CN1518076A - 用于沉积含硅薄膜的前体及其方法 - Google Patents

用于沉积含硅薄膜的前体及其方法 Download PDF

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CN1518076A
CN1518076A CNA2004100029839A CN200410002983A CN1518076A CN 1518076 A CN1518076 A CN 1518076A CN A2004100029839 A CNA2004100029839 A CN A2004100029839A CN 200410002983 A CN200410002983 A CN 200410002983A CN 1518076 A CN1518076 A CN 1518076A
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diazanyl
silane
dimethyl
dimethyl diazanyl
composition
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�Ф
肖满超
���沮��
A·K·霍奇伯格
K·S·库西尔
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Air Products and Chemicals Inc
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Abstract

使用下式的肼基硅烷作为氮化硅、氧化硅和氮氧化硅在基材上的硅电介质沉积的前体的方法：[R1 2N－NH]nSi(R2)4－n其中各R1独立选自C1－C6的烷基；各R2独立选自氢，烷基，乙烯基，烯丙基，和苯基；和n＝1－4。这些肼基硅烷的一些是新型前体。

Description

用于沉积含硅薄膜的前体及其方法 相关申请的相互参照
本申请要求2003年1月23日提出的U.S.临时申请No.60/442,183的权益。
技术领域
本发明涉及用于氮化硅(silicon nitride)、氧化硅(siliconoxide)和氮氧化硅的化学蒸汽沉积的一类新型前体。尤其，本发明涉及肼基硅烷的合成及其作为低温CVD前体用于制造集成电路器件的硅电介质膜的应用。这些前体还可以用于原子层沉积，等离子体增强的化学蒸汽沉积，以及大气压化学蒸汽沉积。
背景技术
含硅介电沉积在制造集成电路上具有重要作用。氮化硅能够在半导体器件上用作扩散隔膜，用作栅极绝缘(gate insulator)，用于沟槽隔离，以及用作电容器电介质。低温CVD方法是被制造氮化硅膜的半导体工业所广泛接受的方法。
在半导体器件的制造中，化学惰性介电材料如氮化硅(Si3N4)的薄钝态层(passive layer)是必需的。氮化硅的薄层起扩散掩蔽，氧化阻隔层，具有高介电击穿电压的金属间化合介电材料和钝化层的作用。氮化物膜用作MOS器件中的侧壁隔片，以及与氧化物和氮氧化物一起可用作IV和II-V类晶体管的栅极电介质。在其它地方报道了含硅电介质在制造半导体器件中的许多其它应用，参阅Semiconductorand Process technology handbook，由Gary E.McGuire编写，Noyers Publication，New Jersey，(1988)，289-301页；和SiliconProcessing for the VLSI ERA，Wolf，Stanley，and Talbert，Richard，N.，Lattice Press，Sunset Beach，California(1990)，20-22，327-330页。
现半导体工业标准氮化硅生长方法是使用二氯硅烷和氨在＞750℃的热壁反应器中的低压化学蒸汽沉积。
氮化硅在大量硅晶片上的沉积使用许多前体来完成。使用二氯硅烷和氨的低压化学蒸汽沉积(LPCVD)需要高于750℃的沉积温度，以获得适当的生长速率和均匀性。一般使用较高的沉积温度来获得最佳膜性能。在这些方法中具有几个缺陷，这些缺陷的一些如下所示：
i)硅烷和二氯硅烷是自燃、毒性压缩气体；和
ii)二氯硅烷的膜具有污染物，如氯和氯化铵，它们作为副产物形成。
几类化学品用作氮化硅膜沉积的前体。属于它们之列的是硅烷，氯硅烷，聚硅氮烷，氨基硅烷，和叠氮基硅烷。
日本专利6-132284描述了使用具有通式(R1R2N)nSiH4-n(其中R1和R2为H-，CH3-，C2H5-，C3H7-，异-C4H9-)的有机硅烷通过在氨或氮的存在下的等离子体增强的化学蒸汽沉积法和热化学蒸汽沉积法来沉积氮化硅的方法。这里所述的前体是叔胺，且不含NH键，如在本发明的情况中那样。沉积实验在单晶片反应器(single wafer reactor)中在400℃和80-100托(Torr)的高压下进行。在这些膜中的Si∶N比率是0.9(在Si3N4膜中的Si∶N比率是0.75)，在沉积膜中含有氢。
Sorita等人，J.Electro.Chem.Soc.，Vol 141，No.12，(1994)，3505-3511页描述了使用二氯硅烷和氨用LPCVD方法沉积氮化硅的方法。在该方法中的主产物是氨基氯硅烷、氮化硅和氯化铵。氯化铵的形成是使用含Si-Cl的前体的主要缺陷。氯化铵的形成导致了颗粒形成和氯化铵在管的尾端以及管道和泵抽系统内的沉积。在前体中含有氯的方法导致了NH4Cl形成。这些方法需要常常清洗和导致了长的反应器停工时间。
B.A.Scott，J.M.Martnez-Duart，D.B.Beach，T.N.Nguyen，R.D.Estes和R.G.Schad.，Chemtronics，1989，Vol 4，230-234页报道了通过LPCVD在250-400℃的温度范围内使用硅烷和氨沉积氮化硅的方法。硅烷是自燃气体，由于部分气相反应，对于清洁的氮化硅沉积难以控制。
J.M.Grow，R.A.Levy，X.Fan和M.Bhaskaran，MaterialsLetters，23，(1995)，187-193页描述了通过LPCVD方法在600-700℃的温度范围内使用二叔丁基硅烷和氨沉积氮化硅的方法。沉积的氮化硅膜被碳杂质污染(10原子％)。这主要归因于直接Si-C键在前体中的存在。
W-C.Yeh，R.Ishihara，S.Moishita以及M.Matsumura，Japan.，J.Appl.Phys.，35，(1996)，1509-1512页描述了使用六氯二硅烷和肼在接近350℃下的硅-氮膜的低温沉积。该膜在空气中不稳定和缓慢转化为硅-氧膜。
A.K.Hoc hberg和D.L.O’Meara，Mat.Res.Soc.Symp.Proc.，Vol.204(1991)，509-514页报道了氮化硅和氮氧化硅通过使用二乙基硅烷与氨和一氧化氮通过LPCVD沉积的方法。沉积在650-750℃的温度范围内进行。该沉积限于在650℃下的沉积和沉积速率在较低的温度下降低到4/min以下。在LPCVD方法中，含有直接Si-C碳键的前体导致了在膜中的碳污染。无碳沉积需要高于5∶1的NH3：前体比率。在较低的氨浓度下，发现膜含有碳。二乙基硅烷和氨一般需要覆盖舟皿(covered boat)或温度斜线上升，以改进在整个晶片上的均匀性。
US专利5,234,869和R.G.Gordon和D.M.Hoffman，Chem.Mater.，Vol.2(1990)，482-484页公开了减少包括碳的氨基硅烷，如四(二甲基胺基)硅烷的量的其它尝试。沉积的温度是在300-1000℃的范围内，压力为1毫托至10托。存在直接Si-N键和不存在Si-C键预期使膜中的碳浓度较低。然而，这类前体具有以下三个主要缺点：
1)它们含有N-甲基，甲基往往容易迁移到硅表面和在CVD方法中膜被碳污染。为了减少碳的量，该方法使用高温(＞700)和高氨比率(＞10∶1)。在氨比率增加的情况下，沉积速度由于反应剂贫乏而急剧降低。
2)它们不含有NH键和它们不包括仲硅烷。
3)在较低的温度下，沉积速率和均匀性是非常差的(＞5％)。
U.S.专利5,874,368描述了我们先前的工作，使用双(叔丁基胺基)硅烷(“BTBAS”)将氮化物沉积温度减低到550℃以下。该温度对于在镀金属的电路和许多III-V和II-VI类器件上的沉积仍然太高。另外，该前体具有高活化能，这使该方法具有高度温度敏感性。
半导体器件微型化和低热平衡的趋势需要较低的工艺温度和较高的沉积速率。涉及典型前体如BTBAS的方法要求至少550℃的加工温度。氯硅烷需要甚至更高的温度。
氨作为氮源在氮化硅CVD中具有重要的作用。肼及其衍生物已作为硅表面氮化(nitradation)的试剂使用[6-10]，还作为氮源替换氨用来与氯硅烷反应[11-13]。
虽然几十年以前首先合成了肼基硅烷[1-2]，但在该领域中进行的研究工作非常少。近年来，一些研究者对环肼基硅烷的化学产生了兴趣[3-5]。然而，一般，那些环肼基硅烷具有高分子量和因此高沸点。对于CVD应用，高沸点或低蒸汽压是不优选的。没有公开过肼基硅烷的含硅的介电应用，尤其对于开链肼基硅烷。
肼基硅烷的不寻常的反应活性一般归因于N-N键的弱键合力和因此它被均裂的事实。
在1，1-二甲基肼(246.9kJ/mol)中的N-N键的键能比在Me3SiH中的Si-H键(377.8kJ/mol)、在s-Bu-SiMe3中的Si-C键(414kJ/mol)，和在叔丁基胺中的N-C键(362kJ/mol)的键能低得多[15]。
发明内容
本发明通过使用仅用于形成在低热条件下(在400℃以下)生长，碳污染减少以及具有低氢污染的含硅电介质膜的一组前体而已经克服了现有技术的问题。另外，该前体具有非常低的活化能，这使加工的温度敏感性降低，避免了氯污染和在如在下面更详细描述的工业分批式炉(batch furnace)或单晶片反应器中在宽压力范围内(10-5托-760托)操作。
本发明是使用下式的肼基硅烷在基材上进行氮化硅的低压化学蒸汽沉积的方法：
[R1 2N-NH]nSi(R2)4-n
其中各R1独立选自C1-C6烷基；各R2独立选自氢，烷基(C1-C6)，乙烯基，烯丙基，和苯基；和n＝1-4。
附图说明
图1是许多氮化硅前体，包括BTBAS(“双(叔丁基胺基)硅烷”)的沉积速率与温度倒数的关系曲线图。
图2是折光指数同氨与双(二甲基肼基)乙基硅烷的比率的关系曲线图。
图3A是各种氨基硅烷的沉积速率与计算能量(-110kcal/mol到-40kcal/mol)的关系曲线图。
图3B是各种氨基硅烷的沉积速率与计算能量(-300kcal/mol到300kcal/mol)的关系曲线图。
图4A是各种肼基硅烷的沉积速率与计算能量(-35kcal/mol到-5kcal/mol)的关系曲线图。
图4B是各种肼基硅烷的沉积速率与计算能量(50kcal/mol到-300kcal/mol)的关系曲线图。
图5是使用双(二甲基胺基)乙基硅烷的等离子体增强的化学蒸汽沉积的折光指数与RF功率的关系曲线图。
图6是使用双(二甲基胺基)乙基硅烷的单层沉积的Arrhenius曲线图。
在超大规模集成电路(VLSI)器件的制造中使用大量的“薄膜”。这些沉积薄膜能够是金属、半导体或绝缘体。这些薄膜可以热生长或由使用LPCVD的气相沉积。对于制造微处理器和随机存取存储器器件的各种应用，VLSI技术需要非常薄的绝缘体。二氧化硅主要用作介电材料，因为它易于沉积和具有在SiO2/Si界面的优异性能。与二氧化硅相比，氮化硅具有其它优点，这些优点的一些包括耐杂质和掺杂剂抗扩散阻隔，高介电击穿电压，优异的机械性能和Si3N4固有的惰性。氮氧化硅在某些应用中具有改进的电特性。
在VLSI制造中，需要满足一大堆的严格的化学、结构、工艺和电方面的要求。膜的纯度、厚度、均匀性和沉积速率是有利于制造器件中的亚微(submicron)特征的严格控制参数中的一些。如果沉积方法能够在低于850℃的温度下进行的话，这是器件制造和性能上的主要优点。用于在这些温度下在LPCVD条件下沉积氮化硅的硅源材料局限于硅烷和二氯硅烷。安全、可靠的低温氮化硅源材料具有在其它技术如：平板显示器件，其它电子和非电子基材或复合半导体器件制造中的应用。
本发明确定，肼基硅烷的挥发性足够作为CVD前体使用，它们能够在相对低的温度下形成含硅电介质膜。它的沉积速率显著高于氨基硅烷的沉积速率。另外，由于温度变化由肼基硅烷对氮化硅膜沉积速率的影响比氨基硅烷的小得多。该特征改进了膜均匀性，当在整个晶片上具有温度变化时。
能够使用本发明的肼基硅烷的方法包括，通过化学蒸汽沉积法(CVD)、等离子体增强的化学蒸汽沉积法(PECVD)、低压化学蒸汽沉积法(LPCVD)和原子层沉积法(ALD)沉积选自氧化硅、氮氧化硅和氮化硅中的材料的方法。
本发明包括使用用下式表示的肼基硅烷类的氮化硅，氧化硅或氮氧化硅沉积方法：
[R1 2N-NH]nSi(R2)4-n
其中各R1独立选自C1-C6的烷基；各R2独立选自氢，烷基，乙烯基，烯丙基，和苯基；和n＝1-4。
优选，各R1独立选自甲基和乙基，各R2独立选自氢，甲基，乙基，丙基，异丙基，正丁基，异丁基，叔丁基，烯丙基和苯基。
优选，肼基硅烷与选自氮、氨、肼和它们的混合物的氮源反应，以用于氮化硅沉积。
虽然对于氮化硅膜前体，许多肼基硅烷是可接受的，但下表1举例说明了设想的肼基硅烷：
                        表1
                  示例性肼基硅烷
Figure A20041000298300101
适合的肼基硅烷包括：(A)双(1，1-二甲基肼基)甲基硅烷，(B)三(1，1-二甲基肼基)硅烷，(C)三(1，1-二甲基肼基)叔丁基硅烷，(D)三(1，1-二甲基肼基)仲丁基硅烷，(E)三(1，1-二甲基肼基)乙基硅烷，(F)双(1，1-二甲基肼基)乙基硅烷，(G)双(1，1-二甲基肼基)异丙基硅烷，(H)双(1，1-二甲基肼基)烯丙基硅烷，(I)双(1，1-二甲基肼基)硅烷，(Y)四(1，1-二甲基肼基)硅烷，N，N′，N″-三(二甲基胺基)环三硅氮烷，N，N′，N″，N-四(二甲基胺基)环三硅氮烷，三(1，1-二甲基肼基)异丙基硅烷，和三(1，1-二甲基肼基)烯丙基硅烷。较低分子量肼基硅烷是优选的，非环状肼基硅烷比环状肼基硅烷优选。这些化合物通过相应氯硅烷与二烷基肼使用有机基胺，如三乙胺作为碱的反应来合成。
在半导体基材上的氮化硅膜由这些化合物在化学蒸汽沉积方法在100-800℃的温度范围和压力为10-5-760托下产生。所形成的薄膜在沟槽内的阶梯覆盖(step coverage)和晶片的厚度均匀性上是优异的。
由于分子的富氮特性，氮化硅膜能够用或不用引入氨或其它添加剂来形成。
沉积膜具有优异的均匀性，其不含氯化铵和氯污染物。肼基硅烷具有通过LPVCD于明显在二氯硅烷和氨方法的温度以下的温度沉积氮化硅的性能。
肼基硅烷的显著优点可以归因于在前体中的配体的固有性能。在这些前体的热解过程中，这些配体可以易于作为挥发性产物消除。肼基硅烷的其它优点能够总结如下：
1)它们是非自燃挥发性稳定液体或低熔点挥发性固体。
2)它们在分子中没有任何氯。在二氯硅烷中的Si-Cl键导致了氯化铵的形成，它们沉积在管的后端或单晶片反应器的壁上，需要经常清洗。
3)所得氮化硅膜是相对无碳的，如由RutherfordBackscattering Spectrometry所示。
4)肼基硅烷获得了优异的沉积均匀性。
5)当与其它可获得的前体，如具有二胺基，二甲基胺基和其它烷基胺的配体的硅烷比较时，使用这些前体的沉积温度能够减低150-300℃。
其它前体沉积温度，前体和膜性能的比较在表2中给出。
表2
前体 蒸汽压(托@℃) 沉积温度(℃) 前体和膜性能
SiH4+NH3 气体，环境温度 200-400等离子体方法 自燃气体，气相反应，在低温下富含硅，膜可能含有氢。
Cl2SiH2+NH3 气体，环境温度 ＞750 腐蚀性气体，直接Si-Cl键，氯污染，氯化铵副产物
(C2H5)2SiH2+NH3 100托，20℃ 650-725 均匀性差，直接Si-C键，直接Si-Cl键，膜中的碳杂质＞2％。可以需要笼形舟皿和温度斜线上升
(t-C4H9)2SiH2+NH3 20.5托，20℃ 600-700 直接Si-C键，膜中碳含量(10％)
[(CH3)2N]3SiR+NH3R＝H或CH3 16托，25℃ 700-1000 直接Si-C键，膜中的碳含量＞2％和需要高氨与源比率(30∶1)。＞5％的不良均匀性
(t-C4H9NH)2SiH2 7.5托，45℃ 500-1000 无Si-C键，无碳污染，良好的均匀性和高沉积速率
肼基硅烷 25托，46℃到1托，56℃ 100-800 良好的均匀性，很少或无碳，非常高的沉积速率
下表3列举了在本发明的开发过程中调查研究的化合物，包括用作SiNxOy膜的前体的合成化合物，另外只考虑用于本发明的那些化合物。
表3
为了形成氮化硅薄膜，让肼基硅烷和任选的氨(或氮或肼)在反应管中在升温(优选100-800℃，但温度能够低于或高于该范围)下反应。反应可以在表面上或非常接近晶片表面的地方发生，以沉积氮化硅薄膜。如果反应在气相(均相反应)中发生，那么形成了氮化硅簇。这种情况在硅烷和氨方法中是典型的。当反应在晶片表面上发生时，那么所得膜具有优异的均匀性。因此，CVD应用的一个重要要求是多相反应比气相反应有利的程度。
CVD方法能够分类为a)气相方法和b)表面反应方法。气相现象与气体在基材上撞击的速度有关。这通过气体穿过分离流动气体的松散区域和基材表面的边界层的速度来模拟。这种传送过程通过气相扩散来发生，它与气体的扩散率和边界层的浓度梯度成正比。当气体达到热表面时，几种表面方法可能是重要的，但表面反应一般能够通过热活化现象来模拟，它以在属于频率系数、活化能和温度的函数的速率下进行。
表面反应速率随温度的增加而增加。对于既定表面反应，温度可以升到足够高，使得反应速率超过反应物质到达表面的速率。在这种情况下，反应进行的速度至多也不能快于反应剂气体通过质量传递供给基材的速度。这被称为质量传递限制沉积方法。在低温下，表面反应速率降低，以及最后反应剂的浓度超过它们被表面反应方法消耗的速率。在这种条件下，沉积速率受反应速率限制。因此，在高温下，沉积通常受质量传递限制，而在低温下，它受表面反应速率限制。在实际的方法中，沉积条件从这些生长状态之一发展到另一种状态的温度取决于反应的活化能，以及反应器中的气体流动条件。因此，难以推断工艺条件或结果从一种压力状况或温度状况到另一种压力状况或温度状况。
在反应速度限制的条件下进行的方法中，该方法的温度是重要参数。即，在整个反应器中的均匀的沉积速率要求保持恒定反应速率的条件。这进而暗示，在所有晶片表面的各个地方必须存在恒定的温度。另一方面，在这些条件下，反应剂到达表面的速率不是重要的，因为它们的浓度不限制生长速率。因此，它不如将反应器设计成以等通量的反应剂供给晶片表面的所有部位那样重要。应该理解的是，在LPCVD反应器中，晶片能够以非常接近的间距堆叠，因为这种系统以反应速率限制的模式操作。其中的原因如下所示：在～1托的LPCVD反应器低压下，气体物质的扩散率比在大气压下增加1000倍，这仅仅部分通过边界层，即反应剂必须扩散的距离增加低于压力的平方根的事实来抵消。净效应是反应器传送到基材表面上和副产物离开基材表面的速度增加一个以上的数量级，以及速率限制步骤因此是表面反应。
低压化学蒸汽沉积方法(LPCVD)包括使其在压力为10-5托到760托下的化学反应。该化学蒸汽沉积(CVD)方法能够在既定温度、压力和反应剂比率下按以下步骤顺序描述：
1)将反应剂引入到反应室中，如果需要，快于用惰性气体稀释；
2)让反应剂扩散到基材上；
3)反应剂吸附在基材上，以及吸附的分子进行迁移；和
4)在表面上发生化学反应，以及反应的气体副产物被吸附，留下沉积薄膜。反应通过几种方法来引发；例如热或光子。在LPCVD方法中使用热能。
水平管热壁反应器最广泛用于制造VLSI的LPCVD。它们用于沉积聚硅(Poly-Si)、氮化硅，未掺杂和掺杂二氧化硅膜。广泛使用这些反应器，因为它们是经济的，具有高产量，它们的沉积膜是均匀的和它们能够容纳大直径晶片(6″-12″)。它们的主要缺点是颗粒污染和低沉积速率的倾向性。
垂直管热壁反应器现在代替水平反应器而用于200mm和200mm以上直径晶片的许多方法。几种其它类型的反应器用喷射方法使用，以避免晶片-晶片反应器消耗效应。它们不需要温度斜线上升，产生了高度均匀的沉积和据报道获得了低颗粒污染。
为了诱发反应器中的低压条件，需要适当的真空系统。适当的真空系统可以由转动叶片泵/roots鼓风机组合和各种冷阱组成。反应器压力通过电容气压计反馈到减压阀控制器来控制。我们的测量反应器载量由在标准扩散舟皿中以9mm间距排列的八十个100mm直径硅片组成。将舟皿安置在滑轨(sled)上，使得晶片中心稍高于反应管中心。这样通过补偿由舟皿和滑轨引起的电导限制而在晶片周围产生了均匀的电导。通过内置多结点热电偶(internal multi-junctionthermocouple)来测量在整个晶片装料(wafer load)上的温度均匀性。通过温度斜线上升改进了在晶片负载以下的沉积均匀性。气体和蒸汽由加料口(load door)或通过喷射器供给。
肼基硅烷是非自燃挥发性液体或低熔点挥发性固体，处理起来比硅烷和二氯硅烷更安全。该沉积方法在优选10-5托到760托下在优选100℃到800℃的温度范围内使用来自肼基硅烷和任选的氨的蒸汽来进行。任选地，能够使用惰性气体稀释剂如氮或氩来稀释和控制反应的速率。使用氨与肼基硅烷的摩尔进料比，来改变膜性能，我们使用0到超过100∶1氨与肼基硅烷。
具体实施方式
实施例1：双(1，1-二甲基肼基)甲基硅烷的合成
在装有两个添加漏斗，冷凝器和机械搅拌器的2000ml三颈圆底烧瓶中，添加500m l的己烷和303g的三乙基胺。在用冰浴冷却和氮气氛围保护的同时，以大约相等的速率通过两个添加漏斗加入115g甲基二氯硅烷在100ml己烷中的溶液和150g 1，1-二甲基肼在50ml己烷中的溶液。然后将反应混合物升至室温，并搅拌过夜。在氮气氛围下，过滤反应混合物和用己烷洗涤固体胺盐。通过真空蒸馏除去溶剂和过量胺。真空蒸馏获得了125g的双(1，1-二甲基肼基)甲基硅烷，沸点45℃/22托。
实施例2：双(1，1-二甲基肼基)乙基硅烷的合成
在装有两个添加漏斗，冷凝器和机械搅拌器的5000ml三颈圆底烧瓶中，添加1500ml的己烷和450g的三乙基胺。在用冰浴冷却和氮气氛围保护的同时，以大约相等的速率通过两个添加漏斗加入200g乙基三氯硅烷在500ml己烷中的溶液和196g 1，1-二甲基肼。然后将反应混合物升至室温，并搅拌过夜。在氮气氛围下，过滤反应混合物和用己烷洗涤固体胺盐。通过真空蒸馏除去溶剂和过量胺。真空蒸馏获得了154g的双(1，1-二甲基肼基)乙基硅烷，沸点40℃/10托。
实施例3：三(1，1-二甲基肼基)-叔丁基硅烷的合成
在装有两个添加漏斗，冷凝器和机械搅拌器的2000ml三颈圆底烧瓶中，添加800ml的己烷和125g的三乙基胺。在用冰浴冷却和氮气氛围保护的同时，以大约相等的速率通过两个添加漏斗加入48g叔丁基三氯硅烷在100ml己烷中的溶液和50g 1，1-二甲基肼在100ml己烷中的溶液。然后将反应混合物升至室温，并搅拌过夜。在氮气氛围下，过滤反应混合物和用己烷洗涤固体胺盐。通过真空蒸馏除去溶剂和过量胺。真空蒸馏获得了30g的三(1，1-二甲基肼基)叔丁基硅烷，沸点56℃/2托。1H NMR 1.19(s，9H)，2.34(s，18H)。
实施例4：三(1，1-二甲基肼基)-异丁基硅烷的合成
在装有两个添加漏斗，冷凝器和机械搅拌器的5000ml三颈圆底烧瓶中，添加1500ml的己烷和400g的三乙基胺。在用冰浴冷却和氮气氛围保护的同时，以大约相等的速率通过两个添加漏斗加入200g异丁基三氯硅烷在200ml己烷中的溶液和240g1，1-二甲基肼。然后将反应混合物升至室温，并搅拌过夜。在氮气氛围下，过滤反应混合物和用己烷洗涤固体胺盐。通过真空蒸馏除去溶剂和过量胺。真空蒸馏获得了170g的三(1，1-二甲基肼基)异丁基硅烷，沸点61℃/2托。
实施例5：三(1，1-二甲基肼基)乙基硅烷的合成
在装有两个添加漏斗，冷凝器和机械搅拌器的5000ml三颈圆底烧瓶中，添加2000ml的己烷和500g的三乙基胺。在用冰浴冷却和氮气氛围保护的同时，以大约相等的速率通过两个添加漏斗加入190g乙基三氯硅烷在100ml己烷中的溶液和290g 1，1-二甲基肼。然后将反应混合物升至室温，并搅拌过夜。在氮气氛围下，过滤反应混合物和用己烷洗涤固体胺盐。通过真空蒸馏除去溶剂和过量胺。真空蒸馏获得了153g的三(1，1-二甲基肼基)乙基硅烷，沸点51℃/2托。
实施例6：四(1，1-二甲基肼基)硅烷的合成
在装有两个添加漏斗，冷凝器和机械搅拌器的5000ml三颈圆底烧瓶中，添加2000ml的己烷和600g的1，1-二甲基肼。在用干冰浴冷却和氮气氛围保护的同时，缓慢添加170g四氯化硅在350ml己烷中的溶液。然后将反应混合物升至室温，并搅拌过夜。在氮气氛围下，过滤反应混合物和用己烷洗涤固体盐。在减压下部分除去溶剂，以及将溶液浓缩到大约1L的容积。一旦一些固体开始从溶液中沉淀出来，将溶液放入冰箱中。过滤固体产物，在真空下干燥。获得了185g的四(1，1-二甲基肼基)硅烷，熔点63℃。
实施例7：三(二甲基肼基)叔丁基硅烷和氨的LPCVD
本方法包括三(二甲基肼基)叔丁基硅烷(TDMHtBS)的热解或该前体与氨在LPCVD条件下的反应(20毫托到2托的低压范围)。经位于入口的注射器将前体和氨(或氮稀释剂)引入到加热反应器(200-800℃)。让反应剂经过晶片的上面流入到真空室中，氨(或氮)与硅源保持在1∶1到10∶1范围内的比率下。氮化硅的连续薄膜沉积在硅片的表面上。这些薄膜适合于集成电路制造。在150mm热壁LPCVD水平管反应器中进行典型试验，但装置构型不是关键的。该方法包括在石英反应器中装载75-100硅片；将该系统抽真空；让硅片达到进行沉积的所需温度。该反应所需的能量能够通过简单的电阻加热来供给。这是有利的，因为设备是廉价的，并且避免了常常与等离子体反应器相关的辐射膜损坏。
典型试验在500℃和400毫托下流出30sccm的TDMHtBS与60sccmNH3。在80件硅片上的平均沉积速率是11.5/min。膜通过红外光谱法和折光指数来表征。FT-IR光谱与由其它已知氮化物前体，例如二氯硅烷+氨沉积的氮化硅膜一致。具有在2100cm-1的Si-H伸展区域中的中等吸收谱带和在870cm-1的强Si-N伸展谱带。然而，这些膜在低温和低氨比率下有些多孔，所以在从反应器取出后具有一些氧化。这些膜的折光指数通过椭圆光度法在632.4nm下测量，折光指数由于多孔隙从＞1.7降低到大约1.6。氮化硅膜通过Rutherford Backscattering分析来表征。测定这些膜的硅、碳、氮和氧含量。在沉积之后的氮化硅的组成是大约1∶1.1硅比氮。这些膜的组成在整个膜的厚度内是均匀的。碳处于检测极限(1-2原子％)，但大多数是来自空气污染。
实施例8：三(二甲基肼基)乙基硅烷和氨的LPCV D
与实施例7相似，本方法涉及三(二甲基肼基)乙基硅烷(TDMHES)的热解或其与氨在LPCVD条件下(20毫托到2托的低压范围)的反应。典型试验在500℃和400毫托下流出30sccm的TDMHES与60sccm NH3。在80件硅片上的平均沉积速率是20/min。RBS分析显示这些膜富含硅，获取MEMS应用的低应力氮化物的先决条件。
实施例9：双(二甲基肼基)甲基硅烷和氨的LPCVD
与实施例7相似，本方法涉及双(二甲基肼基)甲基硅烷(BDMHMS)的热解或其与氨在LPCVD条件下(20毫托到2托的低压范围)的反应。典型试验在500℃和500毫托下流出70sccm的BDMHMS与120sccmN2。在80件硅片上的平均沉积速率是8.5/min。FTIR分析显示这些膜富含氮且密度低，具有在870cm-1下的Si-N伸展带。
实施例10：双(二甲基肼基)乙基硅烷和氨的LPCVD
与实施例7相似，本方法涉及双(二甲基肼基)乙基硅烷(BDMHES)的热解或其与氨在LPCVD条件下(20毫托到2托的低压范围)的反应。典型试验在500℃和400毫托下流出34sccm的BDMHES与60sccmNH3。在80件硅片上的平均沉积速率是11.5/min。RBS分析显示这些膜是氮化硅。椭圆光度法显示这些沉积物具有低到中密度，具有明显不随时间改变的折光指数1.75。在图1中示出了其它沉积速率/温度倒数关系曲线，在图中，它们与使用氨基硅烷的沉积结果比较。
实施例11：双(二甲基肼基)乙基硅烷和氨的PECVD
本方法涉及使用双(二甲基肼基)乙基硅烷(BDMHES)和氨在单晶片等离子体反应器中的等离子体增强的化学蒸汽沉积。典型试验在420℃和1000毫托下流出7sccm的BDMHES与300sccm NH3。对于2.2watt/cm2的平均RF功率，平均沉积速率是85/min和折光指数为1.92。FTIR显示，这些沉积物具有高密度与在860cm-1下的Si-N伸展带。关于在370℃和420℃的标称温度下的沉积的其它数据在图5中给出。
实施例12：双(二甲基肼基)乙基硅烷和氨的LPCVD
本方法涉及使用双(二甲基肼基)乙基硅烷(BDMHES)和氨的在单晶片反应器中的低压化学蒸汽沉积。典型试验在370℃和2000毫托下流出5.5sccm的BDMHES与11sccm NH3。对于2.2watt/cm2的平均RF功率，平均沉积速率是15/min和折光指数为1.73。FTIR显示，这些沉积物具有中到低密度与在872cm-1下的Si-N伸展带。
该化合物(“F”)在单晶片反应器中在2托和8托加工压力下的其它沉积数据在图6中给出。
已经就几个实施方案描述了本发明，然而，本发明的完全范围应该由下面的权利要求书来确定。
参考文献
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[3]Soldner，M.，Riede，J.，Schier，A.，Schmidbaour，H.，“Isomeric Cyclic Dislanediylhydrazines”，Inorg.Chem.，1998，37，601-603
[4]Mitzel，N.W.，Bissinger，P.，Riede，J.，Dreihaupl，K.，Schmidbaur，H.，“Two different cyclization modes in theformation of silylhydrazines”，Organometallics，1993，12，413-416.
[5]Mitzel，N.W.，Hofman，M.，Angermaier，K.，Schier，A.，Schleyer，P.，Schmidbaur，H.，“Cyclic silylhydrazines andtheir borane adducts”，Inorg.Chem.，1995，34，4840-4845.
[6]Seiichi Takami等人，“Monolayernitridation of siliconsurfaces by a dry chemical process using dimethylhydrazine orammonia”，Appl.Phys.Lett.，1995，66(12)，1527-1529
[7]US专利6350708(2000)
[8]US专利6204206
[9]US专利6127287
[10]US专利5939333(1999)
[11]US专利6365231
[12]US专利6146938
[13]US专利6284583
[14]US专利5976991
[15]David R.Lide，“Handbook of Chemistry and Physics”，81st Ed.，2001，CRC.

Claims (30)

1、使用下式的肼基硅烷在基材上进行氮化硅的化学蒸汽沉积的方法：
[R1 2N-NH]nSi(R2)4-n
其中各R1独立选自C1-C6的烷基；各R2独立选自氢，烷基，乙烯基，烯丙基，和苯基；和n＝1-4。
2、权利要求1的方法，其中肼基硅烷选自：双(1，1-二甲基肼基)甲基硅烷，三(1，1-二甲基肼基)硅烷，三(1，1-二甲基肼基)叔丁基硅烷，三(1，1-二甲基肼基)仲丁基硅烷，三(1，1-二甲基肼基)乙基硅烷，双(1，1-二甲基肼基)乙基硅烷，双(1，1-二甲基肼基)异丙基硅烷，双(1，1-二甲基肼基)烯丙基硅烷，双(1，1-二甲基肼基)硅烷，四(1，1-二甲基肼基)硅烷，N，N′，N″-三(二甲基胺基)环三硅氮烷，N，N′，N″，N-四(二甲基胺基)环三硅氮烷，三(1，1-二甲基肼基)异丙基硅烷，三(1，1-二甲基肼基)烯丙基硅烷和它们的混合物。
3、权利要求1的方法，其中基材的温度为大约100至800℃。
4、权利要求1的方法，其中压力为大约10-5托至760托。
5、权利要求1的方法，其中肼基硅烷与选自氮、氨、肼、胺和它们的混合物中的氮源反应。
6、权利要求5的方法，其中氨与肼基硅烷的摩尔比能够大于或等于0。
7、权利要求1的方法，其中基材是硅。
8、权利要求1的方法，其中基材是电子器件。
9、权利要求1的方法，其中基材是平板显示器。
10、权利要求1的方法，其中各R1独立选自甲基和乙基，各R2独立选自氢，甲基，乙基，丙基，异丙基，正丁基，异丁基，叔丁基，烯丙基和苯基。
11、权利要求1的方法，用于通过化学蒸汽沉积法沉积氮化硅。
12、权利要求1的方法，用于通过化学蒸汽沉积法沉积氮氧化硅。
13、权利要求1的方法，用于通过等离子体增强的化学蒸汽沉积法沉积氮化硅。
14、权利要求1的方法，用于通过等离子体增强的化学蒸汽沉积法沉积氧化硅。
15、权利要求1的方法，用于通过等离子体增强的化学蒸汽沉积法沉积氮氧化硅。
16、权利要求1的方法，用于通过原子层沉积法沉积选自氧化硅、氮氧化硅和氮化硅中的材料。
17、氮化硅在反应区中的低温化学蒸汽沉积法，包括以下步骤：
a)在所述反应区内将基材加热到大约100到800℃的温度；
b)在所述反应区内将基材保持在大约10-5托到760托压力的真空下；
c)将下式的肼基硅烷引入到所述反应区内：
[R1 2N-NH]nSi(R2)4-n
其中各R1独立选自C1-C6的烷基；各R2独立选自氢，烷基，烯丙基，和苯基；和n＝1-4；和
d)保持a)到c)的条件，足以使在基材上沉积出氮化硅的膜。
18、权利要求17的方法，其中肼基硅烷选自：双(1，1-二甲基肼基)甲基硅烷，三(1，1-二甲基肼基)硅烷，三(1，1-二甲基肼基)叔丁基硅烷，三(1，1-二甲基肼基)仲丁基硅烷，三(1，1-二甲基肼基)乙基硅烷，双(1，1-二甲基肼基)乙基硅烷，双(1，1-二甲基肼基)异丙基硅烷，双(1，1-二甲基肼基)烯丙基硅烷，双(1，1-二甲基肼基)硅烷，四(1，1-二甲基肼基)硅烷，N，N′，N″-三(二甲基胺基)环三硅氮烷，N，N′，N″，N-四(二甲基胺基)环三硅氮烷，三(1，1-二甲基肼基)异丙基硅烷，三(1，1-二甲基肼基)烯丙基硅烷和它们的混合物。
19、权利要求17的方法，其中肼基硅烷与选自氮、氨、肼和它们的混合物中的氮源反应。
20、组合物，其选自三(1，1-二甲基肼基)硅烷，三(1，1-二甲基肼基)叔丁基硅烷，三(1，1-二甲基肼基)仲丁基硅烷，三(1，1-二甲基肼基)乙基硅烷，双(1，1-二甲基肼基)异丙基硅烷，双(1，1-二甲基肼基)烯丙基硅烷，双(1，1-二甲基肼基)硅烷，四(1，1-二甲基肼基)硅烷，N，N′，N″-三(二甲基胺基)环三硅氮烷，N，N′，N″，N-四(二甲基胺基)环三硅氮烷，三(1，1-二甲基肼基)异丙基硅烷，和三(1，1-二甲基肼基)烯丙基硅烷。
21、包括三(1，1-二甲基肼基)硅烷的组合物。
22、包括三(1，1-二甲基肼基)叔丁基硅烷的组合物。
23、包括三(1，1-二甲基肼基)仲丁基硅烷的组合物。
24、包括双(1，1-二甲基肼基)异丙基硅烷的组合物。
25、包括双(1，1-二甲基肼基)烯丙基硅烷的组合物。
26、包括双(1，1-二甲基肼基)硅烷的组合物。
27、包括四(1，1-二甲基肼基)硅烷的组合物。
28、包括N，N′，N″-三(二甲基胺基)环三硅氮烷的组合物。
29、包括三(1，1-二甲基肼基)异丙基硅烷的组合物。
30、包括三(1，1-二甲基肼基)烯丙基硅烷的组合物。
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