CN101896638A - 基于新型钛、锆和铪前体形成高k介电膜的方法及其在半导体制造中的用途 - Google Patents

基于新型钛、锆和铪前体形成高k介电膜的方法及其在半导体制造中的用途 Download PDF

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CN101896638A
CN101896638A CN2007800204948A CN200780020494A CN101896638A CN 101896638 A CN101896638 A CN 101896638A CN 2007800204948 A CN2007800204948 A CN 2007800204948A CN 200780020494 A CN200780020494 A CN 200780020494A CN 101896638 A CN101896638 A CN 101896638A
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mecp
nme
etcp
formula
net
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CN101896638B (zh
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C·杜萨拉
N·布拉斯科
A·潘沙尔
C·拉绍
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Abstract

在基底上沉积含金属的介电膜的方法，该介电膜包含式(I)的化合物：(M1 1-aM2 a)ObNc (I)其中0≤a<1，0<b≤3，0≤c≤1，M1代表选自(Hf)、(Zr)和(Ti)的金属；且M2代表金属原子，该方法包括下列步骤：步骤a)，将基底供应到反应室中；步骤b)，将式(II)的含M1金属的前体气化，从而形成第一气相金属源：(R1 yOp)x(R2 tCp)zM1R’4-x-z (II)其中：0≤x≤3，优选地x＝0或1，0≤z≤3，优选地z＝1或2，1≤(x+z)≤4，0≤y≤7，优选地y＝2，0≤t≤5，优选地t＝1，(R1 yOp)代表未取代或取代的戊二烯基配体；(R2 tCp)代表未取代或取代的环戊二烯基配体；步骤c)，将第一气相金属源引入反应室中，以使它们与所述基底接触，从而在所述基底上沉积包含如上定义的式(I)化合物的含金属的介电膜。式(II1)的化合物：(R2 tCp)M1[N(R39)(R40)]3 (II1)；其相当于x＝0、z＝1且R’代表基团N(R39)(R40)时的如权利要求1所述的式(II)。

Description

基于新型钛、锆和铪前体形成高k介电膜的方法及其在半导体制造中的用途 
本发明涉及形成高k介电膜(如铪或锆的氧化物或氧氮化物)的方法及其用于制造半导体的用途。 
随着下一代半导体器件的临界尺寸的缩小，需要引入新材料，尤其具有高介电常数的新材料。在CMOS构造中，需要高k电介质代替通常具有大约1纳米SiO2等效厚度的达到其物理极限的SiO2。 
类似地，在用于RAM用途的金属-绝缘体-金属构造中需要高k电介质。多种金属组合物已经被认为既满足材料要求(介电常数、漏电流、结晶温度、电荷俘获)，又满足集成要求(界面处的热稳定性、干蚀刻可行性......)。 
基于第IV族的材料，如HfO2、HfSiO4、ZrO2、ZrSiO4、HfZrO4、HfLnOx(Ln选自钪、钇和稀土元素)，更通常地，HfMOx和ZrMOx，其中M是选自第II族、第IIIa族和第IIIb族的元素或过渡金属，属于最有前途的材料。此外，第IV族金属组合物也可以被考虑用于电极和/或Cu扩散势垒用途，如用于中能隙金属栅极的TiN，和用于MIM电极的HfN、ZrN、HfSi、ZrSi、HfSiN、ZrSiN、TiSiN。 
能以合理生产量和可接受的纯度实现这类膜的沉积的主要工业选择是气相沉积技术，如MOCVD(金属-有机化学气相沉积)或ALD(原子层沉积)。这类沉积法需要必须满足适当工业用途的严厉要求的金属前体。这些方法需要金属-有机或者金属-卤化物前体。多种铪和锆金属-有机化合物已经被视为能够实现这种沉积的前体。 
卤化物，如HfCl4、ZrCl4，是最常见的Hf/Zr前体并且已经广为描述。Kim等人公开了使用HfCl4通过ALD沉积HfO2(Kim等人，Electrochem Soc Proceedings 2005-05，397，2005)。但是，沉积过程中生成的一些副产物，如HCl或Cl2，会造成表面/界面粗糙，这对最终性能有害。根据所用氧源，其它可能的副产物可能是危险的。例如，已经通过QMS，经由OCl片段检出作为HfCl4和O3之间反应副产物的OCl2。此外，在高k氧化物的情况下，Cl或F杂质对最终电性能非常有害。 
Triyoso等人和Chang等人分别研究了Hf(OtBu)4用于HfO2 MOCVD和ALD的用途[Triyoso等人；J.Electrochem.Soc.152(3)G203-G209(2005)；Chang等人；Electrochem.Solid.State Let.，7(6)F42-F44(2004)]。Williams等人已经评测了Hf(mmp)4和Hf(OtBu)2(mmp)2用于HfO2的MOCVD。在WO2003035926中，Jones等人公开了被给体官能化的烷氧基配体(1-甲氧基-2-甲基-2-丙氧基化物[OCMe2CH2OMe，mmp])改进的固体Ti、Hf、Zr和La前体，该配体有助于抑制Zr和Hf的醇盐化合物的低聚，并提高其对湿气的稳定性。但是，如Potter等人所指出，所有这些醇盐前体具有不能在ALD法中实现自限沉积的缺点(R.J.Potter，P.R.Chalker，T.D.Manning，H.C.Aspinall，Y.F.Loo，A.C.Jones，L.M.Smith，G.W.Critchlow，M.Schumacher，Chem.Vap.Deposition，2005，11，N°3，159-167)。 
烷基氨化物前体，如Hf(NEtMe)4、Hf(NMe2)4、Hf(NEt2)4，已经广泛公开在文献中[Senzaki等人，J.Vac.Sci.Technol.A 22(4)，2004年7月/8月；Haussmann等人，Chem.Mater.2002，14，4350-4353；Kawahara等人，J.Appl.Phys.，第43卷，N°7A，2004，第4129-4134页；Hideaki等人，JP2002093804；Metzner等人，US6858547；Dip等人，US20050056219 A1]。第IV族烷基氨化物适用于ALD和MOCVD法。此外，一些在室温下是液体(Hf(NEt2)4和Hf(NEtMe)4)并具有足够挥发性，而且对于有限热预算法，它们能够在低温下进行自限ALD。但是，第IV族烷基氨化物，特别是Zr化合物的烷基氨化物具有几种缺点，包括它们可能在分配过程中在一定程度上分解，可能造成进料管或气化器的堵塞，它们可能在沉积过程中产生粒子，它们可能在深槽沉积法中带来不均匀组成，且它们只适于 窄的自限ALD温度范围，因此降低了工艺操作范围。特别地，Zr(NEtMe)4可能在分配管道中分解，并在高于170℃时产生粒子，而这是常见的分配温度。Hf(NEtMe)4更加热稳定，但在300℃以上由于热分解而不能承受自限原子层沉积。 
WO 2007/055088中，Thenappan等人公开了铪和锆的胍根合络合物及其用于气相沉积的用途。例举了Hf(NEt2)2[(NiPr-CNEt2)2。但是，胍根合铪和锆通常是挥发性非常有限的固体。如热重分析中所例证的那样，不能在没有热分解和后续粒子生成风险的情况下获得蒸气相Hf(NEt2)2[(NiPr-CNEt2)2。 
Lehn等人(Chem.Vap.Deposition，2006，12，280-284)公开了四(三甲基肼合)锆[Zr(NMeNMe2)4]和铪及其用于低温CVD的用途。例举的化合物具有可接受的挥发性(在所报道的0.06Torr，90℃下升华)，但它们在室温下是固体。 
Carta等人公开了双(环戊二烯基)双二甲基铪[HfCp2Me2]的用途(Carta等人在Electrochem Soc Proceedings，260，2005-09，2005中公开)，几位作者(Codato等人，Chem Vapor Deposition，159，5，1995；Putkonen等人，J Mater Chem，3141，11，2001；Niinisto等人，Langmuir，7321，21，2005)提出了作为铪和锆烷基氨化物的替代物的新型Zr和Hf化合物：双(环戊二烯基)双二甲基铪，双(环戊二烯基)双二甲基锆，其能够实现ALD操作范围最高达400℃的的有效ALD沉积法，并在最优化条件中用H2O作为共反应物获得含少于0.2％C的膜。但是，HfCp2Me2和ZrCp2Me2都具有在室温下是固体产品的缺点(HfCp2Me2熔点为57.5℃)。这妨碍了IC制造者以工业方式使用这些前体，即使用离域容器填充，并带来便利性和工艺问题。 
在US 6,743,473中，Parkhe等人公开了(Cp(R)n)xMHy-x用于制造金属和/或金属氮化物层的用途，其中M选自钽、钒、铌和铪，Cp是环戊二烯基，R是有机基团。仅公开了钽和铌环戊二烯基化合物的实例。但是，没有公开液态前体或熔点低于50℃的前体。
Heys等人最近在WO 2006/131751 A1中提出了液态双(环戊二烯基)衍生物。但是，它们具有挥发性有限的缺点并且也构成大的位阻，这可能限制所实现的生长速率。 
现在需要提供液态或低熔点(<50℃)第IV族前体化合物，特别是Hf和Zr化合物，其能够同时实现适当分配(物理状态，在分配温度下的热稳定性)、宽的自限ALD操作范围、和通过ALD或MOCVD沉积纯膜。 
根据本发明，已发现某些基于环戊二烯基或戊二烯基的第IV族金属-有机前体适用于通过ALD或MOCVD法沉积含第IV族金属的膜，并具有下列优点：
-它们在室温下是液体或具有低于50℃的熔点， 
-它们是热稳定的，能够实现适当分配(气相或直接液体注射)，且无粒子生成， 
-它们是热稳定的，具有宽的自限ALD操作范围， 
4)能够通过使用共反应物(选自H2、NH3、O2、H2O、O3、SiH4、Si2H6、Si3H8、TriDMAS、BDMAS、BDEAS、TDEAS、TDMAS、TEMAS、(SiH3)3N、(SiH3)2O、TMA或含铝前体、TBTDET、TAT-DMAE、PET、TBTDEN、PEN、含镧系元素的前体，如Ln(tmhd)3……)中的一种或它们的组合沉积含各种第IV族金属的膜。 
根据第一实施方案，本发明涉及在基底上沉积含至少一种金属的介电膜的方法，该介电膜包含式(I)的化合物： 
(M1 1-a M2 a)ObNc    (I) 
其中： 
0≤a<1， 
0<b≤3，优选地1.5≤b≤2.5； 
0≤c≤1， 
M1代表选自铪(Hf)、锆(Zr)和钛(Ti)的金属；且
M2代表选自镁(Mg)、钙(Ca)、锌(Zn)、硼(B)、铝(A)、铟(In)、硅(Si)、锗(Ge)、锡(Sn)、铪(Hf)、锆(Zr)、钛(Ti)、钒(V)、铌(Nb)、钽(Ta)的金属原子；和镧系原子，更特别地，钪(Sc)、钇(Y)、镧(La)和稀土金属原子， 
该方法包括下列步骤： 
-步骤a)，将基底供应到反应室中； 
-步骤b)，将至少一种式(II)的含M1金属的前体气化，从而形成第一气相金属源： 
(R1 yOp)x(R2 tCp)z M1R’4-x-z    (II) 
其中： 
M1定义如上； 
0≤x≤3，优选地x＝0或1； 
0≤z≤3，优选地z＝1或2； 
1≤(x+z)≤4； 
0≤y≤7，优选地y＝2； 
0≤t≤5，优选地t＝1； 
(R1 yOp)代表戊二烯基(Op)配体，其未被取代或被一个或多个R1基团取代，y代表在所述戊二烯基配体上的R1取代基的数； 
(R2 tCp)代表环戊二烯基(Cp)配体，其未被取代或被一个或多个R2基团取代，t代表在所述环戊二烯基配体上的R1取代基的数； 
R1和R2相同或不同，并独立地选自由下述基团组成的组：氯；具有1至4个碳原子的直链或支链烷基；N-烷基氨基，其中烷基是直链或支链的并具有1至4个碳原子；N，N-二烷基氨基，其中各烷基彼此相同或不同，是直链或支链的并具有1至4个碳原子；具有1至4个碳原子的直链或支链烷氧基；烷基甲硅烷基酰胺基团；脒根(amidinate)基团；和羰基； 
R’代表独立地选自由下述基团组成的组的配体：氢、氟、氯、溴或碘原子；具有1至4个碳原子的直链或支链烷基；N-烷基氨基，其中烷基是直链或支链的并具有1至4个碳原子；N，N-二烷基氨基，其中各烷基彼此 相同或不同，是直链或支链的并具有1至4个碳原子；具有1至4个碳原子的直链或支链烷氧基；烷基甲硅烷基氨基，其中烷基是直链或支链的并具有1至4个碳原子；二烷基甲硅烷基氨基，其中各烷基彼此相同或不同，是直链或支链的并具有1至4个碳原子；三烷基甲硅烷基氨基，其中各烷基彼此相同或不同，是直链或支链的并具有1至4个碳原子；脒根基团；和羰基，要理解的是，如果所述式(II)包含超过一个的R’基团，各R’可以彼此相同或不同； 
-任选地，步骤b’)，将至少一种含M2金属的前体气化，从而形成任选的第二气相金属源，其中M2定义如上； 
-步骤c)，将所述第一气相金属源和所述任选的第二气相金属源引入反应室中以使它们与所述基底接触，从而在所述基底上沉积包含如上定义的式(I)化合物的含金属的介电膜； 
条件是，如果要形成的含至少一种金属的介电膜包含式(I’)的化合物： 
M1 1O2    (I’) 
其相当于a＝0、b＝2且c＝0时的如上定义的式(I)，且如果步骤b)中所涉及的含M1金属的前体是式(II’)的化合物： 
(R2 tCp)2M1R’2    (II’) 
其相当于x＝0且z＝2时的如上定义的式(II)，则在所述式(II’)中，在两个(R2 tCp)配体的至少一个中，t>0。 
在如上定义的方法中，所述至少一种式(II)的含金属的前体和，如果必要，所述至少一种含M2金属的前体，具有通常低于50℃、优选低于35℃的熔点，且它们优选在室温下是液体。 
根据如上定义的方法的一个具体实施方案，气化步骤b)和如果必要，气化步骤b’)通过将载气引入含所述至少一种式(II)的含M1金属的前体和，如果必要，所述至少一种含M2金属的前体的加热容器中而进行： 
(R1 yOp)x(R2 tCp)z M1R′4-x-z  (II) 
该容器优选在能使所述金属源处于液相的温度和足够蒸气压下加热。 如果必要，可以将这两种金属前体之一或二者混入溶剂或混入溶剂混合物和/或混入稳定剂中。所述溶剂例如选自辛烷、己烷、戊烷或四甲基硅烷。金属前体在溶剂或溶剂混合物中的浓度通常为0.01M至0.5M，更特别为大约0.05M。载气选自，但不限于，Ar、He、H2、N2或其混合物。如果必要，该容器可以在80至110℃的温度范围加热。本领域技术人员会理解，可以调节容器温度以控制要气化的前体量。 
载气流速通常为10sccm(标准立方厘米)至500sccm。优选地，载气流速为50sccm至200sccm。 
根据如上定义的本发明的另一具体实施方案，气化步骤b)和，如果必要，气化步骤b’)通过将式(II)的含M1金属的前体和如果必要，含M2金属的前体以液体形式引入气化器(其在此气化)来进行： 
(R1 yOp)x(R2 tCp)z M1R′4-x-z  (II) 
如果必要，可以将这两种金属前体之一或二者混入溶剂或混入溶剂混合物和/或混入稳定剂中。所述溶剂例如选自辛烷、己烷、戊烷或四甲基硅烷。金属前体在溶剂或溶剂混合物中的浓度通常为0.01M至0.5M，更特别为大约0.05M。 
根据更特别的实施方案，气化步骤b)和气化步骤b’)合并成这两种源的一个气化步骤b”)。 
在如上定义的方法的步骤c)中，将气化的含金属的前体引入反应室，其在此接触基底。 
在本发明中，基底是指半导体制造中使用的任何基底，其由于它们的技术功能，要求被含金属的膜涂覆。这类基底例如不仅选自硅基底(Si)、二氧化硅基底(SiO2)、氮化硅基底(SiN)或氧氮化硅基底(SiON)，还选自钨基底(W)或贵金属基底，如铂基底(Pt)、钯基底(Pd)、铑基底(Rh)或金基底(Au)。 
将基底加热至以足够的生长速率和以所需物理状态和组成获得所需膜所需的温度。
步骤c)中的温度通常为150℃至600℃。该温度优选低于或等于450℃。
控制反应室中的压力从而以足够的生长速率获得所需含金属的膜。步骤c)中的压力通常为大约1mTorr(0.1333224Pa)至大约100Torr(13332.24Pa)。 
在本发明中，含M2金属的前体选自由下述物质组成的组： 
硅衍生物或其锗同系物，例如： 
二硅氧烷、三甲硅烷基胺、二硅烷、三硅烷、式(III1)的烷氧基硅烷 
SiHx(OR3)4-x，    (III1) 
其中：0≤x≤3且R3代表具有1至6个碳原子的直链或支链烃基； 
式(III2)的硅烷醇衍生物： 
Si(OH)x(OR4)4-x    (III2) 
其中：1≤x≤3且R4代表具有1至6个碳原子的直链或支链烃基，优选为Si(OH)(OR4)3，更优选为Si(OH)(OtBu)3； 
式(III3)的氨基硅烷衍生物： 
SiHx(NR5R6)4-x    (III3) 
其中：0≤x≤3，且R5和R6相同或不同并独立地代表氢原子或具有1至6个碳原子的直链或支链烷基，优选SiH(NMe2)3(TriDMAS)、SiH2(NHtBu)2(BTBAS)；SiH2(NEt2)2(BDEAS)，及其混合物； 
铝衍生物，例如三甲基铝[Al(CH3)3]、二甲基氢化铝[AlH(CH3)2]、式(IV1)的烷氧基铝烷： 
AlR8 x(OR7)3-x  (IV1) 
其中0≤x≤3，且R7代表具有1至6个碳原子的直链或支链烷基，且R8与R7相同或不同，代表氢原子，或优选AlR9R10(OR7)，其中R9和R10相同或不同，它们独立地代表具有1至6个碳原子的直链或支链烷基，最优选AlMe2(OiPr)； 
式(IV2)的酰氨基铝烷： 
AlR11 x(NR12R13)3-x  (IV2) 
其中：0≤x≤3，且R12和R13相同或不同，代表氢原子或具有1至6个碳原子的直链或支链烷基，且R11与R7相同或不同并代表氢原子或具有 1至6个碳原子的直链或支链烷基； 
钽衍生物，例如：Ta(OMe)5、Ta(OEt)5、Ta(NMe2)5、Ta(NEt2)5、Ta(NEt2)5、式(V1)的钽衍生物： 
Ta(OR14)4[O-C(R15)(R16)-CH2-OR17] 
其中R14、R15、R16和R17相同或不同，独立地代表氢原子或具有1至6个碳原子的直链或支链烷基，优选Ta(OEt)4(OCMe2CH2-OMe)(TAT-DMAE)，式(V2)的钽衍生物： 
Ta(OR18)4[O-C(R19)(R20)-CH2-N(R21)(R22)]    (V2) 
其中R18、R19、R20、R21和R22相同或不同，独立地代表氢原子或具有1至6个碳原子的直链或支链烷基，式(V3)的钽衍生物： 
Ta(＝NR24)(NR25R26)3  (V3) 
其中R24、R25和R26相同或不同，独立地代表氢原子或具有1至6个碳原子的直链或支链烷基； 
铌衍生物，例如：Nb(OMe)5、Nb(OEt)5、Nb(NMe2)5、Nb(NEt2)4、Nb(NEt2)5、式(VI1)的铌衍生物： 
Nb(OR27)4(O-C(R28)(R29)-CH2-OR30)    (VI1) 
其中R27、R28、R29和R30相同或不同，独立地代表氢原子或具有1至6个碳原子的直链或支链烷基，优选Nb(OEt)4(OCMe2CH2-OMe)(NBT-DMAE)，式(VI2)的铌衍生物： 
Nb(OR31)4[O-C(R32)(R33)-CH2-N(R34)(R35)]  (VI2) 
其中R31、R32、R33、R34和R35相同或不同，独立地代表氢原子或具有1至6个碳原子的直链或支链烷基，式(VI3)的铌衍生物： 
Nb(＝NR36)(NR37R38)3    (VI3) 
其中R36、R37和R38相同或不同，独立地代表氢原子或具有1至6个碳原子的直链或支链烷基； 
镧系元素衍生物，例如钪衍生物、钇衍生物、铈衍生物、镨衍生物、钆衍生物、镝衍生物、铒衍生物、镧衍生物、带有至少一个β-二酮配体或至少一个任选被一个或数个具有1至6个碳原子的直链或支链烷基取代的 环戊二烯基配体的衍生物； 
二价金属衍生物，例如锶(Sr)、钡(Ba)、镁(Mg)、钙(Ca)或锌(Zn)衍生物，带有至少一个β-二酮配体或至少一个任选被一个或数个具有1至6个碳原子的直链或支链烷基取代的环戊二烯基配体； 
其它金属衍生物，例如钨(W)、钼(Mo)、铪(Hf)或锆(Zr)衍生物，例如烷氧基衍生物、氨基衍生物或含有这些物质的加合物，要理解的是，所述衍生物不是如上定义的式(II)的化合物。 
根据另一具体实施方案，如上定义的方法包括： 
-步骤d)，其中在步骤c)之前将所述至少一种式(II)的含M1金属的前体和如果必要，所述至少一种含M2金属的前体混入至少一种反应物质中。 
在本发明中，针对的目标金属基膜，选择所述至少一种反应物质。 
根据另一实施方案，反应物质是氧源，更特别是氧(O2)、含氧自由基O·或OH·(例如通过远距等离子体产生的)、臭氧(O3)、湿气(H2O)和H2O2及其混合物。 
根据另一实施方案，反应物质是氮源，更特别是氮(N2)、含氮自由基(例如N·、NH·、NH2 ·)、氨(NH3)、肼(NH2NH2)及其烷基或芳基衍生物、以及它们的混合物。 
根据另一实施方案，反应物质既是氮源和又是氧源，更特别是NO、NO2、N2O、N2O5、N2O4及其混合物。 
根据所需N/O比，如果必要，用在上述方法中的反应物质可以是氧源、氧源的混合物、氮源的混合物、氧和氮的源、或它们的混合物。 
根据本发明的另一实施方案，如果目标金属基膜含有碳，例如但不限于金属碳化物或金属碳氮化物，则至少一种反应物质是碳源，更特别是甲烷、乙烷、丙烷、丁烷、乙烯、丙烯、叔丁烯。 
根据本发明的另一实施方案，如果目标金属基膜含有硅，例如但不限于金属的硅化物、硅-氮化物、硅酸盐或硅-碳-氮化物，则至少一种反应物质是硅源，例如：二硅氧烷、三甲硅烷基胺、二硅烷(Si2H6)、三硅烷(Si3H8)、 上述式(III1)、(III2)或(III3)的烷氧基硅烷，例如SiH(NMe2)3(TriDMAS)；SiH2(NHtBu)2(BTBAS)；SiH2(NEt2)2(BDEAS))及其混合物。 
根据另一具体实施方案，上述方法包括： 
-步骤d′)，其中将所述至少一种式(II)的含M1金属的前体和如果必要，所述至少一种含M2金属的前体在反应室中混入至少一种反应物质中。 
将所述至少一种式(II)的含M1金属的前体和如果必要，所述至少一种含M2金属的前体、和所述至少一种反应物质引入反应室中的模式通常取决于膜在基底上的沉积模式。所述含金属的前体和反应物质通常在化学气相沉积法同时引入，或在原子层沉积法相继引入，或根据几种组合方式引入，例如在脉冲改性原子层沉积法中，其中在一次脉冲中将所述至少一种式(II)的含M1金属的前体和如果必要，所述至少一种含M2金属的前体一起引入，并在单独的脉冲中引入所述至少一种反应物质；或在脉冲化学气相沉积法中，其中脉冲引入所述至少一种式(II)的含M1金属的前体和如果必要，所述至少一种含M2金属的前体，并连续引入所述至少一种反应物质。 
根据本发明的另一实施方案，使所述至少一种反应物质经过远离反应室的等离子系统，并分解成自由基。 
根据另一实施方案，上述方法的步骤(b)由步骤(b 1 )和步骤(b2)构成，其中步骤(b 1 )为将至少一种式(II)的第一含金属的前体与至少下列第二前体混合在一起：M1(NMe2)4、M1(NEt2)4、M1(NMeEt)4、M1(mmp)4、M1(OtBu)4、M1(OtBu)2(mmp)2及其混合物，步骤(b2)为将所述混合物气化。 
根据更特别的实施方案，本发明涉及上述沉积包含式(I)化合物的含金属的介电膜的方法，其中含M1金属的前体具有式(II1)： 
(R2 tCp)M1[N(R39)(R40)]3    (II1) 
其相当于x＝0、z＝1且R’代表基团N(R39)(R40)时的式(II)，其中R39和R40相同或不同，独立地代表氢原子、具有1至4个碳原子的直链或支链烷基、烷基甲硅烷基(其中烷基是直链或支链的并具有1至4个碳原 子)、二烷基甲硅烷基(其中各烷基彼此相同或不同，是直链或支链的并具有1至4个碳原子)、或三烷基甲硅烷基(其中各烷基彼此相同或不同，是直链或支链的并具有1至4个碳原子)。 
根据更特别的实施方案，本发明涉及上述沉积包含式(I1)化合物的含金属的介电膜的方法： 
M1O2    (I1) 
其相当于a＝0、b＝2且c＝0的式(I)，其中式(II)的含金属的前体选自由下述物质组成的组：HfCp2Cl2、Hf(MeCp)2Me2、HfCp(MeCp)Cl2、Hf(MeCp)2Cl2、HfCp(MeCp)Me2、Hf(EtCp)(MeCp)Me2、Hf(EtCp)2Me2、Hf(MeCp)2(CO)2、  ZrCp2Cl2、  Zr(MeCp)2Me2、  ZrCp(MeCp)Cl2、Zr(MeCp)2Cl2、ZrCp(MeCp)Me2、Zr(EtCp)(MeCp)Me2、Zr(EtCp)2Me2、Zr(MeCp)2(CO)2、Zr(MeCp)(NMe2)3、Zr(EtCp)(NMe2)3、ZrCp(NMe2)3、Zr(MeCp)(NEtMe)3  、    Zr(EtCp)(NEtMe)3  、    ZrCp(NEtMe)3  、Zr(MeCp)(NEt2)3、Zr(EtCp)(NEt2)3、ZrCp(NEt2)3、Zr(iPr2Cp)(NMe2)3、Zr(tBu2Cp)(NMe2)3、Hf(MeCp)(NMe2)3、Hf(EtCp)(NMe2)3、HfCp(NMe2)3、Hf(MeCp)(NEtMe)3  、    Hf(EtCp)(NEtMe)3  、    HfCp(NEtMe)3  、Hf(MeCp)(NEt2)3、Hf(EtCp)(NEt2)3、HfCp(NEt2)3、Hf(iPr2Cp)(NMe2)3、Hf(tBu2Cp)(NMe2)3及其混合物。 
根据本发明更特别的实施方案，本发明涉及上述沉积包含式(I2)化合物的含金属的介电膜的方法： 
M1ObNc  (I2) 
其相当于a＝0、1.5≤b≤2.5且0<c≤0.5的式(I)，其中式(II)的含金属的前体选自由下述物质组成的组：HfCp2Cl2、Hf(MeCp)2Me2、HfCp(MeCp)Cl2、Hf(MeCp)2Cl2、HfCp(MeCp)Me2、Hf(EtCp)(MeCp)Me2、Hf(EtCp)2Me2  、  Hf(MeCp)2(CO)2、  ZrCp2Cl2、  Zr(MeCp)2Me2、Zr(MeCp)2Cl2、ZrCp(MeCp)Me2、Zr(EtCp)(MeCp)Me2、Zr(EtCp)2Me2、Zr(MeCp)2(CO)2、Zr(MeCp)(NMe2)3、Zr(EtCp)(NMe2)3、ZrCp(NMe2)3、Zr(MeCp)(NEtMe)3  、    Zr(EtCp)(NEtMe)3  、    ZrCp(NEtMe)3  、 Zr(MeCp)(NEt2)3、Zr(EtCp)(NEt2)3、ZrCp(NEt2)3、Zr(iPr2Cp)(NMe2)3、Zr(tBu2Cp)(NMe2)3、Hf(MeCp)(NMe2)3、Hf(EtCp)(NMe2)3、Hf(p(NMe2)3、Hf(MeCp)(NEtMe)3  、    Hf(EtCp)(NEtMe)3  、    HfCp(NEtMe)3  、Hf(MeCp)(NEt2)3、Hf(EtCp)(NEt2)3、HfCp(NEt2)3、Hf(iPr2Cp)(NMe2)3、Hf(tBu2Cp)(NMe2)3及其混合物。 
根据本发明更特别的实施方案，本发明涉及如上定义的沉积包含式(I3)的化合物的含金属的介电膜的方法： 
(M1 1-a M2 a)Ob  (I3) 
其相当于0≤a<1且c＝0的式(I)，其中式(II)的含金属的前体选自由下述物质组成的组：HfCp2Cl2、Hf(MeCp)2Me2、HfCp(MeCp)Cl2、Hf(MeCp)2Cl2、Hf(p(MeCp)Me2、Hf(EtCp)(MeCp)Me2、Hf(EtCp)2Me2、Hf(MeCp)2(CO)2、  ZrCp2Cl2、  Zr(MeCp)2Me2、  ZrCp(MeCp)Cl2、Zr(MeCp)2Cl2、ZrCp(MeCp)Me2、Zr(EtCp)(MeCp)Me2、Zr(EtCp)2Me2、Zr(MeCp)2(CO)2、Zr(MeCp)(NMe2)3、Zr(EtCp)(NMe2)3、ZrCp(NMe2)3、Zr(MeCp)(NEtMe)3  、    Zr(EtCp)(NEtMe)3  、    ZrCp(NEtMe)3  、Zr(MeCp)(NEt2)3、Zr(EtCp)(NEt2)3、ZrCp(NEt2)3、Zr(iPr2Cp)(NMe2)3、Zr(tBu2Cp)(NMe2)3、Hf(MeCp)(NMe2)3、Hf(EtCp)(NMe2)3、HfCp(NMe2)3、Hf(MeCp)(NEtMe)3  、    Hf(EtCp)(NEtMe)3  、    HfCp(NEtMe)3  、Hf(MeCp)(NEt2)3、Hf(EtCp)(NEt2)3、HfCp(NEt2)3、Hf(iPr2Cp)(NMe2)3、Hf(tBu2Cp)(NMe2)3且含M2金属的前体优选选自如上定义的硅衍生物或其锗同系物、钽衍生物、镧系元素衍生物、和镁衍生物。 
根据本发明的更具体实施方案，本发明涉及如上定义的沉积包含式(I4)的化合物的含金属的介电膜的方法： 
(M1 1-a M2 a)ObNc    (I4) 
其相当于0≤a<1且0<c≤0.5的式(I)，其中式(II)的含金属的前体选自由下述物质组成的组：  HfCp2Cl2、Hf(MeCp)2Me2、HfCp(MeCp)Cl2、Hf(MeCp)2Cl2、HfCp(MeCp)Me2、Hf(EtCp)(MeCp)Me2、Hf(EtCp)2Me2  、  Hf(MeCp)2(CO)2、  ZrCp2Cl2  、  Zr(MeCp)2Me2、 ZrCp(MeCp)Cl2、Zr(MeCp)2Cl2、ZrCp(MeCp)Me2、Zr(EtCp)(MeCp)Me2、Zr(EtCp)2Me2、Zr(MeCp)2(CO)2、Zr(MeCp)(NMe2)3、Zr(EtCp)(NMe2)3、ZrCp(NMe2)3、Zr(MeCp)(NEtMe)3、Zr(EtCp)(NEtMe)3、ZrCp(NEtMe)3、Zr(MeCp)(NEt2)3、Zr(EtCp)(NEt2)3、ZrCp(NEt2)3、Zr(iPr2Cp)(NMe2)3、Zr(tBu2Cp)(NMe2)3、Hf(MeCp)(NMe2)3、Hf(EtCp)(NMe2)3、HfCp(NMe2)3、Hf(MeCp)(NEtMe)3  、    Hf(EtCp)(NEtMe)3  、    HfCp(NEtMe)3  、Hf(MeCp)(NEt2)3、Hf(EtCp)(NEt2)3、HfCp(NEt2)3、Hf(iPr2Cp)(NMe2)3、Hf(tBu2Cp)(NMe2)3，含M2金属的前体优选选自如上定义的硅衍生物或其锗同系物、钽衍生物、镧系元素衍生物和镁衍生物，并向反应器中引入至少一种含氧前体和至少一种含氮前体。 
根据另一实施方案，本发明涉及如上定义的式(II)的化合物的用途，用于制造介电膜、更特别用于集成电路的介电膜，或用于制备随机存取存储器的金属绝缘体金属(MIM)结构。 
根据另一实施方案，本发明涉及式(II1)的化合物： 
(R2 tCp)M1[N(R39)(R40)]3    (II1) 
其相当于x＝0、z＝1且R’代表基团N(R39)(R40)时的式(II)，其中R39和R40相同或不同，独立地代表氢原子、具有1至4个碳原子的直链或支链烷基、烷基甲硅烷基(其中烷基是直链或支链的并具有1至4个碳原子)、二烷基甲硅烷基(其中各烷基彼此相同或不同，是直链或支链的并具有1至4个碳原子)、或三烷基甲硅烷基(其中各烷基彼此相同或不同，是直链或支链的并具有1至4个碳原子)。 
根据一个具体实施方案，本发明涉及如上定义的式(II1)的化合物，其中R2、R39和R40相同或不同，独立地代表选自甲基、乙基、丙基、异丙基、丁基、异丁基、仲丁基和叔丁基的基团，更具体为下列化合物：Zr(MeCp)(NMe2)3、Zr(EtCp)(NMe2)3、ZrCp(NMe2)3、Zr(MeCp)(NEtMe)3、Zr(EtCp)(NEtMe)3、ZrCp(NEtMe)3、Zr(MeCp)(NEt2)3、Zr(EtCp)(NEt2)3、ZrCp(NEt2)3、Zr(iPr2Cp)(NMe2)3、Zr(tBu2Cp)(NMe2)3、Hf(MeCp)(NMe2)3、Hf(EtCp)(NMe2)3、HfCp(NMe2)3、Hf(MeCp)(NEtMe)3、Hf(EtCp)(NEtMe)3、 HfCp(NEtMe)3、Hf(MeCp)(NEt2)3、Hf(EtCp)(NEt2)3、HfCp(NEt2)3、Hf(iPr2Cp)(NMe2)3、Hf(tBu2Cp)(NMe2)3。 
根据更具体的实施方案，本发明涉及下列化合物：Zr(EtCp)(NMe2)3、Zr(MeCp)(NMe2)3、ZrCp(NMe2)3、Hf(EtCp)(NMe2)3、Hf(MeCp)(NMe2)3和HfCp(NMe2)3。 
本领域技术人员会认识到，上述金属-有机化合物可用于气相沉积法以外的任何其它用途，例如催化剂，或需要使用金属-有机化合物的任何其它工业方法或领域。 
根据另一实施方案，本发明涉及制备如上定义的式(II1)化合物的方法，其包括： 
步骤1，包括通过M1Cl4与(R2tCp)Na的反应制备式(VII1)的化合物： 
(R2 tCp)M1 Cl3  (VII1) 
其中M1、R2和t如上文对式(II)所定义； 
步骤2，包括使步骤1中制成的式(VII1)化合物与NH(R39)(R40)反应以产生式(II1)的化合物。 
根据最后一个实施方案，本发明涉及如上定义的式(II)的下列化合物：Hf(EtCp)2Me2、Zr(MeCp)2Me2或Zr(EtCp)2Me2。 
下列实施例是本发明的各种实施方案的示例，而非限制。 
实施例I：沉积金属氧化物膜M 1 O 2 ，其中M 1 优选为铪和锆
要沉积的膜包含a＝0、b＝2且c＝0的式(I)的化合物。 
为了在晶片表面上沉积这种膜或为制造DRAM的MIM结构在深槽中沉积这种膜，需要将如步骤(b)中所定义的M1金属源气化，并将其引入反应器(优选铪或锆)，将氧源(优选湿气)、氧或臭氧注入所述反应器，使产物在适当温度(优选150℃至350℃)和压力(优选25Pa至1000Pa)下反应，反应持续时间为通过ALD或脉冲CVD法实现基底上的薄膜沉积或填满深槽(为了实现氧化物在沟槽中的规则沉积，从而逐渐填满该沟槽，并实现在介电膜中无空隙并因此在电容器介电膜中无缺陷，金属源的相继 脉冲注射是必要的)所必需的时间。 
该介电膜应该具有所需最终组成(在此，b值在2左右的变化基本上改变了前体与氧源的比率)。 
根据下列三个选项a、b或c，选择式(II)化合物的类型的三种实例： 
a)  式(II)的化合物选自Zr(MeCp)2Me2、Zr(EtCp)2Me2、Hf(MeCp)2Me2和Hf(MeCp)2Me2。 
液体形式的分子的输送通常如下进行：将惰性气体(N2、He、Ar等)鼓入该液体，并向反应器供应该惰性气体+液体气体混合物。 
b)  式(II)的化合物选自Zr(2，4-Me2Op)2Me2和Hf(2，4-Me2Op)2Me2。 
c)式(II)的化合物选自  Zr(MeCp)(2，4-Me2Op)Me2和Hf(MeCp)(2，4-Me2Op)Me2。 
氧源应该优选为，但不限于，氧气(O2)、氧自由基(例如O·或OH·，例如通过远距等离子系统产生的自由基)，臭氧、NO、N2O、NO2、湿气(H2O)和H2O2。 
关于沉积法本身，可以将反应物同时(化学气相沉积)、先后(原子层沉积)或以不同的组合方式(一个实例是在一次脉冲中将例如金属源和另一金属源一起引入，并在单独的脉冲中引入氧[改变的原子层沉积]；另一选择是连续引入氧和/或脉冲引入金属源(脉冲化学气相沉积))引入反应器中。 
实施例II：沉积金属氧氮化物膜M 1 ON，其中M 1 优选为铪和锆
要沉积的膜包含a＝0且b和c不同于0的式(I)的化合物。 
实施例I中给出的所有信息都适用于此实施例II，不同的是需要向反应器中引入氮。 
氮应该选自氮源，氮源选自由氮气(N2)、氨、肼和烷基衍生物、含N的自由基(例如N·、NH·、NH2 ·)、NO、N2O、NO2等组成的组。 
实施例III：沉积M 1 M 2 金属氧化物膜，其中M 1 优选为Hf或Zr，M 2 优选为Si或Al
要沉积的膜包含a≠0、b≠0且c＝0的式(I)的化合物。 
实施例I中给出的所有信息都适用于此实施例III，不同的是另外需要M2金属源。 
还向反应器中引入含M2的前体以产生金属的M2源。该含M2的前体源应该优选为： 
a)硅(或锗)源，例如Si(OH)(OtBu)3、SiH(NMe2)3(TriDMAS)；SiH2(NHtBu)2(BTBAS)和SiH2(NEt2)2(BDEAS) 
b)铝源，例如AlMe2(OiPr)；或 
c)  钽  (或铌)  源，  例如  Ta(OMe)5、  Ta(OEt)5  和Ta(OEt)(OCMe2CH2-OMe)(TATDMAE)； 
本发明涉及在反应器中使用ALD、CVD、MOCVD、脉冲CVD法将式I的介电膜沉积到载体如晶片上。 
实施例IV：沉积M 1 M 2 金属氧氮化物膜，其中M 1 优选为Hf或Zr，M 2 优选为Si或Al
要沉积的膜包含a≠0、b≠0且c≠0的式(I)的化合物。 
实施例III中给出的所有信息都适用于这种情况，不同的是需要将氮引入反应器。 
氮源应当选自由氮气(N2)、氨、肼和烷基衍生物、含N的自由基(例如N·、NH·、NH2 ·)、NO、N2O、NO2等组成的组。 
实施例V：合成(乙基环戊二烯基)三(二甲基氨基)锆，Zr(EtCp)(NMe 2 ) 3
在3个步骤中制备Zr(EtCp)(NMe2)3。 
第一步骤是通过(EtCp)Na与ZrCl4的反应制备Zr(EtCp)Cl3； 
第二步骤是LiNMe2与Zr(EtCp)Cl3的反应，制造Zr(EtCp)(NMe2)3。通过蒸馏将所得化合物提纯。总收率为35％。 
已发现(乙基环戊二烯基)三(二甲基氨基)锆是稳定的液态浅黄色化合 物。 
Zr(EtCp)(NMe 2 ) 3 的TGA分析
将热重分析装置存放在湿气和氧含量保持低于1ppmv的氩气手套箱中。通过将35毫克样品装在铝坩锅中，进行热重分析。然后将样品以10℃/分钟升温速率从35℃加热至400℃。监测随着坩锅温度的质量损失。在260℃的完全蒸发温度下，残留含量为2.6％。所得图显示在图1中。 
实施例VI：  使用Zr(EtCp)(NMe 2 ) 3 进行ZrO 2 薄膜的原子层沉积
将Zr(EtCp)(NMe2)3储存在容器中。将该容器在90℃下加热，并以50sccm的流速使用N2作为载气。容器压力控制在50Torr。使用O3作为氧源。将基底在350℃下加热。在第一步骤中，将Zr(EtCp)(NMe2)3在2秒的期间引入反应室。此后作为第二步骤进行5秒N2吹扫。作为第三步骤，然后在2秒的期间向反应室中引入脉冲O3，然后作为第四步骤进行2秒N2吹扫。所有四个步骤重复100次，获得ZrO2膜。获得自限原子层沉积。 
用Hf类似物进行类似实验。用H2O作为氧源进行类似实验。 
实施例VII：  使用Zr(EtCp)(NMe 2 ) 3 进行ZrO 2 的金属-有机化学气相沉积
将Zr(EtCp)(NMe2)3储存在容器中。将该容器在90℃下加热，并以50sccm的流速使用N2作为载气。容器压力控制在50Torr。将Zr(EtCp)(NMe2)3混入进入反应室的O2/N2气体混合物。将基底在500℃下加热。反应室内的压力设定为10Torr。获得氧化锆膜。 
可以用Hf类似物进行类似实验。 
实施例VIII：  Zr(EtCp)(NMe 2 ) 3 和Zr(NEtMe) 4 的热性能的比较
在类似条件下，在Zr(EtCp)(NMe2)3和Zr(NEtMe)4上进行热重分析。将热重分析装置存放在湿气和氧含量保持低于1ppmv的氩气手套箱中。通过将35毫克样品装在铝坩锅中，进行热重分析。然后将样品以10℃/分钟升温速率从35℃加热至400℃。随坩锅温度监测质量损失。在封闭的杯 构造中，将穿孔盘(0.8毫米)放在装有该金属-有机化合物的坩锅上以减缓蒸发。这表现出在较高温度下的热稳定性。这些结果表明，Zr(EtCp)(NMe2)3比Zr(NEtMe)4热稳定得多，这使其进一步有吸引力地用作气相前体。结果显示在图2中。 
实施例IX：Hf(EtCp) 2 Me 2 的合成和热性能
Hf(EtCp)2Cl2容易通过1摩尔HfCl4与EtCpNa的反应获得。 
然后通过在-20℃在1摩尔Hf(EtCp)2Cl2上缓慢加入2摩尔LiMe并将温度升至0℃来获得Hf(EtCp)2Me2。通过蒸馏将所得透明液体Hf(EtCp)2Me2与LiCl和溶剂分离。对于大约30毫克的原料，Hf(EtCp)2Me2在真空条件下的TGA分析留下1.0％残留物(参见图3)。 
实施例X：由Hf(EtCp) 2 Me 2 和O 3 进行HfO 2 的原子层沉积
此实施例涉及氧化铪膜的制造。将硅片安装在沉积室中，该沉积室在其周围带有加热器，并在硅片表面上形成所需膜。用泵将该室抽空。将金属前体(在本例中是二甲基铪茂HfMe2(EtCp)2)储存在加热的液体容器中。使用氮气作为Hf(EtCp)2Me2的载气。通过使氮气流过液化材料，输送液体容器中的Hf(EtCp)2Me2。氮气通过质流控制器送入气化器。由氮气携带Hf(EtCp)2Me2蒸气并一起加入该室，或在可以使前体被引入反应器的阀关闭时转向旁通管。还将氧/臭氧气体混合物(氧化剂)通过质流控制器加入该室或加入旁通管。一侧上的氧/臭氧和另一侧上的Hf(EtCp)2Me2决不一起引入，以避免高度可能的CVD反应。它们通常接连引入，各反应物脉冲被吹扫时间隔开，在该吹扫时间中，仅将N2引入该室。 
使用所述工具在下列条件下在-0.7A/周期下制造氧化铪膜： 
压力＝3torr，温度＝350℃，Hf(EtCp)2Me2流速＝0.5sccm，O2流速＝100sccm。O3流速＝8sccm。N2流速＝100sccm。 
给出所得膜的Auger图作为示例(见图4)。

Claims (18)

1.在基底上沉积含至少一种金属的介电膜的方法，该介电膜包含式(I)的化合物：
(M1 1-a M2 a)ObNc        (I)
其中：
0≤a<1，
0<b≤3，优选地1.5≤b≤2.5；
0≤c≤1，
M1代表选自铪(Hf)、锆(Zr)和钛(Ti)的金属；且
M2代表选自镁(Mg)、钙(Ca)、锌(Zn)、硼(B)、铝(A)、铟(In)、硅(Si)、锗(Ge)、锡(Sn)、铪(Hf)、锆(Zr)、钛(Ti)、钒(V)、铌(Nb)、钽(Ta)的金属原子；和镧系原子，更特别地，钪(Sc)、钇(Y)、镧(La)和稀土金属原子，
该方法包括下列步骤：
-步骤a)，将基底供应到反应室中；
-步骤b)，将至少一种式(II)的含M1金属的前体气化，从而形成第一气相金属源：
(R1 yOp)x(R2 tCp)z M1R’4-x-z      (II)
其中：
M1定义如上；
0≤x≤3，优选地x＝0或1；
0≤z≤3，优选地z＝1或2；
1≤(x+z)≤4；
0≤y≤7，优选地y＝2；
0≤t≤5，优选地t＝1；
(R1 yOp)代表戊二烯基(Op)配体，其未被取代或被一个或多个R1基团取代，y代表在所述戊二烯基配体上的R1取代基的数；
(R2 tCp)代表环戊二烯基(Cp)配体，其未被取代或被一个或多个R2基团取代，t代表在所述环戊二烯基配体上的R1取代基的数；
R1和R2相同或不同，并独立地选自由下述基团组成的组：氯；具有1至4个碳原子的直链或支链烷基；N-烷基氨基，其中烷基是直链或支链的并具有1至4个碳原子；N，N-二烷基氨基，其中各烷基彼此相同或不同，是直链或支链的并具有1至4个碳原子；具有1至4个碳原子的直链或支链烷氧基；烷基甲硅烷基酰胺基团；脒根基团；和羰基；
R’代表独立地选自由下述基团组成的组的配体：氢、氟、氯、溴或碘原子；具有1至4个碳原子的直链或支链烷基；N-烷基氨基，其中烷基是直链或支链的并具有1至4个碳原子；N，N-二烷基氨基，其中各烷基彼此相同或不同，是直链或支链的并具有1至4个碳原子；具有1至4个碳原子的直链或支链烷氧基；烷基甲硅烷基氨基，其中烷基是直链或支链的并具有1至4个碳原子；二烷基甲硅烷基氨基，其中各烷基彼此相同或不同，是直链或支链的并具有1至4个碳原子；三烷基甲硅烷基氨基，其中各烷基彼此相同或不同，是直链或支链的并具有1至4个碳原子；脒根基团；和羰基，要理解的是，如果所述式(II)包含超过一个的R’基团，各R’可以彼此相同或不同；
-任选地，步骤b’)，将至少一种含M2金属的前体气化，从而形成任选的第二气相金属源，其中M2定义如上；
-步骤c)，将所述第一气相金属源和所述任选的第二气相金属源引入反应室中以使它们与所述基底接触，从而在所述基底上沉积包含如上定义的式(I)化合物的含金属的介电膜；
条件是，如果要形成的含至少一种金属的介电膜包含式(I’)的化合物：
M1 1O2      (I’)
其相当于a＝0、b＝2且c＝0时的如上定义的式(I)，且如果步骤b)中所涉及的含M1金属的前体是式(II’)的化合物：
(R2 tCp)2M1R’2       (II’)
其相当于x＝0且z＝2时的如上定义的式(II)，则在所述式(II’)中，在两个(R2 tCp)配体的至少一个中，t>0。
2.根据权利要求1的方法，其中气化步骤b)和气化步骤b’)合并成这两种源的一个气化步骤b”)。
3.根据权利要求1或根据权利要求2的方法，其中含M2金属的前体选自由下述物质组成的组：
硅衍生物或其锗同系物，例如：
二硅氧烷、三甲硅烷基胺、二硅烷、三硅烷、式(III1)的烷氧基硅烷
SiHx(OR3)4-x，     (III1)
其中：0≤x≤3且R3代表具有1至6个碳原子的直链或支链烃基；
式(III2)的硅烷醇衍生物：
Si(OH)x(OR4)4-x    (III2)
其中：1≤x≤3且R4代表具有1至6个碳原子的直链或支链烃基，优选为Si(OH)(OR4)3，更优选为Si(OH)(OtBu)3；
式(III3)的氨基硅烷衍生物：
SiHx(NR5R6)4-x    (III3)
其中：0≤x≤3，且R5和R6相同或不同并独立地代表氢原子或具有1至6个碳原子的直链或支链烷基，优选SiH(NMe2)3(TriDMAS)、SiH2(NHtBu)2(BTBAS)；SiH2(NEt2)2(BDEAS)，及其混合物；
铝衍生物，例如三甲基铝[Al(CH3)3]、二甲基氢化铝[AlH(CH3)2]、式(IV1)的烷氧基铝烷：
AlR8 x(OR7)3-x     (IV1)
其中0≤x≤3，且R7代表具有1至6个碳原子的直链或支链烷基，且R8与R7相同或不同，代表氢原子，或优选AlR9R10(OR7)，其中R9和R10相同或不同，它们独立地代表具有1至6个碳原子的直链或支链烷基，最优选AlMe2(OiPr)；
式(IV2)的酰氨基铝烷：
AlR11 x(NR12R13)3-x       (IV2)
其中：0≤x≤3，且R12和R13相同或不同，代表氢原子或具有1至6个碳原子的直链或支链烷基，且R11与R7相同或不同并代表氢原子或具有1至6个碳原子的直链或支链烷基；
钽衍生物，例如：Ta(OMe)5、Ta(OEt)5、Ta(NMe2)5、Ta(NEt2)5、Ta(NEt2)5、式(V1)的钽衍生物：
Ta(OR14)4[O-C(R15)(R16)-CH2-OR17]
其中R14、R15、R16和R17相同或不同，独立地代表氢原子或具有1至6个碳原子的直链或支链烷基，优选Ta(OEt)4(OCMe2CH2-OMe)(TAT-DMAE)，式(V2)的钽衍生物：
Ta(OR18)4[O-C(R19)(R20)-CH2-N(R21)(R22)]    (V2)
其中R18、R19、R20、R21和R22相同或不同，独立地代表氢原子或具有1至6个碳原子的直链或支链烷基，式(V3)的钽衍生物：
Ta(＝NR24)(NR25R26)3       (V3)
其中R24、R25和R26相同或不同，独立地代表氢原子或具有1至6个碳原子的直链或支链烷基；
铌衍生物，例如：Nb(OMe)5、Nb(OEt)5、Nb(NMe2)5、Nb(NEt2)4、Nb(NEt2)5、式(VI1)的铌衍生物：
Nb(OR27)4(O-C(R28)(R29)-CH2-OR30)     (VI1)
其中R27、R28、R29和R30相同或不同，独立地代表氢原子或具有1至6个碳原子的直链或支链烷基，优选Nb(OEt)4(OCMe2CH2-OMe)(NBT-DMAE)，式(VI2)的铌衍生物：
Nb(OR31)4[O-C(R32)(R33)-CH2-N(R34)(R35)]    (VI2)
其中R31、R32、R33、R34和R35相同或不同，独立地代表氢原子或具有1至6个碳原子的直链或支链烷基，式(VI3)的铌衍生物：
Nb(＝NR36)(NR37R38)3     (VI3)
其中R36、R37和R38相同或不同，独立地代表氢原子或具有1至6个碳原子的直链或支链烷基；
镧系元素衍生物，例如钪衍生物、钇衍生物、铈衍生物、镨衍生物、钆衍生物、或Nd衍生物，带有至少一个β-二酮配体或至少一个任选被一个或数个具有1至6个碳原子的直链或支链烷基取代的环戊二烯基配体的衍生物；
二价金属衍生物，例如锶(Sr)、钡(Ba)、镁(Mg)、钙(Ca)或锌(Zn)衍生物，带有至少一个β-二酮配体或至少一个任选被一个或数个具有1至6个碳原子的直链或支链烷基取代的环戊二烯基配体；
其它金属衍生物，例如钨(W)、钼(Mo)、铪(Hf)或锆(Zr)衍生物，例如烷氧基衍生物、氨基衍生物或含有这些物质的加合物，要理解的是，所述衍生物不是如上定义的式(II)的化合物。
4.根据权利要求1至3之一的方法，其进一步包括：
-步骤d)，其中在步骤c)之前将至少一种式(II)的含M1金属的前体和，如果必要，至少一种含M2金属的前体混入至少一种反应物质中。
5.根据权利要求1至4之一的方法，其进一步包括：
-步骤d′)，其中将至少一种式(II)的含M1金属的前体和，如果必要，至少一种含M2金属的前体在反应室中混入至少一种反应物质中。
6.根据权利要求1至5之一的方法，其中步骤(b)由步骤(b 1 )和步骤(b2)构成，其中步骤(b 1 )为将至少一种式(II)的第一含金属的前体与至少下列第二前体混合在一起：M1(NMe2)4、M1(NEt2)4、M1(NMeEt)4、M1(mmp)4、M1(OtBu)4、M1(OtBu)2(mmp)2及其混合物，步骤(b2)为将所述混合物气化。
7.根据权利要求1至6之一的方法，其中含M1金属的前体具有式(II1)：
(R2 tCp)M1[N(R39)(R40)]3       (II1)
其相当于x＝0、z＝1且R’代表基团N(R39)(R40)时的式(II)，其中R39和R40相同或不同，独立地代表氢原子；具有1至4个碳原子的直链或支链烷基；烷基甲硅烷基，其中烷基是直链或支链的并具有1至4个碳原子；二烷基甲硅烷基，其中各烷基彼此相同或不同，是直链或支链的并具有1至4个碳原子；或三烷基甲硅烷基，其中各烷基彼此相同或不同，是直链或支链的并具有1至4个碳原子。
8.根据权利要求1至7之一的沉积包含式(I1)化合物的含金属的介电膜的方法：
M1O2      (I1)
其相当于a＝0、b＝2且c＝0的式(I)，其中式(II)的含金属的前体选自由下述物质组成的组：HfCp2Cl2、Hf(MeCp)2Me2、HfCp(MeCp)Cl2、Hf(MeCp)2Cl2、HfCp(MeCp)Me2、Hf(EtCp)(MeCp)Me2、Hf(EtCp)2Me2、Hf(MeCp)2(CO)2、ZrCp2Cl2、Zr(MeCp)2Me2、ZrCp(MeCp)Cl2、Zr(MeCp)2Cl2、ZrCp(MeCp)Me2、Zr(EtCp)(MeCp)Me2、Zr(EtCp)2Me2、Zr(MeCp)2(CO)2、Zr(MeCp)(NMe2)3、Zr(EtCp)(NMe2)3、ZrCp(NMe2)3、Zr(MeCp)(NEtMe)3、Zr(EtCp)(NEtMe)3、ZrCp(NEtMe)3、Zr(MeCp)(NEt2)3、Zr(EtCp)(NEt2)3、ZrCp(NEt2)3、Zr(iPr2Cp)(NMe2)3、Zr(tBu2Cp)(NMe2)3、Hf(MeCp)(NMe2)3、Hf(EtCp)(NMe2)3、HfCp(NMe2)3、Hf(MeCp)(NEtMe)3、Hf(EtCp)(NEtMe)3、HfCp(NEtMe)3、Hf(MeCp)(NEt2)3、Hf(EtCp)(NEt2)3、HfCp(NEt2)3、Hf(iPr2Cp)(NMe2)3、Hf(tBu2Cp)(NMe2)3及其混合物。
9.根据权利要求1至7之一的沉积包含式(I2)化合物的含金属的介电膜的方法：
M1Ob Nc         (I2)
其相当于a＝0、1.5≤b≤2.5且0<c≤0.5的式(I)，其中式(II)的含金属的前体选自由下述物质组成的组：HfCp2Cl2、Hf(MeCp)2Me2、HfCp(MeCp)Cl2、Hf(MeCp)2Cl2、HfCp(MeCp)Me2、Hf(EtCp)(MeCp)Me2、Hf(EtCp)2Me2、Hf(MeCp)2(CO)2、ZrCp2Cl2、Zr(MeCp)2Me2、Zr(MeCp)2Cl2、ZrCp(MeCp)Me2、Zr(EtCp)(MeCp)Me2、Zr(EtCp)2Me2、Zr(MeCp)2(CO)2、Zr(MeCp)(NMe2)3、Zr(EtCp)(NMe2)3、ZrCp(NMe2)3、Zr(MeCp)(NEtMe)3、Zr(EtCp)(NEtMe)3、ZrCp(NEtMe)3、Zr(MeCp)(NEt2)3、Zr(EtCp)(NEt2)3、ZrCp(NEt2)3、Zr(iPr2Cp)(NMe2)3、Zr(tBu2Cp)(NMe2)3、Hf(MeCp)(NMe2)3、Hf(EtCp)(NMe2)3、HfCp(NMe2)3、Hf(MeCp)(NEtMe)3、Hf(EtCp)(NEtMe)3、HfCp(NEtMe)3、Hf(MeCp)(NEt2)3、Hf(EtCp)(NEt2)3、HfCp(NEt2)3、Hf(iPr2Cp)(NMe2)3、Hf(tBu2Cp)(NMe2)3及其混合物。
10.根据权利要求1至7之一的沉积包含式(I3)化合物的含金属的介电膜的方法：
(M1 1-a M2 a)Ob        (I3)
其相当于0≤a<1且c＝0的式(I)，其中式(II)的含金属的前体选自由下述物质组成的组：HfCp2Cl2、Hf(MeCp)2Me2、HfCp(MeCp)Cl2、Hf(MeCp)2Cl2、HfCp(MeCp)Me2、Hf(EtCp)(MeCp)Me2、Hf(EtCp)2Me2、Hf(MeCp)2(CO)2、ZrCp2Cl2、Zr(MeCp)2Me2、ZrCp(MeCp)Cl2、Zr(MeCp)2Cl2、ZrCp(MeCp)Me2、Zr(EtCp)(MeCp)Me2、Zr(EtCp)2Me2、Zr(MeCp)2(CO)2、Zr(MeCp)(NMe2)3、Zr(EtCp)(NMe2)3、ZrCp(NMe2)3、Zr(MeCp)(NEtMe)3、Zr(EtCp)(NEtMe)3、ZrCp(NEtMe)3、Zr(MeCp)(NEt2)3、Zr(EtCp)(NEt2)3、ZrCp(NEt2)3、Zr(iPr2Cp)(NMe2)3、Zr(tBu2Cp)(NMe2)3、Hf(MeCp)(NMe2)3、Hf(EtCp)(NMe2)3、HfCp(NMe2)3、Hf(MeCp)(NEtMe)3、Hf(EtCp)(NEtMe)3、HfCp(NEtMe)3、Hf(MeCp)(NEt2)3、Hf(EtCp)(NEt2)3、HfCp(NEt2)3、Hf(iPr2Cp)(NMe2)3、Hf(tBu2Cp)(NMe2)3，且含M2金属的前体优选选自如上定义的硅衍生物或其锗同系物、钽衍生物、镧系元素衍生物、和镁衍生物。
11.根据权利要求1至7之一的沉积包含式(I4)化合物的含金属的介电膜的方法：
(M1 1-a M2 a)ObNc       (I4)
其相当于0≤a<1且0<c≤0.5的式(I)，其中式(II)的含金属的前体选自由下述物质组成的组：HfCp2Cl2、Hf(MeCp)2Me2、HfCp(MeCp)Cl2、Hf(MeCp)2Cl2、HfCp(MeCp)Me2、Hf(EtCp)(MeCp)Me2、Hf(EtCp)2Me2、Hf(MeCp)2(CO)2、ZrCp2Cl2、Zr(MeCp)2Me2、ZrCp(MeCp)Cl2、Zr(MeCp)2Cl2、ZrCp(MeCp)Me2、Zr(EtCp)(MeCp)Me2、Zr(EtCp)2Me2、Zr(MeCp)2(CO)2、Zr(MeCp)(NMe2)3、Zr(EtCp)(NMe2)3、ZrCp(NMe2)3、Zr(MeCp)(NEtMe)3、Zr(EtCp)(NEtMe)3、ZrCp(NEtMe)3、Zr(MeCp)(NEt2)3、Zr(EtCp)(NEt2)3、ZrCp(NEt2)3、Zr(iPr2Cp)(NMe2)3、Zr(tBu2Cp)(NMe2)3、Hf(MeCp)(NMe2)3、Hf(EtCp)(NMe2)3、HfCp(NMe2)3、Hf(MeCp)(NEtMe)3、Hf(EtCp)(NEtMe)3、HfCp(NEtMe)3、Hf(MeCp)(NEt2)3、Hf(EtCp)(NEt2)3、HfCp(NEt2)3、Hf(iPr2Cp)(NMe2)3、Hf(tBu2Cp)(NMe2)3，含M2金属的前体优选选自如上定义的硅衍生物或其锗同系物、钽衍生物、镧系元素衍生物和镁衍生物，并向反应器中引入至少一种含氧前体和至少一种含氮前体。
12.如权利要求1所述的式(II)化合物的用途，用于制造介电膜，特别是用于集成电路的介电膜，或用于制备随机存取存储器的金属绝缘体金属(MIM)构造。
13.式(II1)的化合物：
(R2 tCp)M1[N(R39)(R40)]3        (II1)
其相当于x＝0、z＝1且R’代表基团N(R39)(R40)时的式(II)，其中R39和R40相同或不同，独立地代表氢原子；具有1至4个碳原子的直链或支链烷基；烷基甲硅烷基，其中烷基是直链或支链的并具有1至4个碳原子；二烷基甲硅烷基，其中各烷基彼此相同或不同，是直链或支链的并具有1至4个碳原子；或三烷基甲硅烷基，其中各烷基彼此相同或不同，是直链或支链的并具有1至4个碳原子。
14.如权利要求13所述的式(II1)的化合物，其中R2、R39和R40相同或不同，独立地代表选自甲基、乙基、丙基、异丙基、丁基、异丁基、仲丁基和叔丁基的基团。
15.如权利要求14所述的下列式(II1)的化合物：Zr(MeCp)(NMe2)3、Zr(EtCp)(NMe2)3、ZrCp(NMe2)3、Zr(MeCp)(NEtMe)3、Zr(EtCp)(NEtMe)3、ZrCp(NEtMe)3、Zr(MeCp)(NEt2)3、Zr(EtCp)(NEt2)3、ZrCp(NEt2)3、Zr(iPr2Cp)(NMe2)3、Zr(tBu2Cp)(NMe2)3、Hf(MeCp)(NMe2)3、Hf(EtCp)(NMe2)3、HfCp(NMe2)3、Hf(MeCp)(NEtMe)3、Hf(EtCp)(NEtMe)3、HfCp(NEtMe)3、Hf(MeCp)(NEt2)3、Hf(EtCp)(NEt2)3、HfCp(NEt2)3、Hf(iPr2Cp)(NMe2)3、Hf(tBu2Cp)(NMe2)3。
16.如权利要求15所述的下列式(II1)的化合物：Zr(EtCp)(NMe2)3、Zr(MeCp)(NMe2)3、ZrCp(NMe2)3、Hf(EtCp)(NMe2)3、Hf(MeCp)(NMe2)3和HfCp(NMe2)3。
17.制备如权利要求13至权利要求16之一所述的式(II1)的化合物的方法，其包括：
步骤1，包括通过M1Cl4与(R2 tCp)Na的反应制备式(VII1)化合物：
(R2 tCp)M1Cl3             (VII1)
其中M1、R2和t如上文对式(II)所定义；
步骤2，包括使步骤1中制成的式(VII1)化合物与NH(R39)(R40)反应，以产生式(II1)的化合物。
18.如权利要求1所述的下列式(II)的化合物：Hf(EtCp)2Me2、Zr(MeCp)2Me2或Zr(EtCp)2Me2。
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