CN109642315A - 用于制造低k膜以填充表面特征的前体和可流动cvd方法 - Google Patents

用于制造低k膜以填充表面特征的前体和可流动cvd方法 Download PDF

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CN109642315A
CN109642315A CN201780053056.5A CN201780053056A CN109642315A CN 109642315 A CN109642315 A CN 109642315A CN 201780053056 A CN201780053056 A CN 201780053056A CN 109642315 A CN109642315 A CN 109642315A
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plasma
silicon
branched chain
chain
linear chain
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李建恒
R·N·弗蒂斯
R·G·里德格韦
萧满超
雷新建
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Versum Materials US LLC
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Abstract

一种用于沉积含硅膜的方法，所述方法包括：将包含至少一个表面特征的衬底放入温度为约‑20℃至约400℃的可流动CVD反应器中；向所述反应器中引入至少一种具有至少一个乙酰氧基的含硅化合物，以至少部分地使所述至少一种含硅化合物反应而形成可流动液体低聚物，其中所述可流动液体低聚物在所述衬底上形成氧化硅涂层并至少部分地填充所述至少一个表面特征的至少一部分。一旦固化，所述氧化硅涂层具有低k和优异的机械性能。

Description

用于制造低K膜以填充表面特征的前体和可流动CVD方法
相关申请的交叉引用
本申请要求于2016年8月30日提交的临时申请No.62/381,222和2017年8月18日提交的申请No.15/681,102的权益，其公开内容通过引用整体并入本文。
背景技术
本文描述的是用于制造电子器件的方法。更具体地，本文描述的是用于在沉积工艺(例如，可流动化学气相沉积)中形成含硅膜的组合物。可使用本文所述的组合物和方法沉积的示例性含硅膜包括氧化硅、氮化硅、氮氧化硅或碳掺杂氧化硅或碳掺杂氮化硅膜。
可流动氧化物沉积法通常使用烷氧基硅烷化合物作为含硅膜的前体，所述含硅膜通过受控的水解和缩合反应沉积。这样的膜可以沉积在衬底上，例如，通过向衬底上施加水和烷氧基硅烷的混合物，任选地与溶剂和/或其他添加剂(例如表面活性剂和致孔剂)一起。用于施加这些混合物的典型方法包括旋涂、浸涂、喷涂、丝网印刷、共缩合和喷墨印刷。在施加到衬底上之后并且在施加一种或多种能量源(例如，热、等离子体和/或其他能量源)时，混合物内的水可以与烷氧基硅烷反应以水解烷氧化物和/或芳氧化物基团和产生硅醇物质，其进一步与其他水解的分子缩合并形成低聚物或网络结构。
除了物理沉积或将前体施加到衬底之外，使用水和含硅蒸气源用于可流动电介质沉积(FCVD)的气相沉积工艺已经描述于，例如，美国专利No.7,541,297；8,449,942；8,629,067；8,741,788；8,481,403；8,580,697；8,685,867；7,498,273；7,074,690；7,582,555；7,888,233和7,915,131以及美国公布No.2013/0230987A1中，其公开内容通过引用并入本文。典型方法通常涉及通过在间隙中形成可流动液体膜而用固体介电材料填充衬底上的间隙。可流动膜通过使可具有Si-C键的电介质前体与氧化剂反应以形成电介质材料而形成。在某些实施方式中，电介质前体缩合并随后与氧化剂反应以形成电介质材料。在某些实施方式中，气相反应物反应以形成缩合的可流动膜。由于Si-C键对于与水的反应是相对惰性的，因此所得网络可以用有机官能团有益地官能化，所述有机官能团赋予所得膜期望的化学和物理性质。例如，向网络中添加碳可降低所得膜的介电常数。
使用可流动化学气相沉积工艺沉积氧化硅膜的另一种方法是气相聚合。例如，现有技术已经聚焦于使用诸如三甲硅烷基胺(TSA)的化合物沉积含有Si、H、N的低聚物，所述低聚物随后被用臭氧暴露氧化成SiOx膜。这样的方法的实例包括：美国公布No.2014/0073144；美国公布No.2013/230987；美国专利No.7,521,378，7,557,420和8,575,040；和美国专利No.7,825,040，其公开内容通过引用并入本文。
关于使用三甲硅烷基胺(TSA)的方法，TSA通常作为气体输送到反应室中，与氨混合，并在远程等离子体反应器中活化以产生NH2、NH、H和/或N自由基或离子。TSA与等离子体活化的氨反应并开始低聚以形成更高分子量的TSA二聚体和三聚体或含有Si、N和H的其他种类。将衬底放入反应器中并在特定室压和TSA/活化氨混合物下冷却至约0至约50℃的一个或多个温度，低聚物开始在晶片表面上以使得它们可以“流动”以填充沟槽表面特征的方式缩合。以这种方式，含有Si、N和H的材料沉积在晶片上并填充沟槽。在某些实施方式中，进行预退火步骤以使膜更像SiN。期望的是具有SiN材料，因为下一工艺步骤是使用臭氧或水、在100-700℃的一个或多个温度下的氧化。由于SiN键距和键角，已知当SiN被氧化成SiO2时，存在晶胞体积增加，这阻止膜收缩。
尽管涉及可流动化学气相沉积和其他膜沉积工艺的领域中的最近行动，但问题仍然继续存在。这些问题之一涉及膜组成。例如，在气相聚合工艺中由前体三甲硅烷基胺(TSA)沉积的可流动氧化物膜产生具有高密度的Si-H键和在稀HF溶液中具有比高质量热氧化物快2.2至2.5倍的湿蚀刻速率的膜。这样的膜不适合于低k膜应用。
在许多情况下，可以对可流动膜应用硬化过程，包括热退火、UV固化或离子/自由基致密化。硬化过程可以从沉积的材料中除去碳基团、羟基基团和较小分子量的物质。现在参考图1，这经常在硬化材料中留下空洞、裂缝或空间。这样的膜也不适合于低k膜应用。
因此，需要提供替代性前体化合物以通过流动CVD技术生产具有机械完整性和孔隙率以成功地起到低k含氧化硅的膜材料的功能的含硅膜。
发明内容
本文所述的组合物或制剂和使用该组合物或制剂的方法通过在至少一部分衬底表面上沉积含硅膜而克服现有技术的问题，其在沉积后处理后提供期望的膜性质。本发明可提供含硅膜，其具有：i)按照杨氏模量为约2至约15GPa，约4至约12GPa和在一些情况下约6至约10GPa的机械完整性，ii)约10至约30体积％，约12至约25体积％和在一些情况下约16至约22体积％的孔隙率(例如，如通过椭偏孔隙率测定法所测量的)，和iii)约2.2至约3.0，约2.4至约2.8和在一些情况下约2.5至2.7的介电常数。
在一个方面，本文描述的发明提供了一种用于沉积含硅膜的方法，所述方法包括：将包含至少一个表面特征的衬底放入温度为约-20℃至约400℃的反应器中；向所述反应器中引入至少一种具有至少一个乙酰氧基的含硅化合物，其中所述至少一种含硅化合物选自：
I(a)式(RCOO)mR1 nSiHp的酰氧基硅烷，其中R选自氢、直链或支链C1-C6烷基；R1选自直链或支链C1-C6烷基、直链或支链C2-C6烯基、直链或支链C2-C6炔基；m＝2或3；n＝1或2；p＝0或1；并且m+n+p＝4；
I(b)式(RCOO)m(R2O)nSiHpR1 q的酰氧基烷氧基硅烷，其中R选自氢、直链或支链C1-C6烷基；R1选自直链或支链C1-C6烷基、直链或支链C2-C6烯基、直链或支链C2-C6炔基；R2选自直链或支链C1-C6烷基；m＝2或3；m＝1或2；p＝0或1；q＝0或1，并且m+n+p+q＝4；和
I(c)式(RCOO)m(R3R4NO)nSiHpR1 q的酰氧基氨氧基硅烷，其中R选自氢、直链或支链C1-C6烷基；R1选自直链或支链C1-C6烷基、直链或支链C2-C6烯基、直链或支链C2-C6炔基；和R3选自氢、直链或支链C1-C10烷基；R4选自直链或支链C1-C6烷基；m＝2或3；n＝1或2；p＝0或1；q＝0或1，并且m+n+p+q＝4；和
向所述反应器中提供等离子体以至少部分地使所述至少一种含硅化合物反应而形成可流动液体低聚物，其中所述可流动液体低聚物在所述衬底上形成涂层并至少部分地填充所述至少一个表面特征的至少一部分。
另一方面，本发明的方法还包括在约100℃至约1000℃的一个或多个温度下对所述涂层进行热处理以使至少一部分所述涂层致密化并形成硬化层的步骤。
在又一方面，本发明的方法还包括将所述硬化层暴露于选自等离子体、红外光、化学处理、电子束或紫外光的能量以形成最终含硅膜的步骤。
本发明的另一方面涉及前体组合物，其包含至少一种具有至少一个乙酰氧基的含硅化合物，其中所述至少一种含硅化合物选自：
I(a)式(RCOO)mR1 nSiHp的酰氧基硅烷，其中R选自氢、直链或支链C1-C6烷基；R1选自直链或支链C1-C6烷基、直链或支链C2-C6烯基、直链或支链C2-C6炔基；m＝2或3；n＝1或2；p＝0或1；并且m+n+p＝4；
I(b)式(RCOO)m(R2O)nSiHpR1 q的酰氧基烷氧基硅烷，其中R选自氢、直链或支链C1-C6烷基；R1选自直链或支链C1-C6烷基、直链或支链C2-C6烯基、直链或支链C2-C6炔基；R2选自直链或支链C1-C6烷基；m＝2或3；m＝1或2；p＝0或1；q＝0或1，并且m+n+p+q＝4；和
I(c)式(RCOO)m(R3R4NO)nSiHpR1 q的酰氧基氨氧基硅烷，其中R选自氢、直链或支链C1-C6烷基；R1选自直链或支链C1-C6烷基，直链或支链C2-C6烯基、直链或支链C2-C6炔基；R3选自氢、直链或支链C1-C10烷基；R4选自直链或支链C1-C6烷基；m＝2或3；n＝1或2；p＝0或1；q＝0或1，并且m+n+p+q＝4。
本发明的另一方面涉及通过本发明的方法和组合物获得的膜。
本发明的其他特征和优点将通过以下对优选实施方式更详细的描述并结合通过示例的方式说明本发明的原理的附图而变得显而易见。
本发明的实施方式和特征可以单独或彼此组合使用。
附图说明
本发明将在下文中结合附图加以描述，其中相同的数字表示相同的元件：
图1是SEM显微照片，显示在衬底的沟槽中形成的现有技术的氧化硅膜，其中在硬化过程中形成空洞；
图2是SEM显微照片，显示根据本发明的方法通过二乙酰氧基二甲基硅烷与O2的沉积形成的氧化硅膜。
图3是SEM显微照片，显示根据本发明的方法在300℃下热退火5分钟后图2的氧化硅膜；和
图4是SEM显微照片，显示根据本发明的方法在400℃下UV暴露10分钟后图3的氧化硅膜。
具体实施方式
以下详细描述仅提供了优选示例性实施方式，且不旨在限制本发明的范围、适用性或配置。以下对优选示例性实施方式的详细描述而是将为本领域技术人员提供使得能够实施本发明的优选示例性实施方式的描述。在不脱离如所附权利要求中阐述的本发明的精神和范围的情况下，可以对元件的功能和布置作出各种改变。
在权利要求中，字母可用于识别要求保护的方法步骤(例如，a，b和c)。这些字母用于帮助指称方法步骤，并不旨在表示执行要求保护的步骤的顺序，除非且仅达到在权利要求中具体记载这样的顺序的程度。
本文所述的组合物或制剂和使用该组合物或制剂的方法通过在至少一部分衬底表面上沉积含硅膜而克服现有技术的问题，所述含硅膜在沉积后处理后提供期望的膜性质。
本发明涉及半导体薄膜工艺技术。描述了用于改善在各种器件结构上形态适应的介电膜的质量的方法和系统。更具体地，本发明的实施方式提供了形成具有增加的密度的氧化硅膜，以对于具有高纵横比的沟槽实现无空洞的间隙填充的方法和系统。例如，本发明尤其适用于形成用于填充窄STI沟槽的高质量氧化硅膜。
因此，在一个方面，本发明提供了一种用于沉积含硅膜的方法，所述方法包括：将包含至少一个表面特征的衬底放入温度为约-20℃至约400℃的反应器中；向所述反应器中引入至少一种具有至少一个乙酰氧基的含硅化合物，其中所述至少一种含硅化合物选自：
I(a)式(RCOO)mR1 nSiHp的酰氧基硅烷，其中R选自氢、直链或支链C1-C6烷基；R1选自直链或支链C1-C6烷基、直链或支链C2-C6烯基、直链或支链C2-C6炔基；m＝2或3；n＝1或2；p＝0或1；并且m+n+p＝4；
I(b)式(RCOO)m(R2O)nSiHpR1 q的酰氧基烷氧基硅烷，其中R选自氢、直链或支链C1-C6烷基；R1选自直链或支链C1-C6烷基、直链或支链C2-C6烯基、直链或支链C2-C6炔基；R2选自直链或支链C1-C6烷基；m＝2或3；m＝1或2；p＝0或1；q＝0或1，并且m+n+p+q＝4；和
I(c)式(RCOO)m(R3R4NO)nSiHpR1 q的酰氧基氨氧基硅烷，其中R选自氢、直链或支链C1-C6烷基；R1选自直链或支链C1-C6烷基、直链或支链C2-C6烯基、直链或支链C2-C6炔基；R3选自氢、直链或支链C1-C10烷基；R4选自直链或支链C1-C6烷基；m＝2或3；n＝1或2；p＝0或1；q＝0或1，并且m+n+p+q＝4；和
向所述反应器中提供等离子体以至少部分地使所述至少一种含硅化合物反应而形成可流动液体低聚物，其中所述可流动液体低聚物在所述衬底上形成涂层并至少部分地填充所述至少一个表面特征的至少一部分。
“可流动液体低聚物”是指在沉积条件下可流动的聚硅氧烷材料，其中该聚硅氧烷通过FTIR测量。固化后，可流动液体低聚物形成固体碳掺杂多孔OSG。
含硅膜选自氮化硅、碳化硅、氧化硅、碳掺杂氮化硅、氮氧化硅和碳掺杂氮氧化硅膜。组合物可以是预混合组合物、预混合物(在用于沉积过程之前混合)或原位混合物(在沉积过程中混合)。因此，在本公开中，术语“混合物”、“制剂”和“组合物”是可互换的。
在整个说明书中，如本文所用的术语“氧化硅”是指包含硅和氧的膜，其选自化学计量或非化学计量的氧化硅、碳掺杂氧化硅、碳氧氮化硅及其混合物。
在本发明的方法中，通常第一步是将包含至少一个表面特征的衬底放入温度为约-20℃至约400℃反应器中。合适的衬底包括但不限于半导体材料，例如砷化镓(“GaAs”)、氮化硼(“BN”)硅，以及含硅的组合物，例如晶体硅、多晶硅、非晶硅、外延硅、二氧化硅(“SiO2”)、碳化硅(“SiC”)、碳氧化硅(“SiOC”)、氮化硅(“SiN”)、碳氮化硅(“SiCN”)、有机硅酸盐玻璃(“OSG”)、有机氟硅酸盐玻璃(“OFSG”)、氟硅酸盐玻璃(“FSG”)和其他合适的衬底或其混合物。衬底可以进一步包含膜施加于其上的各种层，例如抗反射涂层、光致抗蚀剂、有机聚合物、多孔有机和无机材料、金属如铜和铝或扩散屏障层，例如TiN、Ti(C)N、TaN、Ta(C)N、Ta、W、WN、TiSiN、TaSiN、SiCN、TiSiCN、TaSiCN或W(C)N。本发明的有机硅酸盐玻璃膜优选能够充分粘附到至少一种前述材料以通过常规拉伸试验，例如ASTM D3359-95a条带拉伸试验。
在一些实施方式中，衬底可以是单晶硅晶片、碳化硅晶片、氧化铝(蓝宝石)晶片、玻璃片、金属箔、有机聚合物膜或者可以是聚合物、玻璃、硅或金属三维制品。衬底可以涂布有本领域公知的各种材料，包括氧化硅、氮化硅、无定形碳、碳氧化硅、氮氧化硅、碳化硅、砷化镓、氮化镓等等的膜。这些涂层可以完全覆盖衬底，可以是各种材料的多个层，并且可以被部分地蚀刻以暴露下方的材料层。表面上还可以具有光致抗蚀剂材料，所述光致抗蚀剂材料已经用图案暴露并显影以部分地覆盖衬底。
在一些实施方式中，衬底包含表面特征。如本文所用，术语“表面特征”是指衬底或部分制造的衬底，其包含以下中的一个或多个：孔、沟槽、浅沟槽隔离(STI)、通孔、凹角(reentrant)特征等等。在一个特定实施方式中，表面特征具有100μm或更小，1μm宽或更小，或0.5μm宽或更小，或50nm宽度或更小的宽度。在这个实施方式或其他实施方式中，如果存在，表面特征的纵横比(深度与宽度的比率)为0.1:1或更大，或1:1或更大，或10:1或更大，或20:1或更大，或40:1或更大。
用于形成本文所述的膜或涂层的方法是可流动化学沉积法。用于本文公开的方法的合适沉积工艺的实例包括但不限于热化学气相沉积(CVD)或等离子体增强循环CVD(PECCVD)法。示例性可流动CVD反应器在US公布No.2014/0073144中公开；其通过引入并入本文。如本文所用，术语“可流动化学气相沉积法”是指其中衬底暴露于一种或多种挥发性前体的任何方法，所述前体在衬底表面上反应和/或分解以提供可流动的低聚含硅物质，然后在进一步处理时产生固体膜或材料。尽管本文中使用的前体，试剂和源有时可描述为“气态”，但应理解前体可以是通过直接蒸发、鼓泡或升华在有或没有惰性气体的情况下输送到反应器中的液体或固体。在某些情况下，蒸发的前体可以通过等离子体发生器。在一个实施方式中，膜使用基于等离子体(例如，远程生成或原位)的CVD法沉积。如本文所用的术语“反应器”包括但不限于反应室或沉积室。
在某些实施方式中，衬底可以暴露于一种或多种沉积前处理，例如但不限于等离子体处理、热处理、化学处理、紫外线曝光、电子束曝光及其组合，以影响一种或多种膜性质。这些沉积前处理可在选自惰性、氧化性和/或还原性的气氛下进行。
虽然本文使用的化学试剂有时可描述为“气态”，但应理解化学试剂可以作为气体直接输送到反应器，使用载气如氮气、氦气或氩气从蒸发液体或鼓泡液体作为蒸气输送，作为来自升华固体的蒸气和/或通过惰性载气输送到反应器中。
本发明的方法包括向反应器中引入具有至少一个乙酰氧基的含硅化合物(在本文中也称为“前体”)的步骤，其中至少一种第二化合物选自下式I(a)至I(c)：
I(a)式(RCOO)mR1 nSiHp的酰氧基硅烷，其中R和R1独立地选自直链或支链C1-C6烷基；m＝2或3；n＝1或2；p＝0或1；并且m+n+p＝4；
I(b)式(RCOO)m(R1O)nSiHp的酰氧基烷氧基硅烷，其中R和R1独立地选自直链或支链C1-C6烷基；m＝2或3；m＝1或2；p＝0或1；并且m+n+p＝4；和
I(c)式(RCOO)m(R2R3NO)nSiHp的酰氧基氨氧基硅烷，其中R选自直链或支链C1-C6烷基；R2选自氢、支链C1-C10烷基和C4-C10芳基；R3选自直链或支链C1-C10烷基；m＝2或3；n＝1或2；p＝0或1；并且m+n+p＝4。
在上式和整个说明书中，术语“直链烷基”表示具有1至10、3至10或1至6个碳原子的直链官能团。在上式和整个说明书中，术语“支链烷基”表示具有3至10或1至6个碳原子的直链官能团。示例性直链烷基包括但不限于甲基、乙基、丙基、丁基、戊基和己基。示例性支链烷基包括但不限于异丙基、异丁基、仲丁基、叔丁基、异戊基、叔戊基、异己基和新己基。在某些实施方式中，烷基可具有一个或多个与其连接的官能团，例如但不限于烷氧基、二烷基氨基或其组合。在其他实施方式中，烷基不具有一个或多个与其连接的官能团。烷基可以是饱和的，或者是不饱和的。
在上式和整个说明书中，术语“芳基”表示具有3至10个碳原子、5至10个碳原子或6至10个碳原子的芳族环状官能团。示例性芳基包括但不限于苯基、苄基、氯苄基、甲苯基和邻二甲苯基。
在上式和整个说明书中，术语“烯基”表示具有一个或多个碳-碳双键并具有2至12、2至10或2至6个碳原子的基团。示例性烯基包括但不限于乙烯基或烯丙基。
术语“炔基”表示具有一个或多个碳-碳三键并具有2至10或2至6个碳原子的基团。示例性炔基包括但不限于乙炔基。
在某些实施方式中，式中的一个或多个烷基或芳基可以是“取代的”或具有代替例如氢原子的取代的一个或多个原子或原子团。示例性取代基包括但不限于氧、硫、卤素原子(例如，F、Cl、I或Br)、氮、烷基和磷。在其他实施方式中，式中的一个或多个烷基、烯基、炔基、芳族基团和/或芳基可以是未取代的。
在某些实施方式中，上述式中的取代基R1、R2和R3中的任何一个或多个可以与上式中的C-C键连接，以在它们不是氢时形成环结构。如技术人员将理解的，取代基可选自直链或支链C1-C10亚烷基部分；C2-C12亚烯基部分；C2-C12亚炔基部分；C4-C10环烷基部分；和C6-C10亚芳基部分。在这些实施方式中，环结构可以是不饱和的，例如环烷基环，或者是饱和的，例如芳环。此外，在这些实施方式中，环结构也可以被取代或不取代。在其他实施方式中，取代基R1，R2和R3中的任何一个或多个未被连接。
在其中含硅前体包含式I(a)化合物的实施方式中，前体的实例包括以下：
式I(a)化合物的实例包括二乙酰氧基二甲基硅烷、二乙酰氧基甲基硅烷、三乙酰氧基甲基硅烷、二乙酰氧基二乙烯基硅烷、二乙酰氧基甲基乙烯基硅烷、三乙酰氧基乙烯基硅烷、二乙酰氧基二乙炔基硅烷、二乙酰氧基甲基乙炔基硅烷和三乙酰氧基乙炔基硅烷。
在其中含硅前体包含式I(b)化合物的实施方式中，前体的实例包括以下：
式I(b)化合物的实例包括二乙酰氧基甲氧基甲基硅烷、二乙酰氧基二甲氧基硅烷和三乙酰氧基甲氧基硅烷。
在其中含硅前体包含式I(c)化合物的实施方式中：
式I(c)化合物的实例包括二乙酰氧基二甲基氨氧基甲基硅烷、二乙酰氧基二(甲基乙基)氨氧基甲基硅烷和二乙酰氧基二乙基氨氧基甲基硅烷。
本文所述的含硅前体化合物可以以各种方式输送至反应室，例如CVD或ALD反应器。在一个实施方式中，可以使用液体输送系统。在替代性实施方式中，可以使用组合的液体输送和闪蒸工艺单元，例如由MSP Corporation，Shoreview，MN制造的涡轮蒸发器，以使低挥发性材料能够被定量地(volumetrically)输送，这导致可重复的输送和沉积而不使前体热分解。在液体输送配置中，本文所述的前体可以以纯液体形式输送，或者可以在包含其的溶剂制剂或组合物中使用。因此，在某些实施方式中，前体制剂可以包含具有合适特性(如在给定的最终用途应用中可能期望和有利的)的溶剂组分，以在衬底上形成膜。
含硅前体化合物优选基本上不含卤离子，例如氯离子或金属离子如Al。如本文所用，术语“基本上不含”在其涉及卤离子(或卤化物)或金属离子例如氯化物、氟化物、溴化物、碘化物、Al3+离子、Fe2+、Fe3+、Ni2+、CR3+时是指每种卤离子或金属离子小于5ppm(按重量计)，优选小于3ppm，更优选小于1ppm，最优选0ppm。已知氯化物或金属离子充当硅前体的分解催化剂。最终产物中显著水平的氯化物可以导致硅前体降解。硅前体的逐渐降解可以直接影响膜沉积过程，使得半导体制造商难以满足膜规格。此外，硅前体的较高降解速率对保质期或稳定性产生负面影响，从而使得难以保证1-2年的保质期。此外，已知硅前体在分解时形成可燃和/或自燃气体，例如氢和硅烷。包含本发明前体化合物的组合物基本上不含这样的分解产物。因此，含硅前体的加速分解带来与这些可燃和/或自燃气态副产物的形成有关的安全性和性能问题。
基本上不含卤化物的根据本发明的含硅前体可以通过(1)在化学合成期间减少或消除氯化物源，和/或(2)实施有效的纯化过程以从粗产物中除去氯化物，使得最终纯化产物基本上不含氯化物而实现。氯化物源可以通过使用不含卤化物的试剂如氯代二硅烷溴代二硅烷或碘代二硅烷而在合成过程中减少，从而避免产生含有卤离子的副产物。此外，上述试剂应基本上不含氯化物杂质，使得所得粗产物基本上不含氯化物杂质。以类似的方式，合成应不使用基于卤化物的溶剂、催化剂或含有不可接受的高水平卤化物污染的溶剂。粗产物还可以通过各种纯化方法处理，以使最终产物基本上不含卤酸根，例如氯酸根。这样的方法在现有技术中充分描述，可包括但不限于纯化方法如蒸馏或吸附。蒸馏通常用于通过利用沸点差异而分离期望产物与杂质。吸附也可用于利用组分的不同吸附性质以实现分离，使得最终产物基本上不含卤化物。吸附剂例如可商购MgO-Al2O3混合物可用于除去卤化物如氯化物。
对于涉及包含本文所述的溶剂和至少一种含硅化合物的组合物的那些实施方式，所选择的溶剂或其混合物不与硅化合物反应。组合物中按重量百分比计溶剂的量为0.5重量％至99.5％或10重量％至75％。在这个实施方式或其他实施方式中，溶剂具有与式I(a)、I(b)和I(c)的前体的沸点(b.p.)相似的沸点，或者溶剂的沸点与式I(a)、I(b)和I(c)的硅前体的沸点之间的差异为40℃或更低，30℃或更低，或20℃或更低，10℃或更低，或5℃或更低。或者，沸点之间的差异的范围开始于以下端点中的任何一个或多个：0、10、20、30或40℃。沸点差异的合适范围的实例包括但不限于0℃至40℃、20℃至30℃或10℃至30℃。组合物中合适溶剂的实例包括但不限于醚(如1,4-二噁烷、二丁醚)、叔胺(如吡啶、1-甲基哌啶、1-乙基哌啶、N,N’-二甲基哌嗪、N,N,N’,N’-四甲基乙二胺)、腈(如苄腈)、烷基烃(如辛烷、壬烷、十二烷、乙基环己烷)、芳族烃(如甲苯、均三甲苯)、叔氨基醚(如双(2-二甲基氨基乙基)醚)，或其混合物。
在一个特定实施方式中，引入步骤(其中将至少一种含硅化合物引入反应器中)是在-20℃至1000℃，或约400℃至约1000℃，或约400℃至约600℃，或约-20℃至约400℃范围的一个或多个温度下进行。在这些或其他实施方式中，衬底包括包含表面特征的半导体衬底。
本发明的方法包括提供原位等离子体或远程等离子体源以至少部分地使至少一种含硅化合物反应而形成可流动液体低聚物的步骤，其中可流动液体低聚物在衬底上形成涂层，并且至少部分地填充至少一个表面特征的至少一部分。能量被施加到至少一种含硅化合物、含氮源(如果采用)、氧源、其他前体或其组合以引发反应并在衬底上形成含硅膜或涂层。这样的能量可以通过但不限于热、等离子体、脉冲等离子体、螺旋波等离子体、高密度等离子体、电感耦合等离子体、X射线、电子束、光子、远程等离子体方法及其组合提供。在某些实施方式中，次级RF射频源可用于改变衬底表面处的等离子体特性。在其中沉积涉及等离子体的实施方式中，等离子体发生工艺可以包括直接等离子体发生工艺，其中等离子体在反应器中直接产生，或者远程等离子体发生工艺，其中等离子体在反应器外部产生并被供应到反应器中。
前体与含氧或含氮源的体积流量比可为约40:1至约0.2:1，约20:1至约1:1，并且在一些情况下约6:1至约2:1。在本发明的一个实施方式中，组合物包含本发明的含硅前体和至少一种含氧或含氮源。在本发明的另一个实施方式中，组合物包含由本发明前体和至少一种含氧或含氮源获得的低聚物。
在一个特定实施方式中，等离子体选自但不限于氮等离子体；包含氮和氦的等离子体；包含氮和氩的等离子体；氨等离子体；包含氨和氦的等离子体；包含氨和氩的等离子体；氦等离子体；氩等离子体；氢等离子体；包含氢和氦的等离子体；包含氢和氩的等离子体；包含氨和氢的等离子体；有机胺等离子体；包含氧的等离子体；包含氧和氢的等离子体，及其混合物。
在另一个实施方式中，等离子体源选自但不限于碳源等离子体，包括烃等离子体、包含烃和氦的等离子体、包含烃和氩的等离子体、二氧化碳等离子体、一氧化碳等离子体、包含烃和氢的等离子体、包含烃和氮源的等离子体、包含烃和氧源的等离子体，及其混合物。
如前所述，该方法将膜沉积在包含表面特征的衬底表面的至少一部分上。将衬底放入反应器中，并将衬底保持在约-20℃至约400℃的一个或多个温度下。在一个特定实施方式中，衬底的温度低于室的壁。衬底温度保持在低于100℃的温度，优选低于25℃的温度，最优选低于10℃且高于-20℃。
在某些实施方式中，反应器在低于大气压或750托(105帕斯卡(Pa))或更低，或100托(13332Pa)或更低的压力下。在其他实施方式中，反应器的压力保持在约0.1托(13Pa)至约10托(1333Pa)的范围内。
在等离子体能量的存在下，含硅化合物彼此反应并形成低聚物，其在衬底表面上作为液体缩合(液体低聚物)并至少部分地填充衬底上的特征。然而，直接使用如此沉积的膜可以导致太多孔并且不具有足够的机械强度的电介质。因此，本发明的某些实施方式被用于对如此沉积的氧化硅层进行进一步处理，以通过增加的密度改善膜质量并仍然实现无空洞的间隙填充。“无空洞”是指通过观察沉积和固化的膜的SEM或TEM获得的视觉确定。
在优选实施方式中，可流动液体低聚物在约100℃至约1000℃的一个或多个温度下热退火以使至少一部分材料致密化，然后在100℃至1000℃的温度下进行宽带UV处理。
为了防止空洞形成，在处理期间需要交联。例如，当加热二乙酰氧基二甲基硅烷时，失去乙酸酐分子并形成Si-O-Si键。乙酸酐分子的失去导致产生纳米级孔隙。由于在每个硅原子上存在两个乙酰氧基，交联形成导致长链。为产生三维交联，需要具有三个乙酰氧基官能团的前体。在其他实施方式中，优选加入氧化剂(O2或CO2)以产生三维交联。膜密度对于氧化硅或碳掺杂氧化硅通常为1.5至2.0g/cm3，且对于氮化硅或碳掺杂氮化硅通常为1.8至2.8g/cm3。因此，这样的膜适合用于低k材料应用。实现的介电常数k对于碳掺杂氧化硅通常为2.5至2.8，或2.5至3.0。
在某些实施方式中，所得含硅膜或涂层可以暴露于沉积后处理，例如但不限于等离子体处理，包括但不限于氢等离子体、氦等离子体、氩等离子体、氨等离子体、水(H2O)等离子体、氧等离子体、臭氧(O3)等离子体、NO等离子体、N2O等离子体、一氧化碳(CO)等离子体、二氧化碳(CO2)等离子体及其组合，化学处理，紫外线暴露，红外暴露，电子束暴露和/或其它处理以影响膜的一种或多种性质。
在一些实施方式中，热处理后材料暴露于等离子体、红外光、化学处理、电子束或UV光以形成致密膜。
上述步骤定义了本文所述方法的一个循环；并且可以重复该循环直到获得含硅膜的期望厚度。在这个实施方式或其他实施方式中，应理解本文所述方法的步骤可以以各种顺序执行，可以顺序地或同时地执行(例如，在另一步骤的至少一部分期间)，及其任何组合。供应化合物和其它试剂的相应步骤可以通过改变供应它们的持续时间而进行，以改变所得含硅膜的化学计量组成。
在本发明的一个实施方式中，以下膜或特征中的至少一种可以在本发明的含硅膜上形成或沉积：i)进行平面化，ii)铜(例如，以填充通孔)，和iii)介电膜。在一个方面，本发明包括衬底，所述衬底包含具有至少一个特征(例如，通孔或沟槽)的图案化结构，本发明的膜(例如，碳掺杂氧化硅)沉积在其上和包含屏障层(例如，钴、碳氮化硅、氮化硅、碳氮氧化物、TiN和TaN中的至少一种)的膜沉积在本发明的膜上。
出于进一步说明本发明的目的提供以下实施例，但决不是旨在限制本发明。
实施例
将可流动化学气相沉积(FCVD)膜沉积到中等电阻率(8-12Ωcm)的单晶硅晶片衬底和Si图案晶片上。在某些实施例中，所得含硅膜或涂层可暴露于沉积前处理，例如但不限于等离子体处理、热处理、化学处理、紫外线暴露、红外暴露、电子束暴露和/或影响膜的一种或多种性质的其他处理。
可以使用硅烷或TEOS工艺套件在Applied Materials Precision 5000系统上的改良FCVD室上进行沉积。该室具有直接液体注射(DLI)输送能力。前体是液体，其输送温度取决于前体的沸点。
为了沉积初始可流动碳掺杂氧化物膜，典型的液体前体流速为100-5000mg/min，氧气(或者二氧化碳)流速为20-40sccm，原位等离子体功率密度为0.25-3.5W/cm2，压力为0.75-12托。为了使如此沉积的可流动膜致密化，使用改良PECVD室在100至1000℃，优选300至400℃下对膜进行热退火和/或UV真空固化。通过SCI反射计或Woollam椭圆偏振仪在632nm下测量厚度和折射率(RI)。典型的膜厚度为10至2000nm。通过Nicolet透射傅立叶变换红外光谱(FTIR)设备测量和分析硅基膜的粘合性质和氢含量(Si-H，CH和NH)。使用X射线反射率(XRR)完成所有密度测量。进行X射线光电子能谱(XPS)和二次离子质谱(SIMS)分析以确定膜的元素组成。通过使用Hitachi S-4800系统的横截面扫描电镜(SEM)在2.0nm分辨率观察图案化晶片上的流动性和间隙填充效果。通过椭偏孔隙率测定法测量膜的孔隙率。
使用实验设计(DOE)方法进行可流动CVD沉积。实验设计包括：前体流量为100至5000mg/min，优选500至2000mg/min；氧气(或CO2)流为0sccm至1000sccm，优选0至100sccm；压力为0.75至12托，优选6至10托；RF功率(13.56MHz)为50至1000W，优选100至500W；低频(LF)功率为0至100W；且沉积温度为-20至400℃，优选-20℃至40℃。DOE实验用于确定哪些工艺参数产生具有良好流动性的最佳膜。
以二乙酰氧基二甲基硅烷为前体沉积低K膜
在该实验中，用于沉积具有最有利的膜性质的可流动多孔低k膜的工艺条件如下：功率＝200W，间距＝200密耳，压力＝6至10托，温度＝30至35℃，二乙酰氧基二甲基硅烷＝1500至2000mg/min，He＝200sccm，O2＝40至60sccm。将可流动膜在300℃下热退火5分钟，然后在400℃下UV固化10分钟。
在空白衬底上获得RI为1.37和k为2.6至2.7的膜。膜的孔隙率为19至20％。加工压力为8托时，膜的模量为10.4GPa；硬度为1.84GPa。该模量和硬度与传统PECVD多孔低k膜一致。
现在参照图2，图2显示横截面SEM，表明通过二乙酰氧基二甲基硅烷与O2的沉积实现良好的间隙填充。现在参考图3，图3显示在300℃下热退火5分钟的图2的膜的横截面SEM。并在400℃下UV固化10分钟(图4)。现在参考图4。图4是SEM显示在400℃下UV暴露10分钟后的图3的氧化硅膜的显微照片。
虽然本发明的原理已在上文中结合优选实施方式描述，但应清楚理解，该描述仅通过示例的方式进行，而非作为对本发明范围的限制。

Claims (17)

1.一种用于沉积含硅膜的方法，所述方法包括：
将包含至少一个表面特征的衬底放入温度为约-20℃至约400℃的反应器中；
向所述反应器中引入至少一种具有至少一个乙酰氧基的含硅化合物，其中所述至少一种含硅化合物选自：
I(a)式(RCOO)mR1 nSiHp的酰氧基硅烷，其中R选自氢、直链或支链C1-C6烷基；R1选自直链或支链C1-C6烷基、直链或支链C2-C6烯基、直链或支链C2-C6炔基；m＝2或3；n＝1或2；p＝0或1；并且m+n+p＝4；
I(b)式(RCOO)m(R2O)nSiHpR1 q的酰氧基烷氧基硅烷，其中R选自氢、直链或支链C1-C6烷基；R1选自直链或支链C1-C6烷基、直链或支链C2-C6烯基、直链或支链C2-C6炔基；R2选自直链或支链C1-C6烷基；m＝2或3；m＝1或2；p＝0或1；q＝0或1，并且m+n+p+q＝4；和
I(c)式(RCOO)m(R3R4NO)nSiHpR1 q的酰氧基氨氧基硅烷，其中R选自氢、直链或支链C1-C6烷基；R1选自直链或支链C1-C6烷基、直链或支链C2-C6烯基、直链或支链C2-C6炔基；和R3选自氢、直链或支链C1-C10烷基；R4选自直链或支链C1-C6烷基；m＝2或3；n＝1或2；p＝0或1；q＝0或1，并且m+n+p+q＝4；和
向所述反应器中提供原位等离子体或远程等离子体源以至少部分地使所述至少一种含硅化合物反应而形成可流动液体低聚物，其中所述可流动液体低聚物在所述衬底上形成涂层并至少部分地填充所述至少一个表面特征的至少一部分。
2.根据权利要求1所述的方法，其中所述等离子体选自基于原位或远程等离子体源的包含氮的等离子体、基于原位或远程等离子体源的包含氮和氦的等离子体、基于原位或远程等离子体源的包含氮和氩的等离子体、基于原位或远程等离子体源的包含氨的等离子体、基于原位或远程等离子体源的包含氨和氦的等离子体、基于原位或远程等离子体源的包含氨和氩的等离子体、氦等离子体、氩等离子体、氢等离子体、基于原位或远程等离子体源的包含氢和氦的等离子体、基于原位或远程等离子体源的包含氢和氩的等离子体、基于原位或远程等离子体源的包含氨和氢的等离子体、基于原位或远程等离子体源的有机胺等离子体、基于原位或远程等离子体源的包含氧的等离子体、基于原位或远程等离子体源的包含氧和氢的等离子体，及其混合物。
3.根据权利要求1所述的方法，其中所述等离子体选自基于原位或远程等离子体源的包含碳或烃的等离子体、基于原位或远程等离子体源的包含烃和氦的等离子体、基于原位或远程等离子体源的包含烃和氩的等离子体、基于原位或远程等离子体源的包含二氧化碳的等离子体、基于原位或远程等离子体源的包含一氧化碳的等离子体、基于原位或远程等离子体源的包含烃和氢的等离子体、基于原位或远程等离子体源的包含烃和氮的等离子体、基于原位或远程等离子体源的包含烃和氧的等离子体，及其混合物。
4.根据权利要求1所述的方法，其还包括在约100℃至约1000℃的一个或多个温度下对所述涂层进行热处理以使至少一部分所述涂层致密化并形成硬化层的步骤。
5.根据权利要求4所述的方法，其还包括将所述硬化层暴露于选自等离子体、红外光、化学处理、电子束或紫外光的能量以形成最终的含硅膜的步骤。
6.根据权利要求5所述的方法，其中上述步骤定义了所述方法的一个循环，并且可以重复所述循环直到获得所述含硅膜的期望厚度。
7.根据权利要求1所述的方法，其中所述至少一种具有至少一个乙酰氧基的含硅化合物包括二乙酰氧基二甲基硅烷。
8.根据权利要求1所述的方法，其中所述式I(a)的酰氧基硅烷选自：
其中R选自甲基、乙基、正丙基、异丙基、叔丁基、正丁基、仲丁基和异丁基；并且R1选自甲基、乙基、乙烯基、烯丙基和乙炔基。
9.根据权利要求1所述的方法，其中所述式I(b)的酰氧基烷氧基硅烷选自：
其中R选自甲基、乙基、正丙基、异丙基、叔丁基、正丁基、仲丁基和异丁基；R1选自甲基、乙基、乙烯基、烯丙基和乙炔基；并且R2选自甲基、乙基、正丙基、异丙基、叔丁基、正丁基、仲丁基和异丁基。
10.根据权利要求1所述的方法，其中所述式I(c)的酰氧基氨氧基硅烷是：
其中R和R1独立地选自甲基、乙基、正丙基、异丙基、叔丁基、正丁基、仲丁基和异丁基；R1选自甲基、乙基、乙烯基、烯丙基和乙炔基；并且R3和R4独立地选自甲基和乙基。
11.根据权利要求1所述的方法，其中所述含硅膜通过电容-电压测量所测定的介电常数为<3.0，通过椭偏孔隙率测定法所测量的孔隙率为>10％。
12.一种含硅膜前体，其包含至少一种含硅化合物，所述含硅化合物选自：
I(a)式(RCOO)mR1 nSiHp的酰氧基硅烷，其中R选自氢、直链或支链C1-C6烷基；R1选自直链或支链C1-C6烷基、直链或支链C2-C6烯基、直链或支链C2-C6炔基；m＝2或3；n＝1或2；p＝0或1；并且m+n+p＝4；
I(b)式(RCOO)m(R2O)nSiHpR1 q的酰氧基烷氧基硅烷，其中R选自氢、直链或支链C1-C6烷基；R1选自直链或支链C1-C6烷基、直链或支链C2-C6烯基、直链或支链C2-C6炔基；R2选自直链或支链C1-C6烷基；m＝2或3；m＝1或2；p＝0或1；q＝0或1，并且m+n+p+q＝4；和
I(c)式(RCOO)m(R3R4NO)nSiHpR1 q的酰氧基氨氧基硅烷，其中R选自氢、直链或支链C1-C6烷基；R1选自直链或支链C1-C6烷基、直链或支链C2-C6烯基、直链或支链C2-C6炔基；和R3选自氢、直链或支链C1-C10烷基；R4选自直链或支链C1-C6烷基；m＝2或3；n＝1或2；p＝0或1；q＝0或1，并且m+n+p+q＝4；
其中所述含硅化合物与等离子体反应以形成所述含硅膜。
13.根据权利要求12所述的前体，其还包含至少一种溶剂。
14.根据权利要求12所述的前体，其还包含含氧源和含氮源中的至少一种。
15.根据权利要求12所述的前体，其还包含至少一种所述含硅化合物的至少一种低聚物。
16.根据权利要求14所述的前体，其包含二乙酰氧基二甲基硅烷和至少一种含氧源。
17.一种通过根据权利要求1所述的方法在具有至少一个表面特征的衬底上获得的含硅膜，所述含硅膜通过电容-电压测量所测定的介电常数为<3.0，通过椭偏孔隙率测定法所测量的孔隙率为>10体积％。
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