CN101248212A - 电介质材料的等离子处理 - Google Patents

电介质材料的等离子处理 Download PDF

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Publication number
CN101248212A
CN101248212A CNA2006800226567A CN200680022656A CN101248212A CN 101248212 A CN101248212 A CN 101248212A CN A2006800226567 A CNA2006800226567 A CN A2006800226567A CN 200680022656 A CN200680022656 A CN 200680022656A CN 101248212 A CN101248212 A CN 101248212A
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China
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substrate
processing procedure
precursor
gas
nitrogen
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Inventor
S·穆图可芮西纳
R·谢芮哥潘尼
T·戈亚尔
P·K·那瓦卡
S·S·凯尔
K·Z·阿哈穆德
Y·马
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Applied Materials Inc
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Applied Materials Inc
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Abstract

本发明的一实施例是提供一种形成电介质材料的方法，其包括：于原子层沉积(ALD)制程中，使基板循序暴露于含金属前驱物以及氧化气体下，而形成氧化金属；接着，使基板暴露于惰性等离子制程以及热退火制程。一般来说，氧化金属包括铪、钽、钛、铝、锆、镧其中之一或其混合物。于一实验例中，基板暴露于不含氮或是实质不含氮的惰性等离子气体中，接着，基板于热退火制程中暴露于氧气环境下。于另一实验例中，基板于ALD制程中循序暴露于金属前驱物以及含水蒸气的氧化气体下，因而形成氧化金属材料，而水蒸气是由消耗氢气气源与氧气气源的催化性水蒸气产生器所形成。

Description

电介质材料的等离子处理
技术领域
本发明涉及一种于基板上沉积物质的方法，特别是一种于形成电介质堆迭(dielectric stack)之时，用以沉积及稳定电介质材料的方法。
背景技术
在半导体制程、平面显示器制程或是其他电子装置的制程当中，气相沉积制程在将材料沉积于基板上扮演一个重要的角色。随着电子装置的几何尺寸日渐减缩，且装置的密度持续增大，因此特征的尺寸与深宽比(aspect ratio)变得更具重要性，举例来说，特征尺寸小于等于65nm以及深宽比大于等于10的装置已列入考量重点。因此，材料以保形沉积(conformal deposition)的方式而形成上述装置已渐趋重要。
传统的化学气相沉积法(CVD)已成功证实可使装置的几何尺寸以及高宽比下降至0.15μm，因此更具竞争力的装置几何尺寸需要另一种沉积技术的出现。原子层沉积法(ALD)引起了广大的注意，于ALD制程中，反应气体不断地导入含有一基板的制程腔中，一般来说，第一反应物是输送至制程腔，并吸附至基板的表面，而第二反应物亦输送至制程腔，并与第一反应物反应而形成一沉积物质。在输送每一个反应气体之间通常会进行净化的步骤，而净化的步骤可以藉由载气(carrier gas)进行连续净化，或是于各个反应气体的输送之间进行脉冲净化。
原子层沉积制程已成功地用以沉积电介质层(dielectric layer)、障壁层(barrier layer)以及传导层(conductive layer)。以ALD制程进行沉积而应用于闸极以及电容器的高介电常数的电介质材料(高K电介质材料)包括有氧化铪(hafnium oxide)、硅酸铪(hafnium silicate)、氧化锆(zirconium oxide)或是氧化钽(tantalum oxide)。电介质材料，如高K电介质材料，于接续的加工制程中暴露于高温之下(＞500℃)，可能会出现形态上的改变。举例来说，氮化钛通常于600℃下藉由化学气相沉积法而沉积于氧化铪或是氧化锆上，而于上述的高温下，氧化铪或是氧化锆可能会结晶、丧失非结晶形与低漏电特性。另外，即使电介质材料的完全结晶情况可避免，暴露于高温下仍会使电介质材料形成晶粒成长以及/或相分离，进而因为高漏电流而导致装置的不良性能表现。
因此，于接续的加工制程中，能够形成一暴露于高温下而其型态仍稳定的电介质材料(特别是高K电介质材料)的制程实为必须。
发明内容
本发明的一实施例中提供了于一基板上形成一电介质材料的方法，其包括：于ALD制程中将基板循序暴露于一含金属前驱物以及一氧化气体下，而于基板上形成氧化金属材料，基板接着再暴露于惰性等离子制程以及热退火制程。惰性等离子制程将基板暴露于惰性气体所形成的等离子下约30秒～5分钟。于一实验例中，基板于热退火制程中加热至约600～1200℃，并持续2分钟，之后，含有氧化金属的基板于惰性等离子制程中暴露于无氮且等离子功率输出约为1800瓦的氩气等离子中约1～3分钟。接着，基板于含有氧气的退火腔中，在800～1100℃下进行热退火约10～30秒。
一般来说，氧化金属材料的厚度介于约5～100，并且含有铪、钽、钛、铝、锆、镧其中之一或其混合物。于一实验例中，氧化铪层的厚度约为40，且其电容至少为2.4μF/cm2。另一实验例中，该方法提供一前处理制程，而自基板表面移除自然氧化物，并接续于湿式清洗制程中形成一化学氧化层。于另一实验例中，该方法提供基板于沉积氧化金属层之后，并于惰性等离子制程之前暴露于一沉积后的退火制程。
本发明所揭露的另一实施例中，氧化金属层于ALD制程中形成，是循序将基板暴露于氧化气体以及至少一金属前驱物下，而于基板上形成氧化金属层。氧化气体包含有水蒸气，其是来自将氢气气源与氧气气源流入一水蒸气产生器所生成。金属前驱物包括铪前驱物、锆前驱物、铝前驱物、钽前驱物、钛前驱物、镧前驱物其中之一或其混合物。于一实验例中，是提供于基板上形成含铪材料的方法，包括使基板暴露于一沉积制程，而在基板上形成含氧化铪的电介质材料；基板利用无氮的氩气等离子而进行一惰性等离子制程；以及进一步于含氧环境中使基板暴露于一热退火制程。
本发明的另一实施例中是提供一于基板上形成电介质材料的方法，包括：基板暴露于一沉积制程而于其上形成一氧化金属层，并接着使基板暴露于一氮化等离子制程以及一热退火制程而形成氮氧化金属层。氧化金属层通常基本上不含有硅，并包括有铪、钽、钛、铝、锆、镧其中之一或其混合物。氮化等离子制程约持续1～3分钟，而等离子功率输出约为900～1800瓦。基板于热退火制程中加热至约600～1200℃，并持续约2分钟。于一实验例中，基板利用含有小于等于50体积％(vol％)氮气的制程气体进行氮化等离子制程，以形成含有氮浓度约5～25原子％(at％)的电介质材料。基板于含有氧气的制程腔中进行热退火约10～30秒，温度范围在800～1100℃。
一般来说，氮氧化电介质材料所具有的厚度约5～100，且其电容约小于等于2.4μF/cm2。于一实验例中，氮氧化电介质材料的厚度为50，电容约为2.35μF/cm2。于部分实验例中，该方法提供一前处理制程以自基板表面移除自然氧化物，并于接续的湿式清洗制程中形成化学氧化层。另一实验例中，该方法提供基板于沉积氧化金属层之后，以及进行氮化等离子制程之前，进行一沉积后的退火制程。
本发明的另一实施例中是提供一于基板上形成含铪材料的方法，包括：基板暴露于一沉积制程而于其上形成一含有氧化铪的电介质材料；基板暴露于一氮化等离子制程，而使氧化铪形成氮氧化铪；以及基板再接续暴露于一热退火制程。
附图说明
本发明于上方所详述的特征可详细地被了解，而针对本发明更特定的描述则简短摘录于上，可参阅实施例所述，且部分的实施例是绘示于附图中。然而，值得注意的是，附图仅绘示本发明的一般实施例，而并非用以限制其范围，其他相同效力的实施例应同属本发明的范畴。
图1，根据本发明的实施例绘示形成电介质材料的流程顺序；
图2A～2C，绘示根据图1所示的流程顺序的多个阶段中的基板状态；
图3，根据本发明的实施例而以图表绘示所形成的电介质材料的电气特性；
图4，根据本发明的另一实施例绘示形成电介质材料的流程顺序；
图5A～5C，绘示根据图4所示的流程顺序的多个阶段中的基板状态；以及
图6A～6B，根据本发明的实施例而以图表绘示所形成的电介质材料的电气特性。
主要元件符号说明
100  方法                    200  基板
201  层                      202  氧化层
204  经等离子处理后的氧化层  206  后退火层
400  步骤                    500  基板
501  层                      502  氧化层
504  氮氧化层                506  后退火层
具体实施方式
本发明的实施例是提供一种制备具有多应用性的电介质材料的方法，特别是应用于电晶体以及电容器加工制程所使用具有高介电常数(K)的电介质材料。原子层沉积(ALD)制程可用于控制所形成的电介质化合物的元素组成。于一实施例中，首先将一含有氧化金属的电介质层于ALD制程中将其沉积于一基板上；并使基板暴露于一惰性气体等离子制程而用以加密电介质层；接着，基板再暴露于一热退火制程，因而制备一电介质材料或是一电介质堆迭。本发明的另一实施例，是将一含有氧化金属的电介质层于ALD制程中将其沉积于一基板上，并使电介质层进行一氮化制程，则氧化金属形成氮氧化金属，接着，基板再暴露于一热退火制程，藉此，而制备一电介质材料或是一电介质堆迭。
电介质层通常包含一氧化金属，并可藉由ALD制程、传统的化学气相沉积(CVD)制程或是物理气相沉积(PVD)制程而被沉积。电介质层包括氧以及至少一额外元素，如：铪(hafnium)、钽(tantalum)、钛(titanium)、铝(aluminum)、锆(zirconium)、镧(lanthanum)其中之一元素或其混合物。举例来说，电介质层包括有氧化铪、氧化锆、氧化钽、氧化铝、氧化镧、氧化钛其中之一，或其衍生物或混合物。于一实施例中，电介质层包括一氧化金属，且基本上不含硅。本发明的实施例提供一种ALD制程，是将一基板循序暴露于一金属前驱物以及一氧化气体，而用以形成一电介质层。而其中一实验例中，氧化气体是包含有水蒸气，而其来自将氢气气源以及氧气气源流入一水蒸气产生器中所得。氢气气源可为氢气或是含氢的混合气体(forming gas)，而氧气气源可为氧气或是氧化亚氮。
电介质材料以惰性等离子进行稳定处理
如「图1」所示，是绘示形成一电介质材料(如：HfOx或TaOx)的范例方法100的流程图。「图2A～2C」与方法100相符，是绘示应用于半导体装置(如：电晶体或电容器)的电介质材料的形成过程。层201是包含一氧化层202设置于其上，并暴露于一惰性等离子制程以形成一经等离子处理后的氧化层204(「图2B」)，并接续暴露于热退火制程而转变为后退火层206(「图2C」)。
于沉积氧化层202之前，层201可先进行一前处理制程，用以使基板表面具有一较佳的官能基团。而有利于起始一沉积制程的官能基团包括有羟基(OH)、烷氧基(alkoxy；OR，其中R＝Me，Et，Pr或是Bu)、卤氧基(haloxyl；OX，其中X＝F，Cl，Br或是I)、卤化物(F，Cl，Br或是I)、氧自由基，以及胺基或是酰胺基(NR或NR2，其中R＝H，Me，Et，Pr或是Bu)。前处理制程可将基板暴露于一试剂下，如：NH3、B2H6、SiH4、SiH6、H2O、HF、HCl、O2、O3、H2O、H2O2、H2、氢原子、氮原子、氧原子、醇、胺其中之一，或其等离子、衍生物或混合物。官能基团是提供一基部而供导入的化学前驱物附着至基板表面。前处理制程可将基板200暴露于试剂下约1秒～2分钟之间，较佳的是介于5～60秒之间。前处理制程亦可包括将基板200暴露于RCA溶液(SC1/SC2)、HF-last溶液、来自WVG或ISSG系统的水蒸气、过氧化氢溶液、酸性溶液、碱性溶液其中之一、或其等离子、衍生物或混合物。有效的前处理制程是描述于本发明受让人所受让的美国专利公告第6858547号，以及同时另案待审的美国申请序号第10/302752号(2002年11月21号申请，公开号为US2003-0232501)，于此处将其整体并为参考文献，用以描述前处理方法以及前处理溶液的组成。
前处理制程的一实验例中，基板200于进行一湿式清洗制程之前会先将一自然氧化层移除，其可采用HF-last溶液来移除的，湿式清洗制程会使基板200上形成厚度约小于等于10(例如介于5～7之间)的化学氧化层，而湿式清洗制程可于TEMPESTTM湿式清洗系统(由加州圣克拉拉的Applied Materials公司所提供)中进行。另一实验例中，基板200于进行ALD制程之前，先暴露于WVG系统所提供的水蒸气中约15秒，而水蒸气可来自将氢气气源(如：氢气或是含氢的混合气体)以及氧气气源(如：氧气或是氧化亚氮)流入WVG系统中所得。
方法100的一实施例中，氧化层202于步骤402中藉由气相沉积制程(如ALD、CVD、PVD、热技术或其组合)而形成于层201上，如「第5A图」所示。于较佳的实施例中，氧化层202藉由本发明受让人所受让与同时另案待审的美国申请序号第11/127767号(2005年5月12号申请，公开号为US 2005-0271813)以及本发明受让人所受让与同时另案待审的美国申请序号第11/127753号(2005年5月12号申请，公开号为US2005-0271812)中所提及的ALD制程以及装置而将其沉积；并于此处将上述发明整体并为参考文献，用以描述ALD制程中所采用的方法与装置。氧化层202一般所沉积的厚度介于5～300之间，较佳为10～200之间，而更佳为20～100之间。于某些实验例中，氧化层202具有一介于10～60之间的厚度，较佳的是介于30～40之间。
氧化层202是沉积于基板200表面上，并可能具有多样的构成型态，包括同质的、异质的、多级的、单层或是多层的堆迭或是薄片。氧化层202是为具有高介电常数的材料，且通常含有氧化金属。因此，氧化层202包括氧以及至少一金属，如：铪(hafnium)、锆(zirconium)、钛(titanium)、钽(tantalum)、镧(lanthanum)、铝(aluminum)其中之一或其混合物。虽然可能会出现基板的硅扩散至氧化层202的现象，但是氧化层202通常基本上不含有硅。氧化层202的组成份可为一含铪材料，如：氧化铪(HfOx或HfO2)、氮氧化铪(HfOxNy)、铝酸铪(HfAlxOy)、氧化镧铪(HfLaxOy)；含锆材料，如：氧化锆(ZrOx or ZrO2)、氮氧化锆(ZrOxNy)、铝酸锆(ZrAlxOy)、氧化镧锆(ZrLaxOy)；其他含铝材料或是含镧材料，如：氧化铝(Al2O3 or AlOx)、氮氧化铝(AlOxNy)、氧化镧铝((LaAlxOy)、氧化镧(LaOx or La2O3)；或为其合金、衍生物或是上述成分的组合。其他可用于氧化层202的电介质材料包括氧化钛(TiOx or TiO2)、氮氧化钛(TiOxNy)、氧化钽(TaOx or Ta2O5)以及氮氧化钽(TaOxNy)。而可用于氧化层202的电介质材料的薄膜包括有HfO2/Al2O3、La2O3/Al2O3以及HfO2/La2O3/Al2O3。
于一实施例中，基板200可选择性地进行沉积后的退火(postdeposition anneal；PDA)制程。含有氧化层202的基板200转移至一退火腔中(如：加州圣克拉拉的Applied Materials公司所提供的CENTURARADIANCERTP chamber)，并进行PDA制程。退火腔可与沉积腔及/或等离子腔为一集结式制程工具(cluster tool)，藉此，基板200可在不接触周遭环境之前提下而进行退火制程。基板200可加热至温度范围600～1200℃，较佳的，介于600～1150℃，更佳的，介于600～1000℃。PDA制程会持续一段时间，约1秒～5分钟，较佳的约1～4分钟，更佳的约2～4分钟。一般来说，腔室的空气中包括至少一种退火气体，如：氧(O2)、臭氧(O3)、氧原子(O)、水(H2O)、一氧化氮(NO)、氧化亚氮(N2O)、二氧化氮(NO2)、五氧化二氮(N2O5)、氮(N2)、氨(NH3)、联胺(N2H4)、其中之一，或是其衍生物或其混合物。通常退火气体含有氮以及至少一种含氧气体，如氧气。腔室的气压介于5～100托(Torr)之间，比方说10托。PDA制程的一实验例中，含有氧化层202的基板200于氧气中加热至600℃并持续约4分钟。
步骤104中，氧化层202暴露于惰性等离子制程以加密电介质材料而形成经等离子处理后的氧化层204，如「图2B」所示。惰性等离子制程亦可包括一解偶惰性气体等离子制程(decoupled inert gas plasmaprocess)，是藉由将一惰性气体流入解偶等离子氮化(DPN)腔中，或是包括一引控式惰性气体等离子制程(remote inert gas plasma process)，是藉由一引控式等离子系统而将惰性气体导入制程腔中。
惰性等离子制程的一实施例中，基板200是转移至DPN腔中，如CENTURADPN chamber(如：加州圣克拉拉的Applied Materials公司所提供)，另一方面，DPN腔与用于沉积氧化层202的ALD腔属于相同的集结式制程工具，藉此，基板200则可在不暴露于周遭环境的条件下而进行惰性等离子制程。在惰性等离子制程中，氧化层202于DPN腔中会受到由流动的氩所形成的离子氩撞击。而惰性等离子制程中可能使用的气体包括氩、氦、氖、氙其中之一，或其混合物。
若任何氮气与惰性气体一起流入，则氮气会使电介质材料氮化，如：使氧化金属转变为氮氧化金属。用于氮化制程而可能存在于DPN腔中的微量氮气，可能会于进行等离子制程时不慎与惰性气体结合。惰性等离子制程所使用的气体包括至少一种惰性气体且不含氮气，或是仅含微量的氮气。于一实施例中，惰性气体中所残留的氮气浓度约小于等于1体积％(vol％)，较佳的，约小于等于0.1％，更佳的，约小于等于100ppm，比方说50ppm。于一实验例中，惰性等离子制程包括氩，且不含有或基本上不含氮气，因此，此惰性等离子制程增加了电介质材料的稳定性与密度，同时，降低了等效氧化层厚度(EOT)。
惰性等离子制程进行约10秒～5分钟，较佳的为30秒～4分钟，而更加的为1～3分钟之间。另外，惰性等离子制程所采用的等离子功率设定为500～3000瓦，较佳的则为700～2500瓦，更佳的为900～1800瓦。一般来说，等离子制程的工作周期约为50％～100％，而脉冲频率约为10kHz。DPN腔中的压力范围为10～80豪托，而惰性气体的流速则为10sccm～5slm，较佳的为50sccm～750sccm，更佳的则为100sccm～500sccm。于较佳的实施例中，惰性等离子制程中的DPN腔是产生无氮的氩气等离子。
另一实施例中，用于沉积氧化层202的制程腔亦可用于惰性等离子制程而形成经等离子处理后的氧化层204，而无须将基板200在制程腔之间搬移。举例来说，引控式氩气等离子可直接于安装有引控式等离子装置的制程腔(如ALD腔或CVD腔)中，与氧化层202接触而形成经等离子处理后的氧化层204。其他形成经等离子处理后的氧化层204的惰性等离子制程仍需仔细评估，如：以雷射退火对基板200进行处理。
于步骤106，基板200暴露于一热退火制程。于一实施例中，基板200转移至退火腔(如：加州圣克拉拉的Applied Materials公司所提供的CENTURARADIANCERTP chamber)中，并进行热退火制程。退火腔可与沉积腔及/或氮化腔属于相同的集结式制程工具，藉此，基板200在不接触周遭环境之前提下而进行退火。基板200可加热至600～1200℃，较佳的为700～1150℃，更佳的为800～1000℃。热退火制程会持续一段时间，约1～120秒，较佳的为2～60秒，更佳的为5～30秒。一般来说，腔室的空气中包括至少一种退火气体，如：氧(O2)、臭氧(O3)、氧原子(O)、水(H2O)、一氧化氮(NO)、氧化亚氮(N2O)、二氧化氮(NO2)、五氧化二氮(N2O5)、氮(N2)、氨(NH3)、联胺(N2H4)其中之一，或是其衍生物或其混合物。通常退火气体含有氮以及至少一种含氧气体，如氧气。腔室的气压介于5～100托之间，比方说10托。热退火制程的一实验例中，基板200于氧气中加热至1050℃并持续约15秒。另一实验例中，基板200于含有等体积的氮气与氧气的环境下加热至1100℃并持续约25秒。
如「图5C」所示，热退火制程将经等离子处理后的氧化层204转变为电介质材料或后退火层206。热退火制程修补了步骤104中等离子冲击所造成的损伤，并降低后退火层206的固定电荷。电介质材料维持非结晶形，并具有一氮浓度介于5～25原子％(at％)，较佳则介于10～20原子％，比方说15原子％。后退火层206的薄膜厚度介于5～300，较佳为10～200，更佳为20～100。于某些实验例中，后退火层206的厚度介于10～60，较佳则介于30～40。
「图3」以图表绘示皆含有氧化铪但暴露于不同等离子制程的二基板的电容相对于电压的表现。基板A暴露于氮化等离子制程，同时，基板B暴露于惰性等离子制程，接着，基板A与B于1000℃下进行本发明所述的热退火制程，并于表面量测电容，结果显示基板B相较于基板A具有较高的电容，基板A的最大电容约2.35μF/cm2，而基板B的最大电容为2.55μF/cm2。
于一实施例中，藉由本发明所述的沉积制程而沉积的电介质材料或后退火层206通常具有范围介于2～4μF/cm2的电容，较佳的是介于2.2～3μF/cm2，更佳的介于2.4～2.8μF/cm2。于一实验例中，不含氮气或是基本上不含氮气的电介质材料具有的电容值至少为2.4μF/cm2。
电介质材料以氮气进行稳定处理
如「图4」所示，是绘示形成一电介质材料(如氮氧化金属材料；HfOxNy或TaOxNy)的范例方法400的流程图。「图5A～5C」与方法骤400相符，是绘示应用于半导体装置(如：电晶体或电容器)的电介质材料的形成过程。层501是包含一氧化层502设置于其上，并暴露于一氮化制程以形成一氮氧化层504(「图5B」)，并接续暴露于一热退火制程而转变为后退火层506(「图5C」)。
于沉积氧化层502之前，层501可先进行一前处理制程，用以使基板500表面具有多样的官能基团。而有利于起始一沉积制程的官能基团包括有羟基(OH)、烷氧基(alkoxy；OR，其中R＝Me，Et，Pr或是Bu)、卤氧基(haloxyl；OX，其中X＝F，Cl，Br或是I)、卤化物(F，Cl，Br或是I)、氧自由基，以及胺基或是酰胺基(NR或NR2，其中R＝H，Me，Et，Pr或是Bu)。前处理制程可将基板暴露于一试剂下，如：NH3、B2H6、SiH4、SiH6、H2O、HF、HCl、O2、O3、H2O、H2O2、H2、氢原子、氮原子、氧原子、乙醇、胺其中之一，或其等离子、衍生物或混合物。官能基团是提供一基部以供导入的化学前驱物附着至基板表面。前处理制程可将基板500暴露于试剂下约1秒～2分钟的时间，较佳的是介于5～60秒之间。前处理制程亦可包括将基板500暴露于RCA溶液(SC1/SC2)、HF-last溶液、来自WVG或ISSG系统的水蒸气、过氧化氢溶液、酸性溶液、碱性溶液其中之一，或其等离子、衍生物或混合物。有效的前处理制程是描述于本发明受让人所受让的美国专利公告第6858547号，以及同时另案待审的美国申请序号第10/302752号(2002年11月21号申请，题目为「Surface Pre-Treatment for Enhancement of Nucleation of HighDielectric Constant Materials」，而公开号为US 2003-0232501)，于此处将其整体并为参考文献，用以描述前处理方法以及前处理溶液的组成。
前处理制程的一实验例中，基板500于进行一湿式清洗制程之前会先将一自然氧化层移除，其可采用HF-last溶液来移除的，湿式清洗制程会使基板500上形成厚度约小于等于10(例如介于5～7之间)的化学氧化层，而湿式清洗制程可于TEMPESTTM湿式清洗系统(加州圣克拉拉的Applied Materials公司所提供)中进行。另一实验例中，基板500于进行ALD制程之前，先暴露于WVG系统所提供的水蒸气中约15秒。
方法400的一实施例中，氧化层502于步骤402中藉由气相沉积制程(如ALD、CVD、PVD、热技术或上述制程的组成)而形成于层501上，如「图5A」所示。于一实施例中，氧化层502藉由ALD制程，以及方法100中所提及的装置而将其沉积。氧化层502一般所沉积的厚度介于5～300之间，较佳的是介于10～200之间，而更佳的是介于20～100之间。于某些实验例中，氧化层502具有一介于10～60之间的厚度，较佳的是介于30～40之间。
氧化层502是沉积于基板表面上，并可能具有多样的构成型态，包括同质的、异质的、多级的、单层或是多层的堆迭或薄片。氧化层502是为具有高介电常数的材料，且通常含有氧化金属或氮氧化金属。因此，氧化层502包括氧以及至少一金属，如：铪、锆、钛、钽、镧、铝其中之一或其混合物。虽然可能会出现基板的硅扩散至氧化层502的现象，但是氧化层502通常基本上不含有硅。氧化层502的组成份可为一含铪材料，如：氧化铪(HfOx或HfO2)、氮氧化铪(HfOxNy)、铝酸铪(HfAlxOy)、氧化镧铪(HfLaxOy)；含锆材料，如：氧化锆(ZrOx or ZrO2)、氮氧化锆(ZrOxNy)、铝酸锆(ZrAlxOy)、氧化镧锆(ZrLaxOy)；其他含铝材料或是含镧材料，如：氧化铝(Al2O3 or AlOx)、氮氧化铝(AlOxNy)、氧化镧铝(LaAlxOy)、氧化镧(LaOx or La2O3)；或为其合金、或衍生物或是上述成分的组合。其他可用于氧化层502的电介质材料包括氧化钛(TiOx or TiO2)、氮氧化钛(TiOxNy)、氧化钽(TaOx or Ta2O5)以及氮氧化钽(TaOxNy)。而可用于氧化层502的电介质材料的薄膜包括有HfO2/Al2O3、La2O3/Al2O3以及HfO2/La2O3/Al2O3。
于一实施例中，基板500可选择性地进行沉积后的退火(postdeposition anneal；PDA)制程。含有氧化层502的基板500转移至一退火腔中(如：加州圣克拉拉的Applied Materials公司所提供的CENTURARADIANCERTP chamber)，并进行PDA制程。退火腔可与沉积腔及/或氮化腔为一集结式制程工具，藉此，基板500可在不接触周遭环境之前提下而进行退火制程。基板500可加热至温度范围为600℃～1200℃，较佳的，介于600℃～1150℃，更佳的，介于600℃～1000℃。PDA制程会持续一段时间，约1秒～5分钟，较佳的，约5秒～4分钟，更佳的，约1～4分钟。一般来说，腔室的空气中包括至少一种退火气体，如：氧(O2)、臭氧(O3)、氧原子(O)、水(H2O)、一氧化氮(NO)、氧化亚氮(N2O)、二氧化氮(NO2)、五氧化二氮(N2O5)、氮(N2)、氨(NH3)、联胺(N2H4)其中之一，或是其衍生物或混合物。通常退火气体含有氮以及至少一种含氧气体，如氧气。腔室的气压介于5～100托(Torr)之间，比方说10托。PDA制程的一实验例中，含有氧化层502的基板500于氧气中加热至600℃并持续约4分钟。
于步骤404中，氧化层502暴露于一氮化制程而使氮原子物理性地并入电介质材料中而形成氮氧化层504，如「图5B」所示，而氮化制程亦使电介质材料的密度增加。氮化制程可包括解偶惰等离子氮化(DPN)、引控式等离子氮化以及于电介质沉积过程中(如：ALD或CVD制程)以热线诱导(hot-wired induced)氮原子及氮气并入。氮氧化层504的表面通常富含氮，而氮氧化层504中氮的浓度约为5～40原子％(at％)，较佳的为10～25原子％。而较佳的实施例是将氧化层502暴露于氮气等离子中，如DPN制程。
氮化制程的一实施例中，基板500是转移至DPN腔中，如CENTURADPN chamber(加州圣克拉拉的Applied Materials公司所提供)，另一方面，DPN腔与用于沉积氧化层502的ALD腔属于相同的集结式制程工具，藉此，基板500则可在不暴露于周遭环境的条件下而进行氮化制程。在DPN制程中，氧化层502会受到共流氮气的氮原子，以及惰性气体等离子(如：氩)的撞击。除了氮气，其他含氮气体亦可用于形成氮气等离子，如：氨(NH3)、联胺(如：N2H4或MeN2H3)、胺(如：Me3N、Me2NH或MeNH2)、苯胺(如：C6H5NH2)以及迭氮化物(azide)。等离子制程中可能使用的气体包括氩、氦、氖、氙其中之一或其混合物。
氮化等离子包括一氮气气源以及一惰性气体，藉此，包含氮气与惰性气体的混合物则成为制程气体而导入等离子腔中，或是氮气与惰性气体会单独流入或共同流入等离子腔中。氮化等离子中氮气的浓度介于5～95体积％，较佳的则为25～70体积％，更佳的为40～60体积％，而其余的部分皆为惰性气体。通常氮化等离子中的氮气浓度约小于等于50体积％。于一实验例中，氮气浓度约50体积％，而氩浓度亦为50体积％；于另一实验例中，氮气浓度约40体积％，而氩浓度为60体积％；又，于另一实验例中，氮气浓度约25体积％，而氩浓度为75体积％。
氮气的流速介于10sccm～5slm之间，较佳则介于50～500sccm，更佳则介于100～250sccm。惰性气体的流速则介于10sccm～5slm之间，较佳为50～750sccm，更佳为100～500sccm。包含氮气与惰性气体(单独流入或共流)的制程气体会形成一结合流速，其范围介于10sccm～5slm之间，较佳为100～750sccm，更佳为200～500sccm。DPN腔中的压力介于10～80豪托。氮化制程进行的时间范围为10秒～5分钟，较佳的则介于30秒～4分钟，更佳的则介于1～3分钟。另外，进行氮化制程的等离子功率设定为500～3000瓦，较佳为700～2500瓦，更佳则为900～1800瓦。一般来说，等离子制程的工作周期约50％～100％，而脉冲频率约为10kHz。于一较佳实施例中，氮化制程是为一DPN制程，并包括由氩和氮所共流形成的等离子。
于另一实施例中，用于沉积氧化层502的制程腔亦用于氮化制程而形成氮氧化层504，而无须将基板500于制程腔之间搬移。举例来说，引控式氮气等离子可直接于安装有引控式等离子装置的制程腔(如ALD腔或CVD腔)中，与氧化层502接触而形成氮氧化层504。氮自由基化合物亦会藉由热或是热线而产生，进而可应用于氮化制程。其他用以形成氮氧化层504的氮化制程仍需仔细评估，如：于含氮环境中对基板进行退火动作，及/或于形成氮氧化层504时，于ALD循环中的额外半反应导入一氮气前驱物。举例来说，ALD循环中用以形成氧化铪的额外半反应可包括在氨的脉冲后紧接着进行净化气体的脉冲。
于步骤406中，基板500是暴露于热退火制程。于一实施例中，基板500转移至退火腔(如：加州圣克拉拉的Applied Materials公司所提供的CENTURARADIANCERTP chamber)中，并进行热退火制程。退火腔可与沉积腔及/或氮化腔属于相同的集结式制程工具，藉此，基板500在不接触周遭环境之前提下而进行退火。基板500可加热至600～1200℃，较佳的为700～1150℃，更佳的为800～1000℃。热退火制程会持续一段时间，约1～120秒，较佳的约2～60秒，更佳的约5～30秒。一般来说，腔室的空气中包括至少一种退火气体，如：氧(O2)、臭氧(O3)、氧原子(O)、水(H2O)、一氧化氮(NO)、氧化亚氮(N2O)、二氧化氮(NO2)、五氧化二氮(N2O5)、氮(N2)、氨(NH3)、联胺(N2H4)其中之一、或是其衍生物或其混合物。通常退火气体含有氮以及至少一种含氧气体，如氧气。腔室的气压介于5～100托之间，比方说10托。热退火制程的一实验例中，基板500于氧气中加热至1050℃并持续约15秒。另一实验例中，基板500于含有等体积的氮气与氧气的环境下加热至1100℃并持续约25秒。
如「图5C」所示，热退火制程将氮氧化层504转变为电介质材料或后退火层506。热退火制程修补了步骤404中等离子冲击所造成的损伤，并降低后退火层506的固定电荷。电介质材料维持非结晶形，并具有一氮浓度介于5～25原子％(at％)，较佳的介于10～20原子％，比方说15原子％。后退火层506的薄膜厚度介于5～300之间，较佳为10～200，更佳则为20～100。于某些实验例中，后退火层506的厚度介于10～60之间，较佳的则介于30～40之间。
「图6A」以图表绘示皆含有氧化铪，但不暴露于或暴露于不同热制程的三基板的电容相对于电压的表现。基板A不暴露于等离子制程或热退火制程，基板B暴露于氮化等离子制程，并在500℃下暴露于热退火制程，基板C暴露于氮化等离子制程，并在1000℃下暴露于热退火制程，接着，于表面量测电容，结果显示，基板C相较于基板B具有较高的电容，而基板B亦相对基板A具有较高的电容。基板A的最大电容约1.75μF/cm2，基板B的最大电容为1.95μF/cm2，而基板C的最大电容为2.35μF/cm2。另外，经过热退火的基板B相对于基板A更具热稳定性。基板A也许在接续的制程中由于升温而结晶，而基板B则维持非结晶形。
「图6B」以图表绘示量测各表面漏电流的现象，其结果显示，基板C的电流密度相较基板A和B低两个层级，基板A和B的电流密度皆大于100A/cm2，而基板C的电流密度小于1A/cm2。
另外，已进行退火的基板B和C相较于基板A更具有热稳定性，而在较高温下进行退火的基板C又较基板B更具热稳定性。基板A在接续的制程中由于升温而结晶，而基板C则维持非结晶形，基板B则当温度高于500℃时可能出现结晶的现象。
于另一实施例中，藉由本发明所提及的沉积制程而沉积的电介质材料或后退火层506通常具有1.5～3μF/cm2的电容值，较佳的为2～2.7μF/cm2，更佳的为2.2～2.5μF/cm2。于一实验例中，电介质材料含有氮，并具有小于等于2.35μF/cm2的电容值。
等效氧化层厚度(EOT)标准是用于比较具有高介电常数的电介质材料于MOS栅极中的效能与氧化硅材料于MOS栅极中的效能。藉由EOT值可了解某一厚度具有高介电常数的电介质材料能够达到与某一厚度的氧化硅材料相同的栅电容。高K电介质材料相对于氧化硅(K值约3.9)具有较高的介电常数，因此材质的厚度与K值之间的关连可藉由EOT值来评估。举例来说，K值约32且层厚度为5nm的含铪材料，其EOT值约为0.6nm。因此，提高电介质材料的K值以及加密电介质材料以降低厚度，则EOT值会降低。亦即是，电介质材料的低EOT值是部分源自高K值以及藉由加密制程而形成的较薄、较密的层。
电介质材料的沉积制程
于此所述的电介质层通常包含一氧化金属材料，包括氧化层202和502，其是藉由ALD制程、传统CVD制程或PVD制程所沉积。于一实施例中，以一原子层沉积制程而于基板上形成电介质材料的方法包括：将基板置入一制程腔中，并接着将基板暴露于氧化气体以及至少一种前驱物，如：铪前驱物、锆前驱物、硅前驱物、铝前驱物、钽前驱物、钛前驱物、镧前驱物其中之一或其混合物。而沉积制程中可能形成的电介质材料包括氧化铪、氧化锆、氧化镧、氧化钽、氧化钛、氧化铝其中之一，或其衍生物或混合物。含有水蒸气的氧化气体可藉由将氢气气源与氧气气源流入水蒸气产生器中所生成。水蒸气产生器含有催化剂，其包含有钯、铂、镍、铁、铬、钌、铑其中之一或其混合物，或为其合金。氢气气源及/或氧气气源可藉由额外气体而将其稀释的，举例来说，于氮气中含有5％氢气的混合气体可用作为氢气气源。于某些实验例中，将过多的氧气气源提供入水蒸气产生器，则可产生含有富含氧气的水蒸气的氧化气体。于某些实验例中，在沉积氧化铪材料或其他氧化金属材料之后，基板于一预浸制程中暴露于一氧化气体。
形成氧化金属材料(如：氧化层202以及502)的ALD制程通常在1～100托的压力下的制程腔中进行，较佳为1～20托，更佳为1～10托。基板的温度通常维持在70～1000℃，较佳的为100～650℃，更佳的为250～500℃。ALD制程的进一步描述是揭露于本发明受让人所受让的美国申请序号第11/127767号(2005年5月12号申请，公开号为US2005-0271813)，并于此处将其整体并为参考文献，用以描述ALD制程中所采用的方法与装置。
于一实验例中，铪前驱物以5～200sccm的速率导入制程腔中，而铪前驱物通常由一载气导入，而其总流速介于50～1000sccm之间。铪前驱物亦可以0.1～10秒的速率脉冲至制程腔中，是视特殊制程条件、铪前驱物或沉积氧化铪材料的期望组成而定。于一实施例中，铪前驱物以1～5秒(如3秒)的速率脉冲至制程腔中；另一实施例中，铪前驱物以0.1～1秒(如0.5秒)的速率脉冲至制程腔中。于一实验例中，铪前驱物较佳为四氯化铪(HfCl4)，而于另一实验例中，铪前驱物较佳为四(二烷胺基)铪化合物，如：四(二乙基胺基)铪((Et2N)4Hf或TDEAH)。
铪前驱物通常藉由将一载气通过一含有铪前驱物的安瓿而导入制程腔中，而安瓿包括一个安瓿瓶、一圆形罩以及一用来容纳或分散化学前驱物的管柱或容器。一个适当的安瓿，如PROE-VAPTM，是由康乃迪克州丹伯里的Advanced Technology Materials公司所提供。于一实验例中，安瓿包含有HfCl4，并维持于150～200℃之下。于另一实验例中，安瓿包含有液体前驱物(如：TDEAH，TDMAH、TDMAS或Tris-DMAS)，并且为包含注射器阀系统的液体输送系统的一部份，用以将液体前驱物以加热的载气来蒸发的。一般来说，安瓿是加压于138kPa(约20psi)～414kPa(约60psi)，并加热至温度小于等于100℃，较佳的温度范围则为20～60℃。
氧化气体导入制程腔的流速约0.05～1000sccm，较佳为0.5～100sccm。氧化气体脉冲至制程腔中的流速约为0.05～10秒，较佳为0.08～3秒，更佳为0.1～2秒。于一实施例中，氧化气体的脉冲速率为1～5秒(如：约1.7秒)；于另一实施例中，氧化气体的脉冲速率为0.1～3秒(如：约0.5秒)。
氧化气体可由与制程腔之间可流通流体的水蒸气产生器(WVG)系统所产生。WVG系统藉由氧气气源(如：O2)与氢气气源(如：H2)于低温下(＜500℃)进行催化反应而产生超高纯度的水蒸气。而氢气与氧气气源流入WVG系统的流速为5～200sccm，较佳为10～100sccm。一般来说，氧气与氢气气源的流速可被单独调整而使氧化气体的流出物存在有氧气或氧气气源以及缺少氢气或氢气气源。
可用于产生含有水蒸气的氧化气体的氧气气源包括氧(O2)、臭氧(O3)、氧原子(O)、臭氧(O3)、氧化亚氮(N2O)、一氧化氮(NO)、二氧化氮(NO2)、五氧化二氮(N2O5)、过氧化氢(H2O2)其中之一，或其衍生物或混合物。可用于产生含有水蒸气的氧化气体的氢气气源包括氢气(H2)、氢原子(H)、含氢的混合气体(N2/H2)、氨(NH3)、碳氢化合物(如：CH4)、醇(如：甲醇)其中之一，或其衍生物或混合物。载气可与氧气气源或氢气气源共流，且载气可为氮气、氦气或氩气其中之一或其混合物。较佳的，氧气气源为氧气或氧化亚氮，氢气气源为氢气或含氢的混合气体(如氮气中含有5体积％的氢气)。
氢气气源以及氧气气源可藉由载气而稀释的，藉此，于沉积制程中提供对氧化气体中水蒸气的敏感控制。于一实施例中，较低的水蒸气流速(＜10sccm水蒸气)较利于完成ALD制程中形成含铪材料或其他电介质材料的化学反应。较低的水蒸气流速稀释了氧化气体中水蒸气的浓度，而稀释后的水蒸气浓度恰可氧化基板表面所吸附的前驱物，因此，较低的水蒸气流速将水蒸气暴露后所进行的净化次数降到最低，进而提升了制造生产力。另外，较低的水蒸气流速藉由避免不期望获得的共反应而降低了微粒污染物的形成。质流控制器(MFC)可用于控制氢气气源的流速为约0.5sccm，而同时产生水蒸气的气流流速为0.5sccm。然而，大多数的MFC系统无法于慢速之下提供一致的流速，因此，稀释的氢气气源(如：含氢的混合气体)可用于WVG系统中以达到较慢的水蒸气流速。于一实验例中，流速为10sccm且为含有5％氢气的混合气体的氢气气源由WVG系统送出流速为0.5sccm的水蒸气。于另一实施例中，较高的水蒸气流速(＞10sccm水蒸气)较利于完成ALD制程中形成含铪材料或其他电介质材料的化学反应。举例来说，约100sccm的氢气传送约100sccm的水蒸气。
含氢的混合气体可选自其氢气浓度相对于载气(如：氩或氮)的体积百分比为1％～95％。一方面，含氢的混合气体的氢气浓度相对于载气的体积百分比为1～30％，较佳为2～20％，更佳为3～10％，举例来说，一种含氢的混合气体是含有5％氢气及95％氮气。另一方面，含氢的混合气体的氢气浓度相对于载气的体积百分比为30～95％，较佳为40～90％，更佳为50～85％，举例来说，一种含氢的混合气体是含有80％氢气及20％氮气。
于一实验例中，WVG系统接收到流速为10sccm且含5％氢气(95％氮气)的氢气气源，以及流速为10sccm的氧气气源(如：氧气)，进而形成流速约为0.5sccm且含有水蒸气的氧化气体，以及流速约为9.8sccm的氧气。于另一实验例中，WVG系统接收到流速约为20sccm且含5％氢气混合气体的氢气气源，以及流速约为10sccm的氧气气源，进而形成流速约为1sccm且含有水蒸气的氧化气体，以及流速约为9sccm的氧气。又另一实验例中，WVG系统接收到氢气流速约为20sccm的氢气气源，以及流速约为10sccm的氧气气源，进而形成流速约为10sccm且含有水蒸气的氧化气体，以及流速约为9.8sccm的氧气。再者，另一实验例中，做为氧气气源的氧化亚氮与氢气气源于ALD制程中形成水蒸气。一般来说，2莫耳当量的氧化亚氮可用来取代1莫耳当量的氧气。
WVG系统含有一催化剂，如：内含催化剂的反应器或是催化剂管柱，于此，含有水蒸气的氧化气体由氢气气源与氧气气源之间的催化性化学反应生成。WVG系统不似热解产生器是藉由燃烧而产生水蒸气，且通常反应温度高于1000℃。WVG系统含有催化剂，且通常于低温下(约100～500℃)产生水蒸气，较佳为小于等于350℃。催化剂反应器中的催化剂可为金属或合金，如：钯、铂、镍、铁、铬、钌、铑其中之一，或其合金或混合物。于本发明中，超高纯度的水为ALD制程的理想所需，于一实施例中，为避免未反应的氢顺流而下，则氧气气源可于WVG系统中流洗5秒，接着，氢气气源再进入反应器5秒。氧气与氢气气源(如H2和O2)之间的催化反应会生成水蒸气。调控氧气与氢气气源的流动可获得对含有水蒸气的氧化气体中氧气与氢气浓度的正确控制。水蒸气中可能含有残留的氢气气源、氧气气源其中之一或其混合物。适合的WVG系统是可购得，如：加州圣克拉拉的Fujikin of America公司的Water Vapor Generator(WVG)system，或是加州蒙罗公园市的Ultra Clean Technology的CatalystSteam Generator System(CSGS)。
净化气体或载气(较佳为氩或氮)的脉冲于ALD循环中铪前驱物、氧化气体或其他前驱物的每次脉冲后，连续地导入制程腔。净化气体或载气的脉冲的流速通常约为2～22slm，较佳为10slm。每一次制程循环的发生时间范围约为0.01～20秒，于一实验例中，制程循环持续约10秒；其他的实验例中，制程循环持续约2秒。持续约10秒的较长制程循环步骤可沉积绝佳的氧化铪薄膜，但却降低了生产率。特殊的净化气体流速与制程循环的持续时间是透过实验而决定的。一实验例中，于相同的持续时间下，300nm直径的晶片相对于200mm直径的晶片需要两倍的流速，藉此才可维持相近的生产效率。
于一实施例中，氢气作为载气、净化气体及/或反应气体以减少卤素对沉积材料的污染。含有卤素原子(如：HfCl4、ZrCl4和TaF5)之前驱物会很快地污染已沉积的电介质材料。氢气为还原剂，并产生卤化氢(如：HCl或HF)，其是具挥发性且为可移除的副产物。因此，在前驱物化合物(如：铪前驱物)的存在下，氢气可作为载气或反应气体，并可再包括另一载气(如：氩气或氮气)。于一实验例中，水/氢混合物于温度范围约100～500℃下用于降低卤素浓度并增加已沉积材料的氧气浓度。于一实验例中，水/氢混合物源自将过量的氢气气源导入WVG系统而形成富含氢的水蒸气。
于此处所提及的用以沉积材料的部分实施例中，可采用另一种氧化气体(如：传统的氧化剂)而取代由WVG系统所生成的含有水蒸气的氧化气体。另一种氧化气体是自含有水的氧气气源而导入制程腔中，而此氧气气源并非源自WVG系统、氧(O2)、臭氧(O3)、氧原子(O)、过氧化氢(H2O2)、氧化亚氮(N2O)、一氧化氮(NO)、五氧化二氮(N2O5)、二氧化氮(NO2)其中之一，或其衍生物或混合物。本发明的实施例所提供的制程是藉由来自WVG系统所形成的含有水蒸气的氧化气体，而亦有其他实施例所提供的制程是于形成含铪材料或其他电介质材料的沉积制程中，利用另一种的氧化气体或传统的氧化剂。
多种前驱物皆列于本发明的可用于沉积电介质材料的实施例范围中。前驱物的一种重要特征需具有适合的蒸汽压力，前驱物于室温及室压下可能为气体、液体或是固体，然而，ALD腔中需使用挥发的前驱物。有机金属化合物含有至少一种金属原子以及至少一种含有机物的官能基团，如：酰胺(amide)、烷基(alkyl)、烷氧基(alkoxyl)、烷基酰胺(alkylamido)或苯胺(anilide)。前驱物可能包括有机金属、无机或卤化物化合物。
铪前驱物的范例包括含有配位基(如：卤化物、烷基酰胺、环戊二烯基、烷基、烷氧化物其中之一，或其衍生物或混合物)的铪化合物。可用作为铪前驱物的卤化铪化合物包括HfCl4、Hfl4和HfBr4；可用作为铪前驱物的烷基酰胺铪包括(RR’N)4Hf，其中R与R’是为独立的氢、甲基、乙基、丙基或丁基。而可用作为沉积含铪材料的铪前驱物包括有(Et2N)4Hf、(Me2N)4Hf、(MeEtN)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，(NO3)4Hf、(tBuO)4Hf、(iPrO)4Hf、(EtO)4Hf、(MeO)4Hf，或其衍生物。其中，于沉积制程中所使用的铪前驱物较佳为HfCl4、(Et2N)4Hf或(Me2N)4Hf。
于另一实施例中，多种的氧化金属或是氮氧化金属可藉由将金属前驱物与源自WVG系统的含水蒸气的氧化气体进行连续脉冲所得。此处所揭露的ALD制程可略做修改，是以其他金属前驱物取代铪前驱物，以形成额外的电介质材料，如：铝酸铪、铝酸钛、氮氧化钛、氧化锆、氮氧化锆、铝酸锆、氧化钽、氮氧化钽、氧化钛、氧化铝、氮氧化铝、氧化镧、氮氧化镧、铝酸镧其中之一，或其合金、衍生物或混合物。于一实施例中，两个以上的ALD制程是共同进行以将层沉积于另一层上。举例来说，一个组合式制程包括形成第一电介质材料的第一ALD制程，以及形成第二电介质材料的第二ALD制程，上述组合式制程是用于产生多样的含铪材料，例如：硅酸铝铪、或是氮氧化硅铝铪。于一实验例中，一电介质堆迭是包括于基板上沉积第一含铪材料之后，再接续于上沉积第二含铪材料，而第一、第二含铪材料在成分上可为不相同，因此一层可能含有氧化铪，而另一层则可能含有硅酸铪。一方面，通常较下方的层含有硅。ALD制程中所使用的其他金属前驱物包括：ZrCl4、Cp2Zr、(Me2N)4Zr、(Et2N)4Zr、TaF5，TaCl5、(tBuO)5Ta、(Me2N)5Ta、(Et2N)5Ta、(Me2N)3Ta(NtBu)、(Et2N)3Ta(NtBu)、TiCl4、Til4、(iPrO)4Ti、(Me2N)4Ti、(Et2N)4Ti、AlCl3、Me3Al、Me2AlH、(AMD)3La、((Me3Si)(tBu)N)3La、((Me3Si)2N)3La、(tBu2N)3La、(iPr2N)3La其中之一，或其衍生物或混合物。
此处所使用的「基板表面」是指基板上方进行薄膜制程的基板或材料表面，举例来说，制程进行的基板表面成分包括有：硅、氧化硅、应变硅、绝缘层上覆硅(SOI)、掺杂碳的氧化硅、氮化硅、掺杂硅、锗、砷化镓、玻璃、蓝宝石，以及其他物质如：金属、氮化金属、金属合金以及其他传导物质，是视其应用而定。障壁层以及基板表面的金属或氮化金属包括钛、氮化钛、钽以及氮化钽。基板不但具有多种尺寸(如：200mm或300mm直径的晶片)以及矩形或正方形的栅格(panes)。除非特别注明，此处所提及的实施例以及实验例较佳以直径200mm或300mm的基板为例，且更佳为300mm。此处所揭露的制程实施例是将含铪材料沉积于多种基板与表面，而本发明的基板可利用于但不限于半导体晶片，如：结晶硅(如：Si<100>或Si<111>)、氧化硅、应变硅、硅锗、掺杂或不掺杂的多晶硅、掺杂或不掺杂的硅晶片以及产品或控片晶片。基板可进行前处理制程以对基板的表面执行磨光、蚀刻、还原、氧化、羟化及/或退火处理。
「原子层沉积」或「循环性沉积」于此处是指连续导入两种以上的反应化合物以将材料层沉积于基板表面。二、三或多种反应化合物可选择性地导入制程腔的反应区中，通常将每一个反应化合物之间以时间作一区分，而使每一个化合物能吸附及/或与基板表面反应。一方面，第一前驱物或是化合物A脉冲进入反应区后，接续一段第一缓冲时间，之后，第二前驱物或化合物B脉冲进入反应区，并同样接续一段第二缓冲时间。于每段缓冲时间内，净化气体(如氮气)会导入制程腔以净化反应区或是移除反应区中任何残留的反应化合物或是副产物。另外，净化气体亦可于沉积制程中持续流动，因此在反应化合物脉冲之间的缓冲时间仅有净化气体在流动。反应化合物亦可选择性地脉冲，直到已达到基板表面所需的薄膜厚度。另一情况是，ALD制程中的脉冲化合物A、净化气体、脉冲化合物B以及净化气体是为一循环，而循环可由化合物A或B开始并接续循环，直到已达到基板表面所需的薄膜厚度。另一实施例，第一前驱物包含化合物A，第二前驱物包含化合物B，第三前驱物包括化合物C，且三者分别脉冲入制程腔，其中，第一前驱物的脉冲亦可与第二前驱物的脉冲时间重迭，而第三前驱物的脉冲则不与第一或第二前驱物的脉冲时间重迭。
「脉冲」是指一特殊的化合物于间歇地或非连续地导入制程腔的反应区中，而特殊化合物于每次脉冲的量随时间会有不同，是视脉冲的持续时间而定，而每一次脉冲的持续时间是依据多个因子而有不同，如：制程腔的体积容量、与制程腔所结合的真空系统以及特殊化合物本身的挥发度/反应度。「半反应」于此处是指前驱物脉冲步骤后，再接续一个净化步骤。
实验例
实验例1～10是于CENTURA基台上进行，包括有TEMPESTTM湿式清洗系统、ALD腔、CENTURADPN(解偶等离子氮化)腔，以及CENTURARADIANCERTP(热退火)腔，上述所有的器材皆可自加州圣克拉拉的Applied Materials公司获得。实验于直径300mm的基板上进行，且基板表面暴露于HF-last溶液以移除自然氧化物，并接续置入湿式清洗系统以形成厚度约为5的化学氧化层。数个与WVG系统连接的ALD腔是进一步描述于本发明受让人所受让及同时另案待审的美国申请序号第11/127753号(2005年5月12号申请，而公开号为US2005-0271812)，于此处将其整体并为参考文献，用以描述ALD制程所使用的方法与装置。另一个可采用的ALD腔是进一步描述于本发明受让人所受让的美国专利公告第6916398号，并同样于此处将其整体并为参考文献，用以描述ALD制程所使用的方法与装置。WVG系统所使用的金属催化剂是自加州圣克拉拉的Fujikin of America公司所获得，而WVG系统是将一氢气气源(含5体积％氢气的氮气)以及一氧气气源(氧气)产生一氧化气体。
实验例1-HfOx沉积-将含有化学氧化物表面的基板置入ALD腔内，藉由将基板循序暴露于铪前驱物(HfCl4)与含有水蒸气的氧化气体中，而使得于ALD制程中形成一氧化铪层。ALD循环包括接连脉冲HfCl4与水蒸气，并以一氮气净化循环分隔每一个前驱物，而重复ALD循环以得到厚度约40的氧化铪层。基板转移至DPN腔中，并暴露于惰性等离子制程(含有氩气等离子)，惰性等离子制程包括流速约200sccm的氩气流，并进行90秒，等离子功率为1800瓦，工作周期50％，脉冲频率10kHz，而用以加密氧化铪层。基板接着转移至热退火腔，并于维持在15托压力的氧气/氮气环境下，于1000℃下加热约15秒。
实验例2-HfOx沉积-将含有化学氧化物表面的基板置入ALD腔内，藉由将基板循序暴露于铪前驱物(TDEAH)与含有水蒸气的氧化气体中，而使得于ALD制程中形成一氧化铪层。ALD循环包括接连脉冲TDEAH与水蒸气，并以一氮气净化循环分隔每一个前驱物，而重复ALD循环以得到厚度约50的氧化铪层。基板转移至DPN腔中，并暴露于惰性等离子制程(含有氩气等离子)，惰性等离子制程包括流速约200sccm的氩气流，并进行90秒，等离子功率为1800瓦，工作周期50％，脉冲频率10kHz，而用以加密氧化铪层。基板接着转移至热退火腔，并于维持在15托压力的氧气/氮气环境下，于1000℃下加热约15秒。
实验例3-TaOx沉积-将含有化学氧化物表面的基板置入ALD腔内，于ALD制程中利用钽前驱物(TaCl5)与水而在基板表面形成氧化钽层。ALD循环包括接连脉冲TaCl5与水蒸气，并以一氮气净化循环分隔每一个前驱物，而重复ALD循环以得到厚度约100的氧化钽层。基板转移至DPN腔中，并暴露于惰性等离子制程(含有氩气等离子)，惰性等离子制程包括流速约200sccm的氩气流，并进行60秒，等离子功率为1800瓦，工作周期50％，脉冲频率10kHz，而用以加密氧化钽层。基板接着转移至热退火腔，并于维持在10托压力的氧气/氮气环境下，于1000℃下加热约15秒。
实验例4-ZrOx沉积-将含有化学氧化物表面的基板置入ALD腔内，藉由将基板循序暴露于锆前驱物(ZrCl4)与含有水蒸气的氧化气体中，而使得于ALD制程中形成一氧化锆层。ALD循环包括接连脉冲ZrCl4与水蒸气，并以一氮气净化循环分隔每一个前驱物，而重复ALD循环以得到厚度约60的氧化锆层。基板转移至DPN腔中，并暴露于惰性等离子制程(含有氩气等离子)，惰性等离子制程包括流速约200sccm的氩气流，并进行2分钟，等离子功率为1800瓦，工作周期50％，脉冲频率10kHz，而用以加密氧化锆层。基板接着转移至热退火腔，并于维持在25托压力的氧气/氮气环境下，于950℃下加热约30秒。
实验例5-HfOxNy沉积-将含有化学氧化物表面的基板置入ALD腔内，藉由将基板循序暴露于铪前驱物(HfCl4)与含有水蒸气的氧化气体中，而使得于ALD制程中形成一氧化铪层。ALD循环包括接连脉冲HfCl4与水蒸气，并以一氮气净化循环分隔每一个前驱物，而重复ALD循环以得到厚度约40的氧化铪层。基板转移至DPN腔中，并暴露于氮化等离子制程，用以加密氧化铪层，并将氮原子并入氧化铪层中以形成氮氧化铪材料。氮化制程包括流速约40sccm的氮气流，并进行180秒，等离子功率为1800瓦，工作周期50％，脉冲频率10kHz。基板接着转移至热退火腔，并于维持在15托压力的氧气/氮气环境下，于1000℃下加热约15秒。
实验例6-HfOxNy沉积-将含有化学氧化物表面的基板置入ALD腔内，藉由将基板循序暴露于铪前驱物(TDEAH)与含有水蒸气的氧化气体中，而使得于ALD制程中形成一氧化铪层。ALD循环包括接连脉冲TDEAH与水蒸气，并以一氮气净化循环分隔每一个前驱物，而重复ALD循环以得到厚度约50的氧化铪层。基板转移至DPN腔中，并暴露于氮化等离子制程，用以加密氧化铪层，并将氮原子并入氧化铪层中以形成氮氧化铪材料。氮化制程包括流速约160sccm的氩气流以及流速约40sccm的氮气流，并进行180秒，等离子功率为1800瓦，工作周期50％，脉冲频率10kHz。基板接着转移至热退火腔，并于维持在15托压力的氧气/氮气环境下，于1050℃下加热约12秒。
实验例7-TaOxNy沉积-将含有化学氧化物表面的基板置入ALD腔内，于ALD制程中利用钽前驱物(TaCl5)与水而在基板表面形成氧化钽层。ALD循环包括接连脉冲TaCl5与水蒸气，并以一氮气净化循环分隔每一个前驱物，而重复ALD循环以得到厚度约100的氧化钽层。基板转移至DPN腔中，并暴露于氮化等离子制程，用以加密氧化钽层，并将氮原子并入氧化钽层中以形成氮氧化钽材料。氮化制程包括流速约120sccm的氩气流以及流速约80sccm的氮气流，并进行120秒，等离子功率为1800瓦，工作周期50％，脉冲频率10kHz，而用以加密氧化钽层。基板接着转移至热退火腔，并于维持在10托压力的氧气/氮气环境下，于1000℃下加热约15秒。
实验例8-ZrOxNy沉积-将含有化学氧化物表面的基板置入ALD腔内，藉由将基板循序暴露于锆前驱物(ZrCl4)与含有水蒸气的氧化气体中，而使得于ALD制程中形成一氧化锆层。ALD循环包括接连脉冲ZrCl4与水蒸气，并以一氮气净化循环分隔每一个前驱物，而重复ALD循环以得到厚度约60的氧化锆层。基板转移至DPN腔中，并暴露于氮化等离子制程，用以加密氧化锆层，并将氮原子并入氧化锆层中以形成氮氧化锆材料，氮化制程包括流速约100sccm的氩气流以及流速约100sccm的氮气流，并进行60秒，等离子功率为1800瓦，工作周期50％，脉冲频率10kHz。基板接着转移至热退火腔，并于维持在25托压力的氧气/氮气环境下，于950℃下加热约30秒。
实验例9-「图3A」的HfOx沉积-氧化铪层于相同的制程条件下沉积于基板A和B上，基板A转移至DPN腔并暴露于氮化等离子制程，氮化制程包括流速约160sccm的氩气流以及流速约40sccm的氮气流，并进行180秒，等离子功率为1800瓦，工作周期50％，脉冲频率10kHz。基板B转移至DPN腔并暴露于惰性等离子制程(含有氩气等离子)，惰性等离子制程包括流速约200sccm的氩气流，并进行90秒，等离子功率为1800瓦，工作周期50％，脉冲频率10kHz，而用以加密氧化铪层。基板A与B接着转移至热退火腔，并于维持在15托压力的氧气/氮气环境下，于1000℃下加热约15秒。
量测二表面的电容，结果显示基板B相对于基板A具有较高的电容，基板A的最大电容约为2.35μF/cm2，而基板B的最大电容为2.55μF/cm2。
实验例10-「图6A～6B」的HfOx沉积-氧化铪层于相同的制程条件下沉积于基板A、B和C上。基板A并未暴露于惰性等离子制程或热退火制程，基板B和C则转移至DPN腔，并分别地暴露于相同的氮化等离子制程，而加密氧化铪层，并将氮原子并入氧化铪层中以形成氮氧化铪材料。氮化制程包括流速约160sccm的氩气流以及流速约40sccm的氮气流，并进行180秒，等离子功率为1800瓦，工作周期50％，脉冲频率10kHz。基板B转移至热退火腔，并于维持在15托压力的氧气/氮气环境(约0.1体积％)下，于500℃下加热约15秒。基板C转移至热退火腔，并于维持在15托压力的氧气/氮气环境(约0.1体积％)下，于1000℃下加热约15秒。
量测各表面的电容，结果显示基板C相对于基板B具有较高的电容，且基板B亦相较于基板A有较高的电容(「图6A」)。基板A的最大电容为1.75μF/cm2，基板B的最大电容为1.95μF/cm2，而基板C的最大电容为2.35μF/cm2。
亦量测各表面的漏电流情形，结果显示基板C的电流密度相较基板A和B低两个层级(「图6B」)，基板A和B的电流密度皆大于100A/cm2，而基板C的电流密度小于1A/cm2。
于一实验例中，「表1」显示含有氧化铪的基板在不经过等离子制程或是热退火制程者，相较于进行该些制程的相似基板而具有较低的电容。虽然二基板皆进行氮化等离子制程，但进行高温热退火制程(如：相对于500℃而较高温的1000℃)的基板具有较高的电容。另外，虽然二基板皆于1000℃下进行热退火制程，但进行惰性等离子制程(如：含氩)的基板相对于进行氮化等离子制程的基板具有较高的电容。
                           表1
  实验例及基板   等离子制程   热退火(℃)   电容(μF/cm2)
  实验例9-基板A   氮气   1,000   2.35
  实验例9-基板B   氩气   1,000   2.55
  实验例10-基板A   无   无   1.75
  实验例10-基板B   氮气   500   1.95
  实验例10-基板C   氮气   1,000   2.35
惟本发明虽以较佳实施例说明如上，然其并非用以限定本发明，任何熟习此技术人员，在不脱离本发明的精神和范围内所作的更动与润饰，仍应属本发明的技术范畴。

Claims (60)

1.一种于基板上形成电介质材料的方法，包括：
将该基板置于制程腔中；
将氢气气源以及氧气气源流入水蒸气产生器中，以形成包含水蒸气的氧化气体；
于原子层沉积制程中，使该基板循序暴露于该氧化气体以及至少一含金属前驱物之中，而于该基板上形成电介质材料；
使该基板暴露于惰性气体等离子，而于惰性等离子制程中加密该电介质材料；以及
使该基板暴露于热退火制程之下。
2.如权利要求1所述的方法，其中该氢气气源为氢气或含氢的混合气体，而该氧气气源为氧气或氧化亚氮。
3.如权利要求2所述的方法，其中该至少一含金属前驱物是选自于由铪前驱物、锆前驱物、铝前驱物、钽前驱物、钛前驱物、镧前驱物以及其混合物所组成的群组。
4.如权利要求3所述的方法，其中该电介质材料包括至少一材料，其是选自于由氧化铪、氧化锆、氧化镧、氧化钽、氧化钛、氧化铝、其合金、其衍生物以及其混合物所组成的群组。
5.如权利要求4所述的方法，其中该基板于形成该电介质材料之前，使该基板进行湿式清洗制程以形成厚度小于等于10的氧化层。
6.如权利要求1所述的方法，其中该惰性气体等离子包括气体，其是选自于由氩、氦、氖以及其混合物所组成的群组。
7.如权利要求6所述的方法，其中该惰性气体等离子包括氩，且不含有或基本上不含有氮。
8.如权利要求7所述的方法，其中该基板暴露于具有功率输出为500～3000瓦的该惰性气体等离子下，持续时间为30秒～5分钟。
9.如权利要求8所述的方法，其中该功率输出为900～1800瓦，而持续时间为1～3分钟。
10.如权利要求7所述的方法，其中该热退火制程的进行时间为1～120秒，进行温度为600～1200℃。
11.如权利要求10所述的方法，其中该进行时间为5～30秒，而该进行温度为800～1100℃。
12.如权利要求11所述的方法，其中该基板于该热退火制程中是暴露于含氧环境下。
13.如权利要求4所述的方法，其中该电介质材料的厚度为5～100。
14.如权利要求13所述的方法，其中该电介质材料包括氧化铪，且厚度为10～60。
15.如权利要求13所述的方法，其中该基板于进行该原子层沉积制程之后，以及该惰性等离子制程之前，进行沉积后的退火制程。
16.如权利要求14所述的方法，其中该含铪材料的电容至少为2.4μF/cm2。
17.一种于基板上形成电介质材料的方法，包括：
于原子层沉积制程中，使该基板循序暴露于至少含金属前驱物以及氧化气体下，而于该基板上形成氧化金属材料；
使该基板暴露于惰性气体等离子，而于惰性等离子制程中加密该氧化金属材料；以及
使该基板暴露于热退火制程之下。
18.如权利要求17所述的方法，其中该原子层沉积制程更包括将氢气气源以及氧气气源流入水蒸气产生器中，以形成该氧化气体以及包含水蒸气的该氧化气体。
19.如权利要求18所述的方法，其中该氢气气源为氢气或含氢的混合气体，而该氧气气源为氧气或氧化亚氮。
20.如权利要求19所述的方法，其中该至少一含金属前驱物是选自于由铪前驱物、锆前驱物、铝前驱物、钽前驱物、钛前驱物、镧前驱物以及其混合物所组成的群组。
21.如权利要求20所述的方法，其中该氧化金属材料包括至少一材料，其是选自于由氧化铪、氧化锆、氧化镧、氧化钽、氧化钛、氧化铝、其合金、其衍生物以及其混合物所组成的群组。
22.如权利要求17所述的方法，其中该惰性气体等离子包括气体，其是选自于由氩、氦、氖以及其混合物所组成的群组。
23.如权利要求22所述的方法，其中该基板暴露于具有功率输出为500～3000瓦的该惰性气体等离子，持续时间为30秒～5分钟。
24.如权利要求23所述的方法，其中该功率输出为900～1800瓦，而持续时间为1～3分钟。
25.如权利要求22所述的方法，其中该惰性气体等离子包括氩，且不含有或基本上不含有氮。
26.如权利要求25所述的方法，其中该热退火制程的进行时间为1～120秒，进行温度为600～1200℃。
27.如权利要求26所述的方法，其中该进行时间为5～30秒，而该进行温度为800～1100℃。
28.如权利要求26所述的方法，其中该基板于该热退火制程中暴露于含氧环境下。
29.如权利要求25所述的方法，其中该氧化金属材料包括至少一元素，其是选自于由铪、钽、钛、铝、锆、镧以及其混合物所组成的群组。
30.如权利要求29所述的方法，其中该氧化金属材料的厚度为5～100。
31.如权利要求30所述的方法，其中该氧化金属材料包括氧化铪，且厚度为10～60。
32.如权利要求30所述的方法，其中该氧化金属材料的电容至少为2.4μF/cm2。
33.如权利要求29所述的方法，其中该基板于形成该电介质材料之前，该基板进行湿式清洗制程以形成厚度小于等于10的氧化层。
34.如权利要求33所述的方法，其中该基板于进行该原子层沉积制程之后，以及该惰性等离子制程之前，进行沉积后的退火制程。
35.一种于基板上形成含铪材料的方法，包括：
使该基板暴露于沉积制程下，而于该基板上形成含氧化铪的电介质材料；
使该基板暴露于惰性气体等离子，而于惰性等离子制程中加密该电介质材料，其中该惰性气体等离子包括氩，且不含有或基本上不含有氮；以及
使该基板暴露于包含有氧气的热退火制程下。
36.如权利要求35所述的方法，其中该含铪材料的电容至少为2.4μF/cm2。
37.如权利要求35所述的方法，其中用以形成该电介质材料的沉积制程为原子层沉积制程，包括将该基板循序暴露于氧化气体以及含铪前驱物下，以形成该含有氧化铪的电介质材料，其中该氧化气体包含水蒸气，且源自将氢气气源以及氧气气源流入水蒸气产生器中所形成。
38.如权利要求37所述的方法，其中该氢气气源为氢气或含氢的混合气体，而该氧气气源为氧气或氧化亚氮。
39.一种于基板上形成电介质材料的方法，包括：
使该基板暴露于沉积制程下，而于该基板上形成氧化金属层；
使该基板暴露于氮化等离子制程下，而于该基板上形成氮氧化金属层；以及
使该基板暴露于热退火制程下，以形成该电介质材料。
40.如权利要求39所述的方法，其中该氮化等离子制程的进行时间为1～3分钟，且功率输出为900～1800瓦。
41.如权利要求40所述的方法，其中该氮化等离子制程包括氮气浓度小于等于50体积％的制程气体。
42.如权利要求41所述的方法，其中该电介质材料的氮浓度为5～25原子％。
43.如权利要求42所述的方法，其中该氧化金属层基本上不含有硅。
44.如权利要求39所述的方法，其中该氧化金属层包括至少一元素，其是选自于由铪、钽、钛、铝、锆、镧以及其混合物所组成的群组。
45.如权利要求44所述的方法，其中该热退火制程的进行时间为5～30秒，进行温度为800～1100℃。
46.如权利要求45所述的方法，其中该基板于该热退火制程中是暴露于含氧环境下。
47.如权利要求39所述的方法，其中该电介质材料的厚度为5～100。
48.如权利要求47所述的方法，其中该电介质材料包括氮氧化铪，且厚度为10～60。
49.如权利要求48所述的方法，其中该电介质材料的电容至少为2.4μF/cm2。
50.如权利要求39所述的方法，其中该氧化金属层是由原子层沉积制程所形成。
51.如权利要求50所述的方法，其中该基板于进行该原子层沉积制程之前，该基板进行湿式清洗制程以形成厚度小于等于10的氧化层。
52.如权利要求51所述的方法，其中该基板于进行该原子层沉积制程之后，以及该氮化等离子制程之前，进行沉积后的退火制程。
53.如权利要求50所述的方法，其中该原子层沉积制程包括将该基板循序暴露于氧化气体以及至少一含金属前驱物下，而在该基板上形成该氧化金属层。
54.如权利要求53所述的方法，其中该氧化气体包含水蒸气，且源自将氢气气源以及氧气气源流入水蒸气产生器中所形成。
55.如权利要求54所述的方法，其中该氢气气源为氢气或含氢的混合气体，而该氧气气源为氧气或氧化亚氮。
56.如权利要求55所述的方法，其中该含金属前驱物是选自于由铪前驱物、锆前驱物、铝前驱物、钽前驱物、钛前驱物、镧前驱物以及其混合物所组成的群组。
57.一种于一基板上形成一含铪材料的方法，包括：
使该基板暴露于沉积制程下，而于该基板上形成含氧化铪的电介质材料；
使该基板暴露于氮化等离子制程，而使氧化铪形成氮氧化铪；以及
使该基板暴露于包含有氧气的热退火制程下。
58.如权利要求57所述的方法，其中该含铪材料的电容至少为2.4μF/cm2。
59.如权利要求57所述的方法，其中用以形成该电介质材料的沉积制程为原子层沉积制程，包括将该基板循序暴露于氧化气体以及含铪前驱物，以形成含氧化铪的该电介质材料，其中该氧化气体包含水蒸气，且源自将氢气气源以及氧气气源流入水蒸气产生器中所形成。
60.如权利要求59所述的方法，其中该氢气气源为氢气或含氢的混合气体，而该氧气气源为氧气或氧化亚氮。
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