DI)水冲刷和CDA干燥步骤210与215；以氮气(N2)或其他相对惰性的气体而不是CDA来执行CDA干燥步骤215、235、250中的任一步骤；利用经加热的CDA(或其他相对惰性的气体)来促进干燥；省略CDA干燥步骤215和/或235，转而从之前的DI水冲刷直接到之后的化学步骤225或240；和/或缩短或加长DI水冲刷或CDA干燥步骤。
以浓HNO3处理而生成的紧密的AlxOy层的示例
现在示出以不同的稀释度、温和时间的HNO3处理的铝等离子体装备部件和/或铝试片的示例。
图3A和图3B是在完全相同的倍率下的扫描电子显微镜(SEM)照片，两图分别显示在类似的工艺条件下、以稀HNO3和浓HNO3处理的Al表面。图3A显示出以稀HNO3处理的Al表面比以浓HNO3处理的Al表面(图3B)显著地更粗糙。
图4A和图4B是在类似倍率下的以先前已知的最佳方法清洁的Al表面的剖面切片的透射电子显微镜(TEM)照片，所述先前已知的最佳方法包括以稀HNO3(图4A)以及在室温下以浓HNO3(图4B)进行的处理。如图4A和图4B中所示，相应的层40A和40B是下方的铝，层42A和42B为通过相应的HNO3处理而形成的AlxOy。进一步的层44A和44B为铱(iridium)，并且46A和46B是用于TEM样本制备的碳层。在42A和42B中的每一者中在恰好大于5纳米厚度处测量AlxOy层。
图5A和图5B各自显示在1万倍(10,000X)的倍率下原始摄取的一系列SEM照片，所述照片分别显示对于不同温度和不同时间以高浓(69％)的HNO3处理的Al表面。图5A显示以从约5℃至约60℃的范围内的温度处理的Al表面的SEM照片，由图中可从视觉上评估，随着增加的温度，具有更不紧密/更粗糙的AlxOy层。SEM照片根据视觉评估(visual evaluation)并根据HNO3处理温度来排列，但是沿温度和紧密度的方向的定位不是按比例的。图5B显示处理达5分钟至400分钟的范围内的时间的Al表面的SEM照片，由图中可从视觉上评估，随着增加的温度，具有更不紧密/更粗糙的AlxOy层。SEM照片根据对紧密度的视觉评估并根据HNO3处理时间来排列；再次地，沿时间和紧密度的方向的定位不是按比例的。
图6A至图6H显示完全相同的倍率下的SEM照片，各图显示在室温或低温(例如，低于10℃)、对于短时间(例如，5至25分钟)或长时间(例如，90至150分钟)，以浓HNO3或高浓HNO3处理的Al表面。在图6A至图6H中显示的表面形貌中，经长时间处理的样本比在相同条件下经短时间处理的那些样本显著地更粗糙，在室温下处理的样本比相同条件下在低温下处理的那些样本更粗糙，并且以浓HNO3处理的样本比在相同条件下以高浓HNO3处理的那些样本更粗糙。
图7是示出使用激光显微法测量的经处理的和未处理的Al样本的表面粗糙度结果的柱状图。所有经处理的样本都是在低温(例如，低于10℃)下以HNO3来处理的。以高浓HNO3处理的Al样本的表面粗糙度非常接近未处理的Al的表面粗糙度，而以浓HNO3和稀HNO3处理的Al样本的表面粗糙度逐步地更高。以浓HNO3和高浓HNO3处理的Al样本的表面粗糙度比未处理的样本的表面粗糙度增加少于0.05微米。人们相信，先前未曾制造出约5纳米的、且表面粗糙度比未处理的部件的表面粗糙度增加少于0.05微米的AlxOy层的铝部件。
图8A和图8B是分别示出以稀HNO3和浓HNO3处理的等离子体部件的工艺稳定度结果的图表。对于图8A，根据先前工艺处理的Al部件被安装在双腔室等离子体处理系统的两个工艺腔室(两“侧(side)”)内。接着，通过工艺循环来使腔室循环在所述工艺循环中，运行典型的等离子体处理配方(recipe)。按时间间隔(interval)测量在标准工艺条件下被蚀刻的氮化硅的量，从而获得图8A中所示的数据。被蚀刻的量显著地改变，直到约3000次工艺循环为止，接着稳定在目标蚀刻量附近，但是一个腔室继续比另一腔室蚀刻得略微更多。对于图8B，根据图3的工艺200处理的Al部件被安装在双腔室等离子体处理系统的两个工艺腔室内。接着，通过与针对图8A中所示的数据相同的工艺循环来使腔室循环。按时间间隔测量在相同的标准工艺条件下被蚀刻的氮化硅的量，从而获得图8B中所示的数据。可以看到，在仅约25次工艺循环之后，被蚀刻的量就在目标蚀刻量附近相对一致，并且具有更好的侧对侧匹配(side-to-side matching)。
已描述了若干实施例，本领域技术人员将认识到，可使用各种修改、替代构造和等效方案而不背离本发明的精神。此外，未描述多个公知的工艺核元件，以避免不必要地混淆本发明。据此，以上描述不应视为对本发明的范围的限制。
在提供了数值范围的情况下，应理解，除非上下文另外清楚地指明，否则也专门公开了在那个范围的上下限值之间的至下限值单位的十分之一的每一个中间值。也涵盖了所陈述的值或所陈述的范围中的中间值与那个所陈述的范围中任何其他陈述值或中间值之间的每一个较小范围。所述较小范围的上限值与下限值可被独立地包含在范围中或被排除在范围外，并且其中限值中的任一个、零个或两个限值被包括在较小范围中的每一个范围都被涵盖在本发明内，受制于在所陈述范围中任何被专门排除的限值。在所陈述的范围包括限值中的一者或两者的情况下，排除那些被包括的限值中的任一个或两个的范围也被包括。
如本文何所附权利要求书中所使用，除非上下文另外明确地指定，否则单数形式“一(a,an)”和“所述(the)”包括复数指示物。因此，例如，提及“一工艺”包括多个此类工艺，并且提及“所述电极”包括提及一个或多个电极以及为本领域技术人员所知的电极等效物，以此类推。此外，当在说明书和所附权利要求书中使用时，词“包含(comprise,comprising)”与“包括(include,including)”等旨在指定所陈述的特征、整数、部件或步骤，但这些词不排除存在或添加一个或多个其他特征、整数、部件、步骤、动作或组。

Claims (4)

1.一种用于在等离子体处理系统中使用的铝部件上生成紧密的氧化铝钝化层的工艺，所述工艺包含以下步骤：
在去离子水中冲洗所述铝部件达至少1分钟；
干燥所述铝部件达至少1分钟；
在5℃或更低的温度下，将所述铝部件暴露于具有至少30％的浓度的硝酸(HNO3)达1分钟与30分钟之间的时间；
在去离子水中冲洗所述铝部件达至少1分钟；
干燥所述铝部件达至少1分钟；
将所述铝部件暴露于NH4OH达1秒与1分钟之间的时间；
在去离子水中冲洗所述铝部件达至少1分钟；以及
干燥所述铝部件达至少1分钟。
2.如权利要求1所述的工艺，其中所述HNO3具有至少60％的浓度。
3.如权利要求1所述的工艺，其中所述暴露步骤包含以下步骤：将所述铝部件浸泡在所述HNO3中达1分钟与15分钟之间的时间。
4.如权利要求1所述的工艺，其中将所述铝部件暴露于NH4OH的步骤包含以下步骤：将所述铝部件浸置在NH4OH中达1秒与10秒之间的时间。
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