CN102177163B - 用于薄膜沉积的铌和钒有机金属前体 - Google Patents
用于薄膜沉积的铌和钒有机金属前体 Download PDFInfo
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- CN102177163B CN102177163B CN200980139579.7A CN200980139579A CN102177163B CN 102177163 B CN102177163 B CN 102177163B CN 200980139579 A CN200980139579 A CN 200980139579A CN 102177163 B CN102177163 B CN 102177163B
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02205—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45553—Atomic layer deposition [ALD] characterized by the use of precursors specially adapted for ALD
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
- H01L21/0228—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition deposition by cyclic CVD, e.g. ALD, ALE, pulsed CVD
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
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Abstract
式Cp(R1)mM(NR2 2)2(=NR3)(I)的化合物:其中:M是独立地选自钒(V)或铌(Nb)的金属,且m≤5;R1是有机配体,各自独立地选自H、包含1至6个碳原子的直链或支化烃基;R2是有机配体,各自独立地选自H、包含1至6个碳原子的直链或支化烃基;R3是选自H、包含1至6个碳原子的直链或支化烃基的有机配体。
Description
本发明涉及新一类化合物及其在含金属的膜沉积中的用途。
与3D拓扑构造相关联的现代集成电路(IC)构件中临界尺寸的持续缩小以工艺复杂性为代价提供最高密度。
根据International Technology Roadmap for Semiconductors(ITRS),半导体工业中常用于薄膜沉积的物理技术不再适合满足未来技术节点中的要求,尤其是对高纵横比结构而言。使用高能粒子的技术,如PVD(物理气相沉积)、i-PVD(离子化-物理气相沉积)或PECVD(等离子体增强的化学气相沉积)引起高粘着系数,这造成差的阶梯覆盖,尤其是沿着侧壁。
能在高纵横比结构中以合理处理量沉积高度均匀和共形的薄膜的主要工业选项是如MOCVD(金属-有机化学气相沉积)或ALD(原子层沉积)之类的技术。
但是,通过MOCVD沉积的薄膜需要高的热预算并通常遵循Volmer-Weber模型所述的3D-生长机制。通过簇成核之类的技术生长薄膜造成阶梯覆盖不足。
典型的ALD法(例如如RITALA M.,LESKELA M.,Atomic LayerDeposition,Handbook of thin films materials中所述)涉及通过被惰性气体吹扫隔开的脉冲引到基底上的气态反应物。在MOCVD中,气态反应物同时注入并通过热自分解反应;而在ALD中,通过与基底上的表面基团反应,热诱发配体损失。在一定温度范围内,该表面反应是自限的,这允许沉积高度均匀和共形的薄膜。前体必须足够挥发性和稳定以便容易在不分解的情况下转移到反应室中。
此外,它们必须足够活性与该表面的化学基团反应以确保合理生长速率。
ALD特别可用于沉积含第V族(V、Nb、Ta)金属的薄膜。如今,仍然需要具有高挥发性并具有高通用性(适用于半导体制造中的各种用途)的在室温(或接近室温)下为液态的金属有机前体。在过去几年中已经开始关注用于几种主要用途的通过ALD沉积的含导电性(电阻率<1000μΩ.cm)第V族(V、Nb、Ta)金属的薄膜,如:BEOL用途中的铜扩散势垒、CMOS金属栅、用于金属-绝缘体-金属用途(DRAM...)的电极和/或在TFT-LCD用途中的类似物。
含第V族(V、Nb、Ta)金属的薄膜也特别可用于存储器件中的高-k层。
已广泛研究了卤化物,如CpNbCl4(CAS 33114-1507)、NbF5、NbBr5(Thin solid films,1981,79,75)、NbCl5(Crystal growth,1978,45,37)和如US 6,268,288中公开的TaCl5。但是,沉积过程中产生的一些副产物,如HCl或Cl2会造成表面/界面粗糙,这对最终性质有害。此外,Cl或F杂质对最终电性质有害。因此期望找到具有足够挥发性但不含Cl、F或Br原子的新化合物。
许多第V族前体被认为能够实现这种沉积。实例如下:
烷氧基化物被广泛使用和描述,如五乙氧基钽(PET)。但是,它们产生含氧膜并且不适于沉积特别用作电极且不应含有即使痕量水平的氧的含金属膜。对于如Cp2Nb(H)(CO)、CpNb(CO)4(J.Organomet.Chem557(1998)77-92)、V(CO)6(Thermochimica Acta,1984,75,71)、(η5-C5H5)V(CO)4(M.L.Green,R.A.Levy,J.Metals 37(1985)63)之类的化合物,观察到同样的问题。
US-A-6,379,748公开了对PET的改进。例如已通过使用TaMe3(OEt)2代替Ta(OEt)5(PET)来引入烷基键。由此在不影响熔点的情况下显著改进挥发性。
但是,TaMe3(OEt)2不允许多用途沉积:特别地,不能获得无氧金属。
US-A-6,368,398公开了借助使用例如Ta[OC(O)C(CH3)3]5的另一改进,但具有如上文公开的同样限制。
WO 02/20870公开了叔丁基亚氨基(三(二乙基酰氨基)钽,TBTDET用于沉积Ta2O5的用途。
US-A-6,593,484、US 2004/0219784公开了通过相继注入TBTDET或TAIMATA和另一N源来沉积氮化钽膜的方法。
US-A-6,379,748公开了Ta(Me3SiCp)2H3,即双环戊二烯基氢化钽,其是具有低挥发性的固体。
根据第一实施方案,本发明涉及式Cp(R1)mM(NR2 2)2(=NR3)(I)的化合物:
其中:
M是独立地选自钒(V)或铌(Nb)的金属,且m≤5;
R1是有机配体,各自独立地选自H、包含1至6个碳原子的直链或支化烃基;
R2是有机配体,各自独立地选自H、包含1至6个碳原子的直链或支化烃基;
R3是有机配体,选自H、包含1至6个碳原子的直链或支化烃基。
或者,R1是有机配体,各自独立地选自H、直链或支化烷基、烷基甲硅烷基、烷基酰胺、烷基甲硅烷基酰胺和/或烷氧化物。R2可以选自烷基、烷基甲硅烷基、烷基酰胺、烷基甲硅烷基酰胺和/或烷氧化物。R3可以选自烷基、烷基甲硅烷基、烷基酰胺、烷基甲硅烷基酰胺和/或烷氧化物,优选地,R3是含3或4个碳原子的烷基,如异丙基或叔丁基。
在一种具体构造中,各R1和R2彼此不同,它们可具有对化合物物理性质有益的特性。
或者,R1选自H、包含1至4个碳原子的烷基,优选地,R1是H或甲基或乙基或异丙基或叔丁基;
R2是包含1至3个碳原子的烷基,更优选地,R2是含1或2个碳原子的烷基;且
R3是含3或4个碳原子的烷基;更优选地,R3是异丙基或叔丁基。
根据另一些实施方案,本发明涉及:
-一种化合物,其中各R1彼此不同且各R2彼此不同。
-一种化合物,其中式(I)中的m=0。
-如下化合物:
(Cp)V(=NtBu)(NEt2)2
(Cp)V(=NtBu)(NMe2)2
(Cp)V(=NtBu)(N(EtMe)2
(Cp)V(=NiPr)(NEt2)2
(Cp)V(=NiPr)(NMe2)2
(Cp)V(=NiPr))(NEtMe)2
(Cp)V(=NC5H11)(NEt2)2
(Cp)V(=NC5H11)(NMe2)2
(Cp)V(=NC5H11)(NEtMe)2
(Cp)Nb(=NtBu)(NEt2)2
(Cp)Nb(=NtBu)(NMe2)2
(Cp)Nb(=NtBu)(N(EtMe)2
(Cp)Nb(=NiPr)(NEt2)2
(Cp)Nb(=NiPr)(NMe2)2
(Cp)Nb(=NiPr)(NEtMe)2
(Cp)Nb(=NC5H11)(NEt2)2
(Cp)Nb(=NC5H11)(NMe2)2
(Cp)Nb(=NC5H11)(NEtMe)2
根据另一实施方案,本发明涉及在基底上形成含金属的层的方法,该方法包括至少下列步骤:
a)提供包含至少一种式(I)的前体化合物的蒸气;
b)根据沉积法,使包含所述至少一种式(I)的化合物的所述蒸气与基底反应以在所述基底的至少一个表面上形成含金属络合物的层。
根据另一些实施方案,本发明涉及:
-一种方法,其中所述沉积法是原子层沉积法。
-一种方法,其中所述沉积法是化学气相沉积法。
-一种方法,进一步包括如下步骤:
c)使步骤b)中获得的络合物与选自另一金属源、还原反应物和/或氮化反应物和/或氧化反应物的试剂反应。
-一种方法,其中步骤a)中提供的蒸气进一步包含一种或多种金属(M′)-有机前体以产生含M和M′的薄膜。
-一种方法,进一步包括提供至少一种反应气体,其中所述至少一种反应气体选自氢、硫化氢、硒化氢、碲化氢、一氧化碳、氨、有机胺、硅烷、乙硅烷、更高级硅烷、甲硅烷基胺、乙硼烷、肼、甲基肼、氯硅烷和氯代聚硅烷、金属烷基、胂、膦、三烷基硼、氧、臭氧、水、过氧化氢、氧化亚氮、一氧化二氮、二氧化氮、醇、包含这些物类的片段的等离子体、以及它们的组合,优选臭氧或水。
-一种方法,其中基底温度为100℃至700℃,优选150℃至450℃,且其中含有该基底的沉积室的压力为1.33Pa(=0.01托)至100kPa(=800托),优选低于25kPa(=200托)。
-一种方法,进一步包括用选自氢气、氮气、氦气、氩气及其混合物的惰性气体从基底上吹除包含所述至少一种式(I)的化合物的过量的蒸气的步骤。
-一种方法,其中该含金属的层具有大于0微米至10微米的厚度。
-制造半导体结构的方法,包括如上定义的方法的步骤,其中基底是半导体衬底。
含钒(V)或铌(Nb)的膜的相关沉积技术
金属源的气化通过将载气引入含有所述金属源的加热容器中来实现。该容器优选在能使所述金属源达到足够蒸气压的温度下加热。载气可选自Ar、He、H2、N2或它们的混合物。所述金属源可以在该容器中混合到溶剂或另一金属源或它们的混合物中。该容器可以例如在25℃-200℃的温度下加热。本领域技术人员认为,可以调节该容器的温度以控制气化前体的量。为了控制该容器中的蒸发程度,可以改变该容器中的压力。通过降低该容器中的压力,可以提高金属源的气化程度。该容器内的压力可以例如在毫托至800托的范围内改变。
所述金属源也可以以液态送入气化器中,在此将其气化。可以将所述金属源混合到溶剂中。可以将所述金属源混合到另一金属源中。可以将所述金属源混合物混合到溶剂或溶剂混合物中。可以将所述金属源混合到稳定剂中。所述溶剂可选自烷烃,如己烷、庚烷、辛烷,芳族溶剂如苯、甲苯、均三甲苯、二甲苯,含硅的溶剂,如六甲基二硅氧烷、六甲基二硅氮烷、四甲基硅烷,含硫的溶剂,如二甲亚砜,含氧的溶剂,如四氢呋喃、二噁烷等。
随后将所述气化金属源引入反应室,在此其与基底表面接触。可以将基底加热至足够温度以便以足够生长速率和所需物理状态和组成获得所需膜。典型温度为100℃至700℃。优选该温度低于或等于450℃。可通过非限制性选择的等离子技术辅助该方法,以改进所述气化金属源的反应性和/或该方法中所用的其它气态物类的反应性。
在一个实施方案中,本发明的方法包括将通式Cp(R1)mM(NR2 2)2(=NR3)的钒(V)或铌(Nb)金属-有机前体与或不与试剂同时引入反应室。所述金属-有机前体通过热自分解与基底表面反应。所述试剂选自还原反应物、氮化反应物、氧化反应物或它们的混合物。
在一个实施方案中,本发明的方法包括将通式Cp(R1)mM(NR2 2)2(=NR3)的钒(V)或铌(Nb)金属-有机前体与或不与试剂和另一金属源同时引入反应室,所述另一金属源独立地选自第II族、第III-A族、第III-B族、硫(S)、钽(Ta)、过渡金属、镧系元素或稀土金属中的任何其它元素。所述金属-有机前体通过热自分解与基底表面反应。所述试剂选自还原反应物、氮化反应物、氧化反应物或它们的混合物。
在一个实施方案中,本发明的方法包括将通式Cp(R1)mM(NR2 2)2(=NR3)的钒(V)或铌(Nb)金属-有机前体与试剂交替引入反应室。在一定温度范围内,所述金属-有机前体以自限方式与基底表面上存在的键反应。优选从反应室中除去未沉积的金属-有机前体分子。引入的试剂也以自限方式反应。一旦基底表面上存在的所有络合物已与所述试剂反应,用吹扫气体从反应室中除去物类。该吹扫气体可以例如选自N2、Ar、He、H2或它们的混合物。该吹扫气体可另外含有不改变所述表面的化学反应性的其它气体物类。或者,可通过真空实现清除。该方法可以根据需要重复许多次以实现所需膜厚度。所述试剂选自还原反应物、氮化反应物、氧化反应物或它们的混合物。
在一个实施方案中,本发明的方法包括交替地首先将通式Cp(R1)mM(NR2 2)2(=NR3)的钒(V)或铌(Nb)金属-有机前体引入反应室,其次引入试剂或另一金属源,所述另一金属源独立地选自第II族、第III-A族、第III-B族、硫(S)、钽(Ta)、过渡金属、镧系元素或稀土金属中的任何其它元素。在一定温度范围内,所述金属-有机前体以自限方式与基底表面上存在的键反应。优选从反应室中除去未沉积的金属-有机前体分子。引入的试剂也以自限方式反应。一旦基底表面上存在的所有络合物与该试剂反应,用吹扫气体从反应室中除去物类。该吹扫气体可以例如选自N2、Ar、He、H2或它们的混合物。该吹扫气体可另外含有不改变所述表面的化学反应性的其它气体物类。或者,可通过真空实现清除。该方法可以根据需要重复许多次以实现所需膜厚度。所述试剂选自还原反应物、氮化反应物、氧化反应物或它们的混合物。
式(I)的化合物或其混合物用于沉积各种成的膜(如下文公开的那样),使用任何公知的使用气相沉积的沉积方法,如MOCVD(金属有机化学气相沉积)、ALD(原子层沉积)、PE-ALD(等离子体增强的原子层沉积)和任何其它沉积方法,如PECVD(等离子体增强的化学气相沉积)或脉冲CVD。
这些新的第V族金属前体因此可用于纯金属、金属氧化物、氧氮化物、氮化物和/或硅化物膜沉积以产生电极和/或高k层,和/或铜扩散膜层等。
在ALD法中,优选温度在100℃至450℃范围内,更优选在150℃至350℃范围内,ALD中的优选脉冲持续时间为1秒,优选压力在0.01托至800托范围内,更优选为0.1托至200托,优选载气选自N2、He、Ar、H2,更优选Ar或N2。优选的N2气罐流速在30-200sccm范围内,优选50sccm至100sccm。
在CVD法中,优选温度在100℃至700℃范围内,更优选200℃至500℃,优选压力在0.01托至800托范围内,优选1托至200托,优选载气选自N2、He、Ar、H2,更优选Ar或N2。优选的N2气罐流速在30-200sccm范围内,优选50sccm至100sccm。
在PECVD法中,优选温度在100℃至700℃范围内,更优选200℃至500℃,优选压力在0.01托至800托范围内,优选1托至200托,优选载气选自N2、He、Ar、H2,更优选Ar或N2,优选的N2气罐流速在30-200sccm范围内,优选50sccm至100sccm。由远程等离子体系统产生H或NH基团并用作共反应物。
在这些上述用途中,如上定义的任何式(I)的化合物可以单独使用或与所述式(I)的一种或多种其它化合物和/或与沉积含金属膜时可用的任何适当添加剂混合使用,如下文所述。根据一个具体实施方案,本发明涉及具有如下特点的这种混合物的如上定义的用途:熔点小于或等于大约50℃,更优选小于或等于35℃,即在室温下将为液体形式或接近液体形式,这使它们更容易输送,和/或具有在100℃下高于0.01托的蒸气压。
可以使用上述前体,如氮化物、碳化物、硅化物、氮硅化物(MSiN)、氧化物(例如MeOj)、氧氮化物(MOxNy)和两种不同金属M1和M2的氧氮化物(M1M2OxNy)在基底上获得各种膜。
可以如下概括本发明的方法:
根据一个实施方案,该新金属源的气化通过将载气引入含有所述新金属源的加热容器来实现。容器优选在使所述金属源达到足够蒸气压的温度下加热。载气可选自,但不限于,Ar、He、H2、N2或它们的混合物。所述金属源可以在该容器中混合到溶剂或另一金属源或它们的混合物中。该容器可以例如在80℃-140℃范围内的温度下加热。本领域技术人员认为,可以调节该容器的温度以控制气化前体的量。
根据另一实施方案,所述金属源以液态送入气化器,在此将其气化。可以将所述金属源混合到溶剂中。可以将所述金属源混合到另一金属源中。可以将所述金属源混合物混合到溶剂或溶剂混合物中。可以将所述金属源混合到稳定剂中。
随后将该气化金属源引入反应室,在此其与基底接触。可以将基底加热至足够温度以便以足够生长速率和所需物理状态和组成获得所需膜。典型温度在100℃至700℃范围内。该温度优选低于或等于450℃。控制反应室中的压力以便以足够生长速率获得所需的含金属的膜。典型压力为1.33Pa(=0.01托)至13.3kPa(=100托)或更高。
根据另一实施方案,可以将金属源混合到反应物物类中,随后将该混合物引入反应室。
在本发明的另一实施方案中,可以在反应室中将该金属源混合到反应物物类中。
根据再一实施方案,金属源和反应物物类同时引入(化学气相沉积)、相继引入(原子层沉积),或它们的任何组合(一种实例是在一次脉冲中一起引入金属源和另一金属源,并在另一脉冲中引入氧[改进的原子层沉积];另一实例是连续引入氧并脉冲引入金属源(脉冲-化学气相沉积))。
也可以将反应物物类引入远离反应室的等离子体系统中以使这些物类在引入反应室之前分解成自由基。
根据其中基于目标金属的膜含有氧,例如,但不限于,金属氧化物或金属氧氮化物的另一实施方案,反应物物类应包括氧源,其选自氧气(O2),氧自由基(例如O·或OH·),其例如由远程等离子体产生,臭氧(O3)、NO、N2O、NO2、水分(H2O)和H2O2或它们的任何混合物。
根据其中基于目标金属的膜含有氮,例如,但不限于,金属氮化物或金属碳氮化物的再一实施方案,反应物物类包括氮源,其选自但不限于,氮气(N2)、氨、肼和烷基衍生物、含N的基团(例如N、NH、NH2 ·)、NO、N2O、NO2、胺。
如果基于目标金属的膜含有碳,例如,但不限于,金属碳化物或金属碳氮化物,反应物物类包括碳源,其选自,但不限于,甲烷、乙烷、丙烷、丁烷、乙烯、丙烯、叔丁烯、异丁烯、CCl4。
如果基于目标金属的膜含有硅,例如,但不限于,金属硅化物、硅氮化物、硅酸盐、硅碳氮化物,反应物物类应包括硅源,其选自SiH4、Si2H6、Si3H8、TriDMAS、BDMAS、BDEAS、TDEAS、TDMAS、TEMAS、(SiH3)3N、(SiH3)2O、三甲硅烷基胺、二硅氧烷、三甲硅烷基胺、乙硅烷、丙硅烷、烷氧基硅烷SiHx(OR1)4-x、硅烷醇Si(OH)x(OR1)4-x(优选Si(OH)(OR1)3);更优选Si(OH)(OtBu)3、氨基硅烷SiHx(NR1R2)4-x(其中x为0至4;R1和R2独立地为H或直链、支化或环状C1-C6碳链);优选TriDMASSiH(NMe2)3、BTBAS SiH2(NHtBu)2);BDEAS SiH2(NEt2)2)及其混合物。或者目标膜可含锗。上述含Si的源可以被类似的含Ge的源替代。
可以在引入反应室之前将金属源混合到另一金属源中以沉积含多金属的薄膜或将这些金属源同时引入反应室并在反应室中将它们和/或与其它反应物物类混合在一起。
但是还可以将第一金属源、第二金属源和反应物物类同时引入(化学气相沉积)、相继引入(原子层沉积)或它们的任何组合(一种实例是在一次脉冲中一起引入第一金属源和第二金属源,并在另一脉冲中引入氧[改进的原子层沉积];另一实例是连续引入氧并脉冲引入金属源(脉冲-化学气相沉积))引入反应室中。
第二金属源应选自钽、镧系元素和稀土金属源(Sc、Y、La、Ce、Pr、Nd、Gd...)源,如稀土二酮化物Ln(-O-C(R1)-C(R2)-C(R3)-O-)(-O-C(R4)-C(R5)-C(R6)-O-)(-O-C(R7)-C(R8)-C(R9)-O-)(其中各Ri独立地为H或直链、支化或环状C1-C6碳链)、环戊二烯基Ln(R1Cp)(R2Cp)(R3Cp)(其中各Ri独立地为H或直链、支化或环状C1-C6碳链)、Ln(NR1R2)(NR3R4)(NR5R6)及其混合物。第二金属源也可以是铝源,其选自三甲基铝、二甲基氢化铝、烷氧基铝烷AlRi x(OR’)3-x(其中x为0至3;R1和R2独立地为H或直链、支化或环状C1-C6碳链;优选AlR1R2(OR’),最优选AlMe2(OiPr))、酰氨基铝烷AIRi x(NR’R”)3-x(其中x为0至3;R1和R2独立地为H或直链、支化或环状C1-C6碳链)及其混合物。所述另一金属源或是钨、钼源。或者所述另一金属源可以是铪、锆或钛源,如M(OR1)4或其它含烷氧化物的金属源,M(NR1R2)4,或含有这些物类的加合物。或者该第二金属源可以是二价金属源(优选Mg、Ca、Zn、Sr、Ba),其选自,但不限于金属β-二酮化物或含这些物类的加合物。
反应物可以同时引入(化学气相沉积)、相继引入(原子层沉积),或它们的任何组合。
实施例
1.使用NbCp(=NtBu)(NEtMe) 2 和氨的CVD法
将NbCp(=NtBu)(NEtMe)2储存到容器中。该容器在120℃下加热并使用50sccm流速的N2作为载气。使用氨(NH3)作为氮源。在400℃下加热基底。将前体与NH3同时引入反应室。获得氮化铌膜。
2.使用NbCD(=NtBu)(NEtMe) 2 和氨的ALD法
将NbCp(=NtBu)(NEtMe)2储存到容器中。该容器在120℃下加热并使用50sccm流速的N2作为载气。使用氨(NH3)作为氮源。在400℃下加热基底。将前体与NH3相继引入反应室:在第一步骤中经8秒引入一脉冲NbCp(=NtBu)(NEtMe)2,接着N2吹扫13秒。随后经8秒向反应室中引入一脉冲NH3,接着N2吹扫13秒。随后再进行第一步骤。由此进行400个周期。获得氮化铌膜。
本发明的前体适用于在原子水平控制厚度和组成的情况下在高纵横比结构中制得极薄、均匀和共形的薄膜。这些薄膜非常适用在半导体工业中,例如作为:
a.BEOL用途中的铜扩散膜
b.CMOS金属栅
c.金属-绝缘体-金属结构中的电极
d.金属-绝缘体-金属结构中的高-k层
实施例:NbNx,VNx,Nb,,V,VOx,NbOx...TaNbN,TaNbOx,BiNbOx,BiTaNbOx。
尽管这些前体看起来非常适用于半导体工业,但其不仅限于该工业。含V和Nb的层例如可尤其用于提高耐磨性、催化应用和传感器。
Claims (16)
1.在基底上形成含金属M的层的方法,该方法包括至少下列步骤:
a)提供包含至少一种选自下组的前体化合物的蒸气:
(Cp)V(=NtBu)(NEt2)2
(Cp)V(=NtBu)(NMe2)2
(Cp)V(=NtBu)(NEtMe)2
(Cp)V(=NiPr)(NEt2)2
(Cp)V(=NiPr)(NMe2)2
(Cp)V(=NiPr)(NEtMe)2
(Cp)V(=NC5H11)(NEt2)2
(Cp)V(=NC5H11)(NMe2)2
(Cp)V(=NC5H11)(NEtMe)2
(Cp)Nb(=NtBu)(NEt2)2
(Cp)Nb(=NtBu)(NMe2)2
(Cp)Nb(=NtBu)(NEtMe)2
(Cp)Nb(=NiPr)(NEt2)2
(Cp)Nb(=NiPr)(NMe2)2
(Cp)Nb(=NiPr)(NEtMe)2
(Cp)Nb(=NC5H11)(NEt2)2
(Cp)Nb(=NC5H11)(NMe2)2
(Cp)Nb(=NC5H11)(NEtMe)2;
b)提供至少一种选自臭氧和水的反应气体;和
c)根据沉积法,使所述蒸气与基底反应以在所述基底的至少一个表面上形成含金属络合物的层。
2.权利要求1的方法,其中所述沉积法是原子层沉积法。
3.权利要求1的方法,其中所述沉积法是化学气相沉积法。
4.权利要求1至3之一的方法,进一步包括步骤:
d)使步骤c)中获得的络合物与选自另一金属源、还原反应物和/或氮化反应物和/或氧化反应物的试剂反应。
5.权利要求1至3之一的方法,其中步骤a)中提供的蒸气进一步包含一种或多种金属(M′)-有机前体以产生含M和M′的薄膜。
6.权利要求1至3之一的方法,其中基底温度为100℃至700℃,且其中含有该基底的沉积室的压力为1.33Pa至100kPa。
7.权利要求6的方法,其中基底温度为150℃至450℃,且其中含有该基底的沉积室的压力低于25kPa。
8.权利要求1至3之一的方法,进一步包括用选自氢气、氮气、氦气、氩气及其混合物的惰性气体从基底上吹除包含所述至少一种前体化合物的过量的蒸气的步骤。
9.制造半导体结构的方法,包括在半导体衬底上形成含金属M的层的步骤:
a)提供包含至少一种选自下组的前体化合物的蒸气:
(Cp)V(=NtBu)(NEt2)2
(Cp)V(=NtBu)(NMe2)2
(Cp)V(=NtBu)(NEtMe)2
(Cp)V(=NiPr)(NEt2)2
(Cp)V(=NiPr)(NMe2)2
(Cp)V(=NiPr)(NEtMe)2
(Cp)V(=NC5H11)(NEt2)2
(Cp)V(=NC5H11)(NMe2)2
(Cp)V(=NC5H11)(NEtMe)2
(Cp)Nb(=NtBu)(NEt2)2
(Cp)Nb(=NtBu)(NMe2)2
(Cp)Nb(=NtBu)(NEtMe)2
(Cp)Nb(=NiPr)(NEt2)2
(Cp)Nb(=NiPr)(NMe2)2
(Cp)Nb(=NiPr)(NEtMe)2
(Cp)Nb(=NC5H11)(NEt2)2
(Cp)Nb(=NC5H11)(NMe2)2
(Cp)Nb(=NC5H11)(NEtMe)2;
b)提供至少一种选自臭氧和水的反应气体;和
c)根据沉积法,使所述蒸气与基底反应以在所述半导体衬底的至少一个表面上形成含金属络合物的层。
10.权利要求9的方法,其中所述沉积法是原子层沉积法。
11.权利要求9的方法,其中所述沉积法是化学气相沉积法。
12.权利要求9至11之一的方法,进一步包括步骤:
d)使步骤c)中获得的络合物与选自另一金属源、还原反应物和/或氮化反应物和/或氧化反应物的试剂反应。
13.权利要求9至11之一的方法,其中步骤a)中提供的蒸气进一步包含一种或多种金属(M′)-有机前体以产生含M和M′的薄膜。
14.权利要求1至3之一的方法,进一步包括用选自氢气、氮气、氦气、氩气及其混合物的惰性气体从基底上吹除包含所述至少一种前体化合物的过量的蒸气的步骤。
15.选自下组的化合物:
(Cp)V(=NtBu)(NEt2)2
(Cp)V(=NtBu)(NMe2)2
(Cp)V(=NtBu)(NEtMe)2
(Cp)V(=NiPr)(NEt2)2
(Cp)V(=NiPr)(NMe2)2
(Cp)V(=NiPr)(NEtMe)2
(Cp)V(=NC5H11)(NEt2)2
(Cp)V(=NC5H11)(NMe2)2和
(Cp)V(=NC5H11)(NEtMe)2。
16.选自下组的化合物:
(Cp)Nb(=NiPr)(NEt2)2
(Cp)Nb(=NiPr)(NMe2)2
(Cp)Nb(=NiPr)(NEtMe)2
(Cp)Nb(=NC5H11)(NEt2)2
(Cp)Nb(=NC5H11)(NMe2)2和
(Cp)Nb(=NC5H11)(NEtMe)2。
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JP2012505177A (ja) | 2012-03-01 |
CN102177163A (zh) | 2011-09-07 |
CN103741119B (zh) | 2017-04-12 |
JP5746034B2 (ja) | 2015-07-08 |
US20130295778A1 (en) | 2013-11-07 |
WO2010040741A1 (en) | 2010-04-15 |
EP2174942A1 (en) | 2010-04-14 |
EP2174942B1 (en) | 2011-11-30 |
KR101602984B1 (ko) | 2016-03-11 |
KR20110081181A (ko) | 2011-07-13 |
US9040372B2 (en) | 2015-05-26 |
CN103741119A (zh) | 2014-04-23 |
US20110195574A1 (en) | 2011-08-11 |
ATE535534T1 (de) | 2011-12-15 |
US8460989B2 (en) | 2013-06-11 |
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