CN103688345A - 用于减少脱气的表面处理及沉积 - Google Patents

用于减少脱气的表面处理及沉积 Download PDF

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CN103688345A
CN103688345A CN201280035181.0A CN201280035181A CN103688345A CN 103688345 A CN103688345 A CN 103688345A CN 201280035181 A CN201280035181 A CN 201280035181A CN 103688345 A CN103688345 A CN 103688345A
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J·梁
X·陈
N·K·英格尔
S·文卡特拉马
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Abstract

描述一种形成介电层的方法。该方法首先通过自由基成分的化学气相沉积（CVD）沉积含硅氮与氢（聚硅氮烷）层。该含硅氮与氢层是通过将自由基前驱物（在远端等离子体中激发）与无激发的无碳的硅前驱物结合而形成。氧化硅覆盖层可由一部分的无碳的含硅氮与氢层形成，以避免底下的层在转换成氧化硅之前该层的性质随时间演变。或者，该氧化硅覆盖层形成于该含硅氮与氢层上。任一形成方法皆涉及在基材处理区域内形成本地等离子体。

Description

用于减少脱气的表面处理及沉积
背景技术
自从数十年前引入半导体元件以来，半导体元件的几何形状在尺寸上已剧烈减少。现代的半导体制造设备例行生产具有45nm、32nm、与28nm的特征尺寸的元件，且正开发及实行新设备以制作具有更小的几何形状的元件。减少的特征尺寸造成元件上的结构性特征具有减少的空间尺度。元件上的间隙与沟槽的宽度变窄至间隙深度对间隙宽度的深宽比（aspect ratio）高得足以造成难以用介电材料填充该间隙的地步。在间隙完全填充前，沉积的介电材料易于在顶部阻塞，在间隙中间产生空隙或缝线（seam）。
过去几年，已开发许多技术去避免使介电材料阻塞间隙顶部或“愈合”已经形成的空隙或缝线。已以高度可流动的前驱物材料开始进行一项解决手段，可以液相施加该高度可流动的前驱物材料至旋转基材表面（例如，SOG沉积技术）。这些可流动的前驱物能够流进非常小的基材间隙并且填充该等间隙，而不形成空隙或脆弱缝线。然而，一旦这些高度可流动的材料被沉积，它们必须被硬化成固体介电材料。
许多例子中，该硬化步骤包括热处理，以从沉积的材料移除碳与氢氧基，而留下诸如氧化硅的固体介电质。不幸的是，离开的碳与氢氧物种经常在硬化的介电质中留下孔隙，这些孔隙降低最终材料的品质。此外，硬化的介电质也倾向在体积上绉缩，这可于介电质与周围基材的介面处留下裂隙与空间。一些例子中，硬化的介电质的体积可减少40%或更多。
旋涂介电质（SOD）也已用于流入图案化基材上的特征。该材料大体上由硅氮烷类型的层转换成氧化硅，该硅氮烷类型的层含有硅、氮、与氢。含有硅、氮、与氢的层一般在高温下于含氧环境中转换成氧化硅。来自环境的氧置换氮与氢以建立氧化硅层。对某些电路构造而言，对氧环境的高温暴露可能摧毁底下的层。此考量导致需要在制造流程期间维持在“热预算”内。热预算的考量已大幅将SOD限制至结合底下的氮化硅层的流程，该氮化硅层能够保护底下的特征免受氧化（例如DRAM应用）。
已开发替代性方法，该等替代性方法藉由自由基成分的CVD沉积含硅氮烷层。自由基成分的CVD可通过激发一种前驱物并且将该前驱物与无激发的含硅前驱物在无等离子体的基材处理区域中结合而建立可流动层。层性质（包括密度）可能随时间会稍微改变，直到含硅氮烷层转变成氧化硅为止。控制层性质的演变（evolve）改善使用这些层的元件的制造能力。因此，需要新的沉积制程与材料以形成不会随时间演变的介电材料。此需要与其他需要在本发明中获得解决。
发明内容
在此描述一种形成介电层的方法。该方法首先通过自由基成分的化学气相沉积（CVD）沉积含硅氮与氢（聚硅氮烷）层。该含硅氮与氢层是通过将自由基前驱物（在远端等离子体中激发）与无激发的无碳的硅前驱物结合而形成。氧化硅覆盖层可由一部分的无碳的含硅氮与氢层形成，以避免底下的层在转换成氧化硅之前该层的性质随时间演变。或者，该氧化硅覆盖层形成于该含硅氮与氢层上。任一形成方法皆涉及在基材处理区域内形成本地等离子体。
本发明的实施例包括在基材上形成介电层的方法。该等方法包括下述依序的步骤：(1)在含有该基材的第一基材处理区域中，于该基材上形成无碳的含硅氮与氢层，以及(2)在该无碳的含硅氮与氢层上形成氧化硅覆盖层。形成该无碳的含硅氮与氢层包括以下步骤：将无激发的前驱物流进远端等离子体区域以产生自由基前驱物，在该第一基材处理区域中将无碳的含硅前驱物与该自由基前驱物结合，以及沉积无碳的含硅氮与氢层于该基材上。在形成该无碳的含硅氮与氢层的操作期间，该第一基材处理区域无等离子体。该无碳的含硅氮与氢层在沉积期间可流动。形成该氧化硅覆盖层包括以下步骤：将含氧前驱物流进含有该基材的第二基材处理区域，将含硅前驱物流进该第二基材处理区域，在该第二基材处理区域中由该含氧前驱物与该含硅前驱物形成等离子体，以及沉积该氧化硅覆盖层于该无碳的含硅氮与氢层上。
本发明的实施例包括在基材上形成介电层的方法。该等方法包括下述依序的步骤：(1)在含有该基材的第一基材处理区域中，于该基材上形成无碳的含硅氮与氢层，以及(2)处理该无碳的含硅氮与氢层，以将该无碳的含硅氮与氢层的一部分转换成氧化硅覆盖层。形成该无碳的含硅氮与氢层包括以下步骤：将无激发的前驱物流进远端等离子体区域以产生自由基前驱物，在该第一基材处理区域中将无碳的含硅前驱物与该自由基前驱物结合，以及沉积无碳的含硅氮与氢层于该基材上。在形成该无碳的含硅氮与氢层的操作期间，该第一基材处理区域无等离子体。该无碳的含硅氮与氢层在沉积期间可流动。处理该无碳的含硅氮与氢层包括以下步骤：将含氧前驱物流进含有该基材的第二基材处理区域，在该第二基材处理区域中由该含氧前驱物形成等离子体，以及将该无碳的含硅氮与氢层的一部分转换成该氧化硅覆盖层。
额外的实施例与特征部分在随后的实施方式中提出，而部分对于本领域技术人员而言，在详阅本说明书后可清楚该等实施例与特征，或者可由操作所揭露的实施例而学得。可通过本说明书中所述的设备、各式组合物及方法而明了及获得所揭露的实施例的特征与优点。
附图说明
通过参考说明书的其余部分及图式，可进一步了解本发明的本质与优点，在该等图式中，相似的附图标记用于全部多幅图式中以指类似部件。一些例子中，次符号与一附图标记相连且置于一破折号后，以标注类似部件之一者。当引用一附图标记而不指定现有次符号时，申请人希望是指所有此类多个类似部件。
图1是流程图，示出用于根据本发明的实施例制做介电层的所选步骤；
图2是流程图，示出用于根据本发明的实施例制做介电层的所选步骤；
图3显示根据本发明实施例的基材处理系统；
图4A显示根据本发明实施例的基材处理腔室；
图4B显示根据本发明实施例的气体分配喷头。
具体实施方式
在此描述一种形成介电层的方法。该方法首先通过自由基成分的化学气相沉积（CVD）沉积含硅氮与氢（聚硅氮烷）层。该含硅氮与氢层是通过将自由基前驱物（在远端等离子体中激发）与无激发的无碳的硅前驱物结合而形成。氧化硅覆盖层可由一部分的无碳的含硅氮与氢层形成，以避免底下的层在转换成氧化硅之前该层的性质随时间演变。或者，该氧化硅覆盖层形成于该含硅氮与氢层之上。任一形成方法皆涉及在基材处理区域内形成本地等离子体。
已发现将自由基成分CVD的含硅氮与氢层定位在氧化硅覆盖层下方可减少及/或消除脱气以及伴随的层性质的随时间演变。没有氧化硅覆盖层，层的性质与化学当量可能随着时间改变。由于含硅物种、氨气、与类似物的脱气，这些层随时间演变。由于吸收存在于一般制造设施内的周围气氛中的水或其他成分，性质也可能演变。改变层性质可能会因需要严密控制层形成与其他基材处理系统或腔室内的处理之间的延迟，而使制造制程复杂化。这些复杂与需求都是不被期望的。已发现此述的氧化硅覆盖层抑制脱气，但仍容许底下的含硅氮与氢层转变成含硅与氧层且转变成氧化硅。
已发现根据在此所含的方法以含氧化硅覆盖层覆盖自由基成分的CVD层在基材暴露至一般清洁室气氛时显现不会演变的性质。现在，将描述关于形成氧化硅覆盖层的方法与系统的额外细节。
第一示范性介电质堆迭制程
图1是流程图，显示根据本发明的实施例制作介电层堆迭的方法100中所选步骤。方法100包括提供无碳的含硅前驱物至基材处理区域102。一些实施例中，该无碳的含硅前驱物不通过等离子体激发，所以该前驱物完整无缺地行进至基材处理区域中。随后仅通过即将要描述的自由基前驱物提供激发。该无碳的含硅前驱物除了其他类的硅前驱物外可以是例如含硅与氮前驱物、含硅与氢前驱物、或含硅氮与氢前驱物。缺乏碳减少了沉积层的绉缩。含硅前驱物除了无碳之外可为无氧。缺乏氧造成由前驱物形成的含硅与氮层中有低浓度的硅烷醇（Si-OH）基。沉积层中过剩的硅烷醇基团（moiety）可能在从沉积层移除氢氧（-OH）基团的后沉积步骤期间引发孔隙度与绉缩增加。
无碳的硅前驱物的特定范例可包括硅烷胺，除了其他硅烷胺之外，可以诸如为H2N(SiH3)、HN(SiH3)2与N(SiH3)3。不同实施例中，硅烷胺的流速可为约200sccm或更大、300sccm或更大、或者约500sccm或更大。在此所给的所有流速是参考双腔室基材处理系统。单一晶圆系统将需要这些流速的一半，而其他晶圆形状/尺寸将需要经过按处理面积缩放（scaled）的流速。这些硅烷胺可与额外气体混合，这些额外气体可做为载气、反应性气体、或前述二者。额外气体除其他气体之外可包括H2、N2、NH3、He、Ne及/或Ar。无碳的含硅前驱物的范例也可包括甲硅烷（SiH4），该甲硅烷可单独存在或与其他含硅气体（例如N(SiH3)3）、含氢气体（例如H2）及/或含氮气体（例如N2、NH3）混合。无碳的含硅前驱物也可包括乙硅烷、丙硅烷、更高等级的硅烷、与氯化硅烷，前述硅烷为单独存在或彼此结合或与先前提及的无碳含硅前驱物结合。
也提供自由基前驱物至基材处理区域104。自由基前驱物描述在基材处理区域外的等离子体激发中由任何稳定物种（惰性或反应性）产生的等离子体流出物。该自由基前驱物可以是含氮自由基前驱物，该含氮自由基前驱物在此是指自由基氮前驱物。该自由基氮前驱物是一种在基材处理区域外由更稳定的氮前驱物所生成的含氮自由基前驱物。稳定的前驱物可在此指无激发的前驱物，以指示该前驱物尚未通过等离子体。可在腔室等离子体区域或另一远端等离子体系统（RPS）中活化含有NH3、联胺（N2H4）及/或N2的稳定的氮前驱物化合物以形成该自由基氮前驱物，该自由基氮前驱物随后被输送进入基材处理区域，以激发含硅前驱物，前述的远端等离子体系统（RPS）是位在处理腔室外。将稳定氮前驱物活化成自由基氮前驱物涉及解离，除其他方法之外，该解离可通过以下方法完成：热解离、紫外光解离、及/或等离子体解离。等离子体解离可涉及：在远端等离子体生成腔室中由氦、氩、氢（H2）、氙、氨（NH3）等点燃等离子体，以及将稳定的氮前驱物导入等离子体区域以生成自由基氮前驱物。
不同实施例中，稳定的氮前驱物也可以是包含NH3与N2、NH3与H2、NH3与N2与H2、以及N2与H2的混合物。也可使用联胺以取代NH3或与NH3结合，且可用于涉及N2与H2的混合物中。不同实施例中，稳定的氮前驱物的流速可为约300sccm或更大、约500sccm或更大、或者是约700sccm或更大。在腔室等离子体区域中产生的自由基氮前驱物可以是·N、·NH、·NH2等之一或多者，且可伴随在等离子体中形成的离子化物种。在本发明的实施例中，氧源也可在远端等离子体中与更稳定的氮前驱物结合。添加氧源预先使层载有氧，同时减少了流动性。氧源可包括O2、H2O、O3、H2O2、N2O、NO、或NO2之一或多者。
在运用腔室等离子体区域的实施例中，自由基氮前驱物在基材处理区域的一区段中生成，该区段自沉积区域划分出来，在该沉积区域，该等前驱物混合并且反应而沉积含硅与氮层于沉积基材上（例如半导体晶圆）。自由基氮前驱物亦可伴随诸如氢（H2）、氮（N2）、氦、氖、氩等载气。在此可将基材处理区域描述为在生长无碳的含硅氮与氢层期间及后续制程期间“无等离子体”。“无等离子体”并非必然指该区域缺乏等离子体。腔室等离子体区域中等离子体的边界是难以界定的，且可能通过喷头中的穿孔（aperture）侵入基材处理区域上。在感应耦合等离子体的情况中，例如可在基材处理区域内启动少量的离子化。大体而言，低强度的等离子体可在基材处理区域中建立，而不至于损害形成的层的可流动的本质。在建立自由基氮前驱物期间，离子密度远低于远端/腔室等离子体区域的等离子体的所有成因不偏离在此所用的“无等离子体”的范畴。
在基材处理区域中，无碳的硅前驱物与自由基氮前驱物混合并且反应，而在沉积基材上沉积含硅氮与氢层106。多个实施例中，所沉积的含硅氮与氢层具有可流动特性，此可流动特性与习知氮化硅（Si3N4）层沉积技术并不类似。形成期间可流动的本质使层得以在固化前流进狭窄的特征中。
含硅氮与氢层中的氮可源自自由基前驱物或无激发的前驱物的任一者（或源自于前述二者）。一些实施例中，该无碳的含硅前驱物可基本上无氮。然而，其他实施例中，无碳的含硅前驱物与自由基氮前驱物二者皆含有氮。在第三套实施例中，自由基前驱物可基本上无氮而用于无碳的含硅氮与氢层的氮可由无碳的含硅前驱物供应。所以，在此自由基前驱物可指“自由基氮及/或氢前驱物”，意味该前驱物含有氮及/或氢。可以此类推，流进等离子体区域而形成自由氮及/或氢前驱物的前驱物可指含氮及/或氢前驱物。此命名法则可应用到在此揭露的每一实施例。在多个实施例中，含氮及/或氢前驱物包含氢（H2），而自由基氮及/或氢前驱物包含·H等。
回到图1所示的特定范例，含硅氮与氢层的可流动性可能是由于从将自由基氮前驱物与无碳的含硅前驱物混合造成的各种性质。这些性质可包括在沉积的层中有显著的氢成分及/或存在短链的聚硅氮烷聚合物。在形成层期间或之后，这些短链生长并且互成网络，而形成更加致密的介电材料。例如沉积层可具有硅氮烷形式的Si-NH-Si骨架，即无碳的Si-N-H层。当含硅前驱物与自由基前驱物二者皆无碳时，沉积的含硅氮与氢层也实质上无碳。当然，“无碳”并非必然意味该层缺乏甚至痕量的碳。碳混入物（contamination）可存在于前驱物材料中而找到进入沉积的含硅与氮前驱物的途径。然而，这些碳杂质的量远低于具有碳基团的硅前驱物（例如TEOS、TMDSO等）中可见的量。
该制程中的此点，在本发明的多个实施例中，制程流出物可由基材处理区域移除。制程流出物可包括任何未反应的含硅前驱物、未反应的自由基氮前驱物、惰性的载气以及来自层生长的反应产物。在所揭露的实施例中，可通过将惰性物种流进基材处理区域及/或通过排放通口排尽来移动制程流出物。
该方法100还包括额外沉积氧化硅于含硅氮与氢层上，以避免底下的层的脱气。氧化硅层在此是指氧化硅覆盖层。氧化硅覆盖层的形成可发生在相同的基材处理区域中，或该基材可传送到分开的处理区域。本发明的多个实施例中，该基材可在传送期间暴露至气氛，或可维持在真空下。形成氧化硅覆盖层的优点是，避免执行后续处理之前，含硅氮与氢层的膜性质随时间演变。就此而言，期望在沉积氧化硅覆盖层之前有可控制且可再现的基材暴露量。通过提供含氧前驱物至基材处理区域而启动氧化硅覆盖层的沉积108。含硅前驱物还流进基材处理区域109，且在基材的附近与含氧前驱物结合。等离子体同步在基材处理区域中形成110，以形成氧化硅覆盖层112。已使用远端等离子体（在基材处理区域外）沉积含硅氮与氢层，而本地等离子体（在基材处理区域内）用于沉积氧化硅覆盖层。
含氧前驱物可包括分子氧（O2）及/或臭氧（O3）。较佳实施例中，含硅前驱物可包括正硅酸乙酯（TEOS）。大体而言，该含硅前驱物可包括正硅酸乙酯（TEOS）、八甲基三硅氧烷（octamethyltrisiloxane,OMTS）、八甲基环四硅氧烷（octamethylcyclotetrasiloxane,OMCTS）、甲基二乙氧基硅烷（methyldiethoxysilane,MDEOS）、双（叔丁基胺基）硅烷（bis(tertiary-butylamino)silane,BTBAS）、三甲基氨基硅烷（tridimethylaminosilane,TriDMAS）、三二甲基氨基硅烷（trisdimethylaminosilane,TrisDMAS）、甲硅烷（silane）、乙硅烷（disilane）、二氯硅烷、三氯硅烷、二溴硅烷、四氯化硅、四溴化硅、二甲基硅烷、三甲基硅烷、四甲基硅烷、二乙基硅烷、正硅酸甲酯（tetramethylorthosilicate,TMOS）、或前述前驱物的组合。施加至基材处理区域的等离子体功率可为约1000W或更低、约500W或更低、或者是约300W或更低。在本发明多个实施例中，施加至基材处理区域的等离子体功率可为约50W或更高，约100W或更高，或者是约200W或更高。等离子体功率的该等上限可与该等下限结合以形成额外实施例。该等离子体功率低于许多等离子体增强化学气相沉积（PE-CVD）制程，以基本上维持底下的含硅氮与氢层的结构。等离子体频率可以是13.56MHz及/或350KHz。视情况与含硅前驱物同时导入腔室的气体包括氦气及/或氩气。氦气或其他惰气可用做为载气，以递送平常为液体的前驱物至基材处理区域。
可用介于约10sccm至约1000sccm之间的流速将该含氧前驱物导进腔室。可用介于约5sccm至约1000sccm之间的流速将该含硅前驱物导进腔室。可用介于约100sccm至约20000sccm之间的流速将可选的载气（例如氦气）导进腔室。进入腔室的含硅前驱物（例如正硅酸乙酯）流速对载气（例如氦气）流速的比为约1:1或更高，诸如介于约1:1至约1:100之间。当含硅前驱物与含氧前驱物流进腔室以沉积氧化硅覆盖层的同时，基材处理区域内的压力可大于约500mTorr（诸如介于约2Torr至约10Torr之间），且腔室中基材支撑件的温度可以介于约100℃至约250℃之间。在所揭露的实施例中，该温度较佳为低于约250℃或低于约200℃。低基材温度也是期望的，以保有含硅氮与氢层的结构。含硅前驱物与含氧前驱物可各自流入腔室一段时间，该段时间足以沉积厚度为约5nm或更大、约10nm或更大、约20nm或更大、或者约50nm或更大的氧化硅覆盖层。
第二示范性介电质堆迭制程
图2是一流程图，该流程图显示根据本发明的实施例制做介电层堆迭的第二方法200的所选步骤。该方法200包括形成含硅氮与氢层，如参考图2所描述。因此，该方法包括提供无碳的含硅前驱物至基材处理区域202，该步骤无等离子体激发且如先前所述的所有实施例。该方法进一步包括提供自由基前驱物至基材处理区域204，如先前所述。该自由基前驱物提供主要的激发，此述的主要的激发是在无等离子体的基材处理区域中“断裂”无碳的含硅前驱物以及产生沉积含硅氮与氢层于沉积基材上206的反应所需。再一次，所沉积的含硅氮与氢层可具有可流动特性，此可流动特性与习知氮化硅（Si3N4）层沉积技术并不类似。形成含硅氮与氢层之后，可由基材处理区域移除制程流出物。制程流出物可包括任何未反应的含硅前驱物、未反应的自由基氮前驱物、惰性的载气以及来自层生长的反应产物。在所揭露的实施例中，可藉由将惰性物种流进基材处理区域及/或藉由通过排放通口排尽来移动制程流出物。
该方法200进一步包括额外处理该含硅氮与氢层，以由该含硅氮与氢层的一部分形成氧化硅。与图1的方法呈对比，此氧化硅覆盖层是通过使用一些含硅氮与氢层的材料形成。但是，所形成的氧化硅覆盖层的目的与图1相同：为了避免从底下的层脱气。氧化硅覆盖层的形成可发生在相同的基材处理区域，或该基材可被传送至分开的处理区域。本发明的多个实施例中，该基材可在传送期间暴露至气氛，或可维持在真空下。形成氧化硅覆盖层的优点是，避免执行后续处理之前，含硅氮与氢层的膜性质随时间演变。就此而言，期望在形成氧化硅覆盖层之前有可控制且可再现的基材暴露量。通过提供含氧前驱物至基材处理区域，而启动氧化硅覆盖层的形成208。等离子体同步在基材处理区域中形成210，以使用来自含硅氮与氢膜的材料以及来自含氧前驱物的氧形成氧化硅覆盖层112。已使用远端等离子体（在基材处理区域外）沉积含硅氮与氢层，而本地等离子体（在基材处理区域内）用于沉积氧化硅覆盖层。
含氧前驱物可包括分子氧（O2）及/或臭氧（O3）。施加至基材处理区域的等离子体功率可为约1000W或更低、约500W或更低、或者是约300W或更低。在本发明多个实施例中，施加至基材处理区域的等离子体功率可为约50W或更高，约100W或更高，或者是约200W或更高。等离子体功率的该等上限可与该等下限结合以形成额外实施例。该等离子体功率低于许多等离子体增强化学气相沉积（PE-CVD）制程，以基本上维持底下的含硅氮与氢层的结构。等离子体频率可以是13.56MHz及/或350KHz。视情况与含硅前驱物同时导入腔室的气体包括氦气及/或氩气。氦气或其他惰气可用做为载气，以递送平常为液体的前驱物至基材处理区域。
可用介于约10sccm至约1000sccm之间的流速将该含氧前驱物导进腔室。当含氧前驱物流进腔室以形成氧化硅覆盖层的同时，基材处理区域内的压力可大于约500mTorr（诸如介于约2Torr至约10Torr之间），且腔室中基材支撑件的温度可以介于约100℃至约250℃之间。在所揭露的实施例中，该温度较佳为低于约250℃或低于约200℃。低基材温度也是期望的（类似低等离子体功率），以保有含硅氮与氢层的结构，故在进一步处理开始的同时可预测层性质。含硅前驱物与含氧前驱物可各字流入腔室一段时间，该段时间足以沉积厚度为约10nm或更大、约20nm或更大、约50nm或更大、或者约100nm或更大的氧化硅覆盖层。
在示范性方法100或200任一者完成后，层堆迭准备受到固化或退火。固化阶段可涉及将氧化硅覆盖层与无碳的含硅氮与氢层暴露至含氧的气氛。本发明的实施例中，该含氧气氛可包括臭氧。沉积基材可留在基材处理区域中以供固化，或该基材可传送到导入含氧的气氛的不同腔室。不同实施例中，基材的固化温度可为约300℃或更低，250℃或更低，约225℃或更低，或者约200℃或更低。在不同实施例中，该基材的温度可以为约室温（25℃）或更高，约50℃或更高，约100℃或更高，约125℃或更高，或约150℃或更高。根据额外揭露的实施例，任一上限可与任一下限结合以形成基材温度的额外范围。
固化操作将无碳的含硅氮与氢层修饰成含硅与氧层。该含硅与氧层可转换成氧化硅层，这是通过在含氧环境中于相对高温下退火基材而完成。当导入含氧气氛时，沉积基材可留在相同的用于固化的基材处理区域，或该基材可传送到导入含氧的气氛的不同腔室。除了其他含氧气体外，含氧气氛可包括诸如为氧气（O2）、臭氧（O3）、水蒸气（H2O）、过氧化氢（H2O2）与氮氧化物（NO、NO-2等）等一或多种含氧气体。含氧气氛也可包括自由基氧与氢氧物种，诸如原子氧（O）、氢氧化物（OH）等，该等物种可远端生成并且输送进入基材腔室。也可存在含氧物种的离子。固化与退火操作的含氧气氛提供氧，以将含硅氮与氢层转换成氧化硅（SiO2）层。基材的氧退火温度在不同实施例中可为约1100℃或更低、约1000℃或更低、约900℃或更低，或者是约800℃或更低。基材的温度在不同实施例中可为约500℃或更高，约600℃或更高、约700℃或更高，或者是约800℃或更高。再一次，根据额外揭露的实施例，任一上限可与任一下限结合以形成基材温度的额外范围。
用于沉积无碳的含硅氮与氢层及覆盖层的基材可为图案化基材且可具有多个间隙以用于基材上形成的元件部件（例如电晶体）的间隔与结构。该等间隙可具有一高度与宽度，该高度与宽度界定该高度对宽度（即H/W）的深宽比（AR），该AR远大于1:1，例如5:1或更大，6:1或更大，7:1或更大，8:1或更大，9:1或更大，10:1或更大，11:1或更大，12:1或更大等。许多范例中，高AR是由于小间隙宽度，该宽度范围为约90nm至约22nm或更小，例如低于90nm、65nm、50nm、45nm、32nm、22nm、16nm等。因为该无碳的含硅氮与氢层可流动，该层能够填充高深宽比的间隙，而不会在填充材料的中心周围建立空隙或脆弱缝线。例如，沉积可流动材料在完全填充之前，不太可能过早地阻塞间隙顶部，而在间隙中间留下空隙。
描述示范性氧化硅沉积系统期间，可引入额外的制程参数。
示范性氧化硅沉积系统
可实施本发明实施例的沉积腔室除其他类型的腔室外特别可包括高密度等离子体化学气相沉积（HDP-CVD）腔室、等离子体增强化学气相沉积（PE-CVD）腔室、次气氛压化学气相沉积（SACVD）腔室、与热化学气相沉积腔室。可实施本发明的实施例的CVD系统的特定范例包括CENTURA
Figure BDA0000457250520000101
HDP-CVD腔室/系统与
Figure BDA0000457250520000102
PECVD腔室/系统，此二者可购自美国加州Santa Clara的应用材料公司。
可与本发明的示范方法一并使用的基材处理腔室的范例可包括显示于及描述于具有共同受让人的Lubomirsky等人的美国临时专利申请案第60/803,499号中的该等腔室，该案于2006年5月30日提出申请，且发明名称为“PROCESS CHAMBER FORDIELECTRIC GAPFILL”，该案全文在此并入作为参考，以供所有目的之用。额外的示范性系统可包括显示于及描述于美国专利第6,387,207号与第6,830,624号中的该等系统，该等专利的全文亦在此并入作为参考，以供所有目的之用。
沉积系统的实施例可结合至较大的制造系统，以生产集成电路芯片。图3显示根据所揭露的实施例的一个此类沉积、烘烤及固化腔室的系统300。在该图中，一对FOUP（前开式晶圆盒）302供给基材（例如300mm直径的晶圆），在该等基材放进基材处理腔室308a-f之一者前，基材是由机械手臂304接收并且放置到低压固持区域306。第二机械手臂310可用于从低压固持区域306传输基材晶圆至基材处理腔室308a-f并且往回传输。
基材处理腔室308a-f可包括一或多个用以在基材晶圆上沉积、退火、固化及/或蚀刻可流动介电层的系统部件。在一个配置方式中，两对处理腔室（例如，308c-d及308e-f）可用于沉积可流动介电材料于基材上，而第三对处理腔室（例如，308a-b）可用于退火沉积的介电质。在另一配置方式中，相同的两对处理腔室（例如308c-d及308e-f）可经装设以在基材上沉积及退火可流动介电层，同时第三对腔室（例如308a-b）可用于UV或电子束固化沉积的层。另一配置方式中，所有三对腔室（例如308a-f）可经装设以于基材上沉积及固化可流动的介电层。尚有另一配置方式，两对处理腔室（例如308c-d及308e-f）可用于沉积及以UV固化或电子束固化可流动介电质，同时第三对腔室（例如308a-b）可用于退火介电层。所述制程的任一者或多者可在与不同实施例中所示的制造系统分开的腔室上执行。
此外，一个或更多个基材处理腔室308a-f可被装设成湿式处理腔室。该等制程腔室包括在含水分（moisture）的气氛下加热该可流动介电层。因此，系统300的实施例可包括湿式处理腔室及退火处理腔室，以在沉积的介电层上执行湿式及干式退火二者。
图4A是根据所揭露的实施例的基材处理腔室400。远端等离子体系统（RPS）410可处理气体，随后该气体行进穿过气体入口组件411。在气体入口组件411中可见两个不同的气体供给通道。第一通道412搭载穿过远端等离子体系统（RPS）410的气体，而第二通道413绕过RPS410。在揭露的实施例中，第一通道412可用于制程气体而第二通道413可用于处理气体（treatment gas）。图中图示盖（或导电的顶部部分）421以及穿孔隔件（或喷头）453之间有一绝缘环424，该绝缘环使AC电位得以相对于喷头453施加到盖421。制程气体行进穿过第一通道412进入腔室等离子体区域420，且可单独在腔室等离子体区域420中（或者与RPS410相结合）的等离子体里受到激发。在此腔室等离子体区域420及/或RPS410的结合可指远端等离子体系统。穿孔隔件（也称为喷头）453将腔室等离子体区域420分隔喷头453下方的基材处理区域470。喷头453使等离子体得以存在于腔室等离子体区域420中，以避免直接于基材处理区域470中激发气体，同时依然使激发的物种得以从腔室等离子体区域420行进至基材处理区域470。
喷头453定位在腔室等离子体区域420与基材处理区域470之间，且使等离子体流出物（前驱物或其他气体的受激发的衍生物）在腔室等离子体区域420产生，而穿过多个横穿板厚的透孔（through hole）456。喷头453亦具有一或多个中空空间451，该空间可被蒸气或气态形式的前驱物（诸如含硅前驱物）填充，并且穿过小孔洞455进入基材处理区域470但不直接进入腔室等离子体区域420。在此揭露的实施例中，喷头453比透孔456的最小直径450的长度还厚。为了维持受从腔室等离子体区域420穿透至基材处理区域470的受激发物种具显著浓度，可通过形成透孔456的较大的直径部分使该较大的直径部分穿过喷头453达某一程度（part way），而限制透孔最小直径450的长度426。在所揭露的实施例中，透孔456的最小直径450的长度可与透孔456的最小直径相同数量级，或者为较小的数量级。
在所示的实施例中，一旦制程气体受到腔室等离子体区域420中的等离子体激发，喷头453可（通过透孔456）分配制程气体，该等制程气体含有氧、氢及/或氮，及/或此类制程气体的等离子体流出物。在实施例中，通过第一通道412导入RPS410中及/或腔室等离子体区域420中的制程气体可含有氧(O2)、臭氧(O3)、N2O、NO、NO2、NH3、包括N2H4的NxHy、甲硅烷、乙硅烷、TSA及DSA的一者或多者。该制程气体亦可包括诸如氦气、氩气、氮气(N2)等之类的载气。第二通道413亦可传递制程气体及/或载气，及/或层固化气体（例如O3），该层固化气体用于从生长中的层或刚沉积的层中移除非期望的成分。等离子体流出物可包括制程气体的离子化或中性衍生物，且在此等离子体流出物亦可指自由基氧前驱物及/或自由基氮前驱物，前述二前驱物所指的是所导入的制程气体的原子的组分。
在实施例中，透孔456的数量可介于约60个至约2000个之间。透孔456可具有多种形状，但最容易做成圆形。在所揭露的实施例中，透孔456的最小直径450可介于约0.5mm至约20mm之间，或介于约1mm至约6mm之间。在选择透孔的截面形状上，亦有范围，截面可做成锥形、圆柱形或该二种形状的组合。不同实施例中，用于将气体导进处理区域470的小孔洞455数目可介于约100至约5000之间，或介于约500至约2000之间。小孔洞455的直径可介于约0.1mm至约2mm之间。
图4B是根据所揭示的实施例与处理腔室一并使用的喷头453的底视图。喷头453对应图3A中所图示的喷头。透孔456被绘成在喷头453底部处具有较大的内径(ID)，而在顶部处具有较小的ID。小孔洞455实质上在喷头表面上均匀分布，甚至分布在透孔456之间，相较于此述的其他实施例，这种分布方式助于提供更均匀的混合。
当穿过喷头453中的透孔456抵达的等离子体流出物与源自中空空间451穿过小孔洞455抵达的含硅前驱物结合时，在基材处理区域470内示范性的层建立在由底座（图中未示）支撑的基材上。虽可将基材处理区域470装配成支持等离子体以供诸如固化之类的其他制程所用，然而在生长示范性层期间无等离子体存在。
等离子体既可在喷头453上方的腔室等离子体区域420中点燃，亦可在喷头453下方的基材处理区域470点燃。等离子体存在于腔室等离子体区域420中，以从含氮与氢的气体的流入中产生自由基氮前驱物。于处理腔室的盖中形成的导电顶部部分421及喷头453之间施加一般在射频（RF）范围的AC电压，以在沉积期间于腔室等离子体区域420中点燃等离子体。RF电源供应器产生13.56MHz的高RF频率，但亦可产生单独其他频率或者与13.56MHz频率结合的频率。
当于第二固化阶段开启基材处理区域470中的底部等离子体或该底部等离子体清洁接壤基材处理区域470的内部表面时，顶部等离子体可处于低功率或无功率。通过在喷头453及底座（或腔室底部）之间施加AC电压，而点燃基材处理区域470中的等离子体。清洁气体可在等离子体存在时导入基材处理区域470。
底座可具有热交换通道，热交换流体流过该热交换通道中以控制基材温度。此配置方式使基材温度得以冷却或加热，以维持相对低的温度（从室温直到约120℃）。热交换流体可包含乙二醇与水。底座的晶圆支撑浅盘（较佳为铝、陶瓷或前述材料的组合）亦可被电阻式加热以达成相对高的温度（从约120℃直到约1100℃），此加热是通过使用嵌入式单回圈嵌入的加热器元件达成，该元件设以造成平行的同心圆形式的两个完整回转。加热器元件的外部可绕于邻接支撑浅盘的周边处，同时内部绕于具有较小半径的同心圆的路径上。至加热器元件的配线穿过底座的心柱。
基材处理系统是由系统控制器控制。在一示范性实施例中，系统控制器包括硬盘驱动器、软盘驱动器及处理器。处理器含有单板电脑(SBC)、模拟数字输入/输出板、介面板及步进马达控制板。CVD系统的各部件符合Versa Modular European(VME)标准，该标准界定电路板、介面卡插件箱(card cage)以及连结器尺寸与类型。VME标准亦界定总线结构为具有16比特数据总线或24比特地址总线。
系统控制器控制所有沉积系统的活动。系统控制器执行系统控制软件，该软件是储存在电脑可读媒体中电脑程序。该媒体较佳为硬盘，但该媒体也可以是其他种类的存储器。电脑程式包括指令集，该等指令集指示时间、气体混合、腔室压力、腔室温度、RF功率层级、基座位置及其他特殊制程参数。储存在其他存储器元件（其他存储器元件包括例如软盘或其他适合的驱动器）上的其他电脑程序亦可用于指示系统控制器。
可使用由系统控制器执行的电脑程序产品实施用于在基材上沉积层堆迭（例如依序沉积无碳的含硅氮与氢层而随后沉积氧化硅覆盖层）、将层转换成氧化硅的制程或者用于清洁腔室的制程。电脑程序代码可用任何习知电脑可读的编程语言撰写，例如68000汇编语言、C、C++、Pascal、Fortran或其他程式语言。使用习知的文本编辑器将适合的程序代码编入单一文件或多个文件，并且储存或收录于电脑可使用媒体（如电脑的存储器系统）。倘若输入的代码文本是高级语言，则编译该代码，而所得的编译代码随后与预先编译的Microsoft
Figure BDA0000457250520000141
函式库例程的目标码连结。为了执行该连结、编译的目标码，系统使用者援用该目标码，使电脑系统载入存储器中的代码。CPU随后读取并且执行该代码，以操作程序中标识的任务。
使用者与控制器之间的介面通过平板接触感应显示器。在较佳实施例中，使用两个显示器，一个安装在清洁室壁以供操作者使用，另一个在壁后以供维修技术人员使用。两个显示器可同时显示相同信息，该情况中，一次仅有一个接受输入。为了选择特殊的屏幕或功能，操作者接触该接触感应显示器的指定区域。接触区域改变该区域的强调色彩，或呈现新的选单或屏幕，以确认操作者和接触感应显示器之间的沟通。取代接触感应显示器，或者是除了接触感应显示器之外，可使用其他装置，例如键盘、滑鼠或其他指示或沟通装置，以让使用者与系统控制器沟通。
在此所使用的“基材”可为具有（或不具有）形成在上面的多个层的支撑基材。该支撑基材可为有各种掺杂浓度及掺杂轮廓的绝缘体或半导体，可例如为用在积体电路制造上的该类型的半导体基材。“氧化硅”层可包括次要浓度的其他元素组份，诸如氮、氢、碳与类似元素。在一些实施例中，氧化硅基本上由氧与硅构成。“前驱物”的用语是用于指任何参与反应从表面移除材料或沉积材料在表面上的制程气体。处于“激发态”的气体描述其中至少有一些气体分子处于振动型式的激发、解离及/或离子化的状态的气体。气体（或前驱物）可以是两种或更多种气体（或前驱物）的组合。“自由基前驱物”是用于描述参与反应从表面移除材料或沉积材料在表面上的等离子体流出物（离开等离子体、处于激发态的气体）。“自由基氮前驱物”是一种含有氮的自由基前驱物，而“自由基氢前驱物”是一种含有氢的自由基前驱物。“惰气”一词是指在蚀刻或被并入层中时不形成化学键结的任何气体。示范性的惰气包括稀有气体，但可包括其他气体，只要当（一般而言）在层中补捉到痕量的该气体时不形成化学键结即可。
全文中所用的“沟槽”（trench）的用语并非暗指经蚀刻的几何形状具有大的水平尺寸比（horizontal aspect ratio）。从表面上方所视，沟槽可显现圆形、卵形、多边形、矩形或各种其他形状。“通孔”（via）的用语用于指低深宽比沟槽，该通孔可或可不被金属填充而形成垂直的电连接。如在此所用，共形层指的是表面上与该表面形状相同的大体上均匀的材料层，即，该层的表面与受覆盖的表面大体上平行。此技术领域中具通常知识者将了解沉积的材料可能不会100%共形，而因此“大体上”一词允许可接受的容忍值。
已在此描述数个实施例，发明所属技术领域中具有通常知识者应知可使用多种修饰例、替代架构与等效例而不背离所揭露的实施例的精神。此外，说明书中不描述多种习知制程与元件，以避免不必要地混淆了本发明。故，上文中的描述不应被视为对本发明范畴的限制。
当提供一范围的数值时，除非文本中另外清楚指明，应知亦具体揭露介于该范围的上下限值之间各个区间值至下限值单位的十分之一。亦涵盖了所陈述数值或陈述范围中的区间值以及与陈述范围中任何另一陈述数值或区间值之间的每个较小范围。这些较小范围的上限值与下限值可独立地被包含或排除于该范围中，且其中在该较小范围内包含任一个极限值、包含两个极限值，或不含极限值的各范围也涵盖于本发明内，取决于在该陈述的范围中的任何特别排除的限制。在所陈述的范围包括极限值的一者或两者之处，也包括该些排除其中任一者或两者被包括的极限值的范围。
在此与如附权利要求书中所使用的单数形式“一”与“该”等用语也包括复数形式，除非文本中另外清楚指明。因此，举例而言，“一种制程”所指的制程包括多个此类制程，而“该前驱物”所指的包括一或多种前驱物以及该领域技术人士所熟知的该等材料的等效例等。
同样，申请人希望此说明书与下述申请专利范围中所用的“包括”与“包含”等用语是指存在所陈述的特征、整体、部件或步骤，但该等用语不排除存在或增加一或多种其他特征、整体、部件、步骤、动作或群组。

Claims (18)

1.一种在基材上形成介电层的方法，所述方法包括下述依序的步骤：
在含有所述基材的第一基材处理区域中，于所述基材上形成无碳的含硅氮与氢层，此步骤通过下述步骤完成：
将无激发的前驱物流进远端等离子体区域以产生自由基前驱物；
在所述第一基材处理区域中将无碳的含硅前驱物与所述自由基前驱物结合，其中在形成所述无碳的含硅氮与氢层的操作期间所述第一基材处理区域无等离子体；以及
沉积无碳的含硅氮与氢层于所述基材上，其中所述无碳的含硅氮与氢层在沉积期间可流动；以及
在所述无碳的含硅氮与氢层上形成氧化硅覆盖层，此步骤通过下述步骤完成：
将含氧前驱物流进含有所述基材的第二基材处理区域；
将含硅前驱物流进所述第二基材处理区域；
在所述第二基材处理区域中由所述含氧前驱物与所述含硅前驱物形成等离子体；以及
沉积所述氧化硅覆盖层于所述无碳的含硅氮与氢层之上。
2.如权利要求1所述的方法，其特征在于，在形成所述无碳的含硅氮与氢层期间，所述基材的温度在约25℃或大于25℃至约125℃或小于125℃之间。
3.如权利要求1所述的方法，其特征在于，进一步包含：在含氧气氛中退火所述介电层，以将所述无碳的含硅氮与氢层转换成氧化硅层。
4.如权利要求3所述的方法，其特征在于，所述退火操作发生在形成所述氧化硅覆盖层之后。
5.如权利要求3所述的方法，其特征在于，所述退火操作发生在形成所述无碳的含硅氮与氢层与形成所述氧化硅覆盖层之间。
6.如权利要求1所述的方法，其特征在于，所述基材温度在形成所述氧化硅覆盖层期间为约200℃或更低。
7.如权利要求1所述的方法，其特征在于，所述氧化硅覆盖层的厚度为约10nm或更厚。
8.如权利要求1所述的方法，其特征在于，所述无激发的前驱物包含氮，且所述自由基前驱物是自由基氮前驱物。
9.如权利要求1所述的方法，其特征在于，所述无激发的前驱物包含N2H2、NH3、N2与H2中的至少一者，且所述无碳的含硅前驱物包含H2N(SiH3)、HN(SiH3)2、或N(SiH3)3中的一者。
10.如权利要求1所述的方法，其特征在于，所述第一基材处理区域是所述第二基材处理区域。
11.如权利要求1所述的方法，其特征在于，在所述第二基材处理区域中由所述含氧前驱物与所述含硅前驱物形成等离子体的步骤包含以下步骤：施加约1000W或更低的等离子体功率。
12.一种在基材上形成介电层的方法，所述方法包括下述依序的步骤：
在含有所述基材的第一基材处理区域中，于所述基材上形成无碳的含硅氮与氢层，此步骤通过下述步骤完成：
将无激发的前驱物流进一远端等离子体区域以产生自由基前驱物；
在所述第一基材处理区域中将无碳的含硅前驱物与所述自由基前驱物结合，其中在形成所述无碳的含硅氮与氢层的操作期间所述第一基材处理区域无等离子体；以及
沉积无碳的含硅氮与氢层于所述基材上，其中所述无碳的含硅氮与氢层在沉积期间可流动；以及
处理所述无碳的含硅氮与氢层，以将所述无碳的含硅氮与氢层的一部分转换成氧化硅覆盖层，此步骤通过下述步骤完成：
将含氧前驱物流进含有所述基材的第二基材处理区域；
在所述第二基材处理区域中由所述含氧前驱物形成等离子体；以及
将所述无碳的含硅氮与氢层的一部分转换成所述氧化硅覆盖层。
13.如权利要求12所述的方法，其特征在于，在形成所述无碳的含硅氮与氢层期间，所述基材的温度在约25℃或大于25℃至约125℃或小于125℃之间。
14.如权利要求12所述的方法，其特征在于，进一步包含以下步骤：在含氧气氛中退火所述介电层，以将所述无碳的含硅氮与氢层转换成氧化硅层。
15.如权利要求14所述的方法，其特征在于，所述固化操作发生在处理所述无碳的含硅氮与氢层之后。
16.如权利要求14所述的方法，其特征在于，所述固化操作发生在形成所述无碳的含硅氮与氢层与处理所述无碳的含硅氮与氢层之间。
17.如权利要求12所述的方法，其特征在于，所述氧化硅覆盖层的厚度为约50nm或更厚。
18.如权利要求12所述的方法，其特征在于，在所述第二基材处理区域中由所述含氧前驱物与所述含硅前驱物形成等离子体的步骤包含以下步骤：施加约1000W或更低的等离子体功率。
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