CN1145632C - 第iv副族元素的络合化合物 - Google Patents

第iv副族元素的络合化合物 Download PDF

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CN1145632C
CN1145632C CNB99813824XA CN99813824A CN1145632C CN 1145632 C CN1145632 C CN 1145632C CN B99813824X A CNB99813824X A CN B99813824XA CN 99813824 A CN99813824 A CN 99813824A CN 1145632 C CN1145632 C CN 1145632C
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complex compound
ligand
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compound
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CN1328562A (zh
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F·欣特迈尔
����ĸ�
R·梅茨格尔
C·维尔纳
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Infineon Technologies AG
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    • 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
    • C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
    • 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 System
    • C07F9/005—Compounds of elements of Group 5 of the Periodic System without metal-carbon linkages
    • 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
    • C23C16/22—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 deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
    • C23C16/405—Oxides of refractory metals or yttrium

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
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Abstract

本发明涉及第IV或V副族元素的新型络合物，该络合物在化学汽相沉积(CVD)-技术中以形成改进型前体组合。这种络合物排除了带α位质子的烷氧化物配位体，这样，通过络合物的水解不再释放任何还原剂。

Description

第IV副族元素的络合化合物
本发明涉及第IV或V副族元素的新型络合物，该络合物构成用于化学汽相淀积(CVD)技术的一种改进型的前体化合物和/或前体组合。前体组合系指在CVD反应开始时汽化的物料混合物(例如金属络合物或前体和溶剂)。
US 5 820 664报导过前体组合。例如，对于SrBi2Ta2O9(SBT)的CVD淀积采用有[Ta(OiPr)4thd](参见Sp.6；Z.42)的前体组合，该组合含有带α-位质子的烷氧化物配位体Ta-络合物，从而含潜在的还原剂(形成相应的酮)。
为了得到稳定的Bi2O3-淀积速率，采用Bi(thd)3代替前体Bi(Ph)3(参见F.Hintermaier等，Vortrag auf dem InternationalSymposium on Integrated Ferroelectrics(一体化铁电体国际讨论会报告)，Monterey，CA，USA，1998)。在有还原剂的存在下，Bi(thd)3容易还原成金属。而且，前体[Ta(OiPr)4thd]例如，通过水解释放HOiPr，后者起还原剂的作用或者按配位体交换反应：Ta(OiPr)4thd+Bi(thd)3-＞Ta(thd)2(oiPr)3+Bi(thd)2(oiPr)生成Bi(thd)2(OiPr)，该化合物在内氧化还原反应中使Bi3+金属离子还原，释放出元素铋。
因此本发明的目的在于提供一种新型络合化合物，该化合物宜作为前体在用Bi3+前体进行CVD淀积时保持稳定和/或在配位体交换反应的情况下有助于在CVD技术的反应条件下形成热稳定的副产物，该副产物所含的铋仍处于氧化态。
本发明通过权利要求1的络合化合物达到此目的，作为络合剂的该化合物只含不带α-位质子的烷氧化物，而且在空间上对配位体有很严格的要求。
本发明的主要目的是提供一种通式为
                     M(L)x(R3C-O-)y-x的络合物，其中
M是稳定的中心原子，来自周期表的第IV或V副族，
L是β-二酮盐；β-酮亚胺盐和/或β-二亚胺盐，
(R3C-O-)是一种烷氧化物配位体，其中R可以是相同的或不同的，代表C-原子为1-24的烷基，可以是支链的或直链的，有时可以是取代的或络合的，
x不等于0，并是1-4之间的数，以及
y不等于0，并根据中心原子的氧化程度可取2、3、4或5。
其次，本发明的目的还在于这种络合物对铁电体层、仲电体层和高ε层淀积中的应用。
最后，本发明的目的在于提供一种包含以新型络合物作前体的前体组合。
本发明优选采用钽或铌作络合物的中心原子。
优选采用叔丁基-和/或叔戊基根作烷氧化物配位体的叔基。
根据一种优选结构，采用thd、2，2，6，6四甲基-3，5-庚二酮盐作在空间有严格要求的配位体。
根据一个优选的实施方案，在络合物的中心原子上形成4个带有(thd)配位体的烷氧化物配位体。
“络合物的稳定中心原子”系指周期表中的元素，其最常见的同位素不进行放射性衰变。优选选自Ti、Zr、Hf、V、Nb和Ta的金属，特别优选Ta。
烷氧化物配位体系指通过醇基的氧原子结合的烷氧基配位体，其通式为
                        -O-CR3其中R可是是相同的或不同的，它表示C-原子为1-24的烷基，它可以是支链的或直链的，有时可以是取代的和/或络合物。而且，例如在烷氧基配位体还含有醚、胺和/或硫基的情况是有利的，这些化合物可对中心原子起辅助供体的作用。
特别优选使用下面通式的烷氧化物配位体：
             -O-C(CH3)3-n[(CH2)m-CH3]n其中n的值可取0-3，和m的值可取0-3。
优选采用β-二酮盐的衍生物、β-酮亚胺盐的衍生物和β-二亚胺盐的衍生物。
优先采用2，2，6，6四甲基-3，5-庚二酮盐(thd)。其它的优选配位体是例如乙酰丙酮盐(acac)；六氟戊二酮盐(hfac)；1，1，1-三氟2，4-戊二酮盐(tfac)；6，6，7，7，8，8-七氟-2，2-二甲基-3，5-辛二酮盐；2，2，7-三甲基-3，5-辛二酮盐；1，1，1，5，5，6，6，7，7，7-十氟-2，4-庚二酮盐；以及1，1，1-三氟-6-甲基-2，4-二酮盐。
络合物的制造按下列模式经过配位体交换反应进行：
从一种低钽-烷氧化物出发，例如Ta(thd)p(OMe)5-p(p可取1-4之间的值)。举例而言，这种氧化物可在添加苯的条件下溶于叔丁醇-或叔戊醇，并在回流下煮沸并同时蒸馏释放出的醇类(平衡朝有利于形成新型络合物的方向转移)，这里指甲醇类。
络合物Ta(thd)(OtBu)4作前体的优点在于，在Bi(thd)3反应的条件下生成热稳定的化合物Bi(thd)a(OtBu)b(其中a和b的总是取1或2)。此外，在有时出现水解的情况下tBuOH作为醇析出，这种化合物无任何α-位质子，因而不起还原剂的作用。
Ta(thd)(OtBu)4具有与Ta(thd)(OiPr)4相似的汽化性质，因为两种化合物具有近似的分子量。
作为用于沉积SBT的前体组合，本发明推荐：
-Sr(thd)2(pmdeta)或Sr(thd)2(四甘醇)，
-Bi(thd)3，和
-Ta(thd)(OtBu)4或Ta(thd)(OtPe)4。
但是所述络合物，特别是Ta的络合物，不仅只用于SBT淀积。总的说来，更多还能用于在金属氧化物基底上进行薄膜的CVD沉积。
例如，这类薄膜可在贮存器技术中找到应用，例如对于动态随机存取记忆器(DRAM)和铁电体随机存取记忆器(FeRAM)。
这里还可考虑用于五氧化钽的淀积，该化合物将在下一代DRAM中作为介电质得到应用。

Claims (1)

1.一种用于SBT淀积的前体组合，它包括下列化合物：
-Sr(thd)2(pmdeta)或Sr(thd)2(四甘醇二甲醚)
-Bi(thd)3，和
-Ta(thd)(OtBu)4或Ta(thd)(OtPe)4。
CNB99813824XA 1998-11-26 1999-11-02 第iv副族元素的络合化合物 Expired - Fee Related CN1145632C (zh)

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DE59904296D1 (de) 2003-03-20
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EP1133499A1 (de) 2001-09-19
WO2000032608A1 (de) 2000-06-08
US6527848B2 (en) 2003-03-04
JP2002531692A (ja) 2002-09-24
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KR100439444B1 (ko) 2004-07-09
US20020000175A1 (en) 2002-01-03
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