CN1293265A - 利用含硝酸盐的前体淀积原子层 - Google Patents

利用含硝酸盐的前体淀积原子层 Download PDF

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CN1293265A
CN1293265A CN00125992A CN00125992A CN1293265A CN 1293265 A CN1293265 A CN 1293265A CN 00125992 A CN00125992 A CN 00125992A CN 00125992 A CN00125992 A CN 00125992A CN 1293265 A CN1293265 A CN 1293265A
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precursor
metal
nitrate
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CN1260403C (zh
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斯蒂芬·M·盖茨
德伯拉·A·纽梅尔
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Abstract

在原子层淀积工艺中使用含金属硝酸盐的前体,形成例如金属、金属氧化物和金属氮化物等含金属的膜,这些膜具有原子突变界面和优异的均一性。

Description

利用含硝酸盐的前体淀积原子层
本发明涉及含金属硝酸盐的前体化合物，这种含金属硝酸盐的前体化合物用于形成含金属的膜(元素金属，金属氧化物或金属氮化物)期间原子层的淀积(ALD)，所说含金属膜可用于许多半导体应用，例如作为半导体晶体管的栅介质，作为存储电路的电容介质，作为反应扩散阻挡层和其它类似应用。具体说，本发明使用含金属硝酸盐的化合物作为原子层淀积的前体化合物，提供具有以下优点的含金属膜：原子突变界面；精细的厚度控制(到约1单层)；优异的均一性。含金属硝酸盐的前体包括硝酸盐、氧代硝酸盐、及取代硝酸盐配合物。
金属氧化物的原子层外延(ALE)一般使例如TiCl4等金属氯化物前体与水起反应形成金属氧化层。一种这样的方法例如记载于T．Suntola & M．Simpson的“Atomic Layer Epitaxy”(Chapamn &Hall，1990，New York，New York)中。授予Ackerman的美国专利5256244中公开了一种使用金属的水解氯化物和水通过AlE淀积金属氧化物膜的方法。
这些现有技术方法具有残留的氯留在氧化物膜中，并可能形成氯化物的缺点。正如所属领域的技术人员了解的，电子器件中是不希望有氯和氯化物的。这是由于由金属氯化物前体形成的金属氧化物会由于离子Cl-的传导而稍有导电性(高漏电流)。另外，氯会从金属氧化物中扩散出来，对电子器件的其它区造成负面影响。
授予Suntola的美国专利4058430公开了一种使用与一种物质反应的单汽相元素形成膜的方法。该方法具有以下缺点：需要物理蒸发元素；某些元素具有低挥发率；在金属氧化物膜的情况下，需要氧化元素。
授予Mochizuki等人的美国专利4861417公开了一种使用例如三甲基铝或三乙基铝等烷基铝前体作通过ALE生长Ⅲ-Ⅴ族化合物半导体的源材料的方法。另一方面，授予Mochizuki等人的美国专利5166092公开了一种使用不同极性的至少含一个甲基的源化合物通过ALE生长Ⅲ-Ⅴ族化合物半导体的方法。这两种现有技术的方法的缺点在于残留碳会由于烷化铝前体的不完全分解而进入膜中。另外，由于会使金属氧化物稍有导电性，所以碳是不希望的，碳会从金属氧化物中扩散出来，对电子器件的其它区造成负面影响。
一般用于形成金属膜的另一技术是分子束外延(MBE)。MBE一般使用蒸发的金属作源材料。MBE包括一般使用金属的碳酸盐、醇盐、β-二酮盐或卤化物作源材料的气体源MBE、有机金属MBE、金属有机MBE及化学束外延。
已有记载，用不需要氧化共反应剂的无水挥发金属硝酸盐作金属氧化物膜的化学汽相淀积(CVD)的前体，见W．L．Gladfelter等人的“Anhydrous Metal Nitrates as Volatile Single Source Precursors forthe CVD of Metal Oxide Films”(Chem．Vap．Dep．1998，4，No．6，p．220)，这里引用该用文献。在CVD应用中使用金属硝酸盐前体的方法还记载于M．L．Galfelter等人的“Low Temperature CVD ofCrystalline Titanium Dioxide Film Using Tetranitratotitanium(iv)”(Chem．Vap．Dep．1998，4，No．1，p．9)和M．L．Galfelter等人的“DoesChemistry Really Matter im the Chemical Vapor Deposition ofTitanium Dioxide？Precursor and Kinetic Effects on theMicrostructure of Polycrystalline Films”(JACS，1999，121，p．5220)。这些文献都公开了可以用含金属硝酸盐的前体通过CVD形成氧化物膜，而不用氧化共反应剂。然而，这些文献中没有公开在ALD应用中通过氧化、氮化或还原共反应剂使用含硝酸盐的前体的方法。
本发明不同于上述文献，本发明中含金属硝酸盐的前体与氧化、氮化和还原共反应剂结合可以通过ALD分别生长氧化物、氮化物和金属膜。
在上述引用的文献中，金属氧化物膜通过CVD而不是氧化共反应剂生长。如这些文献中所述的，由于含金属硝酸盐的前体是强氧化和氮化剂，能够与许多化合物剧烈反应，这是必须的。此外，存在环境空气、水、光时和／或在100℃那么低的温度下，金属硝酸盐前体容易分解。金属硝酸盐的反应性容易产生与其它前体和与例如氧化、氮化和还原剂等共反应剂的汽相反应。汽相反应可导致金属硝酸盐前体和共反应剂的早期分解，可能会汽相形成颗粒，减少引入膜中的反应剂，难以再现膜的化学计量、厚度和晶片上的均一性，由于不可控的分解，造成了输送管道和CVD室的沾污。
例如，为形成氮化膜，需要将例如氨等氮化剂引入气体蒸汽。氨会汽相与金属硝酸盐前体反应，导致汽相早期分解，和很差的生长特性。
如上所述，常规CVD系统中使用金属硝酸盐具有妨碍成功的明显问题。然而，使用含金属硝酸盐的前体利用ALD技术可以避免上述困难。通过改变气体蒸汽中的反应剂，气体反应的机会减少，允许金属硝酸盐与例如氧化、氮化、还原剂等不兼容反应剂及其它含金属前体一起使用，形成利用常规CVD无法制造的多组分金属氧化物、金属氮化物及金属膜。
ALD不同于CVD，因此需要不同于CVD的前体。ALD以顺序改变前体、反应剂和清洗气体脉冲输入的周期性方式进行。ALD前体必须具有自限制效应，以便前体吸收到衬底上直到形成单层。由于自限制效应，每个操作周期只淀积一个单层或亚单层，甚至供应额外的前体时，也不会在生长层上淀积附加的前体。在CVD中，随着膜的生长，由于前体在衬底表面上的连续化学反应，前体和产物同时到达衬底。膜的均一性和再生长取决于如何保持衬底上的合适前体和反应剂流量。生长速率正比于衬底上的前体流量及衬底温度。由于不同的生长机制，ALD和CVD需要的前体不同。在ALD中，前体必须容易在键合点以自限制方式吸附到生长表面，一旦吸附后，必须容易与共反应剂反应形成希望的膜。在CVD中，前体和共反应剂必须同时在衬底表面上适当地反应，以形成希望的膜。所以，许多有用的CVD前体不能用作ALD前体，因而，选择用于ALD方法的前体并非不重要的或是显然的。
本发明的一个目的是提供一种原子层淀积(ALD)方法，该方法利用含金属硝酸盐的前体和氧化剂，淀积用作集成电路中栅介质或电容介质或反应阻挡层的金属氧化膜。
本发明再一目的是提供一种ALD方法，该方法利用含金属硝酸盐的前体和还原剂，淀积用作例如用于高速微处理器中的铜互联等布线互联结构中的布线层或导电阻挡层的高保形金属膜。
本发明又一目的是提供一种ALD方法，该方法利用含金属硝酸盐的前体和氮化剂，淀积用作例如用于高速微处理器中的铜互联等布线互联结构中的阻挡层。金属氮化物层还可以用于光半导体器件。
本发明还一目的是提供一种ALD方法，该方法利用含金属硝酸盐的前体和含金属非硝酸盐的前体(选自烷基金属、金属卤化物、金属β-二酮盐、金属醇盐、金属氢化物、甲硅烷基金属、金属酰胺)及氧化剂，淀积多组分或多层金属氧化物。
本发明再一目的是提供一种ALD方法，该方法利用含金属硝酸盐的前体和含金属非硝酸盐的前体(选自烷基金属、金属卤化物、金属β-二酮盐、金属醇盐、金属氢化物、甲硅烷基金属、金属酰胺)及还原剂，淀积多组分或多层高保形金属膜。
本发明再一目的是提供一种ALD方法，该方法利用含金属硝酸盐的前体和含金属非硝酸盐的前体(选自烷基金属、金属卤化物、金属β-二酮盐、金属醇盐、金属氢化物、甲硅烷基金属、金属酰胺)及氮化剂，淀积多组分或多层高保形金属氮化膜。
本发明再一目的是提供一种ALD方法，该方法利用含金属硝酸盐的前体形成配合多层结构，所说结构含有以任何组合形式交替的金属氧化膜、金属氮化物膜和金属膜。
本发明其它目的包括：
-提供制造晶体管结构的方法，所说晶体管结构含有利用含金属硝酸盐的前体利用ALD法淀积的氧化物栅介质。
-提供制造电容器结构的方法，所说晶体管结构含有利用含金属硝酸盐的前体利用ALD法淀积的无机电容介质。
-提供制造具有例如介质反光镜或抗反射涂层等光学应用的多层结构结构的方法，所说多层结构具有以不同组合交替的金属氧化物、金属和金属氮化物层，这些层是利用含金属硝酸盐的前体利用ALD法淀积的。
应注意，本申请中使用的术语“原子层淀积(ALD)”包括利用前体、共反应剂和清洗气体进行的原子层外延及分子束外延(MBE)、气体源MBE、有机金属MBE、和化学束外延。
由于可以产生原子突变界面和将介质厚度控制在1-10nm范围，并且精度精度为0．1nm，所以利用ALD形成的金属氧化物膜的优点在于可用作具有小特征尺寸(小于150nm)的场效应晶体管(FET)的栅介质。容易实施ALD法在直径为200和300nm的Si晶片衬底上淀积均匀膜。其它应用包括：动态随机存取存储器电路中的电容器，反应扩散阻挡层、绝缘体、去耦电容器及耐磨涂层，但不限于这些。
如上所述，用于形成金属氧化物的前述ALD法利用金属氯化物与水的反应，形成金属氧化物。这些现有技术的ALD法的缺点是残留的氯会留在膜中或形成氯氧化物。利用本发明的方法可以克服这些缺点。
本发明记载了一种使用含金属硝酸盐的前体M(NO3)x利用ALD法形成含金属膜的方法。术语“含金属的膜”包括金属氧化物、金属氮化物、元素金属或它们的任意组合或包括多层和多组分的混合物。在利用ALD形成含金属膜时，本发明的前体与共反应剂气体，例如氧化剂、还原剂或氮化剂等一起使用。在上述分子式中，M是选自Ti、Ga、Zr、Sn、Co、V、Cr、Hf、Cu、Mn、La、Y、Al、Gd、Nd、Sm、Si、Nb、Ta和In中的一种金属，x是M的化合价态。
本发明的前体还可以与含金属非硝酸盐的前体和共反应剂气体一起使用，以便利用ALD生长多组分或多层含金属的膜。
除使用所有配位体为NO3配位体的金属硝酸盐外，本发明还尝试用取代基R代替某些但不是所有NO3，其中R是氢、氧、例如N2O5或NO2等氧代硝酸盐、羟基、芳香剂、酰胺、烷基、甲硅烷基、醇盐、β-二酮或它们的混合物。在许多金属氧化物应用中，引入氮(氧氮化物)是有益的，可以得到优异的介质特性。
ALD法中使用含金属硝酸盐的前体的优点在于，反应的副产物是NOx分子，如果进入膜中并热分解，则会形成不会离子导电的氧氮化物或氮化物物质。通过用其它的配位体例如氢、氧、例如N2O5或NO2等氧代硝酸盐、羟基、芳香剂、酰胺、烷基、甲硅烷基、醇盐、β-二酮取代用于硝酸盐配位体，可以得到例如挥发性和化学热稳定性等优异的前体化学性质。通过避免使用含卤素前体，本发明解决了氯沾污问题。金属膜中的任何残留硝酸盐都可能转变成挥发的NOx或不可能导电的绝缘氧氮化物或氮化物。
所以，本发明提供一种含金属的膜的淀积方法，比起氯沾污的含金属的膜，本发明的膜会具有优异的电特性。
由于本发明可以将金属氮化物的厚度控制在1-10nm范围内，并且精确度为0．1nm，所以本发明形成的金属氮化物膜的优点在于可以用作薄膜布线互联结构中的扩散／反应阻挡层。另外，小通道(100-300nm直径)和沟槽内的ALD氮化物膜的保形性优异(几乎为100％的台阶覆盖)。
本发明的含金属硝酸盐的前体还特别适用于享有与ALD类似的层生长机制生长的层的MBE。金属氧化物的MBE一般使用金属源，结果产生非化学计量的氧化物膜。本发明通过用预氧化的、更易反应的含金属硝酸盐的前体替换低反应性的金属(常常难以氧化金属)解决了这个问题。本发明前体化合物中的硝酸盐配位体容易被含氧物质替代，或硝酸盐可以分解，并给金属膜提供氧原子。
本发明的金属氧化物一般具有约10-约100的介质常数，远大于SiO2。采用了ALD制造的金属氧化物的本发明的FET栅介质厚度比SiO2大，因此具有比具有SiO2栅介质的FET低的栅漏电流和提高的可靠性。
图1A-B是展示薄膜布线结构的剖面图，其中在形成保形地涂敷双镶嵌结构的被腐蚀结构的金属氮化物阻挡层时采用了本发明的ALD法。
如上所述，本发明提供用于包括进行前体和共反应剂的交替脉冲输入的MBE、气体源MBE、有机金属MBE、化学束外延等淀积工艺的ALD工艺中的前体化合物。具体说，本发明的前体化合物包括分子式为M(NO3)x的含金属硝酸盐的化合物，其中M是选自Ti、Ga、Zr、Sn、Co、V、Pt、Pd、Fe、Ni、Mo、W、Ag、Au、Hf、Cr、Cu、Mn、La、Y、Al、Gd、Nd、Sm、Si、Nb、Ta和In中的一种金属，x是M的化合价。
本发明的一个实施例中，某些但不是NO3全部配位体由取代基R取代，其中取代基R选自氢、氧、例如N2O5或NO2等氧代硝酸盐、羟基、芳香剂、烷基、胺、甲硅烷基、醇盐、β-二酮。这里也可以采用所说R取代基的各种组合。
本发明的金属前体化合物用于常规的ALD工艺或相关的原子淀积工艺，例如MBE，并用于代替金属氯化物前体使用。如所属领域的技术人员所了解的，ALD工艺利用至少一种反应剂(即前体)和清洗气体的交替脉冲输入形成含金属的膜。
在本发明的一个实施例中，共反应剂与金属前体化合物一起使用。在本发明的该实施例中，脉冲输入顺序可以是：
金属前体
惰性清洗
共反应剂
惰性清洗
在另一实施例中，可以使用两种以上金属前体化合物。这种情况下该物质中的脉冲输入顺序为：
第一金属前体
惰性清洗
共反应剂
惰性清洗
第二金属前体
惰性清洗
共反应剂
惰性清洗
在另一实施例中，可以使用两种以上的金属前体化合物，前提条件是至少一种金属前体是含金属硝酸盐的前体。另一金属前体可以是含金属非硝酸盐的前体。
本发明也可以采用其它脉冲输入顺序，只要反应剂分别地脉冲输入到衬底上从而在衬底上形成顺序建立的膜便可。例如，脉冲输入顺序可以是共反应剂、惰性清洗、前体和惰性清洗。
本发明中使用的共反应剂可以是一般用于ALD工艺的常规的氧化剂、氮化剂和还原剂。
合适的氧化剂包括但不限于：氧、臭氧、水、过氧化氢、氧化亚氮或任何其它氧化剂或它们的组合。
可用于本发明的合适还原剂包括：氢、形成气体或任何其它还原剂或它们的组合。
可用于本发明的合适氮化剂包括但不限于：氨、联氨、叔丁胺、异丙胺、叠氮化氢或任何其它氮化剂或它们的组合。
合适的含金属非硝酸盐的前体包括但不限于：烷基金属、金属卤化物、金属β-二酮盐、金属醇盐、金属氢化物、甲硅烷基金属、金属酰胺或其它任何含金属非硝酸盐的前体或它们的组合。
如上所述，本发明的前体化合物用于每种反应剂顺序淀积的ALD工艺。在ALD工艺中，前体和共反应剂不必象CVD工艺那样一起反应。相反，每种反应剂一般在低于CVD目前所用温度的低淀积温度下顺序脉冲输入到合适的衬底上。
在本发明中，淀积温度随所用前体化合物和共反应剂而改变，但一般低于400℃(另一方面，CVD淀积一般在500℃以上)。本发明中优选的淀积温度约为200℃-400℃。
如上所述，ALD包括前体、清洗气和共反应剂的顺序淀积。惰性气体清洗分隔开了各种反应剂脉冲输入。本发明所用的惰性气体包括使用例如He、Ar、N2或其它类似气体等惰性气体。前体、共反应剂和惰性气体的脉冲输入时间对于本发明来说不重要，但一般脉冲输入时间为0．1-约5秒，更优选0．2-约1秒。注意，前体和共反应剂的脉冲输入时间一般少于惰性气体清洗的时间。
本发明中，整个一系列脉冲输入(前体／惰性清洗／共反应剂／惰性清洗)称作一个周期。完成一个周期后，在衬底表面上淀积约0．01-约1个单层的含金属的膜。上述单层范围对应于约0．02-约1nm的膜厚。为实现希望厚度，周期可以重复任何次数。
本发明的前体化合物可以脉冲输入于其上的合适衬底包括但不限于：半导体衬底、介质、金属层、有机衬底、玻璃、金属氧化物和塑料聚合物衬底。术语“半导体衬底”包括含Si半导体衬底、绝缘体上硅衬底、锗衬底、SiGe衬底、GaAs衬底和其它类似的半导体衬底。例如Si和SiGe等的层状衬底也可用于本发明。
给出以下实例以展示可从本发明得到的某些优点，并表明本发明可以扩展到的其它领域。
实例1
该例中，在制造FET的栅介质时使用本发明的方法。具体说，该例中，使用含构图结构的Si晶片衬底。衬底的所选区域含有位于两FET之间的浅沟槽隔离(STI)氧化物，其它区域含有场氧化物，裸Si的所选区域暴露于将设置FET的区域中。
然后，将Si晶片衬底设置于用于原子层淀积的合适反应器中，例如Microchemistry制造的市售F-200反应器中，并利用本发明的方法淀积ZrO2层到厚度为1-100nm。
该例中，两种反应剂是Zr(NO3)4和H2O。衬底温度约为350℃，反应剂(前体和共反应剂)及惰性气体清洗按以下顺序脉冲输入到反应器：
1、Zr(NO3)4-0．5秒
2、惰性清洗-2秒
3、H2O-0．5秒
4、惰性清洗-2秒
上述步骤的完整系列即1-4称为一个周期。一个周期完成后，淀积了约0．1-约1个单层的ZrO2，或大致0．03nm的氧化物。该例中，所淀积的ZrO2的优选厚度为10nm，所以进行333次如上所述的气体转换周期。如所属领域的技术人员所了解的，可以淀积希望厚度的ZrO2，形成FET栅介质，并可以调整气体转换周期数，淀积希望膜厚度。
例2
该例中，在形成用作晶体管的栅介质的ZrO2和HfO2膜的双层时使用本发明的方法。具体说，用含有构图结构的Si晶片衬底。所选的衬底区含有浅沟槽隔离(STI)氧化物，其它区含有场氧化物树脂，所选的裸Si区暴露于将要设置FET的区域中。
然后，将衬底设置于Microchemistry制造的市售F-200反应器中，并利用本发明的ALD方法淀积ZrO2层到厚约0．1-约10nm。
然后，利用本发明的工艺淀积HfO2层到厚度也为约0．1-约10nm。可以重复该工艺，以淀积层状介质。
在ZrO2淀积时，衬底温度约为350℃。反应剂及惰性气体清洗按以下顺序脉冲输入到反应器：
1、Zr(NO3)4
2、惰性清洗
3、H2O
4、惰性清洗
反应剂脉冲输入(1和3)约0．5秒。惰性气体清洗脉冲输入(2-4)约2秒。该例中，所淀积ZrO2的希望厚度是5nm，所以要进行167次上述气体转换周期。
在HfO2淀积时，衬底温度约为300℃。反应剂及惰性气体清洗按以下顺序脉冲输入到反应器：
1、Hf(NO3)4
2、惰性清洗
3、H2O
4、惰性清洗
反应剂脉冲输入(1和3)约0．5秒。惰性气体清洗脉冲输入(2-4)约2秒。该例中，所淀积HfO2的希望厚度是5nm，所以要进行167次上述气体转换周期。
该例中所述的本发明方法可以扩展到包括生长由利用含硝酸盐的前体利用ALD淀积的交替金属氧化层构成的任何多层金属氧化膜。
该例中所述的本发明方法可以扩展到包括生长由利用其中至少一种金属前体是含金属硝酸盐前体的ALD淀积的交替金属氧化层构成的任何多层金属氧化膜。
例3
该例中，Si衬底设置于Microchemistry制造的市售F-200反应器中，利用本发明的工艺淀积多组分ZrHfO2层。多组分金属氧化物膜可用作晶体管的栅介质层隔离或电容器。
具体说，该例所用的两种前体是硝酸锆(Zr(NO3)4)和硝酸铪(Hf(NO3)4)，共反应剂气体是水(氧化剂)。衬底温度为约300℃，在形成多组分金属氧化物时使用以下脉冲输入顺序：
1、Hf(NO3)4
2、惰性清洗
3、H2O
4、惰性清洗
5、Zr(NO3)4
6、惰性清洗
7、H2O
8、惰性清洗
反应剂和前体脉冲输入(步骤1、3、5、7)约为0．5秒，每次惰性气体清洗脉冲输入约为2秒。该例中所淀积ZrHf氧化物的希望厚度是50nm，所以进行500次上述气体转换周期。
该例中所述的本发明方法可以扩展到包括生长由利用含硝酸盐的前体利用ALD淀积的交替金属氧化层构成的任何多组分金属氧化膜。优选多组分金属氧化物将是钙钛矿型氧化物，分子式为ABO3，其中B至少是含选自Al、Ti、Zr、Hf、V、Nb、Ta、Cr、Mo、W和Cu中的一种金属的酸性氧化物，A至少是一个具有约1-3个正电荷的附加阳离子。例子包括下述钙钛矿型氧化物：例如钛酸钡、钛酸锶、钛酸锶钡、钛酸铅、钛酸锆铅、钛酸锆酸镧铅、钛酸镧钡等钛酸系材料，例如铌酸镁铅、铌酸锂、钽酸锂、铌酸钾、和铌酸钽钾等铌酸或钽酸系材料，例如铌酸锶钡、铌酸钡铅、铌酸钛钡等钨-青铜系材料，或例如钽酸铋锶、和钛酸铋等双层钙钛矿系材料。利用本发明的ALD方法还可以形成锆酸盐、铪酸盐或例如铝酸钇、铝酸镧等铝酸盐。其它优选多组分金属氧化物包括硅酸铪、硅酸锆、包括掺杂有稀土的硅酸盐等的硅酸铝等含硅氧化物。
该例中介绍的本发明方法可扩展到包括生长由至少一种金属前体是含硝酸盐的前体的ALD淀积的交替金属氧化层构成的任何多组分金属氧化膜。
例4
该例中，在形成FET的栅介质时使用本发明的方法。该例的栅介质由所淀积的SiO2层和所淀积的金属氧化物层构成。具体说，使用含构图结构的Si晶片衬底，使用Microchemistry制造的F-200反应器，淀积SiO2层和金属氧化物层。
首先淀积SiO2层(厚约0．3-约0．5nm)，衬底保持在500℃，然后，利用本发明的工艺，在350℃的温度下淀积HfO2层，至厚约10nm。
在SiO2淀积中，Si前体是三甲基硅烷基硝酸盐(Si(CH3)3(NO3))，共反应剂是水。按以下顺序在反应器中脉冲输入不同的气体：
1、Si(CH3)3(NO3)
2、惰性清洗
3、H2O
4、惰性清洗
反应剂脉冲输入(步骤1和3)约0．5秒，惰性气体清洗脉冲输入约2秒。希望的SiO2厚度是0．2nm，所以进行7次上述气体转换周期。
在HfO2淀积中，衬底温度约300℃，前体、共反应剂和惰性清洗气体按以下顺序脉冲输入到反应器中：
1、Hf(NO3)4
2、惰性清洗
3、H2O
4、惰性清洗
步骤1和3的脉冲输入时间各自约为0．5秒，惰性气体清洗脉冲输入时间约2秒。该例中，希望的HfO2层厚度为5nm，所以在淀积该金属氧化膜时，进行167次上述气体转换周期(重复步骤1-4)。
例5
该例中，制造薄膜布线结构，使用本发明的方法淀积保形地涂敷在双镶嵌结构的被腐蚀结构的金属氮化阻挡层。图1A示出了在介质层14中腐蚀的沟槽10和通道12。介质层14下是金属薄膜布线16和布线层的介质层18。如下所述，使用本发明的工艺，所得结构示于图1B，该结构包括保形金属氮化物层20。
含有图1A所示双镶嵌结构的衬底设于ALD反应器中。该例中阻挡膜是TiN。前体是Ti(NO3)4，衬底温度为300℃。使用以下脉冲输入顺序：
1、Ti(NO3)4-0．5秒
2、惰性清洗-2秒
3、NH3-0．5秒
4、惰性清洗-2秒
在形成厚5nm的TiN层时，使用167次上述脉冲输入周期。
该例中介绍的本发明方法可以扩展到包括生长利用含硝酸盐的前体利用ALD法淀积的任何氮化膜，例如包括分别由Ta(NO3)5或W(NO3)6淀积的TaN或WN。
例6
该例中，将蓝宝石衬底设于ALD反应器(Microchemistry制造的F-200反应器)，并利用本发明的方法淀积GaN层。
该例所用前体是硝酸镓，反应剂是NH3。衬底温度为500℃，形成GaN层是使用以下脉冲输入顺序：
1、NH3-0．5秒
2、惰性清洗-2秒
3、硝酸镓-0．5秒
4、惰性清洗-2秒
该例中，希望的厚度是100nm。所以进行2000次上述气体转换周期。通过调节气体转换周期数，可以得到任何希望厚度的GaN。
例7
该例中，淀积金属膜(Cr)。把将要涂敷Cr的衬底设于Microchemistry制造的F-200反应器，并利用本发明的方法淀积Cr金属层。
衬底温度为400℃，在衬底上淀积Cr金属层时使用以下脉冲输入顺序：
1、氢-0．5秒
2、惰性清洗-2秒
3、氧代硝酸铬-0．5秒
4、惰性清洗-2秒
在形成厚度为80nm的Cr金属膜时，使用2000次上述气体转换周期。
例8
该例中，将Si衬底设于ALD反应器(Microchemistry制造的F-200反应器)，并利用本发明的方法淀积由Mn，Fe／Al2O3／Co构成的多层结构。含有多层膜的所得结构可用于磁RAM或磁隧道阻挡应用。
在第一层中，两种前体是硝酸锰和硝酸铁，还原剂是氢。衬底温度为500℃，形成多层结构时使用以下脉冲输入顺序：
1、氢-0．5秒
2、惰性清洗-2秒
3、硝酸铁-0．5秒
4、惰性清洗-2秒
5、氢-0．5秒
6、惰性清洗-2秒
7、硝酸锰-0．5秒
8、惰性清洗-2秒
希望的FeMn合金厚度是10nm，所以使用200个周期。
第二层中，前体是硝酸铝，氧化剂是水。利用以下顺序脉冲输入前体、反应剂和惰性清洗气体。
1、硝酸铝-0．5秒
2、惰性清洗-2秒
3、水-0．5秒
4、惰性清洗-2秒
在提供厚2nm的氧化铝膜时，使用20个周期。
利用硝酸钴作前体，用氢气作还原剂，形成第三层。衬底温度约500℃，在形成第三层时使用以下脉冲输入顺序：
1、硝酸钴-0．5秒
2、惰性清洗-2秒
3、氢-0．5秒
4、惰性清洗-2秒
在形成厚约100nm的Co层时，使用200次气体转换周期。
尽管结合其优选实施例具体展示和介绍了本发明，但所属领域的技术人员应理解，在不脱离本发明精神和范围的情况下，可以在形式和细节上做出各种改变。因此，并不想将本发明限制于这里所介绍和展示的精确形式和细节，而是落在所附权利要求书范围内。

Claims (53)

1、一种在衬底上形成含金属薄膜的方法，包括原子层淀积工艺，其中在容纳有所说衬底的反应器中引入含金属硝酸盐的前体。
2、根据权利要求1的方法，其中所说含金属硝酸盐的前体的分子式是M(NO3)x，其中M是选自Ti、Ga、Zr、Sn、Co、V、Pt、Pd、Fe、Ni、Mo、W、Ag、Au、Hf、Cr、Cu、Mn、La、Y、Al、Gd、Nd、Sm、Si、Nb、Ta和In中的一种金属，x是M的化合价。
3、根据权利要求2的方法，其中用取代基R代替所说含金属硝酸盐的前体的某些但非全部所说NO3配位体，所说取代基R选自氢、氧、氧代硝酸盐、羟基、芳香剂、烷基、胺、甲硅烷基、醇盐、β-二酮和它们的混合物。
4、根据权利要求1的方法，其中共反应气体与所说含金属硝酸盐的前体一起使用，所说共反应气体独立于所说含金属硝酸盐的前体引入。
5、根据权利要求4的方法，其中所说共反应气体是还原剂、氧化剂或氮化剂。
6、根据权利要求5的方法，其中所说还原剂选自氢、形成气体和它们的组合。
7、根据权利要求5的方法，其中所说氧化剂选自氧、臭氧、水、过氧化氢、氧化亚氮和它们的组合。
8、根据权利要求5的方法，其中所说氮化剂选自氨、联氨、叠氮化氢、叔丁胺、异丙胺和它们的组合。
9、根据权利要求1的方法，其中惰性气体与所说含金属硝酸盐的前体一起使用，所说惰性气体作为清洗气体独立于所说含金属硝酸盐的前体引入。
10、根据权利要求1的方法，其中所说含金属的前体形成金属氮化膜、金属氧化膜、金属膜或它们的任何组合膜、多层膜或多组分膜。
11、根据权利要求1的方法，其中一种以上含金属非硝酸盐的前体与所说含金属硝酸盐的前体一起使用，所说含金属非硝酸盐的前体独立于所说含金属硝酸盐的前体引入。
12、根据权利要求11的方法，其中所说含金属非硝酸盐的前体选自烷基金属、金属醇盐、金属卤化物、金属β-二酮盐、金属氢化物、甲硅烷基金属、金属酰胺和它们的混合物和组合。
13、一种利用原子层淀积在衬底上形成金属氧化膜的方法，包括对所说衬底进行三种或更多不同气体的交替脉冲输入的程序，其中所说气体中的一种包括含金属硝酸盐的前体，所说气体中的另一气体是惰性气体，所说气体中再一气体是氧化剂。
14、根据权利要求13的方法，其中所说含金属硝酸盐的前体的分子式是M(NO3)x，其中M是选自Ti、Ga、Zr、Sn、Co、V、Pt、Pd、Fe、Ni、Mo、W、Ag、Au、Hf、Cr、Cu、Mn、La、Y、Al、Gd、Nd、Sm、Si、Nb、Ta和In中的一种金属，x是M的化合价。
15、根据权利要求14的方法，其中用取代基R代替所说含金属硝酸盐的前体的某些但非全部所说NO3配位体，所说取代基R选自氢、氧、氧代硝酸盐、羟基、芳香剂、烷基、胺、甲硅烷基、醇盐、β-二酮和它们的组合。
16、根据权利要求13的方法，其中所说氧化剂选自氧、臭氧、水、过氧化氢、氧化亚氮和它们的组合。
17、根据权利要求13的方法，其中使用两种或更多所说含金属硝酸盐的前体。
18、一种利用原子层淀积在衬底上形成金属膜的方法，包括对所说衬底进行含金属硝酸盐的前体、清洗气体和还原气体的交替脉冲输入。
19、根据权利要求18的方法，其中所说含金属硝酸盐的前体的分子式是M(NO3)x，其中M是选自Ti、Ga、Zr、Sn、Co、V、Pt、Pd、Fe、Ni、Mo、W、Ag、Au、Hf、Cr、Cu、Mn、La、Y、Al、Gd、Nd、Sm、Si、Nb、Ta和In中的一种金属，x是M的化合价。
20、根据权利要求19的方法，其中用取代基R代替所说含金属硝酸盐的前体的某些但非全部所说NO3配位体，所说取代基R选自氢、氧、氧代硝酸盐、羟基、芳香剂、烷基、胺、甲硅烷基、醇盐、β-二酮和它们的混合物。
21、根据权利要求18的方法，其中所说还原剂选自氢、形成气体和它们的组合。
22、根据权利要求18的方法，其中使用两种或更多所说含金属硝酸盐的前体。
23、一种利用原子层淀积在衬底上形成金属氮化膜的方法，包括对所说衬底进行含金属硝酸盐的前体、清洗气体和氮化剂的交替脉冲输入。
24、根据权利要求23的方法，其中所说含金属硝酸盐的前体的分子式是M(NO3)x，其中M是选自Ti、Ga、Zr、Sn、Co、V、Pt、Pd、Fe、Ni、Mo、W、Ag、Au、Hf、Cr、Cu、Mn、La、Y、Al、Gd、Nd、Sm、Si、Nb、Ta和In中的一种金属，x是M的化合价。
25、根据权利要求24的方法，其中用取代基R代替所说含金属硝酸盐的前体的某些但非全部所说NO3配位体，所说取代基R选自氢、氧、氧代硝酸盐、羟基、芳香剂、烷基、胺、甲硅烷基、醇盐、β-二酮和它们的混合物。
26、根据权利要求23的方法，其中所说氮化剂包括氨、联氨、叠氮化氢、叔丁胺、异丙胺和它们的组合。
27、根据权利要求23的方法，其中使用两种或更多所说含金属硝酸盐的前体。
28、一种形成含金属薄膜的原子层淀积方法，至少包括向容纳有衬底的反应器内引入含金属的前体的步骤，所说含金属的前体的分子式为M(NO3)x，其中M是选自Ti、Ga、Zr、Sn、Co、V、Pt、Pd、Fe、Ni、Mo、W、Ag、Au、Hf、Cr、Cu、Mn、La、Y、Al、Gd、Nd、Sm、Si、Nb、Ta和In中的一种金属，x是M的化合价。
29、根据权利要求28的方法，其中用取代基R代替所说含金属硝酸盐的前体的某些但非全部所说NO3配位体，所说取代基R选自氢、氧、氧代硝酸盐、羟基、芳香剂、烷基、胺、甲硅烷基、醇盐、β-二酮和它们的混合物。
30、根据权利要求28的方法，其中共反应气体与所说含金属硝酸盐的前体一起使用，所说共反应气体独立于所说含金属硝酸盐的前体引入。
31、根据权利要求30的方法，其中所说共反应气体是还原剂、氧化剂或氮化剂。
32、根据权利要求31的方法，其中所说还原剂选自氢、形成气体和它们的组合。
33、根据权利要求31的方法，其中所说氧化剂选自氧、臭氧、水、过氧化氢、氧化亚氮和它们的组合。
34、根据权利要求31的方法，其中所说氮化剂选自氨、联氨、叠氮化氢、叔丁胺、异丙胺和它们的组合。
35、根据权利要求28的方法，其中惰性气体与所说含金属硝酸盐的前体一起使用，所说惰性气体独立于所说含金属硝酸盐的前体引入。
36、一种利用原子层淀积在衬底上形成多组分或多层金属氧化膜的方法，包括对所说衬底进行四种或更多不同气体的交替脉冲输入的程序，其中所说气体中的一种包括含金属硝酸盐的前体，所说气体中的另一气体是惰性气体，所说气体中再一气体是氧化剂，所说气体中的还一种是含金属非硝酸盐的前体。
37、根据权利要求36的方法，其中所说含金属硝酸盐的前体的分子式是M(NO3)x，其中M是选自Ti、Ga、Zr、Sn、Co、V、Pt、Pd、Fe、Ni、Mo、W、Ag、Au、Hf、Cr、Cu、Mn、La、Y、Al、Gd、Nd、Sm、Si、Nb、Ta和In中的一种金属，x是M的化合价。
38、根据权利要求37的方法，其中用取代基R代替所说含金属硝酸盐的前体的某些但非全部所说NO3配位体，所说取代基R选自氢、氧、氧代硝酸盐、羟基、芳香剂、烷基、胺、甲硅烷基、醇盐、β-二酮和它们的组合。
39、根据权利要求36的方法，其中所说氧化剂选自氧、臭氧、水、过氧化氢、氧化亚氮和它们的组合。
40、根据权利要求36的方法，其中使用两种或更多所说含金属硝酸盐的前体。
41、根据权利要求36的方法，其中所说含金属非硝酸盐的前体选自烷基金属、金属醇盐、金属卤化物、金属β-二酮盐、金属氢化物、甲硅烷基金属、金属酰胺和它们的混合物及组合。
42、一种利用原子层淀积在衬底上形成多组分或多层金属膜的方法，包括对所说衬底进行四种或更多不同气体的交替脉冲输入的程序，其中所说气体中的一种包括含金属硝酸盐的前体，所说气体中的另一气体是惰性气体，所说气体中再一气体是还原剂，所说气体中的还一种是含金属非硝酸盐的前体。
43、根据权利要求42的方法，其中所说含金属硝酸盐的前体的分子式是M(NO3)x，其中M是选自Ti、Ga、Zr、Sn、Co、V、Pt、Pd、Fe、Ni、Mo、W、Ag、Au、Hf、Cr、Cu、Mn、La、Y、Al、Gd、Nd、Sm、Si、Nb、Ta和In中的一种金属，x是M的化合价。
44、根据权利要求43的方法，其中用取代基R代替所说含金属硝酸盐的前体的某些但非全部所说NO3配位体，所说取代基R选自氢、氧、氧代硝酸盐、羟基、芳香剂、烷基、胺、甲硅烷基、醇盐、β-二酮和它们的组合。
45、根据权利要求42的方法，其中所说还原剂选自氢、形成气体和它们的组合。
46、根据权利要求42的方法，其中使用两种或更多所说含金属硝酸盐的前体。
47、根据权利要求42的方法，其中所说含金属非硝酸盐的前体选自烷基金属、金属醇盐、金属卤化物、金属β-二酮盐、金属氢化物、甲硅烷基金属、金属酰胺和它们的混合物及组合。
48、一种利用原子层淀积在衬底上形成多组分或多层金属氮化膜的方法，包括对所说衬底进行四种或更多不同气体的交替脉冲输入的程序，其中所说气体中的一种包括含金属硝酸盐的前体，所说气体中的另一气体是惰性气体，所说气体中再一气体是氮化剂，所说气体中的还一种是含金属非硝酸盐的前体。
49、根据权利要求48的方法，其中所说含金属硝酸盐的前体的分子式是M(NO3)x，其中M是选自Ti、Ga、Zr、Sn、Co、V、Pt、Pd、Fe、Ni、Mo、W、Ag、Au、Hf、Cr、Cu、Mn、La、Y、Al、Gd、Nd、Sm、Si、Nb、Ta和In中的一种金属，x是M的化合价。
50、根据权利要求49的方法，其中用取代基R代替所说含金属硝酸盐的前体的某些但非全部所说NO3配位体，所说取代基R选自氢、氧、氧代硝酸盐、羟基、芳香剂、烷基、胺、甲硅烷基、醇盐、β-二酮和它们的组合。
51、根据权利要求48的方法，其中所说氮化剂选自氨、联氨、叠氮化氢、叔丁胺、异丙胺和它们的组合。
52、根据权利要求48的方法，其中使用两种或更多所说含金属硝酸盐的前体。
53、根据权利要求48的方法，其中所说含金属非硝酸盐的前体选自烷基金属、金属醇盐、金属卤化物、金属β-二酮盐、金属氢化物、甲硅烷基金属、金属酰胺和它们的混合物及组合。
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