CN112292477A - 用于形成含金属的材料的循环沉积方法及包含含金属的材料的膜和结构 - Google Patents
用于形成含金属的材料的循环沉积方法及包含含金属的材料的膜和结构 Download PDFInfo
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- CN112292477A CN112292477A CN201980041932.1A CN201980041932A CN112292477A CN 112292477 A CN112292477 A CN 112292477A CN 201980041932 A CN201980041932 A CN 201980041932A CN 112292477 A CN112292477 A CN 112292477A
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- 239000002184 metal Substances 0.000 title claims abstract description 260
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- 125000004122 cyclic group Chemical group 0.000 title claims abstract description 13
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- 238000006243 chemical reaction Methods 0.000 claims description 84
- 239000000758 substrate Substances 0.000 claims description 78
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- NCXUNZWLEYGQAH-UHFFFAOYSA-N 1-(dimethylamino)propan-2-ol Chemical compound CC(O)CN(C)C NCXUNZWLEYGQAH-UHFFFAOYSA-N 0.000 description 3
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- 229910052741 iridium Inorganic materials 0.000 description 3
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 3
- 150000002602 lanthanoids Chemical class 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
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- 239000000178 monomer Substances 0.000 description 3
- DWFKOMDBEKIATP-UHFFFAOYSA-N n'-[2-[2-(dimethylamino)ethyl-methylamino]ethyl]-n,n,n'-trimethylethane-1,2-diamine Chemical compound CN(C)CCN(C)CCN(C)CCN(C)C DWFKOMDBEKIATP-UHFFFAOYSA-N 0.000 description 3
- DIHKMUNUGQVFES-UHFFFAOYSA-N n,n,n',n'-tetraethylethane-1,2-diamine Chemical compound CCN(CC)CCN(CC)CC DIHKMUNUGQVFES-UHFFFAOYSA-N 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
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- 235000012431 wafers Nutrition 0.000 description 3
- UJTDKNZVLGVLFT-UHFFFAOYSA-N 1,2-Bis(methylthio)ethane Chemical compound CSCCSC UJTDKNZVLGVLFT-UHFFFAOYSA-N 0.000 description 2
- WLDGDTPNAKWAIR-UHFFFAOYSA-N 1,4,7-trimethyl-1,4,7-triazonane Chemical compound CN1CCN(C)CCN(C)CC1 WLDGDTPNAKWAIR-UHFFFAOYSA-N 0.000 description 2
- MDAXKAUIABOHTD-UHFFFAOYSA-N 1,4,8,11-tetraazacyclotetradecane Chemical compound C1CNCCNCCCNCCNC1 MDAXKAUIABOHTD-UHFFFAOYSA-N 0.000 description 2
- HRFJEOWVAGSJNW-UHFFFAOYSA-N 1,4,8,11-tetramethyl-1,4,8,11-tetrazacyclotetradecane Chemical compound CN1CCCN(C)CCN(C)CCCN(C)CC1 HRFJEOWVAGSJNW-UHFFFAOYSA-N 0.000 description 2
- MIOCUERTSIJEDP-UHFFFAOYSA-N 2-diethylphosphanylethyl(diethyl)phosphane Chemical compound CCP(CC)CCP(CC)CC MIOCUERTSIJEDP-UHFFFAOYSA-N 0.000 description 2
- UBAYCEQOGPEGJA-UHFFFAOYSA-N 3-(dimethylhydrazinylidene)-2-methylbutan-2-olate manganese(2+) Chemical compound [Mn+2].CN(C)N=C(C)C(C)(C)[O-].CN(C)N=C(C)C(C)(C)[O-] UBAYCEQOGPEGJA-UHFFFAOYSA-N 0.000 description 2
- YHLILMKECDOCMB-UHFFFAOYSA-N 3-(dimethylhydrazinylidene)-2-methylbutan-2-olate nickel(2+) Chemical compound [Ni+2].CN(C)N=C(C)C(C)(C)[O-].CN(C)N=C(C)C(C)(C)[O-] YHLILMKECDOCMB-UHFFFAOYSA-N 0.000 description 2
- UDQOBFJTYHSIPJ-UHFFFAOYSA-N 3-diethylphosphanylpropyl(diethyl)phosphane Chemical compound CCP(CC)CCCP(CC)CC UDQOBFJTYHSIPJ-UHFFFAOYSA-N 0.000 description 2
- SVQCWDDHEAICGG-UHFFFAOYSA-L CC(CC(N)(C)C)(N)C.[Ni](I)I Chemical compound CC(CC(N)(C)C)(N)C.[Ni](I)I SVQCWDDHEAICGG-UHFFFAOYSA-L 0.000 description 2
- STLRZBGWSTVCGW-UHFFFAOYSA-L CN(CCN(C)C)C.[Co](Cl)Cl Chemical compound CN(CCN(C)C)C.[Co](Cl)Cl STLRZBGWSTVCGW-UHFFFAOYSA-L 0.000 description 2
- FNERMLWFVOBRCD-UHFFFAOYSA-L CN(CCN(C)C)C.[Co](I)I Chemical compound CN(CCN(C)C)C.[Co](I)I FNERMLWFVOBRCD-UHFFFAOYSA-L 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- 239000005749 Copper compound Substances 0.000 description 2
- VMQMZMRVKUZKQL-UHFFFAOYSA-N Cu+ Chemical compound [Cu+] VMQMZMRVKUZKQL-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 description 2
- 229910000792 Monel Inorganic materials 0.000 description 2
- CJKRXEBLWJVYJD-UHFFFAOYSA-N N,N'-diethylethylenediamine Chemical compound CCNCCNCC CJKRXEBLWJVYJD-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 239000004721 Polyphenylene oxide Substances 0.000 description 2
- 229910008336 SnCo Inorganic materials 0.000 description 2
- CUJRVFIICFDLGR-UHFFFAOYSA-N acetylacetonate Chemical compound CC(=O)[CH-]C(C)=O CUJRVFIICFDLGR-UHFFFAOYSA-N 0.000 description 2
- 125000003342 alkenyl group Chemical group 0.000 description 2
- 125000000304 alkynyl group Chemical group 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000000277 atomic layer chemical vapour deposition Methods 0.000 description 2
- 238000003877 atomic layer epitaxy Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- FXOMLMRNOFQSII-UHFFFAOYSA-N chromium(2+) 2-methyl-3-propan-2-yliminobutan-2-olate Chemical compound [Cr+2].CC(C)N=C(C)C(C)(C)[O-].CC(C)N=C(C)C(C)(C)[O-] FXOMLMRNOFQSII-UHFFFAOYSA-N 0.000 description 2
- YYAFKBFJFVPSFW-UHFFFAOYSA-N chromium(2+) 3-(dimethylhydrazinylidene)-2-methylbutan-2-olate Chemical compound [Cr+2].CN(C)N=C(C)C(C)(C)[O-].CN(C)N=C(C)C(C)(C)[O-] YYAFKBFJFVPSFW-UHFFFAOYSA-N 0.000 description 2
- 150000001868 cobalt Chemical class 0.000 description 2
- LYVZGNBMSHODPT-UHFFFAOYSA-N cobalt(2+) 2-methyl-3-propan-2-yliminobutan-2-olate Chemical compound [Co+2].CC(C)N=C(C)C(C)(C)[O-].CC(C)N=C(C)C(C)(C)[O-] LYVZGNBMSHODPT-UHFFFAOYSA-N 0.000 description 2
- 150000004696 coordination complex Chemical class 0.000 description 2
- WHGAMOSRQAYXIO-UHFFFAOYSA-N copper 3-(dimethylhydrazinylidene)-2-methylbutan-2-olate Chemical compound [Cu+2].CN(C)N=C(C)C(C)(C)[O-].CN(C)N=C(C)C(C)(C)[O-] WHGAMOSRQAYXIO-UHFFFAOYSA-N 0.000 description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 2
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical group [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910000856 hastalloy Inorganic materials 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- PXNDECJEMKEQEI-UHFFFAOYSA-N iron(2+) 2-methyl-3-propan-2-yliminobutan-2-olate Chemical compound [Fe+2].CC(C)N=C(C)C(C)(C)[O-].CC(C)N=C(C)C(C)(C)[O-] PXNDECJEMKEQEI-UHFFFAOYSA-N 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- 150000002603 lanthanum Chemical class 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 2
- IMHSAVOVOUFBHU-UHFFFAOYSA-N manganese(2+) 2-methyl-3-propan-2-yliminobutan-2-olate Chemical compound [Mn+2].CC(C)N=C(C)C(C)(C)[O-].CC(C)N=C(C)C(C)(C)[O-] IMHSAVOVOUFBHU-UHFFFAOYSA-N 0.000 description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical class [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 2
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- MFIGJRRHGZYPDD-UHFFFAOYSA-N n,n'-di(propan-2-yl)ethane-1,2-diamine Chemical compound CC(C)NCCNC(C)C MFIGJRRHGZYPDD-UHFFFAOYSA-N 0.000 description 2
- DMQSHEKGGUOYJS-UHFFFAOYSA-N n,n,n',n'-tetramethylpropane-1,3-diamine Chemical compound CN(C)CCCN(C)C DMQSHEKGGUOYJS-UHFFFAOYSA-N 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 2
- 150000002902 organometallic compounds Chemical class 0.000 description 2
- UKODFQOELJFMII-UHFFFAOYSA-N pentamethyldiethylenetriamine Chemical compound CN(C)CCN(C)CCN(C)C UKODFQOELJFMII-UHFFFAOYSA-N 0.000 description 2
- 229920000570 polyether Polymers 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000009738 saturating Methods 0.000 description 2
- 125000003808 silyl group Chemical group [H][Si]([H])([H])[*] 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- RXJKFRMDXUJTEX-UHFFFAOYSA-N triethylphosphine Chemical compound CCP(CC)CC RXJKFRMDXUJTEX-UHFFFAOYSA-N 0.000 description 2
- 238000005019 vapor deposition process Methods 0.000 description 2
- 125000004209 (C1-C8) alkyl group Chemical group 0.000 description 1
- PCCAMUMRVQUYQE-UHFFFAOYSA-N 1-tert-butylimino-2,3,3-trimethylbutan-2-ol Chemical compound CC(C)(C)N=CC(C)(O)C(C)(C)C PCCAMUMRVQUYQE-UHFFFAOYSA-N 0.000 description 1
- LETVAZILRYBHKJ-UHFFFAOYSA-N 1-tert-butylimino-2,3,3-trimethylbutan-2-olate chromium(2+) Chemical compound [Cr+2].CC(C)(C)N=CC(C)([O-])C(C)(C)C.CC(C)(C)N=CC(C)([O-])C(C)(C)C LETVAZILRYBHKJ-UHFFFAOYSA-N 0.000 description 1
- BUYKFLADLZOPLS-UHFFFAOYSA-N 1-tert-butylimino-2,3,3-trimethylbutan-2-olate cobalt(2+) Chemical compound [Co+2].CC(C)(C)N=CC(C)([O-])C(C)(C)C.CC(C)(C)N=CC(C)([O-])C(C)(C)C BUYKFLADLZOPLS-UHFFFAOYSA-N 0.000 description 1
- GXFSDRMBKGFQEC-UHFFFAOYSA-N 1-tert-butylimino-2,3,3-trimethylbutan-2-olate iron(2+) Chemical compound [Fe+2].CC(C)(C)N=CC(C)([O-])C(C)(C)C.CC(C)(C)N=CC(C)([O-])C(C)(C)C GXFSDRMBKGFQEC-UHFFFAOYSA-N 0.000 description 1
- CGFSETBVPYTSTO-UHFFFAOYSA-N 1-tert-butylimino-2,3,3-trimethylbutan-2-olate manganese(2+) Chemical compound [Mn+2].CC(C)(C)N=CC(C)([O-])C(C)(C)C.CC(C)(C)N=CC(C)([O-])C(C)(C)C CGFSETBVPYTSTO-UHFFFAOYSA-N 0.000 description 1
- TXOSZPKFXAPIQS-UHFFFAOYSA-N 2-methyl-3-propan-2-yliminobutan-2-olate nickel(2+) Chemical compound [Ni+2].CC(C)N=C(C)C(C)(C)[O-].CC(C)N=C(C)C(C)(C)[O-] TXOSZPKFXAPIQS-UHFFFAOYSA-N 0.000 description 1
- WQICARGMAGGQMT-UHFFFAOYSA-N 3-(dimethylhydrazinylidene)-2-methylbutan-2-olate iron(2+) Chemical compound [Fe+2].CN(C)N=C(C)C(C)(C)[O-].CN(C)N=C(C)C(C)(C)[O-] WQICARGMAGGQMT-UHFFFAOYSA-N 0.000 description 1
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- NQCCFWOBBPLSGD-UHFFFAOYSA-N C(C)(C)(C)N=CC(C(C)(C)C)(O)C.C(C)(C)(C)N=CC(C(C)(C)C)(O)C.[Fe+2] Chemical compound C(C)(C)(C)N=CC(C(C)(C)C)(O)C.C(C)(C)(C)N=CC(C(C)(C)C)(O)C.[Fe+2] NQCCFWOBBPLSGD-UHFFFAOYSA-N 0.000 description 1
- SADZCFSGBJZMPF-UHFFFAOYSA-N C(C)(C)(C)N=CC(C(C)(C)C)(O)C.C(C)(C)(C)N=CC(C(C)(C)C)(O)C.[Mn+2] Chemical compound C(C)(C)(C)N=CC(C(C)(C)C)(O)C.C(C)(C)(C)N=CC(C(C)(C)C)(O)C.[Mn+2] SADZCFSGBJZMPF-UHFFFAOYSA-N 0.000 description 1
- HJKAZUFVAWLTFI-UHFFFAOYSA-N C(C)(C)(C)N=CC(C(C)(C)C)(O)C.C(C)(C)(C)N=CC(C(C)(C)C)(O)C.[Ni+2] Chemical compound C(C)(C)(C)N=CC(C(C)(C)C)(O)C.C(C)(C)(C)N=CC(C(C)(C)C)(O)C.[Ni+2] HJKAZUFVAWLTFI-UHFFFAOYSA-N 0.000 description 1
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- KLELIHZOQYVPNZ-UHFFFAOYSA-L CN(CCCN(C)C)C.[Co](Cl)Cl Chemical compound CN(CCCN(C)C)C.[Co](Cl)Cl KLELIHZOQYVPNZ-UHFFFAOYSA-L 0.000 description 1
- HNUALPPJLMYHDK-UHFFFAOYSA-N C[CH]C Chemical compound C[CH]C HNUALPPJLMYHDK-UHFFFAOYSA-N 0.000 description 1
- QDVBRRUHORJCQY-UHFFFAOYSA-N C[Si](C)(C)[N-][Si](C)(C)C.CC(C)N1CCN(C(C)C)C1=[Cu+] Chemical compound C[Si](C)(C)[N-][Si](C)(C)C.CC(C)N1CCN(C(C)C)C1=[Cu+] QDVBRRUHORJCQY-UHFFFAOYSA-N 0.000 description 1
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- 229910021012 Co2(CO)8 Inorganic materials 0.000 description 1
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 description 1
- 229910020707 Co—Pt Inorganic materials 0.000 description 1
- 229910020709 Co—Sn Inorganic materials 0.000 description 1
- 229910020515 Co—W Inorganic materials 0.000 description 1
- 229910017566 Cu-Mn Inorganic materials 0.000 description 1
- 229910017871 Cu—Mn Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
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- 229910018100 Ni-Sn Inorganic materials 0.000 description 1
- 229910005102 Ni3Sn Inorganic materials 0.000 description 1
- 229910003306 Ni3Sn4 Inorganic materials 0.000 description 1
- 229910018532 Ni—Sn Inorganic materials 0.000 description 1
- 241000233805 Phoenix Species 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
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- 229910002846 Pt–Sn Inorganic materials 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
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- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
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- XAGWGEBOYZWKFR-UHFFFAOYSA-L [Br-].CN(CCN(C)C)C.[Co+2].[Br-] Chemical compound [Br-].CN(CCN(C)C)C.[Co+2].[Br-] XAGWGEBOYZWKFR-UHFFFAOYSA-L 0.000 description 1
- ATORQOBSCIEGLQ-UHFFFAOYSA-N [Cu+].C(C)(CC)NC(C)=NC(C)CC Chemical class [Cu+].C(C)(CC)NC(C)=NC(C)CC ATORQOBSCIEGLQ-UHFFFAOYSA-N 0.000 description 1
- GPOHEWYMQUEFAZ-UHFFFAOYSA-N [Cu].NO Chemical class [Cu].NO GPOHEWYMQUEFAZ-UHFFFAOYSA-N 0.000 description 1
- BOLFPTURUBFEGF-UHFFFAOYSA-N [Ni].[CH]1C=CC=C1 Chemical class [Ni].[CH]1C=CC=C1 BOLFPTURUBFEGF-UHFFFAOYSA-N 0.000 description 1
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 150000004703 alkoxides Chemical group 0.000 description 1
- 125000005103 alkyl silyl group Chemical group 0.000 description 1
- 150000001409 amidines Chemical class 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 150000001621 bismuth Chemical class 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 1
- 229910000085 borane Inorganic materials 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 238000004871 chemical beam epitaxy Methods 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- OSHLRLXESIGNQS-UHFFFAOYSA-N cobalt(2+) 3-(dimethylhydrazinylidene)-2-methylbutan-2-olate Chemical compound [Co+2].CN(C)N=C(C)C(C)(C)[O-].CN(C)N=C(C)C(C)(C)[O-] OSHLRLXESIGNQS-UHFFFAOYSA-N 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000000109 continuous material Substances 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- RXASRYNSUKRBMC-UHFFFAOYSA-N copper 1-tert-butylimino-2,3,3-trimethylbutan-2-olate Chemical compound [Cu+2].CC(C)(C)N=CC(C)([O-])C(C)(C)C.CC(C)(C)N=CC(C)([O-])C(C)(C)C RXASRYNSUKRBMC-UHFFFAOYSA-N 0.000 description 1
- WSFXESFWSSXEFX-UHFFFAOYSA-N copper 2-methyl-3-propan-2-yliminobutan-2-olate Chemical compound [Cu+2].CC(C)N=C(C)C(C)(C)[O-].CC(C)N=C(C)C(C)(C)[O-] WSFXESFWSSXEFX-UHFFFAOYSA-N 0.000 description 1
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- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- VXGHASBVNMHGDI-UHFFFAOYSA-N digermane Chemical compound [Ge][Ge] VXGHASBVNMHGDI-UHFFFAOYSA-N 0.000 description 1
- PZPGRFITIJYNEJ-UHFFFAOYSA-N disilane Chemical compound [SiH3][SiH3] PZPGRFITIJYNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000001678 elastic recoil detection analysis Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
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- 125000000623 heterocyclic group Chemical group 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
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- 230000008018 melting Effects 0.000 description 1
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- 125000002524 organometallic group Chemical group 0.000 description 1
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- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
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- 150000003254 radicals Chemical class 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
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- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
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- 239000011669 selenium Substances 0.000 description 1
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- 239000010703 silicon Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
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- 238000004544 sputter deposition Methods 0.000 description 1
- 238000000629 steam reforming Methods 0.000 description 1
- 159000000008 strontium salts Chemical class 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- MUQNAPSBHXFMHT-UHFFFAOYSA-N tert-butylhydrazine Chemical compound CC(C)(C)NN MUQNAPSBHXFMHT-UHFFFAOYSA-N 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- 239000013638 trimer Substances 0.000 description 1
- CYTQBVOFDCPGCX-UHFFFAOYSA-N trimethyl phosphite Chemical compound COP(OC)OC CYTQBVOFDCPGCX-UHFFFAOYSA-N 0.000 description 1
- VEDJZFSRVVQBIL-UHFFFAOYSA-N trisilane Chemical compound [SiH3][SiH2][SiH3] VEDJZFSRVVQBIL-UHFFFAOYSA-N 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Images
Classifications
-
- 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
- C23C16/06—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 metallic material
-
- 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
- C23C16/06—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 metallic material
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Abstract
公开了一种沉积含金属的材料的方法。所述方法可包括循环沉积技术的使用，如循环化学气相沉积和原子层沉积。含金属的材料可包括金属间化合物。还公开了一种包括所述含金属的材料的结构和一种用于形成所述材料的系统。
Description
联合研究协议的合作对象
本文要求保护的发明是根据或代表和/或结合赫尔辛基大学(the University ofHelsinki)与ASM微量化学公司(ASM Microchemistry Oy.)之间的联合研究协议进行的。所述协议在作出所要求保护的本发明的日期当天和之前有效，并且所要求保护的本发明是作为在所述协议的范围内进行的活动的结果而作出。
技术领域
本公开总的涉及用于在基板的表面上沉积含金属的材料的方法、包含含金属的材料的膜和结构及用于沉积含金属的材料的反应器和系统。
背景技术
含金属的材料的沉积可用于各种器件如半导体器件、平板显示器件、光伏器件、微电子机械系统(MEMS)、磁阻器件、超导电器件、储能(例如，储氢)器件、锂或钠离子电池等的制造中和/或用于形成催化材料。对于许多应用，常常期望以均匀和/或保形的方式在表面上方沉积含金属的材料，所述表面可包括三维特征，如沟道和/或突出部，这些三维特征可能具有相对高的纵横比。
近来，由于它们相对独特的物理和化学性质，人们对各种器件的形成中金属间化合物的可能使用的兴趣已经增长。金属间化合物通常具有特定的、有序的结晶结构，其可不同于由相同金属形成的合金；所述特定的结构可带来优于非金属间化合物的材料性质。这样的性质包括例如磁阻、超导性、催化活性和储氢容量。举例来说，已经研究了以不同的化学计量含Co或Ni和Sn的金属间化合物作为用于Li-和Na-离子电池的阳极材料、作为用于磁器件的铁磁材料以及用于催化的目的。
含金属的材料，如具有不同化学计量的Co-Sn和Ni-Sn，包括材料的金属间Co3Sn2和Ni3Sn2相，通常已通过例如球磨、电弧熔化、不同的基于溶液的技术、溶剂热和水热路线、电沉积、溅射和电子束蒸发来制备。已采用从两种单源反应物Me3SnCo(CO)4和Ph3SnCo(CO)4的化学气相沉积(CVD)来沉积具有1:1的化学计量并仅含微量Co3Sn2的Co和Sn的合金。也已通过使用SnMe4和Ni基板进行CVD、然后在高温下进行氢处理来沉积Ni3Sn、Ni3Sn2和Ni3Sn4。尽管可使用这样的技术来形成金属间化合物，但这样的技术通常不太适合于在基板的表面上形成金属间材料的均匀、保形膜。
可使用循环沉积技术如原子层沉积来以受控且可重现的方式在基板表面上的复杂三维结构上方以相对均匀(例如，均匀的结晶结构、均匀的组成和/或均匀的厚度)且保形的方式沉积材料。然而，这样的技术通常尚未被用于沉积若干含金属的材料，包括金属间化合物。相反，特别地，金属间化合物通常使用其他技术来形成和/或需要额外的、通常高温的工艺。
相应地，需要用于形成含金属的材料如金属间化合物的改进方法。另外，需要用于形成含金属的材料的均匀和/或保形膜的改进技术。
此部分中提供的问题的任何讨论仅出于为本发明提供上下文的目的引入而不应视为承认任何或所有这些讨论在完成本发明时是已知的。
发明内容
提供此概述是为了以简化的形式引入一系列概念。下文将在本公开的实例实施例的详细描述中更详细地描述这些概念。本发明内容无意于一定确定所要求保护的主题的关键特征或必要特征，也无意于用来限制所要求保护的主题的范围。
根据本公开的至少一个实施例，公开了一种用于沉积金属间化合物的方法。根据各种方面，所述方法为循环沉积工艺，其包括：向反应腔室提供包含第一金属的第一气相反应物(在本文中也称为前体)以与基板的表面反应以形成第一金属物种；和向反应腔室提供包含第二金属的第二气相反应物以与第一金属物种反应以从而形成金属间化合物。可类似地使用另外的反应物来形成包含不止两种金属的金属间化合物。如下文更详细地阐述的，可在基板上形成金属间化合物的膜而无需额外的高温和/或还原步骤。循环沉积工艺可包括例如原子层沉积。
根据本公开的至少一个其他实施例，公开了一种用于形成含金属的材料的方法。含金属的材料可如本文所述包含一种、两种或三种或更多种金属。所述方法可以是循环沉积工艺，如原子层沉积或循环化学气相沉积工艺。循环沉积工艺可包括向反应腔室提供包含第一金属的第一气相反应物以形成第一金属物种和提供包含通式为R-M-H(例如，R(X-n)-MX-Hn)的化合物的第二气相反应物以与第一金属物种反应以从而形成含金属的材料，其中在所述通式中，R为有机基团，M为金属。根据各种实例，X为M的形式氧化态，n可在1至5的范围内。根据各种方面，含金属的材料包含金属混合物、合金和金属间化合物中的一种或多种。包含含金属的材料的膜可以是金属性的、导电的、非导电的或半导电的。示例性的膜可以是超导电的、磁阻的、铁磁的或为催化剂。
根据本公开的至少一个另外的实施例，提供了一种用于供给包含第一金属的第一气相反应物和包含第二金属的第二气相反应物(例如，包含通式为R-M-H(例如，R(X-n)-MX-Hn)的化合物，其中R为有机基团，X为金属的形式氧化态，n为1至5，M为金属)的方法。所述方法可包括：提供配置为用于容纳第二气相反应物(例如，任何本文所述的第二气相反应物)的第二气相反应物源容器，将第二气相反应物源容器与反应腔室流体连接；将第二气相反应物源容器中所含的第二气相反应物加热到约0℃至约400℃、约20℃至约200℃、或约20℃至约100℃的温度；生成至少0.001毫巴的第二气相反应物蒸气压；和向反应腔室供给第二气相反应物。
在本公开的一些实施例中，提供了利用反应性挥发性化学物质的反应器系统。所述反应器系统可包括反应腔室、与反应腔室流体连通的第一气相反应物源容器和与反应腔室流体连通的第二气相反应物源容器。第二气相反应物可包括例如通式为R-M-H—例如，R(X-n)-MX-Hn的化合物，其中R为有机基团，X为金属的形式氧化态，n为1至5，M为金属。
出于概述本公开和所取得的优于现有技术的优点的目的，某些目标和优点可能已在本文上述内容中描述。当然，应理解，未必所有这样的目标或优点都可根据本公开的任何特定实施例取得。因此，举例来说，本领域技术人员应认识到，本公开的实施例可以按照实现或优化如本文所教导或提出的一个优点或一组优点的方式进行，而不必实现如本文可能教导或提出的其他目标或优点。
附图说明
本公开的主题在说明书的结论部分中特别指出并明确要求保护。然而，当结合附图考虑时，最好可通过参考详细描述和权利要求来获得对本公开的更完整的理解，在附图中，相同的标号表示相同的元件，并且其中：
图1示意了根据本公开的至少一个实施例的示例性循环沉积方法的工艺流程；
图2示意了根据本公开的至少一个实施例的示例性循环沉积方法的另一工艺流程；
图3示意了包含根据本公开的至少一个实施例沉积的含金属的膜的示例性器件结构的示意图；
图4示意了根据本公开的至少一个实施例在循环沉积工艺中采用的金属卤化物化合物的实例；
图5示意了根据本公开的至少一个实施例的示例性反应器系统的示意图；和
图6示意了根据本公开的至少一个实施例的示例性第二气相反应物。
应理解，图中的元件仅为简单和清晰起见示意而不一定按比例绘制。举例来说，图中的一些元件的尺寸可能相对于其他元件被放大以帮助改善对所示意的本发明实施例的理解。
具体实施方式
下文提供的对本公开的示例性实施例的描述仅是示例性的并意在仅出于示意的目的；以下描述无意于限制本发明的范围。此外，具有所陈述特征的多个实施例的叙述并不意图排除具有额外特征的其它实施例或并入所陈述特征的不同组合的其它实施例。
如下文更详细地阐述的，本公开的示例性实施例涉及用于沉积含金属的材料如金属间化合物的方法和装置，并涉及包含含金属的材料的膜和结构。虽然下文更详细地描述了本公开解决现有系统和方法的各种缺点的方式，但总体上，本文所述的各种系统和方法采用改进的反应物(有时一般称为前体)和/或改进的沉积技术来沉积具有所需性质的含金属的材料。
如本文所用，术语“前体”和/或“反应物”可指参与化学反应的或参与反应的气相物质源自于此的一种或多种气体/蒸气。化学反应可在气相中和/或在气相与基板表面和/或基板表面上的物种之间发生。
如本文所用，术语“循环沉积”可指向反应腔室中依序引入反应物以在基板上方沉积膜并包括沉积技术如原子层沉积和循环化学气相沉积。
如本文所用，术语“循环化学气相沉积”可指其中将基板依序暴露于两种或更多种挥发性反应物的任何工艺，所述挥发性反应物在基板上反应和/或分解而产生期望的材料。
如本文所用，术语“原子层沉积”(ALD)可指其中在反应腔室中进行沉积循环、例如多个连续沉积循环的气相沉积工艺。通常，在每个循环期间，第一反应物被化学吸附到基板的表面，形成不易于与额外的第一反应物反应的单层或亚单层(即，自限性反应)。其后，可随后向工艺腔室中引入另一第二反应物或反应气体以用于将被化学吸附的物质转化为期望的材料。此外，在每个沉积循环期间还可利用吹扫步骤来在化学吸附的第一和/或第二反应物的转化之后从反应腔室去除过量的第一反应物和/或从反应腔室去除过量的第二反应物、反应气体和/或反应副产物。此外，当使用反应物、反应性气体和/或吹扫气体(例如，惰性载气)的交替脉冲进行时，如本文所用，术语“原子层沉积”还意在包括由相关术语如化学气相原子层沉积、原子层外延(ALE)、分子束外延(MBE)、气体源MBE、有机金属MBE和化学束外延所指定的工艺。
如本文所用，术语“基板”可指具有可向其上沉积材料的表面的任何材料。基板可包括本体材料如硅(例如，单晶硅)，并可包括加在本体材料上面的一个或多个层，包括例如化学吸附的物种。另外，基板可包括各种特征，如形成在基板的至少一部分内或基板的至少一部分上的沟道、通孔、线条等。特征可具有例如大于或等于5、大于或等于10、大于或等于15、或大于或等于20的纵横比，纵横比定义为特征的高度除以特征的宽度。
如本文所用，术语“膜”、“薄膜”、“层”和“薄层”可指沉积的——例如通过本文公开的方法沉积的任何连续或非连续材料。例如，“膜”、“薄膜”、“层”和“薄层”可包括2D材料、纳米棒、纳米管或纳米颗粒或甚至部分或完整分子层或者部分或完整原子层或者原子和/或分子的团簇。“膜”、“薄膜”、“层”和“薄层”可包含具有针孔的材料或层，但仍然是至少部分连续的。
如本文所用，术语“含金属的膜”和“含金属的材料”可指含至少一种金属物种的膜或材料。
如本文所用，术语“金属”可包括半金属或类金属。
如本文所用，“金属间”或“金属间化合物”可指包含具有限定的化学计量的两种或更多种金属元素和有序的晶体结构的化合物。金属间化合物与金属合金的不同在于其晶体结构；金属间化合物的结晶结构以特定的结构排列，而合金通常表现出参与的金属组分中之一的晶体结构。当不同原子之间的键强于相同元素的原子之间的键时，将形成金属间化合物。
在整个本公开中给出了大量的实例材料；应指出，针对每一实例材料给出的化学式不应理解为限制性的，并且给出的非限制性实例材料不应受限于所给实例化学计量。
本公开包括用于向基板上沉积含金属的材料——例如，含金属的材料的膜——的方法。可使用循环沉积工艺进行所述方法以沉积含金属的材料来例如在基板上形成含金属的膜。示例性的方法可在相对低的温度下沉积含金属的膜，如包含金属间化合物、基本上由金属间化合物组成或由金属间化合物组成的膜。另外或替代地，所述方法可沉积含金属的材料，包含所述含金属的材料、基本上由所述含金属的材料组成或由所述含金属的材料组成的膜具有大面积厚度、结晶度和/或组成均匀性。
现在转到附图，图1示意了根据本公开的至少一个实施例的循环沉积方法100。方法100可用于在基板表面上形成金属间化合物，如金属间化合物的膜。
方法100以步骤110开始，其包括向反应腔室中提供至少一个基板和加热基板至沉积温度。沉积温度可取决于例如用来形成金属间化合物的一种或多种反应物。作为实例，可将反应腔室加热到高于0℃并低于600℃、低于500℃、低于400℃、低于300℃或低于250℃、或约20℃至约700℃、约50℃至约500℃、或约50℃至约400℃、约75℃至约300℃或约100℃至约250℃之间。作为特定实例，金属间化合物可包含Co3Sn2，在此情况下，温度可在约170℃至约200℃的范围内；类似地，当金属间化合物包含Ni3Sn2时，温度可在约125℃至约175℃、或约140℃至约160℃的范围内。可控制反应腔室内的压力以在反应腔室中为沉积工艺提供期望的压力。例如，在循环沉积工艺期间反应腔室内的压力可小于1000毫巴、或小于100毫巴、或小于10毫巴、或小于5毫巴，或甚至在一些情况下小于1毫巴，或为约10-8毫巴至约1000毫巴、约10-3毫巴至约100毫巴、约10-2毫巴至约50毫巴、或约0.1毫巴至约10毫巴。
方法100可以步骤120继续，其包括向反应腔室提供包含第一金属的第一气相反应物以与基板的表面反应以形成第一金属物种。此步骤可在与上文结合步骤110所述相同的压力和温度下。向反应腔室提供第一气相反应物的脉冲时间或时间可在例如约0.01秒至约60秒之间、或约0.05秒至约10秒之间、或约0.1秒至约5秒之间的范围内。在步骤120期间，第一气相反应物的流率可小于2000sccm、或小于1000sccm、或小于500sccm、或小于200sccm、或甚至小于100sccm，或可在约1至约5000sccm、约5至约2000sccm、或约10至约1000sccm的范围内。
在提供第一气相反应物的步骤之后，可通过吹扫/泵工艺从反应腔室去除任何过量的第一气相反应物和任何反应副产物(步骤125)。步骤125的持续时间可例如在约0.01秒至约60秒之间、或在约0.05秒至约10秒之间、或在约0.1秒至约5秒之间。在步骤125期间，吹扫气体的流率可小于2000sccm、或小于1000sccm、或小于500sccm、或小于200sccm、或甚至小于100sccm，或可在约1至约5000sccm、约5至约2000sccm、或约10至约1000sccm的范围内。尽管分开示意，但步骤125可视为步骤120的一部分。
方法100可以步骤130继续，该步骤是向反应腔室提供包含第二金属的第二气相反应物以与第一金属物种反应以从而形成金属间化合物。此步骤可在与上文结合步骤110所述相同或不同的压力和/或温度下。向反应腔室提供第二气相反应物的脉冲时间或时间可在约0.01秒至约60秒之间、或约0.05秒至约10秒之间、或约0.1秒至约5秒之间的范围内。在步骤130期间，第二气相反应物的流率可与上文在步骤120期间所述的流率相同或相似。
如图1中所示，随着第二气相反应物与基板表面上的物种反应，将形成金属间化合物——例如，包含金属间化合物、基本上由金属间化合物组成或由金属间化合物组成的膜(步骤140)。
在步骤140之后，可通过吹扫/泵工艺从反应腔室去除任何过量的第二气相反应物和任何反应副产物(步骤145)。该步骤中吹扫气体的流量和/或持续时间可与上文在步骤125中所述的那些相同或相似。此外，尽管分开示意，但步骤145可视为步骤130的一部分。
步骤120和130(及任选地吹扫步骤125和/或145)可构成一个沉积循环。在本公开的一些实施例中，方法100可包括将沉积循环重复一次或多次。例如，方法100可以决策门150继续，其决定循环沉积方法100是继续还是经由步骤160退出。决策门150可基于沉积的金属间化合物的厚度或量来作决定。例如，如果金属间化合物的厚度对于期望的器件结构是不够的，则方法100可返回到步骤120，并可重复步骤120-145。一旦金属间化合物已沉积至期望的厚度或量，则方法可在步骤160处结束，并可使基板经受额外的工艺以形成一个或多个器件或器件结构。
根据方法100的各种方面，在使第二气相反应物与步骤120期间在表面上形成的第一金属物种反应时形成金属间化合物。因此，可在没有额外的还原步骤和/或加热步骤的情况下形成金属间化合物或者包含金属间化合物、基本上由金属间化合物组成或由金属间化合物组成的层或膜。此外，如上文所阐述，金属间化合物可在相对低的温度下形成。
第一气相反应物可包括不同于第二金属的任何第一金属。作为实例，第一金属可以是或可包括过渡金属(例如，3-12族金属)、3-6族金属、7-12族金属、镧系金属、8-11族金属和/或9-10族金属。
根据替代的实施例，如下文结合图2描述的那些，第一气相反应物可包括与第二金属相同的第一金属。当第一金属和第二金属相同时，可形成元素金属膜。如上所述，这样的元素金属膜可包括半金属或类金属。
第一气相反应物可以是或可包括金属卤化物化合物，其中所述金属为或包括所述第一金属。金属卤化物化合物可包含金属氯化物、金属碘化物、金属氟化物或金属溴化物。在本公开的一些实施例中，金属卤化物化合物可包含金属物种，包括但不限于钴、镍或铜中的至少之一。在本公开的一些实施例中，金属卤化物化合物可包含氯化钴、氯化镍和氯化铜中的至少之一。在一些实施例中，金属卤化物化合物可包含二齿含氮加合物形成配体。在一些实施例中，金属卤化物化合物可包含包括两个氮原子的加合物形成配体，其中所述氮原子中的每一个键合到至少一个碳原子。在本公开的一些实施例中，金属卤化物化合物包含键合到中心金属原子的一个或多个氮原子，由此形成金属络合物。图4中示意了这样的化合物的一个实例。另外的第一气相反应物可包括包含磷、氧和/或硫的加合物形成配体。
在一些实施例中，第一气相反应物可包含具有加合物形成配体的过渡金属化合物。在一些实施例中，第一气相相反应物可包含过渡金属化合物。在一些实施例中，第一气相反应物可包含过渡金属卤化物化合物。在一些实施例中，第一气相反应物可包含具有加合物形成配体的过渡金属化合物，如单齿、二齿或多齿加合物形成配体。在一些实施例中，第一气相反应物可包含具有加合物形成配体的过渡金属卤化物化合物，如单齿、二齿或多齿加合物形成配体。在一些实施例中，第一气相反应物可包含具有加合物形成配体的过渡金属化合物，如包含氮的单齿、二齿或多齿加合物形成配体。在一些实施例中，第一气相反应物可包含具有包含磷、氧或硫的加合物形成配体的过渡金属化合物，如包含磷、氧或硫的单齿、二齿或多齿加合物形成配体。例如，在一些实施例中，过渡金属卤化物化合物可包含过渡金属氯化物、过渡金属碘化物、过渡金属氟化物或过渡金属溴化物。在本公开的一些实施例中，过渡金属卤化物化合物可包含过渡金属物种，包括但不限于钴、镍或铜中的至少之一。在本公开的一些实施例中，过渡金属卤化物化合物可包含氯化钴、氯化镍或氯化铜中的至少之一。在一些实施例中，过渡金属卤化物化合物可包含二齿含氮加合物形成配体。在一些实施例中，过渡金属卤化物化合物可包含包括两个氮原子的加合物形成配体，其中所述氮原子中的每一个键合到至少一个碳原子。在本公开的一些实施例中，过渡金属卤化物化合物包含键合到中心过渡金属原子的一个或多个氮原子，由此形成金属络合物。
在本公开的一些实施例中，第一气相反应物可包含具有下式的过渡金属化合物：
(加合物)n-M-Xa
其中所述“加合物”中的每一个为加合物形成配体并可独立地选择为单齿、二齿或多齿加合物形成配体或其混合物：在单齿形成配体的情况下，n为1至4，在二齿或多齿加合物形成配体的情况下，n为1至2；M为过渡金属，例如钴(Co)、铜(Cu)或镍(Ni)；其中Xa中的每一个为另一配体，并可独立地选择为卤化物或其他配体；其中a为1至4，在一些情况下a为2。
在本公开的一些实施例中，过渡金属化合物如过渡金属卤化物化合物中的加合物形成配体可包含单齿、二齿或多齿加合物形成配体，其通过氮原子、磷原子、氧原子或硫原子中的至少之一与过渡金属化合物的过渡金属原子配位。在本公开的一些实施例中，过渡金属化合物中的加合物形成配体可包含环状加合物配体。在本公开的一些实施例中，过渡金属化合物中的加合物形成配体可包含单胺、二胺或多聚胺。在本公开的一些实施例中，过渡金属化合物中的加合物形成配体可包含单醚、二醚或多聚醚。在一些实施例中，过渡金属化合物中的加合物形成配体可包含单膦、二膦或多聚膦。在一些实施例中，过渡金属化合物中的加合物形成配体可包含碳和/或除加合物形成配体中的氮、氧、磷或硫之外还包含碳。
在本公开的一些实施例中，过渡金属化合物中的加合物形成配体可包含一个单齿加合物形成配体。在本公开的一些实施例中，过渡金属化合物中的加合物形成配体可包含两个单齿加合物形成配体。在本公开的一些实施例中，过渡金属化合物中的加合物形成配体可包含三个单齿加合物形成配体。在本公开的一些实施例中，过渡金属化合物中的加合物形成配体可包含四个单齿加合物形成配体。在本公开的一些实施例中，过渡金属化合物中的加合物形成配体可包含一个二齿加合物形成配体。在本公开的一些实施例中，过渡金属化合物中的加合物形成配体可包含两个二齿加合物形成配体。在本公开的一些实施例中，过渡金属化合物中的加合物形成配体可包含一个多齿加合物形成配体。在本公开的一些实施例中，过渡金属化合物中的加合物形成配体可包含两个多齿加合物形成配体。
在本公开的一些实施例中，加合物形成配体包含氮，如胺、二胺或多聚胺加合物形成配体。在这样的实施例中，过渡金属化合物可包含以下中的至少之一：三乙胺(TEA)、N,N,N’,N’-四甲基-1,2-乙二胺(CAS:110-18-9)(TMEDA)、N,N,N′,N′-四乙基乙二胺(CAS:150-77-6)(TEEDA)、N,N’-二乙基-1,2-乙二胺(CAS:111-74-0)(DEEDA)、N,N’-二异丙基乙二胺(CAS:4013-94-9)、N,N,N’,N’-四甲基-1,3-丙二胺(CAS:110-95-2)(TMPDA)、N,N,N’,N’-四甲基甲二胺(CAS:51-80-9)(TMMDA)、N,N,N’,N”,N”-五甲基二亚乙基三胺(CAS:3030-47-5)(PMDETA)、二亚乙基三胺(CAS:111-40-0)(DIEN)|、三亚乙基四胺(CAS:112-24-3)(TRIEN)、三(2-氨基乙基)胺(CAS:4097-89-6)(TREN,TAEA)、1,1,4,7,10,10-六甲基三亚乙基四胺(CAS:3083-10-1)(HMTETA)、1,4,8,11-四氮杂环十四烷(CAS:295-37-4)(Cyclam)、1,4,7-三甲基-1,4,7-三氮杂环壬烷(CAS:96556-05-7)或1,4,8,11-四甲基-1,4,8,11-四氮杂环十四烷(CAS:41203-22-9)。
在本公开的一些实施例中，加合物形成配体包含磷，如膦、二膦或多聚膦加合物形成配体。例如，过渡金属化合物可包含三乙基膦(CAS：554-70-1)、亚磷酸三甲酯(CAS：121-45-)、1,2-双(二乙基膦基)乙烷(CAS：6411-21-8)(BDEPE)或1,3-双(二乙基膦基)丙烷(CAS：29149-93-7)中的至少之一。
在本公开的一些实施例中，加合物形成配体包含氧，如醚、二醚或多聚醚加合物形成配体。例如，过渡金属化合物可包含1,4-二氧六环(CAS：123-91-1)、1,2-二甲氧基乙烷(CAS：110-71-4)(DME，单甘醇二甲醚)、二乙二醇二甲醚(CAS：111-96-6)(二甘醇二甲醚)、三乙二醇二甲醚(CAS：112-49-2)(三甘醇二甲醚)或1,4,7,10-四氧杂环十二烷(CAS：294-93-9)(12-冠-4)中的至少之一。
在本公开的一些实施例中，加合物形成配体可包含硫醚或混合醚胺，如例如1,7-二氮杂-12-冠-4:1,7-二氧杂-4,10-二氮杂环十二烷(CAS:294-92-8)或1,2-双(甲基硫基)乙烷(CAS:6628-18-8)中的至少一种。
在一些实施例中，过渡金属卤化物化合物可包含氯化钴N,N,N’,N’-四甲基-1,2-乙二胺(CoCl2(TMEDA))。在一些实施例中，过渡金属卤化物化合物可包含溴化钴四甲基乙二胺(CoBr2(TMEDA))。在一些实施例中，过渡金属卤化物化合物可包含碘化钴四甲基乙二胺(CoI2(TMEDA))。在一些实施例中，过渡金属卤化物化合物可包含氯化钴N,N,N’,N’-四甲基-1,3-丙二胺(CoCl2(TMPDA))。在本公开的一些实施例中，过渡金属卤化物化合物可包含氯化钴N,N,N’,N’-四甲基-1,2-乙二胺(CoCl2(TMEDA))、氯化镍四甲基-1,3-丙二胺(NiCl2(TMPDA))或碘化镍四甲基-1,3-丙二胺(NiI2(TMPDA))中的至少之一。
其他适合的第一气相反应物可基本上不含卤素物种。基本上不含卤素物种的第一气相反应物(不含卤素的金属前体)包括M(dmap)x(dmap＝二甲基氨基-2-丙醇盐)，其中M为金属、β-二酮阴离子、脒阴离子和其他典型的ALD金属前体。在一些实施例中，不含卤素的金属前体可包含铜、钴和镍中的至少一种。不含卤素的金属前体可因此包含Cu(dmap)2、Ni(dmap)2或Co(dmap)2中的至少一种。
在一些实施例中，不含卤素的金属前体可因此包含至少一个二齿配体，其中金属中心原子通过二齿配体中的至少一个氧和至少一个氮原子键合。在一些实施例中，不含卤素的金属前体可因此包含至少一个二齿配体，其中金属中心原子通过二齿配体中的至少一个氮原子键合。在一些实施例中，不含卤素的金属前体可因此包含至少一个二齿配体和至少一个其他配体，如单齿配体。在一些实施例中，不含卤素的金属前体可因此包含至少一个二齿配体和至少两个其他配体，如单齿配体。在一些实施例中，不含卤素的金属前体可因此包含至少一个二齿配体和至少一个其他配体，如单齿配体，其通过N或O键合到金属中心原子。在一些实施例中，不含卤素的金属前体可因此包含至少一个二齿配体，其中金属中心原子通过二齿配体中的至少一个氮原子键合并通过二齿配体中的至少一个非氮的其他原子键合。在一些实施例中，不含卤素的金属前体可因此包含至少一个二齿配体，其中金属中心原子通过二齿配体中的至少两个氮原子键合。在一些实施例中，不含卤素的金属前体包含至少两个二齿配体。在一些实施例中，不含卤素的金属前体包含两个二齿配体。
合适的不含卤化物的β二酮亚胺阴离子配体(例如，Ni(pda)2)(pda＝戊烷-2,4,-二酮亚胺阴离子配体)化合物的一些实例包含至少一个β-二酮亚胺阴离子配体，并具有通式：
其中M为选自镍、钴、钌、铱、钯、铂、银和金的金属。R1-5中的每一个为独立地选自H及C1-C4直链或支链烷基基团、烷基甲硅烷基基团、烷基氨基化物基团、醇盐基团或烷基甲硅烷基氨基化物基团的有机配体。每一个L独立地选自：烃；含氧烃；胺；多聚胺；联吡啶；含氧杂环；含氮杂环；及它们的组合；并且n为0至4的范围内的整数，包括0和4。特定的实例包括Ni(pda)2。
合适的不含卤化物的脒阴离子化合物(例如，Ni(iPr-AMD)2)的一些实例包括具有选自以下的式的化合物：M(I)AMD、M(II)AMD2和M(III)AMD3以及其低聚物，其中M为金属，AMD为脒阴离子部分，如脒阴离子铜(I)盐、脒阴离子钴(II)盐或者镍、铁、钌、锰、铬、钒、铌、钽、钛和/或镧的脒阴离子盐。
在一个或多个实施例中，一价金属的前体包括挥发性脒阴离子金属(I)盐[M(I)(AMD)]x，其中x＝2、3。这些化合物中的一些具有二聚体结构1，
其中R1、R2、R3、R1′、R2′和R3′为由一个或多个非金属原子构成的基团。在一些实施例中，R1、R2、R3、R1′、R2′和R3′可独立地选自氢、烷基、芳基、烯基、炔基、三烷基甲硅烷基或氟烷基基团或其他非金属原子或基团。在一些实施例中，R1、R2、R3、R1′、R2′和R3′各自独立地为含1至4个碳原子的烷基或氟烷基或甲硅烷基基团。合适的一价金属包括铜(I)、银(I)、金(I)和铱(I)。在一个或多个实施例中，脒阴离子金属盐为脒阴离子铜盐，并且所述脒阴离子铜盐包含N,N′-二异丙基乙脒阴离子铜(I)盐，其对应于将通式1中R1、R2、R1′和R2′取为异丙基基团并将R3和R3′取为甲基基团。在一个或多个实施例中，脒阴离子金属(I)盐为具有通式[M(I)(AMD)]3的三聚体。
在一个或多个实施例中，二价金属前体包括挥发性双脒阴离子金属(II)盐[M(II)(AMD)2]x，其中x＝1、2。这些化合物可具有单体结构2，
其中R1、R2、R3、R1′、R2′和R3′为由一个或多个非金属原子构成的基团。在一个或多个实施例中，还可使用该结构的二聚体，例如[M(II)(AMD)2]2。在一些实施例中，R1、R2、R3、R1′、R2′和R3′可独立地选自氢、烷基、芳基、烯基、炔基、三烷基甲硅烷基、或氟烷基基团或其他非金属原子或基团。在一些实施例中，R1、R2、R3、R1′、R2′和R3′各自独立地为含1至4个碳原子的烷基或氟烷基或甲硅烷基基团。合适的二价金属包括钴、铁、镍、锰、钌、锌、钛、钒、铬、铕、镁和钙。在一个或多个实施例中，脒阴离子金属(II)盐为脒阴离子钴盐，并且所述脒阴离子钴盐包含双(N,N′-二异丙基乙脒阴离子)钴(II)盐，其对应于将通式2中R1、R2、R1′和R2′取为异丙基基团并将R3和R3′取为甲基基团。
在一个或多个实施例中，三价金属的前体包括挥发性三脒阴离子金属(III)盐[M(III)(AMD)3]。通常，这些化合物具有单体结构3，
其中R1、R2、R3、R1′、R2′、R3′、R1″、R2″和R3″为由一个或多个非金属原子构成的基团。在一些实施例中，R1、R2、R3、R1′、R2′、R3′、R1″、R2″和R3″可独立地选自氢、烷基、芳基、烯基炔基、三烷基甲硅烷基、卤素或部分氟化的烷基基团。在一些实施例中，R1、R2、R3、R1′、R2′、R3′、R1″、R2″和R3″各自独立地为含1至4个碳原子的烷基基团。合适的三价金属包括镧、镨和其他镧系金属、钇、钪、钛、钒、铌、钽、铬、铁、钌、钴、铑、铱、铝、镓、铟和铋。在一个或多个实施例中，脒阴离子金属(III)盐为脒阴离子镧盐，并且所述脒阴离子镧盐包含三(N,N′-二-叔丁基乙脒阴离子)镧(III)盐，其对应于将通式3中R1、R2、R1′、R2′、R1″和R2′取为叔丁基基团并将R3、R3′和R3″取为甲基基团。
如本文所用，具有与单体相同的金属对脒阴离子比率但化合物中金属-脒阴离子单元的总数不同的脒阴离子金属盐被称为单体化合物的“低聚物”。因此，单体化合物M(R)AMD2的低聚物包括[M(II)(AMD)2]x，其中x为2、3等。类似地，单体化合物M(I)AMD的低聚物包括[M(I)AMD]x，其中x为2、3等。
特定的实例包括(N,N′-二异丙基乙脒阴离子配体)铜([Cu(iPr-AMD)]2)、双(N,N′-二异丙基乙脒阴离子配体)钴([Co(iPr-AMD)2])、双(N,N′-二叔丁基乙脒阴离子)钴盐([Co(tBu-AMD)2])、三(N,N′-二异丙基乙脒阴离子)镧盐([La(iPr-AMD)3])、三(N,N′-二异丙基-2-叔丁基脒阴离子)镧盐([La(iPr-tBuAMD)3].1/2C6H12)、双(N,N′-二异丙基乙脒阴离子配体)铁([Fe(iPr-AMD)2]2)、双(N,N′-二叔丁基乙脒阴离子)铁盐([Fe(tBu-AMD)2])、双(N,N′-二异丙基乙脒阴离子配体)镍([Ni(iPr-AMD)2])、双(N,N′-二异丙基乙脒阴离子配体)锰([Mn(iPr-AMD)2]2)、双(N,N′-二叔丁基乙脒阴离子)锰盐([Mn(tBu-AMD)2])、三(N,N′-二异丙基乙脒阴离子配体)钛([Ti(iPr-AMD)3])、三(N,N′-二异丙基乙脒阴离子配体)钒([V(iPr-AMD)3])、(N,N′-二异丙基乙脒阴离子)银盐([Ag(iPr-AMD)]x(x＝2和x＝3)、N,N′-二仲丁基乙脒阴离子锂盐、双(N,N′-二仲丁基乙脒阴离子)钴盐([Co(sec-Bu-AMD)2])、N,N′-二仲丁基乙脒阴离子铜(I)盐二聚体([Cu(sec-Bu-AMD)]2)、三(N,N′-二叔丁基乙脒阴离子)铋盐二聚体([Bi(tBu-AMD)3]2)、双(N,N′-二叔丁基乙脒阴离子)锶盐([Sr(tBu-AMD)2]n)、氧化铋Bi2O3和三(N,N′-二异丙基乙脒阴离子配体)钌([Ru(iPr-AMD)3])。
合适的不含卤化物的亚氨基醇盐化合物的一些实例由下式描述：
其中M为选自元素周期表第2至12族的金属；并且R1、R2、R3和R4各自独立地为H或C1-C8烷基。在一种细化中，R1、R2、R3和R4各自独立地为甲基、乙基、正丙基、异丙基、正丁基、仲丁基、异丁基或叔丁基。在另一种细化中，M为Cu、Cr、Mn、Fe、Co或Ni。具有该式的化合物的具体实例包括但不限于双(1-(叔丁基亚氨基)-2,3,3-三甲基丁-2-醇酸)镍(II)、双(1-(叔丁基亚氨基)-2,3,3-三甲基丁-2-醇酸)钴(II)、双(1-(叔丁基亚氨基)-2,3,3-三甲基丁-2-醇酸)铁(II)、双(1-(叔丁基亚氨基)-2,3,3-三甲基丁-2-醇酸)锰(II)、双(1-(叔丁基亚氨基)-2,3,3-三甲基丁-2-醇酸)铬(II)、双(1-(叔丁基亚氨基)-2,3,3-三甲基丁-2-醇酸)铜(II)、双(1-(叔丁基亚氨基)-2,3-二甲基丁-2-醇酸)镍(II)、双(1-(叔丁基亚氨基)-2,3-二甲基丁-2-醇酸)钴(II)、双(1-(叔丁基亚氨基)-2,3-二甲基丁-2-醇酸)铁(II)、双(1-(叔丁基亚氨基)-2,3-二甲基丁-2-醇酸)铜(II)、双(3-((叔丁基亚氨基)甲基)-2,2,4,4-四甲基戊-3-醇酸)锰(II)、双(3-((叔丁基亚氨基)甲基)-2,2,4,4-四甲基戊-3-醇酸)铜(II)、双(3-(异丙基亚氨基)-2-甲基丁-2-醇酸)镍(II)、双(3-(异丙基亚氨基)-2-甲基丁-2-醇酸)钴(II)、双(3-(异丙基亚氨基)-2-甲基丁-2-醇酸)铁(II)、双(3-(异丙基亚氨基)-2-甲基丁-2-醇酸)锰(II)、双(3-(异丙基亚氨基)-2-甲基丁-2-醇酸)铬(II)、双(3-(异丙基亚氨基)-2-甲基丁-2-醇酸)铜(II)、双(3-(2,2-二甲基亚联氨基)-2-甲基丁-2-醇酸)镍(II)、双(3-(2,2-二甲基亚联氨基)-2-甲基丁-2-醇酸)钴(II)、双(3-(2,2-二甲基亚联氨基)-2-甲基丁-2-醇酸)铁(II)、双(3-(2,2-二甲基亚联氨基)-2-甲基丁-2-醇酸)锰(II)、双(3-(2,2-二甲基亚联氨基)-2-甲基丁-2-醇酸)铬(II)和双(3-(2,2-二甲基亚联氨基)-2-甲基丁-2-醇酸)铜(II)。特定的实例包括双(1-(叔丁基亚氨基)-2,3,3-三甲基丁-2-醇酸)镍(H)、双(1-(叔丁基亚氨基)-2,3,3-三甲基丁-2-醇酸)钴(II)、双(1-(叔丁基亚氨基)-2,3,3-三甲基丁-2-醇酸)铁(II)、双(1-(叔丁基亚氨基)-2,3,3-三甲基丁-2-醇酸)锰(II)、双(1-(叔丁基亚氨基)-2,3,3-三甲基丁-2-醇酸)铬(II)、双(1-(叔丁基亚氨基)-2,3,3-三甲基丁-2-醇酸)铜(II)、双(1-(叔丁基亚氨基)-2,3-二甲基丁-2-醇酸)镍(II)、双(1-(叔丁基亚氨基)-2,3-二甲基丁-2-醇酸)钴(II)、双(1-(叔丁基亚氨基)-2,3-二甲基丁-2-醇酸)铁(II)、双(1-(叔丁基亚氨基)-2,3-二甲基丁-2-醇酸)铜(II)、双(3-((叔丁基亚氨基)甲基)-2,2,4,4-四甲基戊-3-醇酸)锰(II)、双(3-((叔丁基亚氨基)甲基)-2,2,4,4-四甲基戊-3-醇酸)铜(II)、双(3-(异丙基亚氨基)-2-甲基丁-2-醇酸)钴(II)、双(3-(异丙基亚氨基)-2-甲基丁-2-醇酸)铁(II)、双(3-(异丙基亚氨基)-2-甲基丁-2-醇酸)锰(II)、双(3-(异丙基亚氨基)-2-甲基丁-2-醇酸)铬(II)、双(3-(2,2-二甲基亚联氨基)-2-甲基丁-2-醇酸)镍(II)、双(3-(2,2-二甲基亚联氨基)-2-甲基丁-2-醇酸)钴(II)、双(3-(2,2-二甲基亚联氨基)-2-甲基丁-2-醇酸)铁(II)、双(3-(2,2-二甲基亚联氨基)-2-甲基丁-2-醇酸)锰(II)、双(3-(2,2-二甲基亚联氨基)-2-甲基丁-2-醇酸)铬(II)、双(3-(2,2-二甲基亚联氨基)-2-甲基丁-2-醇酸)铜(II)。
在一些实施例中，不含卤素的金属前体不包含除所需金属外的其他金属原子(例如，Co、Ni、Cu)。在一些实施例中，不含卤素的金属前体中的金属具有为0的氧化态。在一些实施例中，不含卤素的金属前体中的金属具有+I的氧化态。在一些实施例中，不含卤素的金属前体中的金属具有+III的氧化态。在一些实施例中，不含卤素的金属前体中的金属具有+II的氧化态。在一些实施例中，氧化态为前体中的金属在室温下的氧化态。氧化态在不同的条件下可改变，如在不同的压力、温度和/或气氛中以及当在所述不同的条件下与不同的表面材料接触时。在一些实施例中，不含卤素的金属前体不包含卤化物，如F、Cl、Br或I。在一些实施例中，不含卤素的金属前体包含碳、氢和氮及任选地氧。
在一些实施例中，不含卤化物的铜前体可包含例如Cu(dmap)2或N,N′-二异丙基乙脒阴离子铜(I)盐。在一些实施例中，铜前体可选自β二酮阴离子铜盐化合物；β二酮亚胺阴离子配体铜化合物；氨基醇铜化合物，如Cu(dmae)2、Cu(deap)2或Cu(dmamb)2；脒阴离子铜盐化合物，如Cu(sBu-amd)]2；环戊二烯基铜化合物；羰基铜化合物及它们的组合。在一些实施例中，使用X(acac)y或X(thd)y化合物，其中X为铜，y通常为但不一定为2或3，thd为2,2,6,6-四甲基-3,5-庚二酮阴离子配体。在一些实施例中，不含卤化物的铜前体为乙酸铜(II)、[Cu(HMDS)]4或Cu(nhc)HMDS(六甲基二硅叠氮化1,3-二异丙基咪唑啉-2-亚基铜)或Cu-β二酮亚胺阴离子盐，如Cu(dki)VTMS(dki＝二酮亚胺阴离子)。
在一些实施例中，不含卤化物的镍前体可例如为双(4-N-乙基氨基-3-戊烯-2-N-乙基亚胺阴离子配体)镍(II)。在一些实施例中，镍前体可选自β二酮阴离子镍盐化合物、β二酮亚胺阴离子配体镍化合物、氨基醇镍化合物、脒阴离子镍盐化合物、环戊二烯基镍化合物、羰基镍化合物及它们的组合。在一些实施例中，使用X(acac)y或X(thd)y化合物，其中X为镍，y通常为但不一定为2或3，thd为2,2,6,6-四甲基-3,5-庚二酮阴离子配体。
在一些实施例中，Co前体为β-二酮亚胺阴离子配体Co化合物。在一些实施例中，Co前体为酮亚胺阴离子Co盐化合物。在一些实施例中，Co前体为脒阴离子Co盐化合物。在一些实施例中，Co前体为β-二酮阴离子Co盐化合物。在一些实施例中，Co前体含有至少一个酮亚胺配体或其衍生物。在一些实施例中，Co前体含有至少一个脒配体或其衍生物。在一些实施例中，Co前体含有至少一个酮阴离子配体或其衍生物。在一些实施例中，Co前体为Co2(CO)8、CCTBA、CoCp2、Co(Cp-amd)、Co(Cp(CO)2)、tBu-AllylCo(CO)3或Co(HMDS)2。替代地，可使用金属氢化物和/或铝试剂作为第一气相反应物(例如，对于氢化物-氢化物型反应)。
方法100中使用的第二气相反应物可包括含金属的有机化合物。例如，第二气相反应物可包括选自具有式R-M-H(例如，R(X-n)-MX-Hn)的化合物的化合物，其中R为有机基团，M为金属，以与第一金属物种反应以从而形成含金属的材料。根据各种实例，X为M的形式氧化态，n可在1至5的范围内。作为特定的实例，M可以是或可包括Sn、In、Ga、Ge、As、Sb、Pb和Bi。或者，M可包括Al。例如，M可包括Sn、In或Ga。R可以是或可包括烷基基团或环戊二烯基、氨基、烷氧基、脒阴离子配体、胍阴离子配体、亚氨基、羧酸根配体、β-二酮阴离子配体、β-酮亚胺阴离子配体、丙二酸根配体、β-二酮亚胺阴离子配体基团，其具有或不具有另外的供体官能团。示例性的烷基基团可独立地选自C1-C5烷基基团。在一些情况下，第二气相反应物(例如，R-M-H化合物)可以是金属还原剂。图6示意了三丁基氢化锡(TBTH)的特定第二气相反应物实例。
如本文所述包含金属间化合物如Co3Sn2或Ni3Sn2、基本上由其组成或者由其组成的金属间膜可表现出具有超过500Oe的高矫顽力值的磁滞。这样的膜(以及根据方法200形成的膜)的电阻率值可在约10至约106μΩcm、20至104μΩcm、或50至1000μΩcm的范围内，例如80至180μΩcm，具体取决于膜厚度和/或化学计量。另外，根据方法100形成的Ni3Sn2薄膜表现出金属间晶体结构和高纯度。示例性的金属间化合物和膜可用于各种应用中，包括例如磁阻器件、超导器件、作为催化剂、作为能量(例如，氢)存储器等。
图2示意了根据本公开的至少一个实施例的另一循环沉积方法200。方法200可用于沉积含金属的材料以例如形成包含含金属的材料、基本上由含金属的材料组成或者由含金属的材料组成的膜或层。含金属的材料可包括任何上述金属间化合物以及本文所述的其他含金属的化合物。当膜(例如，经由方法100或200形成)基本上由金属间化合物组成或由金属间化合物组成时，膜可如本文所述表现出优异的性质。
方法200开始于步骤210，该步骤可与步骤110相同或相似。例如，反应腔室内的温度和压力可与步骤110中阐述的温度和压力相同或相似。
方法200可以步骤220继续，该步骤包括提供第一气相，如任何上文所述的第一气相反应物。此步骤可在与上文结合步骤210所述相同的压力和温度下。向反应腔室提供第一气相反应物的脉冲时间或时间可在约0.01秒至约60秒之间、或约0.05秒至约10秒之间、或约0.1秒至约5秒之间的范围内。在步骤220期间，第一气相反应物的流率可小于2000sccm、或小于1000sccm、或小于500sccm、或小于200sccm、或甚至小于100sccm，或可在约1至约5000sccm、约5至约2000sccm、或约10至约1000sccm的范围内。
在提供第一气相反应物的步骤220之后，可通过吹扫/泵工艺从反应腔室去除任何过量的第一气相反应物和任何反应副产物(步骤225)。在步骤225期间，吹扫气体的流率可小于2000sccm、或小于1000sccm、或小于500sccm、或小于200sccm、或甚至小于100sccm，或可在约1至约5000sccm、约5至约2000sccm、或约10至约1000sccm的范围内。尽管分开示意，但步骤125可视为步骤120的一部分。
方法200可以步骤230继续，该步骤包括提供第二气相反应物以与第一金属物种(例如，在基板表面上)反应以从而形成含金属的材料，其中所述第二气相反应物包含具有通式R-M-H的化合物，其中R为有机基团，M为金属。具有通式R-M-H的化合物可与上文所述相同。向反应腔室提供第二气相反应物的脉冲时间或时间可在约0.01秒至约60秒之间、或约0.05秒至约10秒之间、或约0.1秒至约5秒之间的范围内。在步骤230期间，第二气相反应物的流率可小于2000sccm、或小于1000sccm、或小于500sccm、或小于200sccm、或甚至小于100sccm，或可在约1至约5000sccm、约5至约2000sccm、或约10至约1000sccm的范围内。尽管分开示意，但步骤225可视为步骤220的一部分。
如图2中所示意，随着第二气相反应物与基板表面上的物种反应，将形成含金属的材料——例如，包含含金属的材料、基本上由含金属的材料组成或由含金属的材料组成的膜。
在步骤230之后，可通过吹扫/泵工艺从反应腔室去除任何过量的第二气相反应物和任何反应副产物(步骤245)。吹扫气体的流率可与上文在步骤225中所述的相同。此外，尽管分开示意，但步骤245可视为步骤230的一部分。
步骤220-245可根据需要以与上文结合图1描述的步骤120-145相同或相似的方式重复。例如，可重复所述步骤直至向基板上沉积了所需的膜厚度或所需量的含金属的材料。
在步骤220中使用的第一气相反应物可以是或可包括任何本文所述的第一气相反应物。如上所述，第一气相反应物和第二气相反应物可包括相同或不同的金属。例如，通过合并第一气相反应物如GeCl3(二噁烷)或一些其他Ge前体与R3GeH，可形成元素Ge膜。可类似地形成其他元素膜(或多金属膜)。
包含具有通式R-M-H的化合物的第二气相反应物可以是或可包括任何本文所述的R-M-H化合物，如上文结合方法100描述的那些，其中在R-M-H中，R为有机基团，M为金属。
根据本公开的一些实施例，方法100和/或方法200可包括原子层沉积(ALD)。ALD通常基于自限制反应，由此使用反应物的依序和交替脉冲来在每一个沉积循环沉积材料的约一个原子(或分子)单层。通常选择沉积条件和反应物以提供自饱和反应，使得一种反应物的吸附层留下不与相同反应物的气相反应物反应的表面终止状态(surfacetermination)。随后使基板与不同的反应物接触，所述不同的反应物与先前的终止状态反应而实现继续沉积。因此，交替脉冲的每个循环通常留下所需材料的不多于约一个单层。然而，如上文所提到，在一个或多个ALD循环中，可沉积材料的不止一个单层(例如如果发生了一些气相反应的话)而不管工艺的交替性如何。
在一些实施例中，使用循环沉积工艺来在基板上形成含金属的膜并且循环沉积工艺可以是ALD型工艺。在一些实施例中，循环沉积可以是混合式ALD/CVD或循环CVD工艺。举例来说，在一些实施例中，相比于CVD工艺，ALD工艺的生长速率可能低。提高生长速率的一个方法可以是相比于通常在ALD工艺中采用的温度在更高的基板温度下操作，从而导致化学气相沉积工艺，但仍利用反应物的依序引入。这样的工艺可被称作循环CVD。
本文所述的循环沉积工艺可在具有经加热基板的ALD或CVD沉积系统中进行。举例来说，在一些实施例中，方法可包括将基板加热到大约80℃与大约150℃之间的温度，或甚至将基板加热到大约80℃与大约120℃之间的温度。当然，对于任何给定循环沉积工艺(如对于ALD反应)的适宜温度窗口将取决于所涉及的表面终止状态和反应物物种。这里，温度随使用的反应物而异并通常处于或低于约700℃。在一些实施例中，对于气相沉积工艺，沉积温度通常处于或高于约100℃，在一些实施例中，沉积温度在约100℃至约300℃之间，并且在一些实施例中，沉积温度在约120℃至约200℃之间。在一些实施例中，沉积温度低于约500℃、或低于约400℃、或低于约350℃、或低于约300℃。在一些情况下，沉积温度可低于约300℃、低于约200℃或低于约100℃。在一些情况下，沉积温度可高于约20℃、高于约50℃、高于约75℃。在本公开的一些实施例中，沉积温度(即，沉积过程中基板的温度)与上文结合方法100和200所述的温度相同或相似。
如图1和2中所示意，包括ALD工艺在内的循环工艺可包括吹扫步骤，如上文描述的吹扫步骤125、145、225和245。在这样的步骤过程中使用的吹扫气体可包括一种或多种惰性气体，如氩气(Ar)或氮气(N2)，以防止或减轻反应物之间、工艺步骤之间的气相反应以及实现自饱和表面反应。然而，在一些实施例中，可另外或替代地移动基板(例如，至另一反应腔室)以分别接触第一气相反应物和第二气相反应物。因此，步骤120/130和/或步骤220/230不需要在同一反应腔室中进行。另外或替代地，可使用真空泵来辅助吹扫。
应理解，在本公开的一些实施例中，提供第一气相反应物和提供第二气相反应物的顺序可以是这样的：先使基板与第二气相反应物接触，然后与第一气相反应物接触。换句话说，步骤120、130和220、230可颠倒。另外，在一些实施例中，循环沉积工艺可包括使基板与第一气相反应物接触一次或多次，然后使基板与第二气相反应物接触一次或多次，并且类似地，作为替代方案，可包括使基板与第二气相反应物接触一次或多次，然后使基板与第一气相反应物接触一次或多次。
本公开的至少一些实施例(例如，方法100和/或方法200)可包括非等离子体反应物，例如，第一和第二气相反应物基本上不含离子化反应性物种。在一些实施例中，第一和第二气相反应物基本上不含离子化反应性物种、受激物种或自由基物种。例如，第一气相反应物和第二气相反应物都可包含非等离子体反应物以防止下面的基板的离子化损伤和由此产生的相关缺陷。当下面的基板含有易碎的制造或至少部分制造的半导体器件结构时，非等离子体反应物的使用可能尤其有用，因为高能等离子体物种可能损伤和/或降低器件性能特性。
虽然图2中未示意，但在本公开的一些实施例中，本公开的示例性方法可包括另外的工艺步骤，其包括使基板与包含还原剂的第三气相反应物接触。在一些实施例中，还原剂可包含以下中的至少之一：氢气(H2)、氢(H2)等离子体、氨气(NH3)、氨(NH3)等离子体、肼(N2H4)、硅烷(SiH4)、乙硅烷(Si2H6)、丙硅烷(Si3H8)、锗烷(GeH4)、乙锗烷(Ge2H6)、硼烷(BH3)、乙硼烷(B2H6)、叔丁基肼(C4H12N2)、硒反应物、硼反应物、磷反应物、硫反应物、有机反应物(例如，醇、醛或羧酸)或氢反应物。在本公开的一些实施例中，本公开的示例性循环沉积方法可包括使基板与为还原剂的第二气相反应物接触(无任何另外的前体/反应物接触步骤)。然而，如上所述，根据至少一些实例，不需要还原剂或还原反应来形成期望的材料如金属间材料。
如果使用，在一种示例性的循环沉积方法中，可向反应腔室中引入包含还原剂的第三气相反应物并在多个工艺阶段与基板接触。在本公开的一些实施例中，可向反应腔室中引入还原剂并与第一气相反应物分开和/或与第二气相反应物分开接触基板。例如，可在使基板与第一气相反应物接触之前、在使基板与第一气相反应物接触之后并在使基板与第二气相反应物接触之前、和/或在使基板与第二气相反应物接触之后向反应腔室中引入还原剂并与基板接触。在本公开的一些实施例中，可与第一气相反应物同时和/或与第二气相反应物同时向反应腔室中引入还原剂并与基板接触。例如，可使还原剂和第一气相反应物共同流动到反应腔室中并同时与基板接触，和/或可使还原剂和第二气相反应物共同流动到反应腔室中并同时与基板接触。
在一些实施例中，含金属的材料和/或金属间化合物的生长速率为约
/循环至约
/循环、约
/循环至约
/循环。在一些实施例中，含金属的材料和/或金属间化合物的生长速率大于约
/循环、大于约
/循环、大于约
/循环、大于约
/循环、大于约
/循环、或大于约
/循环。在一些实施例中，含金属的材料和/或金属间化合物的生长速率小于约
/循环、小于约
/循环、小于约
/循环、小于约
/循环、或小于约
/循环。在本公开的一些实施例中，含金属的材料和/或金属间化合物的生长速率可为大约
/循环。作为特定的实例，在Co3Sn2的情况下，在约170-200℃的沉积温度下，生长在约0.7至
/循环的范围内，而在Ni3Sn2的情况下，当使用NiCl2(TMPDA)作为第一气相反应物时，在160℃下观察到约
/循环的生长速率。
图3示意了包括基板302和层或膜304的结构300。结构300可以是或可包括部分制造的器件结构。如上所述，基板302可包括本体材料，如本体半导体材料，和形成在其上和/或其中的层。膜302可包括金属间化合物或含金属的材料，如根据本文描述的实施例沉积的金属间化合物或含金属的材料。在一些实施例中，膜304可在低于大约100纳米、或低于大约60纳米、或低于大约50纳米、或低于大约40纳米、或低于大约30纳米、或低于大约25纳米、或低于大约20纳米、或低于大约15纳米、或低于大约10纳米、或低于大约5纳米或更低的厚度下是连续的。本文提及的连续性可以是物理连续性或电连续性。在一些实施例中，使膜304可物理连续的厚度可能与使膜电连续的厚度不相同，并且使膜304可电连续的厚度可能与使膜物理连续的厚度不相同。
在一些实施例中，根据一些本文所述的实施例沉积的金属间和/或含金属的膜(例如，膜304)的厚度可为约20纳米至约100纳米。在一些实施例中，根据一些本文所述的实施例沉积的金属间和/或含金属的膜的厚度可为约20纳米至约60纳米。在一些实施例中，根据一些本文所述的实施例沉积的金属间和/或含金属的膜的厚度可大于约20纳米、或大于约30纳米、或大于约40纳米、或大于约50纳米、或大于约60纳米、或大于约100纳米、或大于约250纳米、或大于约500纳米。在一些实施例中，根据一些本文所述的实施例沉积的金属间和/或含金属的膜的厚度可小于约50纳米、小于约30纳米、小于约20纳米、小于约15纳米、小于约10纳米、小于约5纳米、小于约3纳米、小于约2纳米、或甚至小于约1纳米。
在本公开的一些实施例中，可在三维结构例如包含高纵横比特征的非平面基板上沉积金属间和/或含金属的膜。在一些实施例中，在纵横比(高/宽)大于约2、大于约5、大于约10、大于约25、大于约50或甚至大于约100的结构中，金属间和/或含金属的膜的台阶覆盖率可等于或高于约50％、或高于约80％、或高于约90％、或高于约95％、或高于约98％、或高于约99％或更高。
金属间化合物和/或含金属的材料或其对应的膜包含如本文所述的第一金属和第二金属。作为特定的实例，第一金属可包括Co、Ni、Pt或本文提到的任何其他第一金属，第二金属可包括Sn、In、Ga、Ge、As、Sb、Pb和Bi(例如，Sn、In或Fe)或本文提到的任何其他第二金属，包括Al。示例性的金属间和/或含金属的化合物包括(六方)Co3Sn2或Ni3Sn2。金属间和/或含金属的化合物还可具有其他化学计量或其他晶体结构，其可通过例如热处理或通过调节沉积条件来获得。其他示例性的金属间化合物和/或含金属的材料包含In-Sb、Pt-In、Pt-Sn、Pt-Ir、Pd-Pt、Ru-Pt、Ru、Co、Co-W、Ru-Mn、Cu-Mn和Co-Pt的化合物。金属间化合物和/或含金属的材料的其他特定实例包括Co、Ni、Cu和/或Pt以及Sn、In、Ga、Ge、As、Sb、Pb、Al和Bi中的一种或多种。在一些情况下，包含金属间化合物和/或含金属的材料的膜不包含Al、Ga和/或In和过渡金属。
在本公开的一些实施例中，金属间化合物和/或含金属的材料和/或包含其的膜，如本文所述，可包含低于约5原子％的氧、低于约2原子％的氧、低于约1原子％的氧或低于约0.5原子％的氧。在进一步的实施例中，所述化合物、材料或膜可包含低于约5原子％的氢、或低于约2原子％的氢、或低于约1原子％的氢、或甚至低于约0.5原子％的氢。在还进一步的实施例中，所述化合物、材料或膜可包含低于约5原子％的碳、或低于约2原子％的碳、或低于约1原子％的碳、或甚至低于约0.5原子％的碳。在还进一步的实施例中，所述化合物、材料和膜可包含低于约5原子％的卤化物物种、或低于约2原子％的卤化物物种、或低于约1原子％的卤化物物种、或甚至低于约0.5原子％的卤化物物种。在一些实施例中，可利用飞行弹性反冲检测分析(ToF-ERDA)的时间来确定金属间化合物、含金属的材料和包含其的膜的原子％组成。
能够用于沉积含金属的膜的反应器可用于形成本文所述的金属间化合物、含金属的材料和膜。这样的反应器包括ALD反应器以及配备有提供反应物的适宜设备和措施的CVD反应器。根据一些实施例，可使用热壁错流反应器。根据一些实施例，可使用其他错流、批量、小批量或空间ALD反应器。
可使用的合适反应器的实例包括可商购获得的单基板(或单晶片)沉积设备，如可得自美国亚利桑那州菲尼克斯的ASM America,Inc.和荷兰阿尔梅勒的ASM Europe B.V.的
反应器(如
2000和
3000及
XP ALD)以及
XP和
反应器。其他可商购获得的反应器包括以商品名
XP和XP8来自ASMJapan K.K.(日本东京)的反应器。在一些实施例中，反应器为空间ALD反应器，在所述反应器中，基板在加工期间移动或旋转。
在本公开的一些实施例中，可使用批量反应器。合适的批量反应器包括但不限于可自ASM Europe B.V.(荷兰阿尔梅勒)商购获得的商品名为A400和A412 PLUS的
400系列反应器。在一些实施例中，晶片在加工过程中旋转。在其他实施例中，批量反应器包括小批量反应器，其配置为容纳10个或更少基板(例如，半导体晶片)、8个或更少基板、6个或更少基板、4个或更少基板、或者2个或更少基板。在使用批量反应器的一些实施例中，晶片间的不均匀性小于3％(1西格玛)、小于2％、小于1％或甚至小于0.5％。
本文描述的沉积工艺可任选地在连接到丛集工具的反应器或反应腔室中进行。在丛集工具中，因为每一个反应腔室专门用于一种工艺类型，故每个模块中反应腔室的温度可保持恒定，与其中在每次运行前加热衬底直至工艺温度的反应器相比，这将提高生产量。另外，在丛集工具中可以缩短将反应腔室压力变至基板之间所需工艺压力水平的时间。在本公开的一些实施例中，可在包括多个反应腔室的丛集工具中进行沉积工艺，其中每个个别反应腔室可以用于将基板暴露于个别反应物气体，并且基板可在不同的反应腔室之间转移以暴露于多种反应物气体，基板的转移在受控的环境下进行以防止基板的氧化/污染。在本公开的一些实施例中，沉积工艺可在包括多个反应腔室的丛集工具中进行，其中每个单独的反应腔室都可配置为将衬底加热到不同的沉积温度。
独立反应器可配备负载锁。在此情况下，不必在每次运行之间冷却反应空间。
图5示意性地示出了根据本公开的至少一个实施例的反应器系统500。反应器系统500可用于例如进行如本文所述的循环沉积(例如，ALD)方法和/或形成如本文所述的结构、膜、化合物和/或材料。
在所示意的实例中，反应器系统500包括任选的基板处理系统502、反应腔室504、气体分配系统506，并任选地包括设置在反应腔室504与基板处理系统502之间的壁508。系统500还可包括第一气相反应物源512、第二气相反应物源514和排气源510。尽管示意为具有两个气体源512、514，但反应器系统500可包括任何合适数量的反应物气体源。作为实例，示例性的反应器系统可包括至少两个反应物气体源(例如，包括将成为第一或第二气相反应物的化合物的源)和任选地一个或多个载气和/或吹扫气体源516。反应器系统500还包括在处理期间容留一个或多个基板520的承托器518。
反应器系统500可包括任何合适数量的反应腔室104和基板处理系统502。作为实例，反应器系统500的反应腔室504包括错流热壁外延反应腔室。示例性的反应器系统包括可作为系统得自ASM的水平流动反应器。
应指出，图5为反应器系统500的简化示意版本而不含反应器系统500中可能利用的每一个元件，如但不限于阀、电连接、质量流量控制器、密封件和气体导管。
在本公开的一些实施例中，一个或多个反应物源容器522、524经由导管或其他适宜的措施526、528与反应腔室504流体连通并可进一步联接到设置在反应物源容器522、524与反应腔室504之间的气体分配系统506。气体分配系统506可包括例如歧管、阀控制系统、质量流量控制系统和/或其他机构以控制气态反应物源自于的反应物源容器522或524。反应物源容器522、524可配置为用于贮存含金属的化合物(例如,有机金属或金属有机化合物)，所述化合物分别为第一气相反应物和第二气相反应物或者在加热时分别成为第一气相反应物和第二气相反应物。在一些实施例中，反应物源容器522、524可包含石英材料，其可对贮存于源容器522、524内的相应第一反应物和第二反应物基本上化学惰性。在本公开的替代实施例中，反应物源容器522、524可由耐腐蚀金属或金属合金如例如哈氏合金(Hastelloy)、蒙乃尔合金(Monel)或其组合制成。
在本发明的一些实施例中，反应物源容器522、524可还包括一个或多个加热单元526、528，其配置为将贮存在反应物源容器522、524中的化合物加热到所需的温度。在一些实施例中，可利用所述一个或多个加热单元来将化合物加热到大约高于0℃、或大约高于20℃、或大约高于100℃、或大约高于150℃、或大约高于200℃、或大约高于200℃、或大约高于300℃、或甚至大约高于400℃的温度。在一些实施例中，所述一个或多个加热单元526、528可配置为将贮存在反应物源容器522、524中的化合物加热到大致约25℃至约200℃、约25℃至约300℃、或约25℃至约400℃的温度。作为特定的实例，当气相反应物包括Bu3SnH时，温度可在约20℃至约40℃的范围内，或为约30℃；当反应物包括CoCl2(TMEDA)时，温度可在约150℃至约190℃的范围内，或为约170℃；当反应物包括NiCl2(TMPDA)时，温度可在约140℃至约180℃的范围内，或为约157℃；而当反应物包括Ni(dmap)2时，温度可在约50℃至约70℃的范围内，或为约62℃。
在一些实施例中，与反应物源容器522、524相关联的一个或多个加热单元526、528配置为用于将化合物从固体转化成液体或气体以形成第一气相反应物或第二气相反应物。在一些实施例中，可利用分别与反应物源容器522、524相关联的一个或多个加热单元526、528来控制贮存在反应物源容器522、524中的反应物化合物的粘度。在一些实施例中，与相应的反应物源容器522、524相关联的一个或多个加热单元526、528可配置为用于控制由贮存在反应物源容器522、524内的化合物生成的蒸气压。在本公开的一些实施例中，化合物可在高于25℃、或高于50℃、或甚至高于100℃的温度下具有高于0.01毫巴的蒸气压。在本公开的一些实施例中，化合物可在低于350℃、或低于250℃、或低于200℃、或甚至低于150℃的温度下具有高于0.01毫巴的蒸气压。在本公开的一些实施例中，化合物可在高于25℃、或甚至高于100℃的温度下具有高于0.1毫巴的蒸气压。在本公开的一些实施例中，化合物可在低于400℃、或低于200℃、或甚至低于100℃的温度下具有高于0.1毫巴的蒸气压。在本公开的一些实施例中，化合物可在高于25℃、或甚至高于100℃的温度下具有高于1毫巴的蒸气压。例如，可将化合物加热到高于150℃的温度，从而生成高于0.001毫巴的蒸气压。
在本公开的一些实施例中，蒸气通路530可连接到反应物源容器522(和/或反应物源容器524)使得一种或多种载气(例如，来自源516或另一源)可经由蒸气通路530从载气贮存容器输送到反应物源容器522中。在一些实施例中，可将质量流量控制器(未示出)布置在蒸气通路530上并靠近反应物源容器522设置。例如，可校准质量流量控制器以控制进入反应物源容器522的载气的质量通量，从而允许更好地控制反应物蒸气从反应物源容器522流出并进入反应腔室504的后续流动。
在一些实施例中，载气(例如，氢气、氮气、氦气、氩气或其任何混合物)可在化合物的暴露表面上方流动，从而从化合物拾取一部分蒸气并与载气一道将化合物(现在为第一或第二气相反应物)输送到反应腔室504。在本公开的替代实施例中，载气可例如通过任选的蒸气通路(未示意)对化合物“鼓泡”，从而搅拌和拾取一部分含金属的化合物，并经由气体导管526将含金属的化合物蒸气(现在为第一或第二气相反应物)输送到反应腔室504。
在本公开的一些实施例中，反应器系统500还可包括系统操作和控制机构532，其提供电子电路和机械部件以选择性地操作阀、歧管、泵以及与反应器系统500相关联的其他设备。这样的电路和化合物用以从相应的反应物源容器522、524和吹扫气体容器534引入反应物、吹扫气体和/或载气。系统操作和控制机构532还可控制气体脉冲序列的时序、基板和/或反应腔室的温度、反应腔室的压力以及提供反应器系统500的适当操作所必需的各种其他操作。操作和控制机构532可包括控制软件和电控制或气动控制的阀以控制反应物、载气和/或吹扫气体进出反应腔室504的流动。系统操作和控制机构532可包括执行某些任务的模块，如软件和/或硬件部件，例如FPGA或ASIC。模块可不利地配置为位于系统操作和控制机构532的可寻址存储介质上并配置为执行一个或多个工艺。
反应器系统的各种其他配置是可能的，包括不同数目和种类的反应物源和吹扫气体源。此外，存在阀、导管、反应物源、吹扫气体源的许多布置，其可用来实现向反应腔室504中选择性地进给气体的目标。
实例
下文提供的实例示意了根据本公开的示例性实施例的特定工艺、膜和结构。这些实例是示意性的而不意图限制本公开的范围。
1.一种用于沉积金属间化合物的循环沉积工艺，所述循环沉积方法包括以下步骤：
向反应腔室提供包含第一金属的第一气相反应物以与基板的表面反应以形成第一金属物种；以及
向所述反应腔室提供包含第二金属的第二气相反应物以与所述第一金属物种反应以从而形成所述金属间化合物。
2.实例1的循环沉积工艺，其还包括重复提供所述第一气相反应物和提供所述第二气相反应物的步骤直至达到所需的膜厚度。
3.实例1的循环沉积工艺，其还包括一个或多个吹扫步骤，其中所述吹扫步骤中的至少一个在提供所述第一气相反应物的步骤之后并在提供所述第二气相反应物的步骤之前进行。
4.实例1的循环沉积工艺，其中所述循环沉积工艺包括原子层沉积。
5.实例1的循环沉积工艺，其中所述循环沉积工艺包括循环化学气相沉积。
6.实例1的循环沉积工艺，其中在提供所述第一气相反应物和提供所述第二气相反应物的步骤期间反应腔室内的温度高于0℃并低于600℃、低于500℃、低于400℃、低于300℃或低于250℃，或在约20℃至约700℃、约50℃至约500℃、或约50℃至约400℃、约75℃至约300℃、或约100℃至约250℃之间。
7.实例1的循环沉积工艺，其中所述第二气相反应物包含含金属的有机化合物。
8.实例1的循环沉积工艺，其中所述第二气相反应物选自具有式R-M-H的化合物，其中R为有机基团并且M为金属。
9.实例1的循环沉积工艺，其中所述第二金属选自Sn、In、Al、Ga、Ge、As、Sb、Pb和Bi。
10.实例1的循环沉积工艺，其中所述第二金属选自Sn、Ge、As、Sb、Pb和Bi。
11.实例1的循环沉积工艺，其中所述第二金属包含Sn。
12.实例1的循环沉积工艺，其中所述第二金属包含In。
13.实例1的循环沉积工艺，其中所述第二金属包含Ga。
14.实例8的循环沉积工艺，其中具有式R-M-H的化合物具有式R(X-n)-MX-Hn，其中X为金属的形式氧化态并且n为1至5。
15.实例8和14中任一项的循环沉积工艺，其中R包含烷基基团或其他有机基团。
16.实例8和14中任一项的循环沉积工艺，其中R独立地选自C1-C5烷基基团。
17.实例8和14中任一项的循环沉积工艺，其中R为环戊二烯基、氨基、烷氧基、脒阴离子配体、胍阴离子配体、亚氨基、羧酸根配体、β-二酮阴离子配体、β-酮亚胺阴离子配体、丙二酸根配体、β-二酮亚胺阴离子配体基团，其具有或不具有另外的供体官能团。
18.实例1的循环沉积工艺，其中所述第二气相反应物包含金属还原剂。
19.实例1的循环沉积工艺，其中所述第一金属选自过渡金属。
20.实例1的循环沉积工艺，其中所述第一金属选自3-6族金属。
21.实例1的循环沉积工艺，其中所述第一金属选自7-12族金属。
22.实例1的循环沉积工艺，其中所述第一金属选自镧系元素。
23.实例1的循环沉积工艺，其中所述第一金属选自8-11族金属。
24.实例1的循环沉积工艺，其中所述第一金属选自9-10族金属。
25.实例1的循环沉积工艺，其中所述第一气相反应物选自金属卤化物。
26.实例1的循环沉积工艺，其中所述第一气相反应物包含M(dmap)x(dmap＝二甲基氨基-2-丙醇盐)，其中M为金属。
27.实例1的循环沉积工艺，其中所述第一气相反应物选自金属氢化物和铝试剂。
28.实例1的循环沉积工艺，其中所述第一气相反应物包含相应的金属氯化物的二胺加合物。
29.实例1的循环沉积工艺，其中所述第一气相反应物包含金属卤化物化合物，所述金属卤化物化合物包含二齿含氮加合物配体。
30.实例29的循环沉积工艺，其中所述加合物配体包含两个氮原子，并且其中每个氮原子与至少一个碳原子键合。
31.实例1的循环沉积工艺，其中所述第一气相反应物包含氯化钴(TMEDA)和氯化镍(TMPDA)中的至少一种。
32.实例1的循环沉积工艺，其中所述第二气相反应物包含TBTH。
33.实例1的循环沉积工艺，其中所述金属间化合物不包含Al、Ga和/或In以及过渡金属。
34.一种用于形成含金属的材料的循环沉积工艺，所述循环沉积工艺包括：
向反应腔室提供包含第一金属的第一气相前体以形成第一金属物种；以及
提供第二气相反应物以与第一金属物种反应以从而形成含金属的材料，其中所述第二气相反应物包含具有通式R-M-H的化合物，其中R为有机基团并且M为金属。
35.实例34的循环沉积工艺，其中所述第一金属和所述第二金属是相同的。
36.实例34的循环沉积工艺，其中所述含金属的材料包含元素金属。
37.实例1或34的循环沉积工艺，其中所述含金属的材料包括例如In和Ge或其他第一金属和/或第二金属的混合物。
38.实例34的循环沉积工艺，其还包括重复提供所述第一气相反应物和提供所述第二气相反应物的步骤直至达到所需的膜厚度。
39.实例34的循环沉积工艺，其还包括一个或多个吹扫步骤，其中所述吹扫步骤中的至少一个在提供所述第一气相反应物的步骤之后并在提供所述第二气相反应物的步骤之前进行。
40.实例34的循环沉积工艺，其中所述循环沉积工艺包括原子层沉积。
41.实例34的循环沉积工艺，其中所述循环沉积工艺包括循环化学气相沉积。
42.实例34的循环沉积工艺，其中在提供所述第一气相反应物和提供所述第二气相反应物的步骤期间反应腔室内的温度高于0℃并低于600℃、低于500℃、低于400℃、低于300℃或低于250℃，或在约20℃至约700℃、约50℃至约500℃、或约50℃至约400℃、约75℃至约300℃、或约100℃至约250℃之间。
43.实例34的循环沉积工艺，其中所述第一金属选自Sn、In、Ga、Al、Ge、As、Sb、Pb和Bi。
44.实例34的循环沉积工艺，其中所述第二金属选自Sn、Ge、As、Sb、Pb和Bi。
45.实例34的循环沉积工艺，其中所述第二金属包含Sn。
46.实例34的循环沉积工艺，其中所述第二金属包含In。
47.实例34的循环沉积工艺，其中所述第二金属包含Ga。
48.实例34的循环沉积工艺，其中所述含金属的材料包含金属混合物、合金和金属间化合物中的一种或多种。
49.实例34的循环沉积工艺，其中所述含金属的材料是金属、导电、非导电、半导电、超导电、催化、铁磁和磁阻材料中的一种或多种。
50.实例34的循环沉积工艺，其中具有通式R-M-H的化合物具有式R(X-n)-MX-Hn，其中X为金属的形式氧化态并且n为1至5。
51.实例34的循环沉积工艺，其中R包含烷基基团或其他有机基团。
52.实例34的循环沉积工艺，其中R独立地选自C1-C5烷基基团。
53.实例34-52中任一项的循环沉积工艺，其中R为环戊二烯基、氨基、烷氧基、脒阴离子配体、胍阴离子配体、亚氨基、羧酸根配体、β-二酮阴离子配体、β-酮亚胺阴离子配体、丙二酸根配体、β-二酮亚胺阴离子配体基团，其具有或不具有另外的供体官能团。
54.实例34的循环沉积工艺，其中所述第二气相反应物包含金属还原剂。
55.实例34的循环沉积工艺，其中所述第一金属选自过渡金属。
56.实例34的循环沉积工艺，其中所述第一金属选自3-6族金属。
57.实例34的循环沉积工艺，其中所述第一金属选自7-12族金属。
58.实例34的循环沉积工艺，其中所述第一金属选自镧系元素。
59.实例34的循环沉积工艺，其中所述第一金属选自8-11族金属。
60.实例34的循环沉积工艺，其中所述第一金属选自9-10族金属。
61.实例34的循环沉积工艺，其中所述第一气相反应物选自金属卤化物。
62.实例34的循环沉积工艺，其中所述第一气相反应物包含M(dmap)x(dmap＝二甲基氨基-2-丙醇盐)，其中M为金属。
63.实例34的循环沉积工艺，其中所述第一气相反应物选自金属氢化物和铝试剂。
64.实例34的循环沉积工艺，其中所述第一气相反应物包含相应的金属氯化物的二胺加合物。
65.实例34的循环沉积工艺，其中所述第一气相反应物包含金属卤化物化合物，所述金属卤化物化合物包含二齿含氮加合物配体。
66.实例65的循环沉积工艺，其中所述加合物配体包含两个氮原子，并且其中每个氮原子与至少一个碳原子键合。
67.实例34的循环沉积工艺，其中所述第一气相反应物包含氯化钴(TMEDA)和氯化镍(TMPDA)中的至少一种。
68.实例34的循环沉积工艺，其中所述第二气相反应物包含TBTH。
69.一种根据实例1-33中任一项的工艺形成的膜。
70.实例69的膜，其中所述膜是金属、导电、半导电或非导电的。
71.实例69的膜，其中所述膜是超导电的。
72.实例69的膜，其中所述膜是磁阻的。
73.实例69的膜，其中所述膜是铁磁的。
74.实例69的膜，其中所述膜为催化剂。
75.一种根据实例34-68中任一项的工艺形成的膜。
76.实例75的膜，其中所述膜包含金属混合物、合金和金属间化合物中的一种或多种。
77.一种包括根据实例69和76中一项或多项的膜的器件结构。
上文描述的本公开的实例实施例不限制本发明的范围，因为这些实施例仅是本发明的实施例的实例，本发明由附随的权利要求书及其法律等同物限定。任何等同的实施例均意在包括在本发明的范围内。实际上，除本文示出和描述的那些外，本公开的各种修改，如所述要素的替代的可用组合，本领域技术人员可从说明书显而易见。这样的修改和实施例也意在落在附随的权利要求书的范围内。
Claims (20)
1.一种用于沉积金属间化合物的循环沉积工艺，所述循环沉积方法包括以下步骤：
向反应腔室提供包含第一金属的第一气相反应物以与基板的表面反应以形成第一金属物种；以及
向所述反应腔室提供包含第二金属的第二气相反应物以与所述第一金属物种反应以从而形成所述金属间化合物。
2.根据权利要求1所述的循环沉积工艺，其中所述第二气相反应物包含含金属的有机化合物。
3.根据权利要求1所述的循环沉积工艺，其中所述第二气相反应物选自具有式R-M-H的化合物，其中R为有机基团并且M为金属。
4.根据权利要求1所述的循环沉积工艺，其中所述第二金属选自Sn、In、Al、Ga、Ge、As、Sb、Pb和Bi。
5.根据权利要求3所述的循环沉积工艺，其中具有式R-M-H的化合物具有式R(X-n)-MX-Hn，其中X为金属的形式氧化态并且n为1至5。
6.根据权利要求3和5中任一项所述的循环沉积工艺，其中R独立地选自C1-C5烷基基团。
7.根据权利要求3和5中任一项所述的循环沉积工艺，其中R为环戊二烯基、氨基、烷氧基、脒阴离子配体、胍阴离子配体、亚氨基、羧酸根配体、β-二酮阴离子配体、β-酮亚胺阴离子配体、丙二酸根配体、β-二酮亚胺阴离子配体基团，其具有或不具有另外的供体官能团。
8.根据权利要求1所述的循环沉积工艺，其中所述第二气相反应物包含金属还原剂。
9.根据权利要求1所述的循环沉积工艺，其中所述第一气相反应物包含相应的金属氯化物的二胺加合物。
10.根据权利要求1所述的循环沉积工艺，其中所述第一气相反应物包含金属卤化物化合物，所述金属卤化物化合物包含二齿含氮加合物配体。
11.根据权利要求1所述的循环沉积工艺，其中所述第一气相反应物包含氯化钴(TMEDA)和氯化镍(TMPDA)中的至少一种。
12.根据权利要求1所述的循环沉积工艺，其中所述第二气相反应物包含TBTH。
13.一种用于形成含金属的材料的循环沉积工艺，所述循环沉积工艺包括：
向反应腔室提供包含第一金属的第一气相前体以形成第一金属物种；以及
提供第二气相反应物以与所述第一金属物种反应以从而形成所述含金属的材料，其中所述第二气相反应物包含具有通式R-M-H的化合物，其中R为有机基团并且M为金属，
其中所述反应腔室内的温度高于0℃并且低于600℃。
14.根据权利要求13所述的循环沉积工艺，其中所述含金属的材料包含元素金属。
15.根据权利要求13所述的循环沉积工艺，其中所述第一金属选自Sn、In、Ga、Al、Ge、As、Sb、Pb和Bi。
16.根据权利要求13所述的循环沉积工艺，其中具有通式R-M-H的化合物具有式R(X-n)-MX-Hn，其中X为金属的形式氧化态并且n为1至5。
17.根据权利要求13所述的循环沉积工艺，其中所述第一气相反应物包含相应的金属氯化物的二胺加合物。
18.根据权利要求13所述的循环沉积工艺，其中所述第一气相反应物包含氯化钴(TMEDA)和氯化镍(TMPDA)中的至少一种。
19.根据权利要求13所述的循环沉积工艺，其中所述第二气相反应物包含TBTH。
20.一种器件结构，所述器件结构包括根据权利要求1-19中一项或多项所述的膜。
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| TWI815915B (zh) | 2023-09-21 |
| KR20210027265A (ko) | 2021-03-10 |
| JP2021529880A (ja) | 2021-11-04 |
| WO2020003000A1 (en) | 2020-01-02 |
| US11952658B2 (en) | 2024-04-09 |
| US20210269914A1 (en) | 2021-09-02 |
| US20230067660A1 (en) | 2023-03-02 |
| US11499222B2 (en) | 2022-11-15 |
| TW202000966A (zh) | 2020-01-01 |
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