CN1328562A - 第iv副族元素的络合化合物 - Google Patents
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 11
- 239000003446 ligand Substances 0.000 claims abstract description 20
- 239000002243 precursor Substances 0.000 claims abstract description 18
- 150000004703 alkoxides Chemical class 0.000 claims abstract description 10
- 125000004429 atom Chemical group 0.000 claims description 12
- 230000008021 deposition Effects 0.000 claims description 10
- 229910052715 tantalum Inorganic materials 0.000 claims description 4
- 125000004213 tert-butoxy group Chemical group [H]C([H])([H])C(O*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 4
- 230000000737 periodic effect Effects 0.000 claims description 3
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 2
- CUJRVFIICFDLGR-UHFFFAOYSA-N acetylacetonate Chemical compound CC(=O)[CH-]C(C)=O CUJRVFIICFDLGR-UHFFFAOYSA-N 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical group [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 2
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 2
- 230000007704 transition Effects 0.000 claims description 2
- SQNZLBOJCWQLGQ-UHFFFAOYSA-N 6,6,7,7,8,8,8-heptafluoro-2,2-dimethyloctane-3,5-dione Chemical class CC(C)(C)C(=O)CC(=O)C(F)(F)C(F)(F)C(F)(F)F SQNZLBOJCWQLGQ-UHFFFAOYSA-N 0.000 claims 1
- 125000000217 alkyl group Chemical group 0.000 claims 1
- 125000004432 carbon atom Chemical group C* 0.000 claims 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- ZUHZGEOKBKGPSW-UHFFFAOYSA-N tetraglyme Chemical compound COCCOCCOCCOCCOC ZUHZGEOKBKGPSW-UHFFFAOYSA-N 0.000 claims 1
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 9
- 239000003638 chemical reducing agent Substances 0.000 abstract description 5
- 230000007062 hydrolysis Effects 0.000 abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 3
- 238000000151 deposition Methods 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 6
- 125000003253 isopropoxy group Chemical group [H]C([H])([H])C([H])(O*)C([H])([H])[H] 0.000 description 4
- MSXVEPNJUHWQHW-UHFFFAOYSA-N 2-methylbutan-2-ol Chemical compound CCC(C)(C)O MSXVEPNJUHWQHW-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 125000003545 alkoxy group Chemical group 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- -1 tert-amyl groups Chemical group 0.000 description 2
- 125000003158 alcohol group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical group [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000005258 radioactive decay Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 125000004149 thio group Chemical group *S* 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
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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 Table
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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
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/005—Compounds of elements of Group 5 of the Periodic Table 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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- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
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- Chemical Vapour Deposition (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
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)。
US5820664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: 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 (9)
1.一种下列通式的络合物
M(L)x(R3C-O-)y-x其中
M是稳定的中心原子,它取自周期表第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-)是烷氧化物配位体,其中R可以是相同的或不同的,并表示碳原子为1-24的烷基,它可以是支链直链的,有时是取代的和/或络合的,
x不等于0,其值介于1-4之间,和
y不等于0,根据中心原子的氧化程度为2、3、4或5。
2.权利要求1的络合物,其中心原子为钽。
3.权利要求1或2的络合物,其中配位体L为2,2,6,6四甲基-3,5-庚二酮盐[thd];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);6,6,7,7,8,8,8-七氟-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;和1,1,1-三氟-6-甲基-2,4-二酮盐。
4.上述权利要求之-的络合物,其中R是甲基和/或乙基。
5.上述权利要求之一的络合物,其中除4个烷氧化物配位体之外还有[thd]-配位体络合在中心原子上。
6.一种用于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)2,和
-Ta(thd)(OtBu)4或Ta(thd)(OtPe)4。
7.权利要求1-5之一的络合物在淀积铁电体SrBi2Ta2O9层时作为前体的应用。
8.权利要求1-5之一的络合物在淀积高εTa2O5层时作为前体的应用。
9.权利要求1-5之一的络合物在制造FRAMS和/或DRAMS时作为前体的应用。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19854640.8 | 1998-11-26 | ||
DE19854640 | 1998-11-26 |
Publications (2)
Publication Number | Publication Date |
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CN1328562A true CN1328562A (zh) | 2001-12-26 |
CN1145632C CN1145632C (zh) | 2004-04-14 |
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Application Number | Title | Priority Date | Filing Date |
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CNB99813824XA Expired - Fee Related CN1145632C (zh) | 1998-11-26 | 1999-11-02 | 第iv副族元素的络合化合物 |
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Country | Link |
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US (1) | US6527848B2 (zh) |
EP (1) | EP1133499B1 (zh) |
JP (1) | JP3566211B2 (zh) |
KR (1) | KR100439444B1 (zh) |
CN (1) | CN1145632C (zh) |
DE (1) | DE59904296D1 (zh) |
WO (1) | WO2000032608A1 (zh) |
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US6303391B1 (en) * | 1997-06-26 | 2001-10-16 | Advanced Technology Materials, Inc. | Low temperature chemical vapor deposition process for forming bismuth-containing ceramic films useful in ferroelectric memory devices |
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-
1999
- 1999-11-02 EP EP99960855A patent/EP1133499B1/de not_active Expired - Lifetime
- 1999-11-02 KR KR10-2001-7006517A patent/KR100439444B1/ko not_active IP Right Cessation
- 1999-11-02 CN CNB99813824XA patent/CN1145632C/zh not_active Expired - Fee Related
- 1999-11-02 DE DE59904296T patent/DE59904296D1/de not_active Expired - Fee Related
- 1999-11-02 JP JP2000585249A patent/JP3566211B2/ja not_active Expired - Fee Related
- 1999-11-02 WO PCT/DE1999/003495 patent/WO2000032608A1/de active IP Right Grant
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107743417A (zh) * | 2015-07-14 | 2018-02-27 | Lg 纳米水公司 | 用于水通量提高的化学添加剂 |
CN107743417B (zh) * | 2015-07-14 | 2021-08-10 | Lg 纳米水公司 | 用于水通量提高的化学添加剂 |
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WO2000032608A1 (de) | 2000-06-08 |
DE59904296D1 (de) | 2003-03-20 |
EP1133499B1 (de) | 2003-02-12 |
JP3566211B2 (ja) | 2004-09-15 |
KR20010080559A (ko) | 2001-08-22 |
EP1133499A1 (de) | 2001-09-19 |
US6527848B2 (en) | 2003-03-04 |
JP2002531692A (ja) | 2002-09-24 |
CN1145632C (zh) | 2004-04-14 |
KR100439444B1 (ko) | 2004-07-09 |
US20020000175A1 (en) | 2002-01-03 |
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