CN1663031A - 半导体装置的制造方法 - Google Patents

半导体装置的制造方法 Download PDF

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CN1663031A
CN1663031A CN03814509XA CN03814509A CN1663031A CN 1663031 A CN1663031 A CN 1663031A CN 03814509X A CN03814509X A CN 03814509XA CN 03814509 A CN03814509 A CN 03814509A CN 1663031 A CN1663031 A CN 1663031A
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film
semiconductor device
manufacture method
metal oxide
oxide film
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CN100388438C (zh
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神力博
久保万身
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Tokyo Electron Ltd
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Abstract

一种半导体装置的制造方法，其包括：在硅基板上形成含有Si和氧的绝缘膜的工序；利用使用了有机金属原料的化学气相堆积法、在上述绝缘膜上堆积金属氧化物膜的工序，其中：进行上述堆积金属氧化膜的工序，使得上述金属氧化膜在堆积后不久的状态下成为结晶质。

Description

半导体装置的制造方法
技术领域
本发明涉及半导体装置，特别是涉及具有高电介质膜或所谓high-K电介质膜的超微细化高速半导体装置的制造方法。
在现今的超高速半导体装置中，在微细化加工处理进步的同时，栅极长度可以做到0.1μm以下。通常在微细化的同时，半导体装置的动作速度提高，然而在这种作得非常微细的半导体装置中，随着微细化使栅极长度缩短，根据比例法则，需要减小栅极绝缘膜的膜厚。
但是，当栅极长度在0.1μm以下时，在使用SiO2的情况下，栅极绝缘膜的厚度需要设定为1～2nm或其以下。这样，在非常薄的栅极绝缘膜中，隧道电流增大，其结果是不能回避栅极泄漏电流增大的问题。
对于这个问题，目前提出了在栅极绝缘膜上采用比介电率远比SiO2膜的比介电率大、因而即使实际的物理膜厚大而换算为SiO2膜时的膜厚小的Ta2O5或Al2O3、ZrO2、HfO2、再就是ZrSiO4或HfSiO4那样的high-K电介质材料。通过使用这种high-K电介质材料，当栅极长度在0.1μm以下时，即使在非常短的超高速半导体装置中，也可以使用物理膜厚为10nm左右的栅极绝缘膜，可以抑制由隧道效果产生的栅极泄漏电流。
在栅极绝缘膜上使用这种high-K电介质膜的半导体装置中，直接在硅基板上形成high-K电介质膜，对于减小绝缘膜换算为SiO2实际膜厚是较好的，但这样，当直接在硅基板上形成high-K电介质膜时，金属元素会从high-K电介质膜扩散至硅基板中，在隧道区域中产生载流子散乱的问题。
从提高沟道区域中的载流子流动性的观点来看，最好在high-K电介质栅极氧化膜和硅基板之间，放入厚度在1nm以下、最好为0.8nm以下的厚度极薄的基极氧化膜。上述基极氧化膜需要非常薄，当厚度厚时，在栅极绝缘膜上使用high-K电介质膜的效果被抵消。
背景技术
图1A～1C表示目前提出的具有high-K电介质栅极绝缘膜的半导体装置的制造工序。
从图1A可看出，在硅基板11上，通过使用例如紫外光激发氧自由基的自由基氧化处理，形成非常薄的最好膜厚在1nm以下的SiO2膜构成的基极氧化膜12。在图1B的工序中，在上述基极氧化膜12上，利用原子层堆积(ALD)法或有机金属化学气相堆积(MOCVD)法等，形成HfO2或ZrO2等的金属氧化膜13。
在图1A的工序中，可以使用例如特开2002-100627号公报所述的方法，进行上述自由基氧化处理。通过硅基板的紫外光激发自由基氧化处理，可以稳定地再现性良好地形成膜厚相当于2～3个分子层的基极氧化膜。另外，当使用上述特开2002-100627号公报所述的方法时，可在这样形成的非常薄的硅氧化膜中导入氮原子，将上述基极氧化膜12作成硅氧氮化膜。
在图1B的工序中，可以使用特开2002-151489号公报中所述的ALD法或MOCVD法进行上述金属氧化膜13的堆积。
然而，上述金属氧化膜13是作为high-K电介质膜形成的，但为了显现出上述金属氧化膜13作为high-K电介质膜的功能，不利用SiO2膜那样的非晶质膜，而需要进行结晶化。因此，目前，如图1C所示，对在图1B的工序中得出的结构进行热处理，使金属氧化膜13结晶化的工序。由于金属氧化膜13在非晶质的基极氧化膜12上形成，所以在结晶化时，成为由微结晶的集合构成的多晶体。这种结晶化的金属氧化膜13，可以作为高速半导体装置的high-K电介质栅极绝缘膜使用。
然而，如上所述，要求这种high-K电介质栅极绝缘膜13和硅基板11之间的界面上形成的基极氧化膜12要求尽可能薄。当上述基极氧化膜12的膜厚增大时，使用high-K电介质栅极绝缘膜13的效果被抵消。
另一方面，在图1B的金属氧化膜13的堆积工序中，特别是在使用MOCVD法的情况下，成为在氧的气氛中的处理，在堆积时的基板温度高的情况下，上述基极氧化膜12的膜厚可能由于基极的氧化而增大。另外，在图1C所示的结晶化热处理时，上述基极氧化膜12的膜厚也增大。
另外，在图1C的结晶化工序中，在金属氧化膜13结晶化的同时，在上述金属氧化膜13中，产生微结晶的粒成长。当在膜13中产生这种粒成长时，在其下的与基极氧化膜12的界面变成不规则或不稳定，容易产生栅极泄漏电流增大等问题。
发明内容
本发明的目的是要解决上述问题，提供一种新颖的有用的半导体装置的制造方法。
本发明的更具体的目的是要提供一种在具有high-K电介质栅极绝缘膜的半导体装置的制造中、可以回避在上述high-K电介质栅极绝缘膜结晶化时基极氧化膜的膜厚增加的制造方法。
本发明的其它目的是要提供一种在具有high-K电介质栅极绝缘膜的半导体装置的制造中、在上述high-K电介质栅极绝缘膜结晶化时、可以抑制上述high-K电介质栅极绝缘膜中的金属氧化物微结晶的粒成长的制造方法。
本发明的再一个目的是要提供一种在具有high-K电介质栅极绝缘膜的半导体装置的制造中、可以有效地控制上述high-K电介质栅极绝缘膜的膜厚的制造方法。
本发明的其它目的是要提供一种半导体装置的制造方法，它包含下述工序：
在硅基板上形成含有Si和氧的绝缘膜的工序；
利用使用了有机金属原料的化学气相堆积法、在上述绝缘膜上堆积金属氧化物膜的工序；
其特征在于：进行上述堆积金属氧化膜的工序，使得上述金属氧化膜在堆积后不久的状态下成为结晶质。
采用本发明，可形成为构成high-K电介质栅极绝缘膜的金属氧化膜在堆积后不久已成为结晶质，但在本发明中，可抑制上述金属氧化膜中的粒成长，即使在进行了结晶化工序之后，金属氧化物结晶的粒径也不超过10nm。另外，即使进行这种金属氧化膜的堆积，实质上也不会使基极氧化膜的膜厚增加。特别是，在本发明中，在使用含有氨基的有机金属原料的情况下，在上述金属氧化膜中，氮向晶界偏析，这样向晶界偏析的氮，可抑制原子沿着晶界的移动。
本发明的其它目的和特征，从以下参照附图对本发明的详细说明中可以了解。
附图说明
图1A～1C是表示目前的高介电率栅极绝缘膜的形成工序的图。
图2是表示在本发明第一实施例中使用的MOCVD装置的结构的图。
图3是详细地表示图2的MOCVD装置的一部分的图。
图4是表示本发明第一实施例的HfO2膜的堆积速度和基板温度之关系的图。
图5是表示本发明第一实施例的HfO2膜的堆积速度和气相原料分压之关系的图。
图6是表示由本发明第一实施例得到的HfO2膜的X射线衍射图案的图。
图7A～7C是表示包含由本发明第一实施例得到的HfO2膜的试料的剖面TEM像的图。
图8是表示由本发明第一实施例得到的HfO2膜的C-V特性的图。
图9是表示由本发明第一实施例得到的HfO2膜中的碳浓度的图。
图10是表示由本发明第一实施例得到的HfO2膜中的氮浓度的图。
图11A～11E是说明本发明第二实施例的半导体装置的制造工序的图。
具体实施方式
[第一实施例]
图2表示本发明使用的MOCVD装置20的结构。
从图2中可看出，MOCVD装置20具有由泵21排气的反应容器22，在上述反应容器22中设置保持被处理基板W的保持台22A。
在图2的MOCVD装置20中设置有将氧气供给上述反应容器22的管路22a，另外还设置有将保持在起泡器23A中的Hf[N(C2H5)2]4等的液体有机金属原料、通过气相原料控制器22b和管路22c、供给上述反应容器22的原料供给系统I。另外，在上述MOCVD装置20中。还设置有将保持在瓶子23B中的Hf[N(C2H5)2]4等的液体有机金属原料、通过液体流量控制器22d和气化器22e、供给上述反应容器22的原料供给系统II。上述原料供给系统I和原料供给系统II，通过切换阀V1和V2进行切换。
图3表示上述原料供给系统I的气相原料控制器22b的结构。
从图3可看出，上述气相原料控制器22b包含被供给Ar气的质量流量控制器(以下简称MFC)31、32，上述MFC31将供给的Ar气作为载气供给至保持上述有机金属原料的起泡器23A中。
在上述起泡器23A中形成有机金属原料的蒸气，将所形成的有机金属原料蒸气，与来自上述MFC32的Ar载气一起，供给至浓度传感器33。
利用上述浓度传感器33测量有机金属原料相对于所供给的Ar载气浓度，将表示其结果的输出信号供给至控制部件34。另一方面，上述控制部件34根据规定的程序，形成与上述浓度传感器33的输出信号相应的第一和第二控制信号，分别将这些控制信号供给至上述MFC31和MFC32。由此，可将上述浓度传感器33中的有机金属原料相对于载气的浓度比控制为规定值。这样，将控制了有机金属原料浓度比的气相原料气体，由压力计35和阀36设定为规定压力后，通过上述管路22c供给至反应容器22。
图4表示在图2的MOCVD装置20中，对于使用Hf[N(C2H5)2]4作为原料进行在基板温度为480℃的硅基板上堆积HfO2膜的情况，在使用图2所示的原料供给系统I的情况和使用原料供给系统II的情况下比较堆积速度。
从图4中可看出，在使用原料供给系统II的情况下，随着堆积时基板温度的升高，堆积速度也增大，在480℃的基板温度下进行堆积时，可得到每分钟100nm左右的非常大的堆积速度。在这种非常大的堆积速度下，高精度地形成膜厚为数十nm的金属氧化膜较困难。
与此相对，在使用利用起泡器23A的原料供给系统I的情况下，在堆积时的基板温度为480℃时，堆积速度为每分钟1nm左右，可以高精度地形成非常薄的金属氧化膜。
图5表示在图2的MOCVD装置中使用原料供给系统I时的通过管路22c供给至上述反应容器22的气相原料中的Hf[N(C2H5)2]4的分压和基板上的堆积速度的关系。图5的关系是将基板温度设定为480℃时的关系。
从图5中可以看出，在使用图2的原料供给系统I的情况下，当Hf[N(C2H5)2]4的分压降低时，基板上的HfO2膜的堆积速度同时降低。通过利用图3所示的气相原料控制器22b控制Hf[N(C2H5)2]4的分压，可以控制HfO2膜在被处理基板W上的成膜速度。
图6表示在堆积后不久的状态下求出这样形成的HfO2膜X射线衍射图案的结果。图6中表示对这样得到的HfO2膜，在氮气氛中，在500～700℃范围内的各种温度下进行热处理时的X射线衍射图案。在图6的实验中，如上所述，利用在特开2002-100627号公报中所述的方法，在HF洗净了的硅基极表上形成由SiO2膜或SiON膜构成的膜厚约为0.8nm的基极氧化膜，在这样形成的基极氧化膜上进行HfO2膜的堆积。这时，如上所述，使用Hf[N(C2H5)2]4作为原料，设定堆积时的基板温度为480℃，进行HfO2膜的堆积。
从图6可看出，在堆积后不久的状态下，HfO2膜显示出Hf(111)的衍射峰值，成为结晶化状态。
作为与上述的图1(C)的工序相对应，在对这样形成的HfO2膜进行热处理的情况下，Hf(111)的衍射峰值多少增高一些，进行结晶化，但衍射峰值的强度变化不显著，即使进行热处理，HfO2膜的微结构也不太变化。实际上，测定了膜中的HfO2结晶的粒径分布的结果是，在480℃，在堆积后不久的状态下，平均粒径约为4.7nm，在500℃的热处理后的状态下，约为8.5nm，在600℃的热处理后，约为7.5nm，在700℃的热处理后约为6.3nm，若考虑误差时，可以认为在HfO2膜中几乎不会产生由热处理造成的粒径超过10nm的粒成长。
图7A表示用透过型电子显示微镜观察堆积了HfO2膜后的试料的剖面的结果，图7B表示同样利用透过型电子显微镜观察在氮气氛中、在700℃下热处理HfO2膜时的剖面的结果。图7A、7B用相同的比例表示。可看出，在硅基板中，各个Si原子被解像。
从图7A可看出，在形成HfO2膜后不久，SiO2基极氧化膜的膜厚约为1.3nm，相对于初期膜厚(0.8nm)，膜厚增加0.5nm。
与此相对，在图7B中，SiO2基极氧化膜的膜厚约为0.9nm，相对于图7A的状态，膜厚增加约0.1nm。
图7C表示在480℃下、在膜厚为0.8nm的SiON基极膜上形成HfO2膜、再在氮气氛中、在500℃下热处理该膜时的试料剖面。在这种情况下，SiON基极模的膜厚几乎不增加，这已被确认了。
这样，根据本发明，通过使用Hf[N(C2H5)2]4作为原料的MOCVD法，在480℃的基板温度下堆积HfO2膜的情况下，在堆积后不久，可得到结晶化的HfO2膜，并且在热处理这样得到的HfO2膜时，实质上没有HfO2结晶的粒成长，并且其下面的基极氧化膜的膜厚实质上不增加。
目前，得到这种效果的理由还不十分了解，但可以认为可能是原料中所含的氮原子，在HfO2膜中，向晶界偏析，敲击沿结晶晶界的氧原子或Hf原子的移动。该氮原子的量为0.5～5原子％。
图8表示使用这样在480℃下的堆积得到的HfO2膜形成电容器、测定C-V特性的结果。在图8中，为了比较，还表示了对350℃下堆积的HfO2膜同样求出的C-V特性。在480℃下，堆积上述HfO2膜时，设定氧浓度为87％，而在350℃下堆积上述HfO2膜时，设定氧浓度为56％。
从图8中可看出，在基板温度480℃、氧浓度87％的条件下形成的HfO2膜中，得到泄漏电流少的优异的C-V特性，而在基板温度350℃、氧浓度56％条件下形成的HfO2膜，得到泄漏电流多的特性不好的特性。这是由于膜中所含有的杂质元素的浓度两者不同。
图9表示对于在350～480℃范围内的各种基板温度下堆积的HfO2膜、求出了膜中的碳浓度的结果。
从图9中可看出，在氧浓度为56％的条件下堆积的HfO2膜中，在任意一个基板温度下，膜中的碳浓度都超过1×103/cm3，而在氧浓度为84％的条件下堆积的HfO2膜中，特别是在480℃的基板温度下堆积的情况下，膜中的碳浓度在1×102/cm3以下，可以认为这对图8的C-V特性有贡献。这可以认为是，图8的C-V特性反映了在由Hf[N(C2H5)2]4原料堆积HfO2膜时，通过在高温、高氧浓度条件下进行堆积，减小膜中的残留碳量的效果。
图10表示对于在350～480℃范围内的各种基板温度下堆积的HfO2膜、求出了膜中的氮浓度的结果。
从图10中可看出，在氧浓度为56％的条件下堆积的HfO2膜中，在任意一个基板温度下，膜中的氮浓度都超过1×103/cm3，而在氧浓度为84％的条件下堆积的HfO2膜中，特别是在480℃的基板温度下堆积的情况下，膜中的氮浓度在1×102/cm3以下。认为这反映出了具有如下结构式的Hf[N(C2H5)2]4原料中的Hf-N键容易被热切断的情形以及在上述Hf[N(C2H5)2]4原料中不含氧的情形。
这样，在本发明中，特别是通过使用包含Hf[N(C2H5)2]4这样氨基的有机金属化合物作为原料，在结晶化了状态下产生堆积的条件下进行金属氧化膜的堆积时，不论是在金属氧化膜堆积时和在热处理所堆积的金属氧化物时，都可有效地抑制金属氧化膜下的基极氧化膜的膜厚增加。另外，即使在金属氧化膜热处理时，也可抑制膜中的结晶粒成长，使与薄的基极氧化物的界面形态稳定。另外，通过在高温、高氧浓度条件下进行堆积，可使膜中所含的杂质的浓度最小化。
[第二实施例]
图11A～11E表示本发明的第二实施例的半导体装置的制造工序。
从图11A中可看出，通过进行例如使用紫外光激发氧自由基的自由基氧化处理、或者通过继续上述自由基氧化处理进行等离子体自由基氧化处理，可在硅基板41上形成由膜厚为1nm以下的SiO2膜或SiON膜构成的基极氧化膜42，在图1B的工序中，通过使用包含Hf[N(C2H5)2]4、Hf[N(CH3)2]4、Zr[N(C2H5)2]4及Zr[N(CH3)2]4的优选氨基的有机金属原料的有机金属化学气相堆积(MOCVD)法，在为了使上述金属氧化膜43以结晶质状态堆积的400～600℃的基板温度下，并且在80％以上的氧浓度条件下，将HfO2或ZrO2等金属氧化膜13堆积在上述基极氧化膜42上。
其次，在图11C的工序中，在氮气氛中，在500～700℃的温度下，热处理所得到的结构，使上述金属氧化膜43充分结晶化。这时，由于上述金属氧化膜43在堆积后不久已结晶化，所以原料中的氮原子向晶界偏析，可抑制金属氧化膜43中的结晶粒成长，还可抑制上述基极氧化膜42的残留氧造成的膜厚增加。特别是，如果利用SiON膜形成上述基极氧化膜42，则实质上可避免在图11B、11C的工序中的基极氧化膜42的膜厚增加。
接着，在图11D的工序中，在上述金属氧化膜43上堆积聚硅膜44，再在图11E的工序中，通过将该膜图案化，从而形成栅极电极44A。再通过在掩模中对上述栅极电极44A进行离子注入，从而在上述硅基板41中、上述栅极电极44A的两侧形成扩散区域41A、41B。
采用本实施例，可使由基极氧化膜42和金属氧化膜43构成的栅极绝缘膜的膜厚，与栅极长度的缩短而相应地减小，可以实现非常高速地进行动作的半导体装置。
以上说明了本发明的优选实施例，但本发明不是仅限于此，在本发明的要旨内，可作各种变形和变更。
产业上的可利用性
采用本发明，可以使构成high-K电介质栅极绝缘膜的金属氧化膜在堆积后不久已经成为结晶质，但利用本发明，还可抑制上述金属氧化膜中的粒成长，即使进行结晶化工序后，金属氧化物结晶的粒径不超过10nm。另外，即使进行这种金属氧化膜的堆积，基极氧化膜实质上不增厚。特别是，利用本发明，在使用含有氨基的有机金属原料的情况下，在上述金属氧化膜中，氮向晶界偏析，这样，向晶界偏析了的氮，可抑制原子沿着晶界的移动。

Claims (11)

1.一种半导体装置的制造方法，其包括：在硅基板上形成含有Si和氧的绝缘膜的工序；利用使用了有机金属原料的化学气相堆积法、在所述绝缘膜上堆积金属氧化物膜的工序；其特征在于：
进行所述堆积金属氧化膜的工序，使得所述金属氧化膜在堆积后不久的状态下成为结晶质。
2.如权利要求1所述的半导体装置的制造方法，其特征在于：所述金属氧化膜含有Hf或Zr中的任一种。
3.如权利要求1或2所述的半导体装置的制造方法，其特征在于：所述堆积金属氧化膜的工序在400～600℃的基板温度下进行。
4.如权利要求1～3中任一项所述的半导体装置的制造方法，其特征在于：所述有机金属原料包含氨基。
5.如权利要求1～4中任一项所述的半导体装置的制造方法，其特征在于：所述有机金属原料选自Hf[N(C2H5)2]4、Hf[N(CH3)2]4、Zr[N(C2H5)2]4和Zr[N(CH3)2]4。
6.如权利要求1～5中任一项所述的半导体装置的制造方法，其特征在于：所述有机金属原料通过液体原料的起泡供给。
7.如权利要求1～6中任一项所述的半导体装置的制造方法，其特征在于：所述堆积金属氧化膜的工序，在含有氧的气氛中进行。
8.如权利要求1～7中任一项所述的半导体装置的制造方法，其特征在于：所述堆积金属膜的工序，在超过80％的氧浓度气氛中进行。
9.如权利要求1～8中任一项所述的半导体装置的制造方法，其特征在于：所述金属氧化膜在堆积后不久的状态下，由粒径为10nm以下的微结晶构成。
10.如权利要求1～9中任一项所述的半导体装置的制造方法，其特征在于：还包括对所堆积的所述金属氧化膜进行热处理的工序，所述金属氧化膜在热处理后的状态下，由粒径为10nm以下的微结晶构成。
11.如权利要求1～10中任一项所述的半导体装置的制造方法，其特征在于：所述金属氧化膜以5原子％以下的范围含有氮。
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