CN102089861B - 低k电介质材料的汽相修复和孔密封 - Google Patents

低k电介质材料的汽相修复和孔密封 Download PDF

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CN102089861B
CN102089861B CN2008801230605A CN200880123060A CN102089861B CN 102089861 B CN102089861 B CN 102089861B CN 2008801230605 A CN2008801230605 A CN 2008801230605A CN 200880123060 A CN200880123060 A CN 200880123060A CN 102089861 B CN102089861 B CN 102089861B
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詹姆斯·德扬
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Abstract

提供一种处理半导体基片上形成的纳米孔隙低k电介质材料的方法。该低k电介质材料具有蚀刻出的开口，其在该蚀刻出的开口的外部表面和互连孔的内部表面上具有包含硅烷醇基团的蚀刻受损区域。首先，该低k电介质材料与汽相催化剂以可有效在该催化剂和该蚀刻受损区域中的硅烷醇基团之间形成氢键的量相接触，而形成催化中间体。其次，该低k电介质材料与汽相烷氧硅烷修复剂以可有效与大约50％或更多的该蚀刻受损区域中的硅烷醇基团反应的量相接触，从而该烷氧硅烷修复剂与该催化中间体反应；以及/或该低k电介质材料与汽相烷氧硅烷密封剂以可有效防止上覆阻挡层扩散进入该互连孔的量相接触，从而该烷氧硅烷密封剂与该催化中间体反应。

Description

低K电介质材料的汽相修复和孔密封
背景技术
随着集成电路器件尺寸持续减小，多个晶体管之间信号传播的延时(即，传播延迟)已经变成决定器件性能中越来越重要的参数。传播延迟与金属连线的电阻(R)与该层间介电绝缘材料的电容(C)乘积成比例，(也称作RC延迟)。因此，为了最小化传播延迟，将包含低介电常数材料的绝缘材料与高导电率金属组合(或电阻率金属)组合是有益的。低k电介质(LKD)材料(k＜3.0)，如有机硅酸盐玻璃(OSG)、有机硅酸盐玻璃(OSG)、四乙氧硅烷(TEOS)、氟硅玻璃(FSG)和碳掺杂氧化物，也正受到重视以作为氧化硅(k＝3.8-4.0)的替代物。为了获得较低的介电值，该LKD材料可包含互连的纳米孔隙结构，其吸附空气(k＝1)以降低大块LKD总的k值。类似地，铜(Cu)因为其较低的电阻率值(R＜2μΩ-cm)而受到相当大的重视以作为互连线金属，作为更加常见的铝(Al)互连金属(R＝3.0-5.0μΩ-cm)的替代物。
因为铜不容易形成挥发性副产物，所以传统或习知的蚀刻技术是不适当的。因此，镶嵌制造工艺对于形成图案化的铜互连线是必要的，需要涉及先前图案化的开口(例如，沟槽或过孔)中沉积导电材料的工艺。因此，镶嵌处理使得蚀刻该LKD材料中先前图案化的开口成为必要。其这样进行：将电介质层上掩模层(如光刻胶)中的开口图案化为沟槽或过孔的形状，然后湿法或干法蚀刻。然而，LKD材料的蚀刻、灰化或清洁都有可能损伤该LKD材料。
发明内容
提供一种处理半导体基片上形成的纳米孔隙低k电介质材料的方法。该低k电介质材料具有蚀刻的开口，其在该蚀刻出的开口的外部表面和互连孔的内部表面上具有包含硅烷醇基团的蚀刻受损区域。首先，将该低k电介质材料与汽相催化剂以可有效在该催化剂和该蚀刻受损区域中该硅烷醇基团之间形成氢键的量相接触，而形成催化中间体。其次，该低k电介质材料与汽相烷氧硅烷修复剂以可有效与该蚀刻受损区域中大约50％或更多的硅烷醇基团反应的量相接触，从而该烷氧硅烷修复剂与该催化中间体反应；以及/或该低k电介质材料与汽相烷氧硅烷密封剂以可有效防止上覆阻挡层扩散进入该互连孔的量相接触，从而该烷氧硅烷密封剂与该催化中间体反应。
在另一实施例中，提供一种处理半导体基片上形成的纳米孔隙低k电介质材料的方法。该低k电介质材料具有蚀刻出的开口，其在该蚀刻出的开口的外部表面上和互连孔的内部表面上具有包含硅烷醇基团的蚀刻受损区域。首先，该低k电介质材料与汽相有机酸催化剂以可有效在该催化剂和该蚀刻受损区域中的硅烷醇基团之间形成氢键的量相接触，而形成催化中间体。其次，该低k电介质材料与汽相烷氧硅烷修复剂以可有效与大约50％或更多的该蚀刻受损区域中的硅烷醇基团反应的量相接触，从而该烷氧硅烷修复剂与该催化中间体反应；以及/或该低k电介质材料与汽相烷氧硅烷密封剂以可有效防止上覆阻挡层扩散进入该互连孔的量相接触，从而该烷氧硅烷密封剂与该催化中间体反应。
附图说明
图1说明镶嵌制造工艺的示范实施例。
图2说明硅烷水解沉积物。
图3说明在存在Lewis碱胺的情况下，表面约束Si-OH基团和n-丙基三甲氧基硅烷(n-PTMS)之间形成硅烷化合物的反应。
图3B说明烷氧基至Si-OH基团的转换。
图3C说明邻近硅烷化合物之间水平网状物的形成。
图4A-4D说明在存在有机酸的情况下，邻近硅烷化合物之间的水平网状物的形成。
图5说明修复和/或密封带有纳米孔隙LKD材料半导体基片的工艺室和化学制剂蒸汽输送系统。
图5B说明用于液体制剂的蒸发和输送的化学制剂蒸汽输送系统。
图6A-6C是表征汽相修复的样品、超临界CO2修复的样品以及没有修复的样品的蚀刻沟槽侧壁的修复程度的扫描电子显微镜(SEM)图像。
图7说明汽相修复的样品、超临界CO2修复的样品、没有修复的样品和沉积(as-deposited)的样品的次级离子质谱(SIMS)分析得到的碳和硅的比与深度的函数。
具体实施方式
图1是镶嵌制造工艺的示范实施例。图1A说明带有上覆的纳米孔隙LKD材料层110的半导体基片100。使用掩模层120，在纳米孔隙LKD材料110中形成开口130。为了说明目的，仅示出一个开口130，其可以是许多过孔或沟槽之一。例如，掩模层120可以是有机光刻胶，开口130可以通过等离子蚀刻形成。一经完成等离子蚀刻，掩模层120可以通过灰化去除(即，在氧基等离子中干蚀刻)。
图1B中，阻挡层140可以形成在该开口130的侧壁和底面上方以保护邻近该铜连线的该纳米孔隙LKD材料110不会受到扩散进邻近的电介质材料的铜原子侵害。示范性的阻挡材料包括钛(Ti)、氮化钛(TiN)、钽(Ta)、氮化钽(TaN)、钌(Ru)、氧化钌(RuOx)及其合金。例如，该阻挡材料可以通过物理气相沉积(PVD)，原子层沉积(ALD)等涂覆。
图1C中，开口130填充大块的铜层150。例如，大块的铜层150可以这样形成：沉积种子层，接着无电镀铜。如图1D中所示，该结构可通过任何合适的技术平坦化以去除大块的铜层150的多余部分，如通过化学机械平坦化(CMP)。
该镶嵌制造工艺可以是单或双镶嵌工艺的任一个。对于后一工艺，可使用先过孔方法或先沟槽方法的任一个。
在成功的将纳米孔隙LKD材料植入镶嵌结构之前，必须克服多个障碍。首先，通过蚀刻形成开口130(例如，过孔或沟槽)以及通过灰化去除掩模层120的工艺可能会损伤该纳米孔隙LKD材料。其次，该阻挡材料140(例如，Ti，TiN，Ta，TaN，Ru或RuOx)可能会渗透进入纳米孔隙LKD材料110的互连孔，影响低介电值。第三，由于在许多纳米孔隙LKD材料中存在互连孔，纳米孔隙LKD材料形成的结构缺少随后的处理步骤(例如，CMP)所需的机械强度。因此，需要修复受损的纳米孔隙LKD材料，密封该开口130的表面，以及增强该LKD材料的机械强度。
等离子蚀刻和灰化过程中，可以去除至少一部分含碳基团(即，甲基或-CH3基团)，导致纳米孔隙LKD材料疏水性降低。当该含碳基团从该纳米孔隙LKD材料去除，Si-C键被Si-OH(“硅烷醇”)键或基团替代，所得到的电介质层失去了其疏水性，因为来自空气或随后的湿法清洁步骤的水分子与该硅烷醇基团形成很强的氢键作用。水(其k值大约70)的存在导致该纳米孔隙LKD材料的k值显著增加。例如，该纳米孔隙LKD材料中开口(例如，过孔或沟槽)的等离子蚀刻期间，等离子损伤可能延伸到该开口的侧壁中大约30nm的深度。在该等离子损伤的纳米孔隙LKD材料的大约5nm深度，失去大约25％的甲基(-CH3)(即，25％Si-C键被Si-OH键或基团替代)。
蚀刻损伤的纳米孔隙LKD材料可利用烷氧硅烷制剂处理，其与Si-OH反应。然而，使用烷氧硅烷制剂的一个缺陷是在缩合步骤中与该表面约束Si-OH基团缩合之前需要水来水解该烷氧基。因此，与化合物(如烷氧硅烷制剂)的使用相关的挑战之一是修复的一致性。这涉及在烷氧硅烷和Si-OH基团之间的化学反应中水所扮演的关键角色。如图2中所示，需要水在与Si-OH基团缩合之前在水解步骤中水解该烷氧基。
空气湿度导致的表面上不同的氢键合水程度直接影响反应效率。在不使用催化剂的情况下，该烷氧基硅烷和该Si-OH基团之间的化学反应要求存在一些水。进而，如果需要一致的结果，则样品和样品之间必须保持基本上相同程度的水合作用。
Lewis碱胺(例如，氨，甲胺，双甲胺或三甲胺)可以用作催化剂以在没有水解步骤的情况下增强烷氧基硅烷和Si-OH基团之间的缩合速率。如图3中所示，该Lewis碱胺通过与该Si-OH基团形成催化中间体而用作催化剂。形成该催化中间体是因为在该Lewis碱胺和该Si-OH基团之间形成氢键。这个氢键的形成驱使该反应向前进行，允许Si-OH基团与该烷氧硅烷制剂的烷氧基直接反应。该催化中间体本身极容易受到与该烷氧硅烷制剂反应的影响。该反应产生对应的醇作为副产物，释放该胺以再次与额外的Si-OH基团氢键合。另外，该烷氧硅烷化合物可以横向网化以形成三维横向网化的结构，恢复该纳米孔隙LKD材料的机械强度。
有机酸也可通过水解烷氧基硅烷以形成Si-OH基团而用作催化剂，其在加热的情况下与表面约束Si-OH基团缩合。另外，如图4中所示，有机酸可以用来催化水与大多数留在该修复的和/或横向网化的纳米孔隙LKD材料上的残余烷氧基基团之间的反应。图4A中，有机酸催化水和该残余烷氧基之间的水解反应，该反应如图4B中所示产生Si-OH基团。图4C，邻近硅烷化合物的Si-OH基团然后缩合以形成水平网状物。该有机酸可以是任何pKa高达大约7的有机酸，更优选地高达大约4，最优选地高达大约3。该有机酸可包括乙酸、三氟乙酸、三氯乙酸、柠檬酸、其他完全卤化或部分卤化的弱酸及其各种组合。
已经证明这种Lewis碱胺和有机酸催化剂动态增强烷氧基硅烷和表面约束Si-OH基团之间的缩合速率，而不需要在超临界CO2(或SCCO2)介质中的初步水解步骤，如在共同转让的美国专利申请No.11/475,206中描述的，通过引用结合其全部内容。
这里描述的是一种新的方法。其使用与蒸汽相Lewis碱胺或有机酸催化剂结合的蒸汽相单、双或三功能烷氧硅烷制剂修复和/或密封蚀刻损伤的纳米孔隙LKD材料。修复剂和密封剂通常可以表示为Si-(R)x(OR′)y，其中y≥1，x+y＝4，R是烷基、芳基或羟基，R是烷基或芳基，优选地是甲基或乙基。
烷氧硅烷修复剂特征在于大约80至大约125原子质量单位(AMU)的更小尺寸的分子，其可通过互联的多孔网状物分散进该大块的该纳米孔隙LKD材料中，并与硅烷醇基团反应。在修复完成之后，50％或更多的失去的甲基通过烷基(例如，乙基、丙基、丁基)补充，优选地补充大约75％至大约90％的甲基。
修复剂的示例可包括甲基三甲氧基硅烷(CH3-Si-(O-CH3)3)，二甲氧基二甲基硅烷((CH3)2-Si-(OCH3)2)，甲氧基三甲基硅烷((CH3)3-Si-OCH3)或n-丙基三甲氧基硅烷(CH3-CH2-CH2-Si-(OCH3)3)或n-PTMS。
烷氧硅烷密封剂特征在于大约200至大约400AMU的较大的分子。该纳米孔隙LKD材料的毛孔密封通过尺寸排阻的原理进行，其中大尺寸的烷氧硅烷密封剂与表面约束Si-OH基团碰撞反应，而不是通过该纳米孔隙LKD材料孔开口进入多孔网状物。烷氧硅烷密封剂在小于大约3至4nm的深度，优选地在大约1至2nm的深度，与表面硅烷醇基团反应。在该密封工艺完成后，该开口的侧壁和底面用厚度高达大约2nm的膜覆盖。这个膜有效防止上覆的阻挡材料分散到该纳米孔隙LKD材料的互连孔中，然而，应当注意蒸汽相化的催化剂由于较小的分子大小可继续分散到该纳米孔隙LKD材料中。
密封剂的示例可包括双(二甲氧基甲基)硅氧烷，二(甲基双甲基硅氧丙基)-N-甲胺，双(三乙氧基硅)乙烷，1，2-双(三甲氧基硅)己烷，双(三甲氧基硅丙基)胺或二(3-三乙氧基)丙基)二硫化物。
如图5A中所示，带有纳米孔隙LKD材料110的半导体基片100设在工艺室200中，用以处理蚀刻和/或光刻胶灰化导致的损伤。工艺室200可以运行在大约1毫托至大约3750托(即，大约5巴)的压强以及高达大约300℃的温度。
纳米孔隙LKD材料110包括之前蚀刻出的开口130(例如，沟槽或过孔)。由于之前蚀刻和/或去除上覆的掩模层，该电介质层110的暴露表面受到蚀刻损伤。尽管在图5A中未示，但是纳米孔隙LKD材料110可覆盖中间层(如阻挡层)和导电或半导电层。
纳米孔隙LKD材料的示例可包括，但不限于，
Figure BPA00001168416300081
和
Figure BPA00001168416300082
(由Honeywell International制造)，掺杂碳的氧化物，如BLACK
Figure BPA00001168416300083
(APPLIED MATERIALS制造)，
Figure BPA00001168416300084
(由NOVELLUS制造)，(由ASM制造)，(由Trikon制造)，LKD-5109(由JSR制造)，和纳米簇硅石或NCS(由FUJITSU制造)。许多纳米孔隙LKD材料的一个特征是存在互连孔结构，其具有平均孔尺寸大约2纳米的较窄的孔尺寸分布。
半导体基片100可以设在基片支撑件210上。基片支撑件210可包括静电卡盘(ESC)、机械卡具或其他卡紧机构，以及一个或多个加热元件，用于将半导体基片100加热至高达300℃的温度。
化学制剂蒸汽输送系统220A、220B、220C可用于顺次分别输送催化剂、烷氧硅烷修复剂和烷氧硅烷密封剂至工艺室200。一旦利用该催化剂、烷氧硅烷修复剂或烷氧硅烷密封剂的处理完成，真空泵240可用于从工艺室200排出气体。通过背压调节器250保持工艺室200中的静态气体压强，其作用是当气体压强超过预先选定的压强时，将该蒸汽释放进化学缓冲系统。
图5B说明用于液体制剂(例如，催化剂、烷氧基硅烷修复剂或烷氧硅烷密封剂)的化学制剂蒸汽输送系统220的实施例。来自制剂源224的液体制剂222可以设在起泡器226中，将该起泡器加热至高温以汽化该液体制剂222。来自气体源228的惰性气体(例如氮气或氩气)将该液体制剂222吹起泡泡，以便通过气体管线230将该蒸汽化的制剂输送至工艺室200。可以加热气体管线230以防止该蒸汽化的制剂在该气体管线230内冷凝。
半导体基片100设为在任何修复和/或密封工艺之前接触蒸汽相催化剂。如上所述，该Lewis碱胺或有机酸催化剂的作用是动态增强烷氧基硅烷和Si-OH基团之间的缩合速率，在Lewis碱胺催化剂的情况下没有初步水解步骤，在该有机酸的情况下则是通过加快水解。工艺室200和基片支撑件210的温度可以加热至大约60℃至大约275℃的第一温度，优选地大约100℃至大约200℃。为了防止蒸汽相制剂的冷凝，该半导体基片100的温度优选地在整个工艺中保持大于该蒸汽相制剂的温度。
最初，该工艺室200的压强保持在真空压强(例如，大约0.5托至大约10托)以促进该催化剂的汽化。化学制剂蒸汽输送系统220A将蒸汽相催化剂输送至该工艺室200以处理半导体基片100。半导体基片100设为与该蒸汽相催化剂以可有效与该蚀刻受损区域中的硅烷醇基团相互作用的量相接触。例如，该蒸汽相催化剂可在该纳米孔隙LKD材料110中的开口130的外部表面(即，侧壁表面)以及该互连孔的内部表面上形成催化剂子单层或单层。在一个实施例中，等离子损伤区域可在该开口130的侧壁中延伸至大约30nm的深度。
在一个实施例中，将该催化剂输送至该工艺室200中以将工艺室200中该蒸汽相催化剂的静态压强增加至大约20托至大约1500托(即，大约2巴)，优选地大约100托至大约760托。工艺室200的容积是大约1.1升。该蒸汽相催化剂的接触时间可以是大约10秒至大约60秒，优选地大约20至大约30秒。在利用该蒸汽相催化剂的处理完成之后，其余的蒸汽相催化剂由惰性气体的流体流或真空泵240任一个从该工艺室200去除，直到压强低于大约5托。在另一实施例中，通过将该蒸汽相催化剂通入处理室而在真空泵240和/或背压调节器250同时运行期间保持动态真空。
示范性的Lewis碱胺可包括氨(NH3)、甲胺(CH3NH2)、双甲胺((CH3)2NH)或三甲胺(N(CH3)3)，或对应的伯、仲或叔-乙基取代胺。示范性的有机酸可包括乙酸、三氟乙酸、三氯乙酸、柠檬酸、其他完全卤化或部分卤化弱酸。在一个实施例中，该有机酸可以与水混合以形成水溶液，其被蒸汽化。取决于该具体的Lewis碱胺或有机酸，该工艺室200和基片支撑件210的温度和静态压强选择为防止该Lewis碱胺催化剂或有机酸冷凝。如果使用有机酸催化剂，为了最大化烷氧硅烷与表面约束Si-OH基团的反应，在引入烷氧硅烷修复和/或密封剂之前，优选地排出过量的汽相有机酸，以防止汽相的有机酸和烷氧硅烷之间的反应。
在利用该蒸汽相催化剂的处理完成之后，该工艺室200的压强降低至真空压强(例如，大约0.5托至大约10托)以促进该烷氧硅烷修复剂的蒸汽化。工艺室200可选地在排空至真空压强之前以惰性气体(例如，氮气或氩气)回填充。工艺室200和基片支撑件210的温度保持在该大约60℃至大约275℃的第一温度，优选地大约100℃至大约200℃。化学制剂蒸汽输送系统220B将该烷氧硅烷修复剂输送至该工艺室200以处理半导体基片100。半导体基片100设为与该烷氧硅烷修复剂以可有效利用烷基(例如，乙基，丙基，丁基)恢复至少50％的损失甲基的量相接触，优选地大约75％至大约90％的损失甲基。
在一个实施例中，输送固定量的烷氧硅烷修复剂从而工艺室200中该修复剂的静态压强是大约20托至大约1500托(即，大约2巴)，优选地大约100托至大约760托。半导体基片100与该第一温度的蒸汽相烷氧硅烷修复剂的总的接触时间可以是大约10秒至大约180秒，优选地大约20秒至大约60秒。在另一实施例中，可以通过将蒸汽相修复剂通入处理室200而在真空泵240和/或背压调节器250的同时运行期间保持动态真空。
为提高该烷氧硅烷修复剂与该硅烷醇基团在该大块的纳米孔隙LKD材料110中的反应性，在与第一温度的烷氧硅烷修复剂的接触完成后，该纳米孔隙LKD材料110优选地设为接触在第二温度的烷氧硅烷修复剂。该晶片支撑件210的温度可以从该第一温度增加到大约80℃至大约300℃的第二温度，优选地大约150℃至大约250℃。半导体基片100与该第二温度的蒸汽相烷氧硅烷修复剂的总接触时间可以是大约10秒至大约180秒，优选地大约20秒至大约60秒。
示范性的烷氧硅烷修复剂可包括甲基三甲氧基硅烷(CH3-Si-(O-CH3)3)、二甲氧基二甲基硅烷((CH3)2-Si-(OCH3)2)、甲氧基三甲基硅烷((CH3)3-Si-OCH3)或n-丙基三甲氧基硅烷(CH3-CH2-CH2-Si-(OCH3)3)或n-PTMS。取决于具体的烷氧硅烷修复剂，该工艺室200和基片支撑件210的温度和静态压强选择为防止该烷氧硅烷修复剂冷凝。该烷氧硅烷修复剂在该LKD材料表面冷凝是有害的，会阻止该烷氧硅烷修复剂均匀地渗入该纳米孔隙LKD材料。为了确保该制剂处于其蒸汽态，该纳米孔隙LKD材料设为接触低于饱和点(即，给定温度的蒸汽压强小于760托)的制剂。在这些情况下，该纳米孔隙LKD材料上不会出现饱和(即，形成液体制剂)。
为了从半导体基片100去除过量的制剂和副产物，将真空室的压强降低至大约0.5托，持续大约30秒至大约180秒。或者，该室中的压强可以保持在静止水平，以及惰性冲刷气体的动态流可用于去除残余的制剂。
如果需要，上述用于将该蒸汽相催化剂和蒸汽相烷氧硅烷修复剂与该纳米孔隙LKD材料接触的工艺步骤可以在第二温度的同一半导体基片100上重复一次或多次以增加该烷氧硅烷修复剂的反应性。例如，将该蒸汽相催化剂和该烷氧硅烷修复剂与该纳米孔隙LKD材料接触可以重复高达十次。
一旦完成利用该蒸汽相修复剂的处理，可以通过将半导体基片100与烷氧硅烷密封剂接触来密封该LKD材料110的表面。如上所述，这个密封步骤用厚度高达大约2nm的烷氧硅烷膜覆盖该开口的侧壁和底面，有效防止上覆的阻挡材料分散进该纳米孔隙LKD材料的互连孔。该LKD材料110可以是可选地设为在该密封工艺之前接触该蒸汽相催化剂。
密封工艺与上述修复工艺完全相同，包括利用该蒸汽相催化剂的处理。然而，烷氧硅烷密封剂用来替代该烷氧硅烷修复剂。示范性的烷氧硅烷密封剂可包括双(二甲氧基甲基)硅氧烷、双(甲基二甲氧基硅丙基)-N-甲胺、双(三乙氧基硅)乙烷、1，2-双(三甲氧基硅)己烷、双(三甲氧基硅丙基)胺或双(3-(三乙氧基硅)丙基)二硫化物。
如果对开口130的侧壁和底部的等离子损伤最小并且不需要修复，则可以通过使LKD材料110的表面与烷氧硅烷密封剂接触来密封该表面而不需要初始修复步骤。在这个例子中，在该密封工艺之前，将该半导体基片100和LKD材料110设为接触该蒸汽相催化剂。
如果需要，在该修复和/或密封工艺完成之后，该烷氧硅烷化合物可以横向网化以形成三维横向网化结构，恢复该纳米孔隙LKD材料的机械强度。这个横向网化步骤可以利用上述的有机酸(例如，乙酸，三氟乙酸，三氯乙酸，柠檬酸)处理该LKD材料以催化水和该残余烷氧基之间的水解反应来执行，如图4中所示。在优选实施例中，该有机酸蒸汽可以使用该化学制剂蒸汽输送系统220、以上述的温度范围、压强范围和时间范围输送至工艺室200。该LKD材料设为与汽相催化剂以可有效横向网化该烷氧硅烷修复和/或密封剂的量相接触。
在利用该有机酸蒸汽的处理完成之后，将该半导体基片100的温度增加到大约200℃至大约300℃，持续大约60秒至大约360秒。这个加热步骤促进邻近烷氧硅烷分子之间的缩合反应以形成三维横向网化结构，恢复该纳米孔隙LKD材料的机械强度。这个加热步骤可以在工艺室200中进行，或半导体基片100可以去除并在加热板上加热。
在蒸汽相修复和密封完成之后，半导体基片100可以经受随后的镶嵌处理步骤，包括在开口130中沉积阻挡层140、在开口130形成大块的金属层150和平坦化整个结构，如图1B-1D中所示。纳米孔隙LKD材料110中开口130的侧壁和底面的蒸汽相密封防止用来形成阻挡层140的材料(例如，Ti，TiN，Ta，TaN，Ru或RuOx)渗入该纳米孔隙LKD材料110的互连孔。纳米孔隙LKD材料层110的蒸汽相修复和密封产生更稳定的结构，其可经受进一步的机械处理步骤，包括CMP。
示例1
在一个示范实施例中，使用蒸汽相甲基三甲氧基硅烷(CH3-Si-(O-CH3)3)作为修复剂和蒸汽相二乙基胺((CH3)2NH)作为催化剂来修复具有蚀刻损伤的纳米孔隙LKD材料110的半导体基片100。
具有蚀刻损伤的低k电介质层110的半导体基片100设在工艺室200的基片支撑件210上。将该工艺室200排空至低于50托的压强，以及该基片支撑件210和工艺室200加热到大约100℃的第一温度。二乙基胺蒸汽从化学制剂蒸汽输送系统220A输送至工艺室200，至静态压强为700托。该半导体基片100设为接触该二乙基胺蒸汽大约20秒。
在该二乙基胺蒸汽处理完成后，利用真空泵240在动态真空排出该蒸汽以将该工艺室200的压强降低至大约5托或更低，以去除残余的胺并促进该甲基三甲氧基硅烷的蒸汽化，其在大气条件下是液体。
甲基三甲氧基硅烷蒸汽(CH3-Si-(O-CH3)3)从化学制剂蒸汽输送系统220B流进工艺室200，直到静态压强达到400托。半导体基片100设为在大约100℃的第一温度接触该蒸汽相甲基三甲氧基硅烷大约20秒。
基片支撑件210的温度从该大约100℃的第一温度增加到大约150℃的第二温度，该半导体基片100设为接触该蒸汽相甲基三甲氧基硅烷持续额外的30秒。
在该甲基三甲氧基硅烷蒸汽处理完成后，利用真空泵240在动态真空下排出该蒸汽以将该工艺室200的压强降低至大约0.5托或更少，持续大约60秒，以便去除过量的甲基三甲氧基硅烷蒸汽和副产物。
示例2
在另一实施例中，具有蚀刻损伤的纳米孔隙LKD材料110的半导体基片100使用蒸汽相双(3-甲基二甲氧基硅-丙基)-N-甲胺作为密封剂以及蒸汽相甲胺(CH3NH2)作为催化剂来密封。
具有蚀刻损伤的低k电介质层110的半导体基片100设在工艺室200的基片支撑件210上。将该工艺室200排空至压强低于50托，基片支撑件210和工艺室200加热至大约150℃的第一温度。从化学制剂蒸汽输送系统220A将甲胺蒸汽输送进工艺室200至1800托的静态压强。该半导体基片100设为接触该甲胺蒸汽持续大约60秒。
在该甲胺蒸汽处理完成后，利用真空泵240在动态真空下排出该蒸汽以将该工艺室200的压强降低至大约300托或更低。
使用干氮气作为载体气体以近似3000sccm将二(3-甲基二甲基硅氧烷基-丙基)-N-甲胺流从化学制剂蒸汽输送系统220C引入工艺室200。通过同时运行真空泵240将该压强保持在至400托。半导体基片100设为接触双(3-甲基二甲氧基硅-丙基)-N-甲胺流在大约150℃持续大约180秒。
在该二(3-甲基二甲基硅氧烷基-丙基)-N-甲胺蒸汽处理完成后，利用真空泵240在动态真空下排出该蒸汽以将该工艺室200的压强降低至大约2托或更低持续大约60秒。
示例3
准备好具有上覆的纳米孔隙LKD材料(JSR LKD-5109，由JSRCorporation制造)的硅基片样品。该样品涂覆有光刻胶、图案化并且经受反应性离子蚀刻(RIE)以形成沟槽，然后进行氧气灰化以去除该光刻胶。该RIE和光刻胶去除在图案化区域中蚀刻出的开口周围产生等离子损伤区域。
具有等离子损伤的JSR LKD-5109层的第一样品设为在接触蒸汽相n-丙基三甲氧基硅烷(n-PTMS)修复剂之前接触汽相三氟乙酸催化剂。带有等离子损伤的JSR LKD-5109层的第二样品使用n-PTMS修复剂和溶解在超临界CO2(SCCO2)中的三氟乙酸催化剂来处理。第三样品是控制样品，具有未修复的等离子损伤的JSRLKD-5109层。第四样品是另一控制样品，具有沉积状态的JSRLKD-5109层(即，未经受等离子蚀刻)。通过扫描电子显微镜(SEM)来分析这些样品以表征沿所蚀刻的沟槽的侧壁的修复程度，以及通过次级离子质谱(SIMS)分析以表征该JSR LKD-5109层表面至大约150nm的深度中碳与硅的比率。
将含有该等离子蚀刻损伤的JSR LKD-5109的第一样品设在工艺室200的基片支撑件210上。将该工艺室200排空至压强低于50托，将该基片支撑件210和工艺室200加热至大约135℃的第一温度。从化学制剂蒸汽输送系统220A将三氟乙酸与水3∶1的混合物蒸汽化并引入工艺室200至900托的压强。该第一样品设为在工艺室200利用氮气回填之前接触该三氟乙酸蒸汽持续大约120秒，以及排空。通过化学制剂蒸汽输送系统220B将蒸汽相n-PTMS修复剂输送进工艺室200，以在大约1000托的静态压强处理该第二样品持续大约5分钟。该工艺室200回填氮气，该第一样品保持在135℃的温度持续大约2分钟。该第一样品然后从该工艺室去除并在加热板上在大约250℃加热大约120秒。
该第二样品设在加热的压力容器(即，大约140℃)中，其随后密封并利用超临界二氧化碳(SCCO2)加压至大约97500托(大约130巴)。使用高压喷射回路通过将额外的SCCO2泵入该容器并将催化剂冲入该容器来添加三氟乙酸与水的3∶1混合物。该催化剂在完成添加后的浓度大约为1％体积份，所得到的压强是在大约140℃、大约150000托(大约200巴)。在大约60秒的时间后，通过添加纯SCCO2将含有酸催化剂的SCCO2溶液从该室冲离。该冲洗导致在大约2分钟的时间有大约6流体周转(即，一定时间等于该容器容积所需的流量)。冲洗之后，该容器中的压强通过去除SCCO2降低至大约140℃、大约97500托(大约130巴)。然后将n-丙基三甲氧基硅烷(n-PTMS)修复剂添加到该容器，使用高压喷射回路通过将额外的SCCO2泵入该容器。该修复剂的浓度大约2％体积份，该容器中最终的压强是140℃、大约150000托(大约200巴)。在5分钟的时间后，该容器利用纯SCCO2冲洗，所持续的时间和流率使得在大约2分钟的时间内有8流体周转。该容器中的压强降低到大气压强，然后去除该第二样品。
该第一样品(即，n-PTMS蒸汽相修复的)、第二样品(即，n-PTMS SCCO2修复的)和第三样品(即，未修复的)通过SEM来描述。每个样品在1％的HF溶液中蚀刻大约60秒，并在去离子水中冲洗。因为该1％HF溶液优先蚀刻来自该纳米孔隙LKD材料的Si-OH基团，所以修复可以通过沿该沟槽的侧壁的低切深度量化。图6A说明该第一样品(即，n-PTMS汽相修复)的SEM图像，其中在进入该沟槽的侧壁大约11nm的深度测量低切。图6B说明该第二样品(即，n-PTMS SCCO2修复)的SEM图像，其中在进入该沟槽的侧壁大约11nm的深度测量低切。图6C说明该第三样品(即，未修复)的SEM图像，其中在进入该沟槽的侧壁大约43nm的深度测量低切。因此，图6B-6C说明该汽相修复与SCCO2在修复蚀刻损伤的纳米孔隙LKD材料中一样有效。
该第一样品(即，n-PTMS蒸汽相修复)、第二样品(即，n-PTMSSCCO2修复)、第三样品(即，未修复)和第四样品(即，沉积的JSRLKD-5109)通过SIMS表征以确定碳与硅的比与深度的关系，其中溅射每个样品表面，并且利用质谱仪分析在这个溅射过程中形成的次级离子。
如图7中所示，该第四样品(图7中的填充方块)、沉积状态的JSR LKD-5109的碳与硅的比大约0.55。对于该第三样品(图7中的空心方块)，在蚀刻该沟槽和光刻胶去除完成后，该碳与硅的比降至大约0.45至大约0.55。然而，对于该第二样品(图7中空心圆)，该碳与硅的比升至大约0.6至大约0.8，高于该沉积状态的JSRLKD-5109的碳与硅的比。这是因为该修复工艺用丙基(-C3H7)替换了损失的甲基(-CH3)，因此增加该受损区域的碳与硅的比。对于第一样品(图7中实心圆)，该碳与硅的比显著增加到高达大约1.45。这可能表明该蒸汽相修复更有效地使n-PTMS和/或多孔表面的密封致密。
尽管本发明参照其多个实施方式详细描述，但是对于本领域技术人员来说，显然可进行各种不同的改变和修改，以及采用等同方式，而不背离所附权利要求的范围。

Claims (20)

1.一种处理半导体基片上形成的纳米孔隙低k电介质材料的方法，该低k电介质材料具有蚀刻出的开口，其在该蚀刻出的开口的外部表面上和在互连孔的内部表面上具有包含硅烷醇基团的蚀刻受损区域，该方法包括：
(a)将该低k电介质材料与汽相催化剂以可有效在该催化剂和该蚀刻受损区域中的硅烷醇基团之间形成氢键的量相接触，形成催化中间体，然后是：
(b)将该低k电介质材料与汽相烷氧硅烷修复剂以可有效与50％或更多的该蚀刻受损区域中的硅烷醇基团反应的量相接触，从而该烷氧硅烷修复剂与该催化中间体反应；以及/或
(c)将该低k电介质材料与汽相烷氧硅烷密封剂以可有效防止上覆阻挡层扩散进入该互连孔的量相接触，从而该烷氧硅烷密封剂与该催化中间体反应。
2.根据权利要求1所述的方法，其中：(i)该催化剂是Lewis碱胺或有机酸；(ii)在步骤(c)之前重复步骤(a)和步骤(b)十次；(iii)该密封剂在该蚀刻出的开口的外部表面上形成厚度高达2nm的烷氧硅烷膜；以及/或该烷氧硅烷修复剂具有80至125的原子质量单位，该烷氧硅烷密封剂具有200至400的原子质量单位。
3.根据权利要求1所述的方法，进一步包括在步骤(c)之前重复步骤(a)。
4.根据权利要求2所述的方法，其中该Lewis碱胺是氨(NH3)、甲胺(CH3NH2)、二甲胺((CH3)2NH)或三甲胺(N(CH3)3)；或该有机酸是乙酸，三氟乙酸，三氯乙酸或柠檬酸的水溶液。
5.根据权利要求2所述的方法，进一步包括，在步骤(a)之后以及在步骤(b)之前从该低k电介质材料去除汽相有机酸催化剂以防止在：(i)该汽相有机酸催化剂和(ii)烷氧硅烷修复剂和/或烷氧硅烷密封剂之间的汽相反应。
6.根据权利要求5所述的方法，其中该烷氧硅烷修复剂是甲基三甲氧基硅烷(CH3-Si-(O-CH3)3)，二甲氧基二甲基硅烷((CH3)2-Si-(OCH3)2)，甲氧基三甲基硅烷((CH3)3-Si-OCH3)或n-丙基三甲氧基硅烷(CH3-CH2-CH2-Si-(OCH3)3)；以及该烷氧硅烷密封剂是双(二甲氧基甲基)硅氧烷，双(甲基二甲氧基硅丙基)-N-甲胺，双(三乙氧基硅)乙烷，1，2-双(三甲氧基硅)己烷，双(三甲氧基硅丙基)胺或双(3-(三乙氧基硅)丙基)二硫化物。
7.根据权利要求1所述的方法，其中(a)将该低k电介质材料与该气相催化剂接触包括：
将该半导体基片设在处理室中和排空该处理室；
将该半导体基片加热至60℃至275℃的第一温度；
将该催化剂引入压强20托至1500托的该室，持续时间10秒至60秒；以及
排空该室。
8.根据权利要求7所述的方法，其中该第一温度是100℃至200℃，该压强是100托至760托，时间是20秒至30秒。
9.根据权利要求7所述的方法，其中(b)将该低k电介质材料与该气相修复剂接触和/或(c)将该低k电介质材料与该气相密封剂接触包括：
将该半导体基片加热至60℃至275℃的第一温度；
将该烷氧硅烷修复剂或烷氧硅烷密封剂引入压强20托至1500托的室，持续时间10秒至180秒；以及
排空该室。
10.根据权利要求9所述的方法，其中该第一温度100℃至200℃，该压强100托至760托，以及该时间20秒至60秒。
11.根据权利要求9所述的方法，其中(b)将该低k电介质材料与该气相修复剂接触和/或(c)将该低k电介质材料与该气相密封剂接触进一步包括：
在排空该室之前，将该半导体基片加热至80℃至300℃的第二温度，持续10秒至180秒的额外时间；以及
排空该室之后，将该半导体基片保持在该第二温度持续10秒至180秒。
12.根据权利要求11所述的方法，其中该第二温度是150℃至250℃，该额外的时间是20秒至60秒。
13.根据权利要求7所述的方法，进一步包括：
(d)将该低k电介质材料与汽相有机酸催化剂以可有效横向网化该烷氧硅烷修复和/或密封剂的量相接触；以及
(e)加热该低k电介质材料至有效横向网化该烷氧硅烷修复和/或密封剂的温度。
14.根据权利要求13所述的方法，其中(d)将该低k电介质材料与汽相有机酸催化剂以可有效横向网化该烷氧硅烷修复和/或密封剂的量相接触，包括：
将该半导体基片加热至60℃至275℃的第一温度；
将该汽相有机酸催化剂引入压强20托至1500托的室，持续时间10秒至60秒；以及
排空该室。
15.根据权利要求13所述的方法，其中(e)加热该低k电介质材料至有效横向网化该烷氧硅烷修复和/或密封剂的温度包括：
在该室中，将该半导体基片加热至200℃至300℃的温度持续60秒至180秒；或
从该室去除该半导体基片并将该半导体基片设在热板上，以及将该半导体基片加热至200℃至300℃的温度持续60秒至180秒。
16.一种处理半导体基片上形成的纳米孔隙低k电介质材料的方法，该低k电介质材料具有蚀刻出的开口，其在该蚀刻出的开口的外部表面上和在互连孔的内部表面上具有包含硅烷醇基团的蚀刻受损区域，该方法包括：
(a)将该低k电介质材料与汽相有机酸催化剂以可有效在该催化剂和该蚀刻受损区域中的硅烷醇基团之间形成氢键的量相接触，形成催化中间体，接着：
(b)将该低k电介质材料与汽相烷氧硅烷修复剂以可有效与50％或更多的该蚀刻受损区域中的硅烷醇基团反应的量相接触，从而该烷氧硅烷修复剂与该催化中间体反应；以及/或
(c)将该低k电介质材料与汽相烷氧硅烷密封剂以可有效防止上覆阻挡层扩散进入该互连孔的量相接触，从而该烷氧硅烷密封剂与该催化中间体反应。
17.根据权利要求16所述的方法，其中该有机酸是乙酸、三氟乙酸、三氯乙酸或柠檬酸的水溶液。
18.根据权利要求16所述的方法，其中该烷氧硅烷修复剂是甲基三甲氧基硅烷(CH3-Si-(O-CHs)3)，二甲氧基二甲基硅烷((CH3)2-Si-(OCH3)2)，甲氧基三甲基硅烷((CH3)3-Si-OCH3)或n-丙基三甲氧基硅烷(CH3-CH2-CH2-Si-(OCH3)3)；以及该烷氧硅烷密封剂是双(二甲氧基甲基)硅氧烷，双(甲基二甲氧基硅丙基)-N-甲胺，双(三乙氧基硅)乙烷，1，2-二(三甲氧基硅烷)正己烷，双(三甲氧基硅丙基)胺或双(3-(三乙氧基硅)丙基)二硫化物。
19.根据权利要求16所述的方法，其中(a)将该低k电介质材料与汽相有机酸催化剂接触包括：
将该半导体基片设在处理室中和排空该处理室；
将该半导体基片加热至60℃至275℃的第一温度；
将该汽相有机酸催化剂引入压强20托至1500托的室，持续时间10秒至60秒；以及
排空该室。
20.根据权利要求16所述的方法，进一步包括：
(d)将该低k电介质材料与汽相有机酸催化剂以可有效横向网化该烷氧硅烷修复和/或密封剂的量相接触；以及
(e)加热该低k电介质材料至有效横向网化该烷氧硅烷修复和/或密封剂的温度。
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