CN1768159A - 氮化铪沉积方法 - Google Patents

氮化铪沉积方法 Download PDF

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CN1768159A
CN1768159A CNA2004800084270A CN200480008427A CN1768159A CN 1768159 A CN1768159 A CN 1768159A CN A2004800084270 A CNA2004800084270 A CN A2004800084270A CN 200480008427 A CN200480008427 A CN 200480008427A CN 1768159 A CN1768159 A CN 1768159A
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hafnium
precursor
reaction
silicon
sih
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C·梅慈耐
S·赫尔
Y·K·金
M·N·罗克利恩
S·M·乔治
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Applied Materials Inc
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Applied Materials Inc
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Abstract

本发明提供一种形成高k介电层的方法，该方法包括：利用原子层沉积将一种铪化合物沉积到衬底上，包括，将一种铪前体发送至衬底的表面，使铪前体发生反应，生成含铪层，将一种氮前体发送至含铪层，生成至少一个氮铪键，并将铪化合物沉积到表面上。

Description

氮化铪沉积方法
背景技术
技术领域
本发明的具体实施例一般涉及在衬底上沉积物质的方法，更具体地，涉及利用原子层沉积工艺，沉积金属氧化物、金属氮化物、金属氧氮化物、金属硅酸盐以及金属氧氮化硅的方法。
在半导体处理、平板显示器处理或其他电子器件处理领域，化学气相沉积对在衬底上形成膜起了非常重要的作用。由于电子器件的形状不断地缩小，而其密度却持续地增长，因此器件的大小和纵横比则变得越来越重要，例如，器件尺寸为0.07微米和纵横比为10或者更大正在被考虑。相应地，形成这些器件的材料的共形沉积正变得日益重要起来。
尽管传统的化学气相沉积业已证明可成功地适用于低于0.15微米的器件形状和纵横比，更具挑战性的器件几何尺寸需要新型的、创新的沉积技术。一种受到广泛关注的技术是原子层沉积(ALD)。在该技术中，反应物被顺序导入处理室，在该处理室中，每一种反应物化学吸附到衬底的表面，并发生表面反应。在每种反应气体的发送之间，典型地执行清洗步骤。清洗步骤可以是用载气进行持续地冲洗，或者是在发送两种反应气体之间脉冲清洗。
美国专利6287965描述了一种可形成结构为A-B-N的金属氮化物的ALD方法，此处A代表一种金属，B是一种可防止结晶的元素，N是氮。优选的具体实施方式教授了一种制备TiAlN的方法。该专利公开了这些膜中没有被加入氧；事实上，该发明是通过顺序在用于氧保护的金属氮化物层之间堆集氧扩散阻碍层而去除氧的。
美国专利6200893，名称为“Raical-assisted Sequential CVD(自由基协助的顺序CVD)”，描述了一种CVD衬底沉积方法，在该方法中，自由基诸如氢和氧或者氢和氮被交替使用，与分子前体形成一个循环。利用本发明重复的循环产生一种复合一体膜。在一种优选的具体实施例中，来自分子前体的被沉积物质是金属和自由基，在交替步骤中，用于去除金属前体或母体反应残留的配位体。自由基氧化或者氮化在后续层中的金属表面，目的是分别产生金属氧化物或者氮化物。在参考文献各种的具体实施例中，金属铪和氧化铪是由一种含卤素的前体制备的。然而，参考文献没有提出由金属有机化合物制备的络合铪化合物(三元、四元和五元)。而且，参考文献要求使用自由基将氧和/或氮加入膜中。
因此，需要一种方法，可从有机金属化合物中沉积铪化合物，例如氮化物、硅酸盐、氧氮化物、氮化硅、氧氮化硅、氧氮化铝以及氧氮化硅铝。
发明内容
在一个实施例中，本发明是关于在衬底表面形成含铪层的方法，顺序包括：a)将衬底表面暴露于铪前体或母体，以在衬底表面形成含铪层；b)用一种清洗气清洗处理室；c)使第二个前体与含铪层发生反应；d)用清洗气清洗处理室；e)使第三个前体与含铪层发生反应；f)用清洗气清洗处理室；g)使第四个前体与含铪层发生反应；和h)用清洗气清洗处理室。
在另一个实施例中，本发明是关于生成一种含铪层的方法，包括：在ALD循环中，将衬底顺序暴露于至少四种前体，用来沉积一种含铪的化合物薄膜，该薄膜也包含至少三种选自硅、铝、氧和氮的元素。
在另一个实施例中，本发明描述的是在原子层沉积过程中，将一种含铪化合物沉积到处理室的衬底上的方法，包括：进行含有铪前体的第一个半反应，进行含有氧前体的第二个半反应，进行含有氮前体的第三个半反应，和进行含有硅前体的第四个半反应。
在另一个实施例中，本发明是一种半导体材料的合成物，含有HfSixOyNz，此处x至少为0.2但要小于4，y至少为0.5但要小于4，z至少为0.05但要小于2。
附图说明
为了更为详细地了解上述本本发明的特征，通过参照具体实施例，可以得到一个比上述简括的本发明更为详尽的描述，其中一部分在附图中进行了说明。然而，要注意到，附图仅仅说明了本发明典型的具体实施例，因此不应当是被认为限定其范围，因为本发明可能容许其它同等有效的具体实施例。
图1是生长氮化铪薄膜的半反应实例；
图2是生长氧化铪薄膜的半反应实例；
图3A-3D是生长硅酸铪薄膜的半反应实例；
图4A-4D是生长氧氮化硅铪薄膜的半反应实例。
优选的实施例详述
本发明提供了制备用途广泛的铪化合物的方法，包括用于k介电材料。这些方法利用原子层沉积(ALD)对铪化合物的组成进行元素控制。元素控制通常利用半反应进行区分。
下面的反应简要的说明了半反应：
此处AB为产品化合物，CD为第二化合物或者第二产物。
例如，下列每一步反应都说明了一个半反应：
(1)
(2)
此处，第一步的半反应由官能团NH2引发，*代表原子或者分子，其为衬底、薄膜或表面基的一部分。铪前体与NH2基反应生成一个Hf-N键。来自铪前体的配位体质子化形成第二产物。在第二步的半反应中，氨与铪络合物反应在表面结合。当另一个Hf-N键与另一个官能团(NH)生成产物时，剩下的配位体质子化并被去除。在第一步和第二步的每个半反应中，二乙胺(HNEt2)作为第二产物被制备。其它第二产物为氨和肼，以及自由基、离子、和各种配位体变体，例如Et2N、(Et2N)2、EtNH和(EtNH)2。通常，这些第二产物很容易被去除，例如可利用真空和/或清洗。反应配比不一定要按化学计量，但要具备一个宽范围的原子比。在本公开中，反应实例缺乏特定的化学计量、结合级数以及产品化合物与第二产物的成键连接。
下列每步反应说明了另一个半反应实例：
(3)
(4)
此处第三步半反应由官能团OH基引发，并生成一个Hf-O键。第四步继续反应生成另一个Hf-O键以及最终产物和官能团OH。
因此，通常来说，第一个半反应随着第一个官能团的反应而开始，生成了至少一个产品化合物键和生成了第二个官能团。第二个半反应随着第二个官能团的反应而开始，生成了至少一个产品化合物键和生成了第三个官能团。在许多实例里，第三个官能团与第一个官能团相同或相似。然而，即使第三个官能团不同，第二个半反应仍旧完成了。生成三元、四元以及更多元的产品化合物的实例要求半反应有两个以上的前体。因此，半反应并没有被限制在只有二元产品化合物，而是可以包含任意数量的半反应。大多数半反应被气体和/或真空清洗顺序分隔。
在此所描述的方法的实施例是在许多衬底和表面沉积含铪物质。本发明的实施例可用的衬底包括，但并非被限制在半导体晶片，例如晶体硅(例如Si<100>或者Si<111>)、二氧化硅、锗化硅、掺杂或未掺杂多晶硅、掺杂或未掺杂硅晶片、氮化硅以及图案化化或未图案化的晶片。表面包括裸硅晶片、膜、层和具有绝缘、传导和阻碍特性的材料，也包括氧化铝和多晶硅。表面预处理包括抛光、蚀刻、还原、氧化、羟基化、退火和烘烤。
可对衬底作预处理，以各种各样的官能团作为其终端，官能团包括羟基(OH)、烷氧基(RO，此处R＝Me、Et、Pr或Bu)、卤氧基(OX，此处X＝F、Cl、Br或I)、卤化物(F、C1、Br或I)、氧自由基、氨基(NH或NH2)和酰胺基(NR或NR2，此处R＝Me、Et、Pr或Bu)。可通过使用一种试剂来完成预处理，例如使用NH3、B2H6、SiH4、SiH6、H2O、HF、HCl、O2、O3、H2O2、原子氢、原子氧、乙醇或者胺。
一旦衬底的表面被预处理过，ALD循环就开始了。对于许多铪化合物而言，在某种工艺条件下，铪前体吸附具有自限性，通常必须在低温下(＜500℃)来抑制这种行为。一些自限性的铪前体的反应实例包括：
        
        
        
此处，加入铪，生成*O-Hf(NEt2)x或*N-Hf(NEt2)x。原子，例如氮或氧，能将铪原子固着在衬底或者表面。*Hf(NEt2)x是自限性的，因为铪前体不能进一步反应。因此，这是第一个半反应。要继续进行其它的半反应，要加入氧源(例如水)或者氮源(例如氨)。
含有铪前体的第一个半反应引发了一系列半反应，生成二元、三元、四元以及更复杂的化合物。第一个半反应不一定要包含铪前体，而是能包括任何一个其特殊的元素被加入膜中的前体。下列实例将展示铪前体作为第一个半反应，目的是更清晰地解释发明方面。
本发明的一个实施例是关于一个过程，该过程继续进行NH3对*Hf(NEt2)x的反应，以生成*Hf-NH，通过顺序进行铪前体的半反应和一种氮源的半反应而生成氮化铪。图1描述了在大约0.01-10s之间，优选0.25s，加入(Et2N)4Hf，和在大约0.01-20s之间，优选0.25s，加入一种惰性清洗气体所引发的半反应。然后，在大约0.01-10s之间，优选0.25s，加入NH3，在大约0.01-20s之间，优选0.25s，加入一种惰性清洗气体，引发第二个半反应。这两个半反应被循环数次，在每个循环为50ng/cm2的速率下生成氮化铪膜。通过改变循环时间、温度、压力和/或浓度，可以对产品化合物的化学计量进行控制。化学计量的轻微变动就能影响电性能。例如Hf3N4是一种绝缘材料，而HfN是一种导电材料。在一个具体实施例中，HfN由不含硝酸的铪前体制备。氮化铪膜可能会出现氧污染，因为硝酸含有3∶1的氧/氮比。
在一个实施例中，一种利用原子层沉积生成一种半导体材料的方法包括顺序循环的脉冲加入一种铪前体和氮前体。氮化铪被沉积到衬底表面，此处氮化铪的分子式为HfNx，x至少为0.1但要小于1.3。一方面，铪前体为TDEAH，氮前体为NH3。另一方面，铪前体为HfCl4，氮前体为自由基氮，例如氮原子。
本发明的另一个实施例是继续进行一个H2O对*Hf(NEt2)x的半反应，并生成Hf-OH。通过顺序进行铪前体的半反应和一种氧源的半反应，合成氧化铪。图2描述了一个半反应，通过在大约0.01-10s之间，加入(Et2N)4Hf，在大约0.01-20s之间加入一种惰性清洗气而引发。接着，在大约0.01-10s之间加入H2O，在大约0.01-20s之间加入一种惰性清洗气，引发第二个半反应。这两个半反应循环反应数次，在每个循环大约为1.2的速率下生成氧化铪膜。
可对如上所述的生成氮化铪和氧化铪的方法进行修改，来得到其它的产物，也就是三元化合物。氮化铪多孔，可与水反应生成氧氮化铪，Hf-O-N。因此，对氮化铪循环而言，一个氧源(例如水)的半反应被加入用来合成氧氮化铪。Hf∶O∶N的比例可以控制，并根据所需的产品化合物的特征加以变动。在一个具体实施例中，氧前体半反应被包括进半反应循环中。这样的一个循环包含一个铪前体半反应、一个氮前体半反应、另一个铪前体半反应和一个氧前体半反应。相对于铪和氮前体半反应，氧前体半反应可以按任意比例加入到循环中。在一个实例中，每10个完整的铪和氮前体半反应中加入1个氧前体半反应。而且，比例可以改变，以便可根据膜厚控制氧的化学计量。因此，可以形成渐变膜(graded film)。在一个实施例中，工艺条件如下所述，压力大约为1torr，温度约为225℃，氩载气流为200sccm，H2O和NH3在大约1s-4s之间被加入到氩载气流中，在大约20s时加入TDEAH。
渐变膜可用于不同材料之间的过渡。一个实施例采用本方法，在氮化铪与氧化铪之间过渡。在氮化铪膜内，N∶Hf∶O的元素比例开始为10∶10∶0，然后是10∶10∶1，接着是5∶10∶5，接着是1∶10∶10，最后为0∶10∶10，这样经历沉积之后暴露于表面的膜为氧化铪。渐变膜具备有利的特征，例如，允许控制整个膜厚的电性能，以及具有较高的膜附着度。
其它具体实施例包括合成氧氮化铪的方法。由于氮化铪的多孔特性，多重氮化铪层对氧富集敏感。不通过半反应将氧加入每一层表面层中，一种过量氧前体(例如水)被用于渗透到氮化铪的多重层中，并生成一种氧氮化铪渐变膜，如下所示：
因此，可利用ALD、CVD、PVD或其他技术形成氮化铪。随后用氧前体氧化。
本发明的其它实施例包括合成加入硅的三元氮化铪化合物的方法。优选的硅前体化合物包括(Me2N4)Si和(MeN3)SiH。在一个实施例中，一个硅前体半反应被加入到生成氮化铪的半反应循环中。该循环包括一个铪前体半反应、一个氮前体半反应、一个硅前体半反应和另一个氮前体半反应。相对于铪和氮前体半反应，硅前体半反应可按任意比例加入到循环中。在一个实例中，每两个完整的铪和氮前体半反应循环加入一个硅前体半反应。而且，此比例可以改变，目的是根据膜厚控制所加入的硅的比例。与氧氮化铪相似，本方法能够控制Hf∶Si∶N的化学计量。
本发明的其它实施例是关于合成加入氮的三元氧化铪化合物的方法。与上述讨论相似，本方法对换使用氧和氮来合成氧氮化铪。在一个实施例中，一个氮前体半反应被加入到氧化铪的半反应循环中。该循环包括一个铪前体半反应、一个氧前体半反应、另一个铪前体半反应和一个氮前体半反应。相对于铪和氧前体半反应，氮前体半反应可按任意比例加入到循环中。在一个实例中，每两个完整的铪和氧前体半反应循环加入一个氮前体半反应。而且，比例可以改变，目的是根据所生成的膜的厚度控制所加入的氮的比例。
本发明其他的实施例包括合成加入硅的三元氧化铪的方法，即硅酸铪，如图3A-3D所示。在一个实施例中，一个硅源半反应被加入到氧化铪的半反应循环中去。该循环包括一个硅前体半反应、一个氧前体半反应、一个铪前体半反应和另一个氧前体半反应。在每个半反应之间进行清洗。相对于铪和氧前体的半反应，硅前体半反应能够按任意比例加入到循环中。在一个实例中，每两个完整的铪和氧前体半反应循环加入一个硅前体半反应。而且，比例可以改变，目的是根据膜厚控制所加入的硅的比例。
本发明的实施例包括多种合成四元化合物尤其是氧氮化硅铪(HfSiON)的方法，如图4A-4D所示。修改合成两种三元化合物(HfSiO和HfSiN)的方法，分别在循环中进行氮化和氧化，以生成四元络合物HfSiON。在特殊的循环中，加入氮、氧或硅前体的半反应，相对于铪提供对N∶O∶Si比例的完全控制。
在一个实施例中，一个氮源半反应被加入到硅酸铪的半反应循环中。这样的循环包括硅前体半反应、氧前体半反应、铪前体半反应和氮前体半反应。相对于铪、硅和氧前体半反应，氮前体半反应能够按任意比例加入。在一个实例中，每两个完整的铪、硅和氧前体半反应循环加入氮前体半反应。而且，此循环比例可以改变，目的是控制膜厚度内加入的氮的比例。一些实施例生成膜顶部氮浓度较高的氧氮化硅铪渐变膜。
在本发明的一方面，表面以*SiOH基终止。半反应循环包含铪前体、氮前体、硅前体和氧前体，每个半反应之间用清洗分隔。这些前体可分别为TDEAH、氨、Tris-DMAS和水。在本发明的另一方面，这些前体可分别为HfCl4、自由基氮、Si2Cl6和O3。控制其组成，可形成一种半导体材料，该半导体材料结构为HfSixOyNz，其中x至少为0.2，但要小于4，y至少是0.5但要小于4，z至少为0.05但要小于2。
本发明的实施方式包括多种合成五元化合物的方法，尤其是氧氮化硅铝铪(HfAlSiON)。在特定的循环中加入铪、铝、氧和硅前体半反应，相对于铪提供对Al∶N∶O∶Si的比例的完全控制。在本方法的一方面，半反应脉冲的循环依次包括水、TDEAH、氨、Tris-DMAS、水和TMA。在本方法的另一方面，半反应脉冲的循环依次包括水、HfCl4、氨、Tris-DMAS、水和TMA。
因此，利用本工艺的方法，可以制备下列化合物的任何一种化学计量：HfO、HfN、HfON、HfSiO、HfSiN、HfSiON、HfAlO、HfAlN、HfAlON、HfSiAlO、HfSiAlN、HfSiAlON。因此，在产品化合物的沉积过程中，ALD可提供化学计量控制。可以通过沉积工艺后各种不同的步骤来改变化学计量，例如在Hf3N4热退火生成HfN的时候。也可以利用在沉积过程中改变前体比例来控制化学计量。
利用本发明各种不同的实施方式所合成的产品化合物有着许多的工业用途。在微电子工业中，产品化合物可用于高k晶体管门电介质材料、晶体管门界面工程、高k电容器介电材料(DRAMs)、种子层、扩散阻碍层、粘附层、绝缘体层、导电层以及图案化表面的功能化表面基(functionalized surface group)(例如选择性沉积)。在微电机系统领域，利用本发明所制备的材料被用作绝缘、电导或者结构薄膜。这些材料也可用作功能性表面基用来降低粘附作用。表面基其它的功能是用在气相或液相色谱中、化学附着中的化学传感器和活性部位、图案化表面(例如组合化学)。氮化硅可作为一种硬化膜，用在工具上以及光学器件中。
许多前体都在本发明的范围内。一个重要的前体特征是要具备一个合适的蒸汽压。前体可以是环境温度和压力下等离子体、气体、液体或者固体。然而，在ALD室内，前体被蒸发。有机金属化合物或者络合物包括任何一种含有一种金属和一个有机基团，例如烷基、烷氧基、烷基酰氨基和N-(某)酰苯胺的化学品。前体由有机金属和卤化物构成。
铪前体实例包括含有配位体诸如烷基酰氨基、环戊二烯基、卤化物、烷基、醇盐以及其结合体的铪化合物。用作铪前体的烷基酰氨基铪化合物含有(RR’N)4Hf，其中R或R’是独立的氢、甲基、乙基、丙基或者丁基。特定的铪前体包括：(Et2N)4Hf、(Me2N)4Hf、(EtMeN)4Hf、(tBuC5H4)2HfCl2、(C5H5)2HfCl2、(EtC5H4)2HfCl2、Me5C5)2HfCl2、(Me5C5)HfCl3、(iPrC5H4)2HfCl2、(iPrC5H4)HfCl3、(tBuC5H4)2HfMe2、(acac)4Hf、(hfac)4Hf、(tfac)4Hf、(thd)4Hf、Br4Hf、Cl4Hf、I4Hf、(NO3)4Hf、(tBuO)4Hf、(iPrO)4Hf、(EtO)4Hf和(MeO)4Hf。
硅前体实例包括：烷基酰氨基硅(例如(Me2N)4Si、(Me2N)3SiH、(Me2N)2SiH2、(Me2N)SiH3、(Et2N)4Si、(Et2N)3SiH、Si(NCO)4、MeSi(NCO)3、SiH4、Si2H6、SiCl4、Si2Cl6、MeSiCl3、HSiCl3、Me2SiCl2、H2SiCl2)、硅烷醇(例如MeSi(OH)3、Me2Si(OH)2、(EtO)4Si)以及各种烷氧基硅(例如(RO)4-nSiLn，此处R＝甲基、乙基、丙基和丁基，L＝H、OH、F、Cl、Br、I以及其混合物)。而且，本发明的方法也采用了高级硅作为硅前体。美国临时专利申请60/419426、60/429376以及60/419504公开了高级硅，均于2002年10月18日提出申请，授予应用材料有限公司，名称为“Low temperature deposition with siliconcompounds(硅化合物低温沉积)”，在这里这些专利被收录作为参考文献，目的是描述硅前体。
氮前体实例包括：NH3、N2、肼(例如N2H4或MeN2H3)、胺(例如Me3N、Me2NH、或MeNH2)、苯胺(例如C6H5NH2)、有机氮化物(例如MeN3或Me3SiO3)、无机氮化物(例如NaN3或Cp2CoN3)和自由基氮化合物(例如N3、N2、N、NH或NH2)。可以利用热、热丝和/或者等离子体产生自由基氮化合物。
氧前体实例包括：H2O、H2O2、O3、O2、NO、N2O、NO2、N2O5、乙醇(例如ROH，此处R＝Me、Et、Pr和Bu)、过氧化物(有机和无机)羧酸和自由基氧化合物(例如O、O2、O3、和OH自由基)。可以利用热、热丝和/或者等离子体产生自由基氧化合物。
铝前体实例包括：烷基铝，例如：Me3Al、Et3Al、Pr3Al、Bu3Al、Me2AlH、Et2AlH、Me2AlH、Et2AlCl，烷氧基铝，例如：(MeO)3Al、(EtO)3Al、(PrO)3Al和(BuO)3Al、电气(dimmer)铝、卤化铝和氢化铝。
本发明的过程可以在ALD工艺所熟知的设备中进行。装置使原料和被加热的要在其上生成膜的衬底接触。用来沉积膜的硬件器件是美国专利申请10/251715所公开的一种ALD装置，该专利于2002年9月20日提出申请，转让给位于加利福尼亚州Santa Clara的应用材料有限公司，其名称为“An Apparatus for the Deposition of High DielectricConstant Films(一种用于沉积高介电常数膜的装置)”，在这里其被全部收录以做参考，目的是描述该装置。载气或者清洗气包括N2、Ar、He、H2、生成气及其混合物。
在某个实施例中，氢气被用作一种载气、清洗气和/或一种反应气体，以降低来自膜的卤素污染。含有卤素原子(例如HfCl4、SiCl4和Si2Cl6)的前体容易地污染膜。氢为一种还原剂，会生成一种易挥发的、可去除的副产品氯化氢。因此，当氢与一种前体化合物(例如铪、硅、铝、氧或氮前体)结合时，氢被用作一种载气或者反应气体，而且能够包括另一种载气(例如Ar或N2)。在本发明的一方面，提供一种水/氢混合物，在250℃-650℃的温度范围内，被用于降低膜的卤素浓度并增加氧的浓度。
本发明提供了制备下列化合物的方法。下标(w、x、y、z)表明，根据生成下列化合物的ALD进料顺序，可随意改变化学计量(组成可控)。
铝酸铪：HfAlxOy
氧化铪：HfO2和HfOx
氮化铪：Hf3N4、HfN和HfNx
氧氮化铪：HfOxNy
氧氮化铝铪：HfAlOxNy
硅酸铪：HfSiO4、Hf4SiO10、Hf3SiO8、Hf2SiO6、HfSiO2、HfxSiyO2(x+y)和HfxSiyO
硅酸铝：Al6Si2O13和AlxSiyO
硅酸铝铪：Hf2Al6Si4O21和HfxAlySizO
氮化硅铪：HfxSiyN
氧氮化硅铪：HF2Si2N2O5和HfSixOyNz
氧氮化硅铝：AlSixOyNz
氧氮化硅铝铪：HfAlwSixOyNz
本列表化合物只代表部分产品，其它的材料可用本发明的方法制备。其它元素，例如碳、钛、钨、钌、钽、锆、钼、铱、镍、铜、锡、硼或磷，可作为产品化合物加入到膜中。因此，产品化合物可能包括氧氮化硅铪和碳。下面列举了半反应的实例。注意，*＝表面物质。
前体与表面羟基(-OH)的反应：
表面产物与H2O(g) 反应再次生成表面羟基(-OH)：
表面产物与NH3(g) 、反应生成表面胺基(-NH2 ，-NH)：
前体与表面胺基(-NH或-NH2 )的反应：
表面产物与NH3 反应再次生成表面胺基：
表面产物与H2O(g) 反应生成表面羟基：
                             实例：
TDEAH＝四二乙基酰氨铪                          (Et2N)4Hf
TDMAS＝四二甲基酰氨硅                          (Me2N)4Si
TrisDMAS＝三二甲基酰氨硅                       (Me2N)3SiH
TMA＝三甲基铝                                  Me3Al
ALD过程可维持在大约20-650℃的温度范围内，优选温度范围为大约150-300℃，更优选温度为225℃。假如维持饱和的ALD行为，所生成的物质在一个较广的温度范围内是相似的。ALD过程在大约O.1-100torr的压力范围内操作，优选压力范围为大约1-10torr。假如维持饱和的ALD行为，从高真空到高压范围内，所生成的产物是相似的。维持反应流的粘性，以促进反应物分离。载气(例如氮气)维持在大约50sccm到1000sccm的范围内，优选300sccm左右，速度为1m/s左右。高速可能引发粒子转移问题，而低速则因为无效清洗的因素可能可使粒子形成，从而影响薄膜的电行为。所沉积的薄膜的厚度在2-1000左右，优选为5-100左右，而更优选厚度为10-50左右。
在一个实例中，氧化铪膜在氢气存在情况利用ALD生成。氢用于降低含铪膜内卤素污染物(例如F或Cl)的水平。A流，含有四氯化铪和至少一种载气(例如Ar、N2和H2)与B流，含有水、氢和任选载气，被顺序脉冲加入。A流和B流每个被脉冲加入1s左右，氩清洗流在A流和B流的每个脉冲之间被脉冲1s左右。温度维持在大约250-650℃之间。
在另一个实例中，硅酸铪膜在氢气存在情况利用ALD生成。A流，含有四氯化铪和至少一种载气(例如Ar、N2和H2)与B流，含有水、氢和任选载气，以及C流，含有Tris-DMAS和至少一种载气被顺序脉冲加入。A、B、C流每个被脉冲1s左右，氩清洗流在A、B和C流的每个脉冲之间被脉冲加入1s左右。温度维持在大约450-650℃之间。
在另一个实例中，氧氮化硅铪膜在氢气存在情况利用ALD生成。A流，含有四氯化铪和至少一种载气(例如Ar、N2和H2)与B流，含有水、氢和任选载气，和C流，含有Tris-DMAS和至少一种载气，以及D流，含有氮等离子体和一种任选载气被顺序脉冲加入。A、B、C和D流每个被脉冲1s左右，氩清洗流在A、B、C和D流的每个脉冲之间被脉冲1s左右。温度维持在大约450-650℃之间。
通过以一种交替的模式单独加入化学品来沉积物质，利用选择的半反应获得所需的膜组成或者特征。然而，上述半反应并没有规定确切的所生成膜的成键连接或者化学计量。化学计量主要是由热力学控制的；然而，也可以获得动力学控制生成的膜。因此，可以修改进料顺序，从而影响膜的总体组成和质量。能够利用ALD半反应生成的薄膜物质的种类通常如下：
1.二元产物：反应物{A+B}重复循环：例如Hf3N4
2.直接合金：反应物{A+B+C+D}重复循环：例如HfSiO4
3.组成可控的合金：反应物{y(A+B)+z(C+D)}重复循环(此处y或者z等于1，z或者y大于1)：例如HfxSi(2-x)O4
4.组成可控的渐变产物：与3相似，然而，在沉积过程中，y或者z可变化
5.分层或者薄片产物：两种不同的物质在不连续的物理层沉积。反应物{y(A+B+C+D)+z(E+F)}重复循环(此处y和z典型地大于等于4)：例如纳米薄片氧化铪和氧化铝
铝酸铪(HfxAlyO)的ALD
直接：1循环＝(TDEAH+H2O+TMA+H2O)
半反应＝4.03+5.03+4.08+5.08
组成可控：1循环＝n(TDEAH+H2O)+m(TMA+H2O)此处n典型为1而m是变化的，或者m为1而n是变化的。
半反应(第二个)(例如n＝3，m＝1)＝4.03+5.03+4.07+5.07+4.07+5.07+4.08+5.08
分层：1层＝p(TDEAH+H2O)+q(TMA+H2O)此处p和q典型地≥4
半反应(第二个)(例如n＝4，m＝4)＝4.03+5.03+(4.07+5.07+4.07+5.07+4.07+5.07)+4.08+5.08+(4.04+5.04+4.04+5.05+4.04+5.04)
氮化铪(Hf3N4或HfN)的ALD
直接：1循环＝(TDEAH+NH3)
半反应(第二个)＝7.02+8.02
在本例中，这些温度下的沉积可以产生Hf3N4。退火至高温可以产生HfN。
氧氮化铪(HfOxNy )的ALD
直接：1循环＝(TDEAH+H2O+TDEAH+NH3)
半反应(第二个)＝7.02+9.02+4.07+6.07
组成可控：1循环＝n(TDEAH+H2O)+m(TDEAH+NH3)此处典型地n为1而m是变化的，或者m为1而n是变化的。
分层：1层＝p(TDEAH+H2O)+q(TDEAH+NH3)此处p和q典型地≥4
氧氮化铝铪(HfwAlxOyNz )的ALD
直接：1循环＝(TDEAH+NH3+TMA+H2O)氧氮化铪/氧氮化氧化铝合金(alumina oxynitride alloy)
可能的变化：1循环＝(TDEAH+NH3+TDEAH+H2O+TMA+H2O)
注意：不同进料顺序影响成键连接，尤其在较低温度＜300℃和没有高温退火的情况下。在顶部的实例中，可预测为-O-Hf-N-Al-O-连接。这可以被认为是一种氧氮化铪/氧氮化氧化铝合金。在底部的实例中，可预测为-O-Hf-N-Hf-O-Al-O-连接。这可以被认为是一种氧氮化铪/氧化铝合金(alumina alloy)。
硅酸铪(HfSiO4 和HfxSiyO)的ALD
直接：1循环＝(TDEAH+H2O+TrisDMAS+H2O)＝HfSiO4
富硅(silica-rich)硅酸铪：1循环＝(TDEAH+H2O)+3(TrisDMAS+H2O)＝Hf2Si5O14
从纯HfO2到富硅(＞70％)硅酸铪，组成控制(Hf∶Si)是可能的。
硅酸铝(Al6Si2O13 和AlxSiyO)的ALD
直接：1循环＝(TMA+H2O+TrisDMAS+H2O)＝Al6Si2O13
富硅硅酸铝：1循环＝(TMA+H2O)+3(TrisDMAS+H2O)＝Al2Si2O7
从纯Al2O3到富硅(＞50％)硅酸铝，组成控制(Al∶Si)是可能的。
硅酸铝铪(Hf2Al6Si4O21 和HfxAlySizO)的ALD
例如：1循环＝(TDEAH+H2O+TrisDMAS+H2O+TMA+H2O+TrisDMAS+H2O)＝Hf2Al6Si4O21
氮化硅铪(HfxSiyN)的ALD
直接：1循环＝(TDEAH+NH3+TrisDMAS+NH3)
氧氮化硅铪(HfSixOyNz )的ALD
例如：(TDEAH+H2O+TrisDMAS+NH3)
例如：
(TDEAH+NH3+TDEAH+H2O+TrisDMAS+H2O+TrisDMAS+NH3)
氧氮化硅铝(AlSixOyNz )的ALD
例如：(TMA+H2O+TrisDMAS+NH3)
氧氮化硅铝铪(HfAlwSixOyNz )的ALD
例如：(TDEAH+NH3+TMA+H2O+TrisDMAS+H2O)
例如：(TDEAH+NH3+TDEAH+H2O+TrisDMAS+NH3+TMA+H2O3)
二氧化硅(SiO2 )连续ALD
例如：直接：1循环＝Si(NCO)4+H2O
本过程可以生成纯SiO2薄层，或者更易于控制混合物中的硅的浓度。Si(NCO)4易于与Hf-OH*基发生反应，从而能够轻松地加入氧化硅(因为TDEAH与SiOH*发生反应)
例如，考虑几个(TrisDMAS+H2O)循环与一个偶发的(TDEAH+H2O)或(TMA+H2O)循环或(闪光退火＞700℃+H2O)，以改变表面Hydroxal基，从而再次开始生长。
Si3N4 ，(例如非连续性种子层或者封端层)
例如，直接：1循环＝(TrisDMAS+NH3)
SixOyN，(例如非连续性种子层或者封端层)
例如，直接：1循环＝(TrisDMAS+NH3+TrisDMAS+H2O)
AlN
例如，1循环＝(TMA+NH3)
AlxSiyN
AlxOyN
HfxAlyN
尽管上述内容指的是本发明的具体实施例，本发明其它的以及进一步的实施例可以在不偏离其基本范围的情况下进行修改，苯发明的范围由所附权力要求确定。

Claims (25)

1.一种在衬底表面形成含铪层的方法，顺序包括：
a)将衬底表面暴露在铪前体下，在衬底表面形成含铪层；
b)用清洗气清洗处理室；
c)第二种前体与含铪层发生反应；
d)用清洗气清洗处理室；
e)第三种前体与含铪层发生反应；
f)用清洗气清洗处理室；
g)第四种前体与含铪层发生反应；和
h)用清洗气清洗处理室。
2.根据权利要求1所述的方法，其中，含铪层为氧氮化硅铪。
3.根据权利要求1所述的方法，进一步包括：重复步骤a-h，沉积含铪层，其厚度大约在2-1000之间。
4.根据权利要求3所述的方法，其中，厚度大约在10-50之间。
5.根据权利要求1所述的方法，其中，铪前体选自(Et2N)4Hf、(Me2N)4Hf、(EtMeN)4Hf和Cl4Hf。
6.根据权利要求5所述的方法，其中，第二种前体选自氨、肼、叠氮化物和自由基氮化合物。
7.根据权利要求6所述的方法，其中，第三种前体选自SiH4、Si2H6、Si3H8、Si2Cl6、、(Et2N)4Si、(Me2N)4Si、(Et2N)3SiH和(Me2N)3SiH。
8.根据权利要求7所述的方法，其中，第四种前体选自H2O、H2O2、有机过氧化物、O、O2、O3和自由基氧化合物。
9.根据权利要求1所述的方法，进一步包括：
i)第五种前体与含铪层发生反应；和
j)用清洗气清洗处理室。
10.根据权利要求9所述的方法，其中，第五种前体选自Me3Al、Me2AlH、AlCl3、Me2AlCl和(PrO)3Al。
11.一种制备含铪层的方法，包括：
在ALD循环过程中，顺序将衬底暴露于至少四种前体，以沉积含铪的化合物薄膜，并且要从硅、铝、氧和氮中选择至少三种元素。
12.根据权利要求11所述的方法，其中，至少四种前体选自(Et2N)4Hf、(Me2N)4Hf、(EtMeN)4Hf和Cl4Hf的铪前体。
13.根据权利要求11所述的方法，其中，至少四种前体含有选自SiH4、Si2H6、Si3H8、Si2Cl6、、(Et2N)4Si、(Me2N)4Si、(Et2N)3SiH和(Me2N)3SiH的硅前体。
14.根据权利要求11所述的方法，其中，至少四种前体含有选自氨、肼、叠氮化物和自由基氮化合物的氮前体。
15.根据权利要求11所述的方法，其中，至少四种前体含有选自H2O、H2O2、有机过氧化物、O、O2、O3和自由基氧化合物的氧前体。
16.根据权利要求11所述的方法，其中，至少四种前体含有选自Me3Al、Me2AlH、AlCl3、Me2AlCl和(PrO)3Al的铝前体。
17.根据权利要求11所述的方法，其中，所沉积的含铪层的厚度大约在2-1000之间。
18.根据权利要求17所述的方法，其中，膜后大约在10-50之间。
19.一种在原子层沉积过程中将一种铪化合物沉积到室内衬底上的方法，包括：
进行第一个包括铪前体的半反应；
进行第二个包括氧前体的半反应；
进行第三个包括氮前体的半反应；和
进行第四个包括硅前体的半反应。
20.根据权利要求19所述的方法，其中，铪前体选自(Et2N)4Hf、(Me2N)4Hf、(EtMeN)4Hf和Cl4Hf。
21.根据权利要求20所述的方法，其中，硅前体选自SiH4、Si2H6、Si3H8、Si2Cl6、、(Et2N)4Si、(Me2N)4Si、(Et2N)3SiH和(Me2N)3SiH。
22.根据权利要求21所述的方法，其中，氮前体选自氨、肼、叠氮化物和自由基氮化合物。
23.根据权利要求22所述的方法，其中，氧前体选自H2O、H2O2、有机过氧化物、O、O2、O3和自由基氧化合物。
24.根据权利要求19所述的方法，进一步包括：进行第五个包含铝前体的半反应，该前体选自Me3Al、Me2AlH、AlCl3、Me2AlCl和(PrO)3Al。
25.一种半导体材料的组合物，包括HfSixOyNz，
此处x至少为0.2但要小于4；
y至少为0.5但要小于4；和
z至少为0.05但要小于2。
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