TW202409324A - 用於形成含金屬材料之循環沉積製程 - Google Patents
用於形成含金屬材料之循環沉積製程 Download PDFInfo
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- TW202409324A TW202409324A TW112143596A TW112143596A TW202409324A TW 202409324 A TW202409324 A TW 202409324A TW 112143596 A TW112143596 A TW 112143596A TW 112143596 A TW112143596 A TW 112143596A TW 202409324 A TW202409324 A TW 202409324A
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- metal
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- cyclic deposition
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 278
- 239000002184 metal Substances 0.000 title claims abstract description 277
- 125000004122 cyclic group Chemical group 0.000 title claims abstract description 132
- 239000000463 material Substances 0.000 title claims abstract description 107
- 238000005137 deposition process Methods 0.000 title claims description 112
- 239000000376 reactant Substances 0.000 claims description 225
- 239000007789 gas Substances 0.000 claims description 172
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- 238000006243 chemical reaction Methods 0.000 claims description 80
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- -1 metal halide compound Chemical class 0.000 claims description 50
- 239000002243 precursor Substances 0.000 claims description 49
- 229910052757 nitrogen Inorganic materials 0.000 claims description 32
- 229910052759 nickel Inorganic materials 0.000 claims description 31
- 239000010949 copper Substances 0.000 claims description 30
- 150000002739 metals Chemical class 0.000 claims description 25
- 150000003624 transition metals Chemical class 0.000 claims description 24
- 229910052723 transition metal Inorganic materials 0.000 claims description 22
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- 125000004433 nitrogen atom Chemical group N* 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 17
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- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims description 16
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- 125000004665 trialkylsilyl group Chemical group 0.000 description 2
- RXJKFRMDXUJTEX-UHFFFAOYSA-N triethylphosphine Chemical compound CCP(CC)CC RXJKFRMDXUJTEX-UHFFFAOYSA-N 0.000 description 2
- 125000006527 (C1-C5) alkyl group Chemical group 0.000 description 1
- 125000004169 (C1-C6) alkyl group Chemical group 0.000 description 1
- 125000006701 (C1-C7) alkyl group Chemical group 0.000 description 1
- 125000004209 (C1-C8) alkyl group Chemical group 0.000 description 1
- NAHLQCFWWVZWDY-UHFFFAOYSA-N 1,4-dioxane;ethane-1,2-diol Chemical compound OCCO.C1COCCO1 NAHLQCFWWVZWDY-UHFFFAOYSA-N 0.000 description 1
- NCXUNZWLEYGQAH-UHFFFAOYSA-N 1-(dimethylamino)propan-2-ol Chemical compound CC(O)CN(C)C NCXUNZWLEYGQAH-UHFFFAOYSA-N 0.000 description 1
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- LBQSNYLQPZOXLY-UHFFFAOYSA-N CC(C)NC(C)=NC(C)C.CC(C)NC(C)=NC(C)C.[Co+2] Chemical compound CC(C)NC(C)=NC(C)C.CC(C)NC(C)=NC(C)C.[Co+2] LBQSNYLQPZOXLY-UHFFFAOYSA-N 0.000 description 1
- 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 1
- 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
- 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 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
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910000531 Co alloy Inorganic materials 0.000 description 1
- 229910020646 Co-Sn Inorganic materials 0.000 description 1
- 229910021297 Co3Sn2 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
- 239000012691 Cu precursor Substances 0.000 description 1
- 229910017566 Cu-Mn Inorganic materials 0.000 description 1
- 229910017871 Cu—Mn Inorganic materials 0.000 description 1
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 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
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910000792 Monel Inorganic materials 0.000 description 1
- 101100386623 Mus musculus Amd2 gene Proteins 0.000 description 1
- 229910005099 Ni3Sn2 Inorganic materials 0.000 description 1
- 241000233805 Phoenix Species 0.000 description 1
- 229910002835 Pt–Ir Inorganic materials 0.000 description 1
- 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
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 229910001128 Sn alloy Inorganic materials 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- OGUKRJFREVKPRL-UHFFFAOYSA-N [Ag].C(C)(C)NC(C)=NC(C)C Chemical compound [Ag].C(C)(C)NC(C)=NC(C)C OGUKRJFREVKPRL-UHFFFAOYSA-N 0.000 description 1
- 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
- MKDSBEPLGGHMLO-UHFFFAOYSA-N [Cu+].C(C)(C)NC(C)=NC(C)C Chemical compound [Cu+].C(C)(C)NC(C)=NC(C)C MKDSBEPLGGHMLO-UHFFFAOYSA-N 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
- JAZCEXBNIYKZDI-UHFFFAOYSA-N [Ir+] Chemical compound [Ir+] JAZCEXBNIYKZDI-UHFFFAOYSA-N 0.000 description 1
- HBGWCTDZGWFEJZ-UHFFFAOYSA-N [Li].C(C)(CC)NC(C)=NC(C)CC Chemical compound [Li].C(C)(CC)NC(C)=NC(C)CC HBGWCTDZGWFEJZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 125000005103 alkyl silyl group Chemical group 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000001409 amidines Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 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
- RGTXVXDNHPWPHH-UHFFFAOYSA-N butane-1,3-diamine Chemical compound CC(N)CCN RGTXVXDNHPWPHH-UHFFFAOYSA-N 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- XKLVLDXNZDIDKQ-UHFFFAOYSA-N butylhydrazine Chemical group CCCCNN XKLVLDXNZDIDKQ-UHFFFAOYSA-N 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004871 chemical beam epitaxy Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 229960003280 cupric chloride Drugs 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 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
- ZOCHARZZJNPSEU-UHFFFAOYSA-N diboron Chemical compound B#B ZOCHARZZJNPSEU-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
- 230000000694 effects Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000003302 ferromagnetic material Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 238000000171 gas-source molecular beam epitaxy Methods 0.000 description 1
- 229910000078 germane Inorganic materials 0.000 description 1
- SCCCLDWUZODEKG-UHFFFAOYSA-N germanide Chemical compound [GeH3-] SCCCLDWUZODEKG-UHFFFAOYSA-N 0.000 description 1
- 150000002291 germanium compounds Chemical class 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- ZBKIUFWVEIBQRT-UHFFFAOYSA-N gold(1+) Chemical compound [Au+] ZBKIUFWVEIBQRT-UHFFFAOYSA-N 0.000 description 1
- 125000002795 guanidino group Chemical group C(N)(=N)N* 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 229910000856 hastalloy Inorganic materials 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 150000002466 imines Chemical group 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 150000004658 ketimines Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 230000005291 magnetic effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 229910001509 metal bromide Inorganic materials 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 229910001512 metal fluoride Inorganic materials 0.000 description 1
- 229910001511 metal iodide Inorganic materials 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 238000001208 nuclear magnetic resonance pulse sequence Methods 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- HMWORNISPHRSQN-UHFFFAOYSA-N oxomethylidenecopper Chemical class O=C=[Cu] HMWORNISPHRSQN-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 229940002612 prodrug Drugs 0.000 description 1
- 239000000651 prodrug Substances 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 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
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 229910021558 transition metal bromide Inorganic materials 0.000 description 1
- 229910021381 transition metal chloride Inorganic materials 0.000 description 1
- 229910021561 transition metal fluoride Inorganic materials 0.000 description 1
- 229910021573 transition metal iodide Inorganic materials 0.000 description 1
- KTSWILXIWHVQLR-UHFFFAOYSA-N tributylgermane Chemical compound CCCC[GeH](CCCC)CCCC KTSWILXIWHVQLR-UHFFFAOYSA-N 0.000 description 1
- 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
- 238000005019 vapor deposition process Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-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
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
- C23C16/44—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
-
- 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
- C23C16/08—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 from metal halides
-
- 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
- C23C16/18—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 from metallo-organic compounds
-
- 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]
- C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
- G11B5/85—Coating a support with a magnetic layer by vapour deposition
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N50/00—Galvanomagnetic devices
- H10N50/80—Constructional details
- H10N50/85—Magnetic active materials
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N60/00—Superconducting devices
- H10N60/80—Constructional details
- H10N60/85—Superconducting active materials
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
- Physical Vapour Deposition (AREA)
- Electrodes Of Semiconductors (AREA)
Abstract
揭露一種沉積含金屬材料的方法。方法可包含循環沉積技術的使用，諸如化學氣相沉積及原子層沉積。含金屬材料可包含金屬間化合物。亦揭露包含含金屬材料的結構以及用於形成該材料的系統。
Description
本發明主要關於用於在基板表面上沉積含金屬材料之方法、關於包含該含金屬材料的膜及結構及關於用於沉積該含金屬材料的反應器及系統。
聯合研究協定之各方
本文所主張之發明係由、或代表及/或關於赫爾辛基大學(University of Helsinki)與ASM微量化學公司(ASM Microchemistry Oy)之間的聯合研究協定而作出。該協定在所主張之本發明作成之日及之前生效，且所主張之本發明係由於在該協定範疇內所進行之活動而作成。
含金屬材料的沉積可用於各種裝置的製造，諸如半導體裝置、平板顯示裝置、光伏裝置、微機電系統（MEMS）、磁阻裝置、超導裝置、能量（例如氫）儲存裝置、鋰或鈉離子電池等和/或形成催化材料。針對許多應用，經常需要在一表面上以均勻及/或保角的方式沉積含金屬材料，該表面可包括三維特徵，諸如溝渠及/或突起，其可有相對高的高寬比。
近年來，由於其相對獨特的物理及化學性質，人們對於可能使用包括兩或更多金屬的金屬材料，諸如金屬間化合物、鍺化物（例如，鍺化鎳(Ni
xGe
y)或(Co
xGe
y)）等來形成各種裝置的興趣日益增長。金屬間化合物通常具有特定有序的晶體結構，其可能與以相同材料所形成的合金不同；特定結構可能造成比非金屬間化合物更優異的材料性質。這種性質包含，例如，磁阻、超導性、催化活性及儲氫能力。舉例而言，已有研究將含有具有不同化學計量之Co或Ni及Sn之金屬間化合物作為Li及Na離子電池的陽極材料、作為磁性裝置的鐵磁材料及作為催化用。
通常藉由球磨、電弧熔化、不同的溶液為基之技術、溶劑和水熱路線、電沉積、濺射及電子束蒸發來製備含金屬材料，諸如具有不同的化學計量之Co-Sn及Ni-Sn，包含材料之金屬間Co
3Sn
2及Ni
3Sn
2相。已有採用源自兩個單源反應物（Me
3SnCo(CO)
4及Ph
3SnCo(CO)
4）之化學氣相沉積（CVD）來沉積具有1:1化學計量和僅有次要組分的Co
3Sn
2之Co及Sn合金。也已有藉由CVD使用SnMe
4及Ni基板來沉積Ni
3Sn、Ni
3Sn
2及Ni
3Sn
4，接著進行在高溫下的氫處理。雖然這種技術可用來形成金屬間化合物，這種技術一般不適合在基板上形成金屬間材料之均勻且保角的膜。
近年來，將金屬鍺化物和其他金屬-IIIA族及金屬-IVA族材料（IUPAC金屬-第13族及金屬-第14族材料）作為裝置形成中尤其是低電阻接點之應用已備受關注。通常藉由在鍺基板或層上退火經物理氣相沉積（PVD）之金屬（如鎳）來製備金屬-IIIA族(IUPAC金屬-第13族)及金屬-IVA族材料（IUPAC金屬-第14族)材料，諸如金屬(如鎳)鍺化物。雖然這種技術可用來形成金屬-IIIA族(IUPAC金屬-第13族)及金屬-IVA族(IUPAC金屬-第14族)材料，這種技術一般不適合用來形成金屬-IIIA族及金屬-IVA族材料（IUPAC第13及14族）之均勻且保角的膜及/或在相對低溫下形成這種材料。
可使用循環沉積技術，諸如原子層沉積，來以受控且可重複的方式在基板表面上之複雜的三維結構上方以相對均勻（例如均勻晶體結構、均勻成分及/或均勻厚度）且保角的方式沉積材料。然而，這種技術一般尚未用來沉積若干含金屬的材料，包含金屬間化合物及/或金屬-IIIA族(IUPAC金屬-第13族)及/或金屬-IVA族(IUPAC金屬-第14族)材料。更確切地來說，通常使用其他技術及/或需要額外經常高溫的製程來形成特別是這種化合物及材料。某些含金屬薄膜的直接沉積，諸如包括金屬間或鍺化物或其他僅僅金屬/半金屬的膜迄今為止仍充滿挑戰。
依此，需要能用於形成含金屬材料（諸如金屬-IIIA族(IUPAC金屬-第13族)及金屬-IVA族材料（IUPAC金屬-第14族)材料）金屬間化合物及之改進方法。此外，需要用於形成含金屬材料之均勻及/或保角膜的改進技術。
此章節中所提供之問題的任何論述僅為了提供本發明的背景而包括於本發明中，且不應視為承認在完成本發明時已知任何或所有的論述。
本發明內容以簡化形式來介紹一系列之概念。這些概念會在下面本發明的示例實施例之詳細敘述中做進一步詳述。本發明內容沒有意欲要確認所主張之標的的關鍵特徵或必要特徵，亦沒有意欲用來限制所主張之標的的範圍。
根據本發明的至少一個實施例，揭露一種用於沉積金屬間化合物的方法。根據各種態樣，該方法為循環沉積製程，其包含提供包括一第一金屬的第一氣相反應物（在此亦稱為前驅物）至反應室以與基板的表面反應而形成第一金屬物種；以及提供包括第二金屬的的第二氣相反應物至反應室以與第一金屬物種反應，藉此形成金屬間化合物。可同樣地使用額外的反應物來形成包含超過兩種金屬的金屬間化合物。如下更詳細提出，可在基板表面上形成金屬間化合物的膜而無須高溫及/或還原步驟。循環沉積製程可包含，例如，原子層沉積。
根據本發明的至少一個其他實施例，揭露一種用於形成含金屬材料的方法。含金屬材料可包含一種、兩種或三種或更多金屬，如本文中所述。該方法可為循環式沉積製程，諸如原子層沉積製程或循環化學氣相沉積製程。循環沉積製程可包含提供包括第一金屬的第一氣相反應物至反應室以形成第一金屬物種，以及提供第二氣相反應物；第一及/或第二反應物可包括具有R-M-H（例如R
(X-n)-M
X-H
n)之通式的化合物，其中R為有機基而M為金屬，以與第一金屬物種反應而形成含金屬材料。根據各種範例，X為M的正式氧化態而n的範圍可以是從1到5。根據各種態樣，含金屬材料包括元素金屬、金屬混合物、合金及金屬間化合物的一或多者。包括含金屬材料的膜可為金屬型、導電型、非導電型或半導電型。示範膜可為超導型、磁阻型、鐵磁型或催化劑。
根據本發明的至少一個額外的實施例，提供一種用於供應包括第一金屬之第一氣相反應物及包括第二金屬的第二氣相反應物（例如第一及/或第二氣相反應物包括具有R-M-H（例如R
(X-n)-M
X-H
n)之通式的化合物，其中R為有機基、X為金屬的正式氧化態、n是1到5、而M為金屬）之方法。該方法可包括：提供第二氣相反應物來源容器，其構造成含有第二氣相反應物（例如本文中所述之第二氣相反應物的任何者）、流體式連接第二氣相反應物來源容器至反應室、加熱包含在第二氣相反應物來源容器中的第二氣相反應物到約0°C至約400°C、約20°C至約200°C、約20°C至約100°C的溫度、產生至少0.001 mbar的第二氣相反應物之蒸汽壓力以及供應第二氣相反應物至反應室。
在本發明之一些實施例中，提供利用反應性揮發化學物之反應器系統。反應器系統可包含反應室、與反應室流體連通的第一氣相反應物來源容器以及與反應室流體連通的第二氣相反應物來源容器。第一及/或第二氣相反應物可包含，例如，具有R-M-H（例如
(X-n)-M
X-H
n）之通式的化合物，其中R為有機基、X為金屬的正式氧化態、n是1到5、而M為金屬。
為了概述本發明及相較於習知技藝所實現之優點，本發明之某些目的及優點已描述於上文中。當然，應明瞭無須根據本發明之任何特定實施例來達成所有該等目的或優點。因此，例如，熟悉本技術領域者將認識到，本發明可以以實現或最佳化本文所教示或建議之一個優點或一組優點而不一定實現本文可能教示或建議之其他目的或優點的方式來具體化或實施。
以下提供之本發明的示範實施例的說明僅係例示性且僅係意欲用於說明之目的；以下說明不意欲限制本發明之範疇。此外，敘述具有所述特徵之多個實施例不意欲排除具有額外特徵之其他實施例或納入所述特徵之不同組合的其他實施例。
如下更詳細提出，本發明的示範實施例關於用於沉積含金屬（諸如元素金屬、混合物、金屬合金及金屬間化合物）材料的方法及設備，以及關於包含含金屬材料之膜及結構。雖於下詳述其中本發明解決現有系統及方法的各種缺點的方式，一般而言，本文所述之各種系統及方法採用改進的反應物（有時概述為前驅物）及/或改善的沉積技術，以沉積具有希望性質之含金屬材料。
如本文所使用，術語「前驅物」及/或「反應物」可指一或多種氣體/蒸氣，其參與一化學反應或從其衍生出參與一反應之氣相物質。化學反應可在氣相中及/或氣相與基板表面及/或基板表面上的物種之間發生。
如本文所使用，術語「循環沉積」可指將反應物依序引入反應室中以在基板上方沉積一層膜且包含諸如原子層沉積及循環化學氣相沉積之沉積技術。
如本文所使用，術語「循環化學氣相沉積」可指任何一個製程，其中將基板依序暴露於兩種或更多種揮發性反應物，該等前驅物在基板上反應及/或分解，以產生所要的材料。
如本文所使用，術語「原子層沉積(ALD)」可指氣相沉積製程，其中在反應室中實施多個沉積循環，例如複數個連續的沉積循環。通常，在每一個循環期間，第一反應物化學吸附至基板表面，形成不會與額外的第一反應物反應之一單層或亞單層（亦即自限性反應）。之後，可以接著將另一個第二反應物或反應氣體引入處理室中，以用於將經化學吸附之物質轉化為所要材料。此外，在每一個沉積循環期間亦可使用清除步驟，以在經化學吸附的第一及/或第二反應物的轉化後，從反應室移除多餘的第一反應物及/或從反應室移除多餘的第二反應物、反應氣體及/或反應副產物。再者，如本文所使用之術語「原子層沉積」，當以交替脈衝的反應物、反應性氣體及/或清除（如惰性承載）氣體執行時，亦意指包括由相關術語所表示之製程，諸如，化學氣相原子層沉積、原子層磊晶(ALE)、分子束磊晶(MBE)、氣體源MBE、有機金屬MBE及化學束磊晶。
如文中所用，「基板」一詞可指具有材料可沉積於其上之表面的任何材料。基板可包含塊體材料，諸如矽（如單晶矽）或鍺（如單晶鍺），並可包含覆蓋於塊體材料的一或多層，包含，例如在將基板暴露至TMA下而得之例如經化學吸附之物種。此外，基板可包含各種特徵，諸如形成於基板之至少一部分之內或之上的溝渠、通孔、線條等等。特徵可具有例如大於或等於5、大於或等於10、大於或等於15或大於或等於20之高寬比，其界定為特徵之高度除以特徵之寬度。
如本文所使用，術語「膜」、「薄膜」、「層」及「薄層」可以意指例如藉由本文揭露之方法所沉積之任何連續或不連續的材料。例如，「膜」、「薄膜」、「層」及「薄層」可以包括2D材料、奈米棒、奈米管或奈米粒子或者甚至部分或完全分子層或部分或完全原子層或原子及/或分子之團簇。「膜」、「薄膜」、「層」及「薄層」可以包括具有針孔之材料或層，但仍然是至少部分連續的。
如本文中所用，術語「含金屬膜」及「含金屬材料」可指含有至少一個金屬物種的膜或材料。
如本文中所用，術語「金屬」可包含半金屬或類金屬。
如本文中所用，「金屬間」或「金屬間化合物」可指包含具有確定的化學計量及有序晶體結構的兩或更多金屬元素之化合物。金屬間化合物與金屬合金的差別在於其之晶體結構；金屬間化合物之晶體結構排列成特定結構，而合金通常表現出所參與的金屬組分之一的晶體結構。當不同原子之間的鍵比同一元素原子之間的鍵更強時，形成金屬間化合物。
在整份本發明給出一些示範材料；應注意針對每個示範材料所給出之化學式不應被視為限制性，且所給出之非限制性示範材料不應受給定的示範化學計量所限制。
本發明包含用於在基板上沉積含金屬材料（例如含金屬材料的膜）之方法。可使用循環沉積製程來進行該方法來沉積含金屬材料，以例如在基板上形成含金屬膜。示範方法可在相對低溫度下沉積含金屬膜，諸如由金屬間化合物構成、基本上由金屬間化合物組成或由金屬間化合物組成的膜。另外或替代地，方法可沉積含金屬材料，其具有大面積的厚度、結晶及/或組成均勻性之包含含金屬材料、基本上由含金屬材料組成或由含金屬材料組成的膜。
茲參考圖式，圖1繪示出根據本發明的至少一個實施例之循環沉積方法100。方法100可用來形成金屬間化合物，諸如在基板表面上之金屬間化合物的膜。
方法100可以從步驟110開始，其包括提供至少一個基板至反應室中且加熱基板至沉積溫度。沉積溫度可取決於，例如，用於形成金屬間化合物之一或多個反應物。舉例來說，反應室可加熱至大於0°C及小於600°C、小於500°C、小於400°C、小於300°C或小於250°C，或在約20°C至約700°C之間、在約50°C至約500°C之間，或在約50°C至約400°C之間、在約75°C至約300°C之間或在約100°C至約250°C之間。舉特定範圍而言，金屬間化合物可包含Co
3Sn
2，且在此情況中，溫度可在從約170°C至約200°C的範圍內；類似地，當金屬間化合物包含Ni
3Sn
2時，溫度可在從約125°C至約175°C或約140°C至約160°C的範圍內。可控制反應室內的壓力以在反應室中提供一沉積製程所需的壓力。例如，在循環沉積製程期間反應室內的壓力可小於1000 mbar、小於100 mbar、小於10 mbar、小於5 mbar，或甚至，在某些情況中，小於1 mbar，或從約10
-8mbar至約1000 mbar、從約10
-3mbar至約100 mbar、從約10
-2mbar至約50 mbar或從約0.1 mbar至約10 mbar。
方法100可進至步驟120，其包含提供包括第一金屬的第一氣相反應物至反應室以與基板表面反應而形成第一金屬物種。此步驟可在與於上連同步驟110所述之相同壓力及溫度。脈衝時間或將第一氣相反應物提供至反應室之時間可介於，例如，約0.01秒及約60秒之間、約0.05秒及約10秒之間或約0.1秒及約5秒之間。在步驟120期間，第一氣相反應物之流速可小於2000 sccm、小於1000 sccm、小於500 sccm、小於200 sccm、或甚至小於100 sccm、或可在從約1至約5000 sccm、從約5至約2000 sccm或從約10至約1000 sccm的範圍之間。
在提供第一氣相反應物的步驟之後，可藉由清除/泵送程序（步驟125）從反應室移除任何多餘的第一氣相反應物及任何反應副產物。步驟125的持續期間可為，例如，在約0.01秒及約60秒之間、在約0.05秒及約10秒之間或在約0.1秒及約5秒之間。在步驟125之清除氣體流可小於2000 sccm、小於1000 sccm、小於500 sccm、小於200 sccm或小於100 sccm，或可在從約1至約5000 sccm、從約5至約2000 sccm或從約10至約1000 sccm的範圍之間。雖分別繪示，步驟125可視為步驟120的一部分。
方法100可進至步驟130，提供包括第二金屬的第二氣相反應物至反應室以與第一金屬物種反應而形成金屬間化合物。此步驟可在與先前連同步驟110所述之相同或不同的壓力及/或溫度。脈衝時間或將第二氣相反應物提供至反應室之時間可介於，例如，約0.01秒及約60秒之間、約0.05秒及約10秒之間或約0.1秒及約5秒之間。在步驟130期間，第二氣相反應物之流速可與於上所述在步驟120期間之流速相同或類似。
如圖1中所示，當第二氣相反應物與基板表面上的物種反應時，可形成金屬間化合物，例如包含金屬間化合物、基本上由金屬間化合物所組成、由金屬間化合物所組成的膜（步驟140)。
在步驟140之後，可藉由清除/泵送程序（步驟145）從反應室移除任何多餘的第二氣相反應物及任何反應副產物。在此步驟中之清除氣體的流動及/或持續時間可與於上所述在步驟125中的同或類似。此外，雖分別繪示，步驟145可視為步驟130的一部分。
步驟120及130（及可選地清除步驟125及/或145）可構成一個沉積循環。在本發明之一些實施例中，方法100可包括重複這個沉積循環一或多次。例如，方法100可進至決定閘150，其判定循環沉積方法100是否要繼續或經由步驟160離開。可根據所沉積之金屬間化合物的厚度或量來判定決定閘150。例如，若金屬間化合物的厚度針對所要的裝置結構而言不夠的話，則方法100可返回到步驟120，並可重複步驟120-145。一旦金屬間化合物已沉積至所要的厚度或量，方法可在步驟160終止，並可使基板受到額外的製程來形成一或多個裝置或裝置結構。
根據方法100的各個態樣，金屬間化合物在當第二氣相反應物與於步驟120期間形成於表面上的第一金屬物種反應時形成。因此，可在無額外還原步驟及/或加熱步驟下形成包含金屬間化合物、基本上由金屬間化合物組成或由金屬間化合物組成之金屬間化合物或層或膜。此外，如上所提出，可在相對低溫下形成金屬間化合物。
第一氣相反應物可包含與第二金屬不同的任何第一金屬。舉例來說，第一金屬可以是或包含過渡金屬（例如第3-12族金屬），諸如第3-6族金屬、第7-12族金屬、鑭係金屬、第8-11族金屬及/或第9-10族金屬或第13-15族金屬，其中族編號是指IUPAC族編號。
根據替代實施例，諸如於下連同圖2所述的那些，第一氣相反應物可包含與第二金屬相同的第一金屬。當第一金屬及第二金屬相同時，可形成元素金屬膜。如上所示，該等元素金屬膜可包含半金屬或類金屬。
第一氣相反應物可為或包含金屬鹵化物，其中金屬為或包含第一金屬。金屬鹵化物化合物可包括金屬氯化物、金屬碘化物、金屬氟化物或金屬溴化物。在本發明的一些實施例中，金屬鹵化物化合物可包括一個金屬物種，包含，但不限於，鎳、鈷或銅的至少一者。在本發明的一些實施例中，金屬鹵化物化合物可包括一個金屬物種，包含，但不限於，氯化鎳、氯化鈷或氯化銅的至少一者。在一些實施例中，金屬鹵化物化合物可包括含雙牙氮的加成物形成配位子（ligand）。在一些實施例中，金屬鹵化物化合物可包括包含兩個氮原子的加成物形成配位子（例如，相應金屬鹵化物的二胺加成物），其中每一個氮原子鍵結到至少一個碳原子。在本發明的一些實施例中，金屬鹵化物化合物包括鍵結至一中央金屬原子的一或多個氮原子，藉此形成一金屬錯合物。在圖4中繪示這種化合物的一個範例。額外的第一氣相反應物可包含加成物形成配位子，其包含磷、氧及/或硫。
在一些實施例中，第一氣相反應物可包括具有加成物形成配位子的過渡金屬化合物。在一些實施例中，第一氣相相反應物可包括過渡金屬化合物。在一些實施例中，第一氣相反應物可包含過渡金屬鹵化物化合物。在一些實施例中，第一氣相相反應物可包括具有加成物形成配位子（諸如單牙、雙牙或多牙加成物形成配位子）的過渡金屬化合物。在一些實施例中，第一氣相相反應物可包括具有加成物形成配位子（諸如單牙、雙牙或多牙加成物形成配位子）的過渡金屬鹵化物化合物。在一些實施例中，第一氣相相反應物可包括具有包括氮之加成物形成配位子（諸如包括氮之單牙、雙牙或多牙加成物形成配位子）的過渡金屬化合物。在一些實施例中，第一氣相相反應物可包括具有包括磷、氧或硫之加成物形成配位子（諸如包括磷、氧、硫之單牙、雙牙或多牙加成物形成配位子）的過渡金屬化合物。例如，在一些實施例中，過渡金屬鹵化物化合物可包括，過渡金屬氯化物、過渡金屬碘化物、過渡金屬氟化物或過渡金屬溴化物。在本發明的一些實施例中，過渡金屬鹵化物化合物可包括過渡金屬物種，包含，但不限於，鈷、鎳或銅的至少一者。在本發明的一些實施例中，過渡金屬鹵化物化合物可包括氯化鈷、氯化鎳或氯化銅的至少一者。在一些實施例中，過渡金屬鹵化物化合物可包括含雙牙氮的加成物形成配位子。在一些實施例中，過渡金屬鹵化物化合物可包括包含兩個氮原子的加成物形成配位子，其中每一個氮原子鍵結到至少一個碳原子。在本發明的一些實施例中，過渡金屬鹵化物化合物包括鍵結至一中央過渡金屬原子的一或多個氮原子，藉此形成一金屬錯合物。
在本發明的一些實施例中，第一氣相反應物可包括具有下列式子的過渡金屬化合物：
（加成物）
n-M-Xa
其中每一個「加成物」為一加成物形成配位子並可獨立地選擇成單牙、雙牙或多牙加成物形成配位子或上述之混合物：n在單牙形成配位子情況中為從1至4、n在雙或多牙加成物形成配位子情況中為從1至2；M為過渡金屬，諸如，例如，鈷（Co）、銅（Cu）或鎳（Ni）；其中每一個Xa為另一個配位子並可獨立地選擇成鹵化物或其他配位子；其中a為從1至4，且在某些情況中a為2。
在本發明的一些實施例中，在過渡金屬化合物的加成物形成配位子，諸如過渡金屬鹵化物化合物，可包括透過氮原子、磷原子、氧原子或硫原子的至少一者與過渡金屬化合物的過渡金屬原子配位的單牙、雙牙或多牙加成物形成配位子。在本發明的一些實施例中，在過渡金屬化合物中的加成物形成配位子可包括環狀加成物配位子。在本發明的一些實施例中，在過渡金屬化合物中的加成物形成配位子可包括單胺、二胺或多胺。在本發明的一些實施例中，在過渡金屬化合物中的加成物形成配位子可包括單醚、二醚或聚醚。在一些實施例中，在過渡金屬化合物中的加成物形成配位子可包括單膦、二膦或聚膦。在一些實施例中，除了加成物形成配位子中的氮、氧、磷或硫，在過渡金屬化合物中的加成物形成配位子還可/或可包括碳。
在本發明的一些實施例中，在過渡金屬化合物中的加成物形成配位子可包括一個單牙加成物形成配位子。在本發明的一些實施例中，在過渡金屬化合物中的加成物形成配位子可包括兩個單牙加成物形成配位子。在本發明的一些實施例中，在過渡金屬化合物中的加成物形成配位子可包括三個單牙加成物形成配位子。在本發明的一些實施例中，在過渡金屬化合物中的加成物形成配位子可包括四個單牙加成物形成配位子。在本發明的一些實施例中，在過渡金屬化合物中的加成物形成配位子可包括一個雙牙加成物形成配位子。在本發明的一些實施例中，在過渡金屬化合物中的加成物形成配位子可包括兩個雙牙加成物形成配位子。在本發明的一些實施例中，在過渡金屬化合物中的加成物形成配位子可包括一個多牙加成物形成配位子。在本發明的一些實施例中，在過渡金屬化合物中的加成物形成配位子可包括兩個多牙加成物形成配位子。
在本發明的一些實施例中，加成物形成配位子包括氮，諸如胺、二胺或多胺加成物形成配位子。在該等實施例中，過渡金屬化合物可包括三乙胺（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’-二異丙基乙二胺（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’-四甲基甲烷二胺（CAS：51-80-9）（TMMDA），N,N,N’,N”,N”-五甲基二亞乙基三胺（CAS：3030-47-5）（PMDETA）、二亞乙基三胺（CAS：111-40-0）（DIEN）、三亞乙基四胺（CAS：112-24-3）（TRIEN）、三（2-胺基乙基）胺（CAS：4097-89-6）（TREN，TAEA）、1,1,4,7,10,10-六甲基三乙烯四胺（CAS：3083-10-1）（HMTETA）、1,4,8,11-四氮雜環十四烷（CAS：295-37-4）（Cyclam）、1,4,7-三甲基-1,4,7-三氮雜環壬烷（CAS：96556-05-7）或1,4,8,11-四甲基-1,4,8,11-四氮雜環十四烷（CAS：41203-22-9）之至少一者。
在本發明的一些實施例中，加成物形成配位子包括磷，諸如膦、二膦或多膦加成物形成配位子。例如，過渡金屬化合物可包括三乙基膦（CAS：554-70-1）、亞磷酸三甲酯（CAS：121-45-）、1,2-雙（二乙基膦基）乙烷（CAS：6411-21-8）（BDEPE）或1,3-雙（二乙基膦基）丙烷（CAS：29149-93-7）之至少一者。
在本發明的一些實施例中，加成物形成配位子包括氧，諸如醚、二醚或聚醚加成物形成配位子。例如，過渡金屬化合物可包括1,4-二噁烷（CAS：123-91-1）、1,2-二甲氧基乙烷（CAS：110-71-4）（DME，單甘醇二甲醚）、二甘醇二甲醚（CAS：111-96-6）（diglyme）、三甘醇二甲醚（CAS：112-49-2）（triglyme）或1,4,7,10-四氧雜環十二烷（CAS：294-93-9）（12-冠-4）之至少一者。
在本發明的一些實施例中，加成物形成配位子可包括硫醚或混合醚胺，諸如，例如1,7-二氮雜-12-冠-4中的至少一者：1,7-二氧雜-4,10-二氮雜環十二烷（CAS：294-92-8）或1,2-雙（甲硫基）乙烷（CAS：6628-18-8）。
在一些實施例中，過渡金屬鹵化物化合物可包括氯化鈷N,N,N’,N’-四甲基-1,2-乙二胺（CoCl
2（TMEDA））。在一些實施例中，過渡金屬鹵化物化合物可包括溴化鈷四甲基乙二胺（CoBr
2（TMEDA））。在一些實施例中，過渡金屬鹵化物化合物可包括碘化鈷四甲基乙二胺（CoI
2（TMEDA））。在一些實施例中，過渡金屬鹵化物化合物可包括氯化鈷N,N,N’,N’-四甲基-1,3-丙二胺（CoCl
2（TMPDA））。在一些實施例中，過渡金屬鹵化物化合物可包括氯化鈷N,N,N’,N’-四甲基-1,2-乙二胺（CoCl
2（TMEDA））、氯化鎳四甲基-1,3-丙二胺（NiCl
2（TMPDA））或碘化鎳四甲基-1,3-丙二胺（NiI
2（TMPDA））之至少一者。
其他適合的第一氣相反應物可為實質上無鹵素物種。實質上無鹵素物種（不含鹵素之金屬前驅物）的第一氣相反應物包含M（dmap）
x（dmap＝二甲基胺基-2-丙醇鹽），其中M為金屬、β-二酮酸鹽、脒鹽及其他典型的ALD金屬前驅物。在一些實施例中，不含鹵素之金屬前驅物可包括銅、鈷及鎳的至少一者。不含鹵素之金屬前驅物可因此包括Cu(dmap)
2、Ni(dmap)
2或Co(dmap)
2的至少一者。
在一些實施例中，不含鹵素之金屬前驅物可因此包括至少一個雙牙配位子，其中金屬中央原子透過雙牙配位子中的至少一個氧及至少一個氮原子鍵結。在一些實施例中，不含鹵素之金屬前驅物可因此包括至少一個雙牙配位子，其中金屬中央原子透過雙牙配位子中的至少一個氮原子鍵結。在一些實施例中，不含鹵素之金屬前驅物可因此包括至少一個雙牙配位子及至少一個其他的配位子，諸如單牙配位子。在一些實施例中，不含鹵素之金屬前驅物可因此包括至少一個雙牙配位子及至少兩個其他的配位子，諸如單牙配位子。在一些實施例中，不含鹵素之金屬前驅物可因此包括至少一個雙牙配位子及至少一個其他的配位子，諸如單牙配位子，其透過N或O鍵結至金屬中央原子。在一些實施例中，不含鹵素之金屬前驅物可因此包括至少一個雙牙配位子，其中金屬中央原子在雙牙配位子中透過至少一個氮原子鍵結及透過至少另一個非氮的原子鍵結。在一些實施例中，不含鹵素之金屬前驅物可因此包括至少一個雙牙配位子，其中金屬中央原子在雙牙配位子中透過至少兩個氮原子鍵結。在一些實施例中，不含鹵素之金屬前驅物可包括至少兩個雙牙配位子。在一些實施例中，不含鹵素之金屬前驅物可包括兩個雙牙配位子。
合適的不含鹵化物之β二酮亞胺基（betadiketiminato）（例如，Ni（pda）
2），（pda＝戊烷-2,4,-二酮亞胺基）化合物的一些範例包含至少一個β-二酮亞胺基配位子，且具有以下通式：
[化學式1]
其中M為選自鎳、鈷、釕、銥、鈀、鉑、銀及金的金屬。每一個R
1-5為獨立地選自H以及C
1-C
4直鍊或支鏈烷基、烷基甲矽烷基、烷基醯胺基、醇鹽基或烷基甲矽烷基醯胺基的有機配位子。每一個L獨立地選自：碳氫化合物、含氧烴、胺、多胺、聯吡啶、含氧雜環、含氮雜環及其組合；且n是0到4的整數，包括0和4。一個具體範例包含Ni(pda)
2。
適合的不含鹵化物之脒鹽化合物（例如Ni(iPr-AMD)
2）的一些範例包含具有選自由M(I)AMD、M(II)AMD
2及M(III)AMD
3及上述之低聚物所組成之群組的式子之化合物，其中M為金屬且AMD為脒鹽部分，諸如銅（I）脒鹽、鈷（II）脒鹽或鎳、鐵、釕、錳、鉻、釩、鈮、鉭、鈦及/或鑭的脒鹽。
在一或多個實施例中，單價金屬的前驅物包括揮發性金屬（I）脒鹽，[M（I）（AMD）]x，其中x＝2, 3。這些化合物的一些具有二聚體結構1，
[化學式2]
其中R
1、R
2、R
3、R
1'、R
2'及R
3'為從一或多個非金屬原子製成的基。在一些實施例中，R
1、R
2、R
3、R
1'、R
2'及R
3'可獨立地選自氫、烷基、芳基、烯基、炔基、三烷基甲矽烷基或氟烷基或其他非金屬原子或基。在一些實施例中，R
1、R
2、R
3、R
1'、R
2'及R
3'各可獨立地為含有1到4個碳原子的烷基或氟烷基或甲矽烷基烷基。適合的單價金屬包含銅（I）、銀（I）、金（I）及銥（I）。在一或多個實施例中，金屬脒鹽為銅脒鹽，且銅脒鹽包括銅（I）N,N’-二異丙基乙脒，相當於取R1、R
2，R
1'及R
2'作為通式1中的異丙基，而R
3及R
3'作為甲基。在一或多個實施例中，金屬（I）脒鹽為具有通式[M（I）（AMD）]
3的三聚體。
在一或多個實施例中，二價金屬前驅物包含揮發性金屬（II）雙脒鹽，[M（II）（AMD）
2]
x，其中x＝1, 2。這些化合物可具有單體結構2，
[化學式3]
其中R
1、R
2、R
3、R
1'、R
2'及R
3'為從一或多個非金屬原子製成的基。在一或多個實施例中，亦可使用此結構的二聚體，例如，[M(II)(AMD)
2]
2。在一些實施例中，R
1、R
2、R
3、R
1'、R
2'及R
3'可獨立地選自氫、烷基、芳基、烯基、炔基、三烷基甲矽烷基或氟烷基或其他非金屬原子或基。在一些實施例中，R
1、R
2、R
3、R
1'、R
2'及R
3'各可獨立地為含有1到4個碳原子的烷基或氟烷基或甲矽烷基烷基。適合的二價金屬包含鈷、鐵、鎳、錳、釕、鋅、鈦、釩、鉻、銪、鎂及鈣。在一或多個實施例，金屬（II）脒鹽為鈷脒鹽，且鈷脒鹽包括鈷（II）雙（N,N’-二異丙基乙脒），相當於取R
1、R
2、R
1'及R
2'作為通式2中的異丙基，而R
3及R
3'作為甲基。
在一或多個實施例，三價金屬的前驅物包含揮發性金屬（III）三脒鹽，M(III)(AMD)
3。通常，這些化合物具有單體結構3，
[化學式4]
其中R
1、R
2、R
3、R
1'、R
2'、R
3'、R
1"、R
2"及R
3"為由一或更多非金屬原子製成之基。在一些實施例，R
1、R
2、R
3、R
1'、R
2'、R
3'、R
1"、R
2"及R
3"可獨立地選自氫、烷基、芳基、鏈烯基炔基、三烷基甲矽烷基、鹵素或部分氟化的烷基。在一些實施例，R
1、R
2、R
3、R
1'、R
2'、R
3'、R
1"、R
2"及R
3"各自獨立地為含有1至4個碳原子的烷基。合適的三價金屬包括鑭、鐠及其他鑭係金屬、釔、鈧、鈦、釩、鈮、鉭、鉻、鐵、釕、鈷、銠、銥、鋁、鎵、銦及鉍。在一或更多實施例中，金屬（III）脒鹽是鑭脒鹽，且鑭脒鹽包含鑭（III）三（N,N’-二（三級丁基乙脒）），相當於取R
1、R
2、R
1'、R
2'、R
1"及R
2'作為通式3中的三級丁基而R
3、R
3'及R
3"作為甲基。
如本文中所用，具有與單體相同的金屬與脒酸鹽比例，但化合物中金屬脒鹽單元（metallamidinate units）總數不同的金屬脒鹽被稱為單體化合物的“低聚物”。因此，單體化合物的低聚物M(R)AMD
2包含[M(II)(AMD)
2]
x，其中x為2、3等等。同樣地，單體化合物的低聚物M(I)AMD包含[M(I)AMD]
x，其中x為2、3等等。
具體實例包括（N,N’-二異丙基乙醯胺基）銅（[Cu（iPr-AMD）]
2）、雙（N,N’-二異丙基乙醯胺基）鈷（[Co（iPr-AMD）
2]）、鈷雙（N,N’-二（三級丁基乙脒））（[Co（tBu-AMD）
2]）、鑭三（N,N’-二異丙基乙脒）（[La（iPr-AMD）
3]）、鑭三（N,N’-二異丙基-2-三級丁基脒）（[La（iPr-tBuAMD））
3]。½C
6H
12）、雙（N,N’-二異丙基乙醯胺基）鐵（[Fe（iPr-AMD）
2]
2）、雙（N,N’-二（三級丁基乙脒））（[Fe（
tBu-AMD）
2]）、雙（N,N’-二異丙基乙醯胺基）鎳（[Ni（
iPr-AMD）
2]）、雙（N,N’-二異丙基乙醯胺基）錳（[Mn（
iPr-AMD）
2]
2）、錳雙（N,N’-二（三級丁基乙脒）（[Mn（
tBu-AMD）
2]）、三（N,N’-二異丙基乙醯胺基）鈦（[Ti（
iPr-AMD）
3]）、三（N,N’-二異丙基乙醯胺基）釩（[V（
iPr-AMD）
3]）、銀（N,N’-二異丙基乙脒）（[Ag（
iPr-AMD）]
x（x＝2及x＝3）、N,N’-二仲丁基乙脒鋰、鈷雙（N,N’-二仲丁基乙脒）（[Co（sec-Bu-AMD）
ㄉ]）、銅（I）N,N’-二仲丁基乙脒二聚體（[Cu（sec-Bu-AMD）]
ㄉ）、鉍三（N,N’-二（三級丁基乙脒））二聚體（[Bi（
tBu-AMD）
3]
2）、鍶雙（N,N’-二（三級丁基乙脒））（[Sr（
tBu-AMD）
2]
n）、氧化鉍、Bi
2O
3及三（N,N’-二異丙基乙醯胺基）釕（[Ru（
iPr-AMD）
3]）。
由下列式子敘述之合適的不含鹵化物亞胺基醇鹽化合物之一些範例：
[化學式5]
其中M為選自週期表之第2至12族的金屬；且R1、R2、R3及R4各自獨立地為H或C1至C8烷基。在一細化方案中，R1、R2、R3及R4各自獨立地為甲基、乙基、正丙基、異丙基、正丁基、二級丁基、異丁基或三級丁基（t-butyl）。在另一細化方案中，M為Cu、Cr、Mn、Fe、Co或Ni。具有此式子的化合物之具體範例包含，但不限於，雙（1-（叔丁基亞胺基）-2,3,3-三甲基丁-2-醇）鎳（II）、雙（1-（叔丁基亞胺基）-2,3,3-三甲基丁-2-醇）鈷（II）、雙（1-（叔丁基亞胺基）-2,3,3-三甲基丁-2-醇）鐵（II）、雙（1-（叔丁基亞胺基）-2,3,3-三甲基丁-2-酮））錳（II）、雙（1-（叔丁基亞胺基）-2,3,3-三甲基丁-2-醇）鉻（II）、雙（1-（叔丁基亞胺基）-2,3,3-三甲基丁-2-醇）銅（II）、雙（1-（叔丁基亞胺基）-2,3-二甲基丁-2-醇）鎳（II）、雙（1-（叔丁基亞胺基）-2,3-二甲基丁-2-醇）鈷（II）、雙（1-（叔丁基亞胺基）-2,3-二甲基丁-2-醇）鐵（II）、雙（1-（叔丁基亞胺基）-2,3-二甲基丁-2-醇）銅（II）、雙（3-（（叔丁基亞胺基）甲基）-2,2,4,4-四甲基戊烷-3-醇）錳（II）、雙（3-（（叔丁基亞胺基）甲基）-2,2,4,4-四甲基戊-3-醇鹽）銅（II）、雙（3-（異丙基亞胺基）-2-甲基丁-2-醇）鎳（II）、雙（3）-（異丙基亞胺基）-2-甲基丁-2-醇）鈷（II）、雙（3-（異丙基亞胺基）-2-甲基丁-2-醇）鐵（II）、雙（3-（異丙基亞胺基）-2-甲基丁-2-醇）錳（II）、雙（3-（異丙基亞胺基）-2-甲基丁-2-醇）鉻（II）、雙（3-（異丙基亞胺基）-2-甲基丁-2-醇）銅（II）、雙（3-（2,2-二甲基亞肼基）-2-甲基丁-2-醇）鎳（II）、雙（3-（2,2-二甲基亞肼基）-2-甲基丁-2-醇）鈷（II）、雙（3-（2,2-二甲基亞肼基）-2-甲基丁-2-醇）鐵（II）、雙（3-（2,2-二甲基亞肼基）-2-甲基丁-2-醇）錳（II）、雙（3-（2,2-二甲基亞肼基）-2-甲基丁-2-醇）chrolium（II）以及雙（3-（2,2-二甲基亞肼基）-2-甲基丁-2-醇）銅（II）。具體範例包括雙（1-（三級丁基亞胺基）-2,3,3-三甲基丁-2-醇）鎳（H）、雙（1-（三級丁基亞胺基）-2,3,3-三甲基丁-2-醇）鈷（II）、雙（1-（三級丁基亞胺基）-2,3,3-三甲基丁-2-醇）鐵（II）、雙（1-（三級丁基亞胺基）-2,3,3-三甲基丁-2-醇）錳（II）、雙（1-（三級丁基亞胺基）-2,3,3-三甲基丁-2-醇）鉻（II）、雙（1-（三級丁基亞胺基））-2,3,3-三甲基丁-2-醇）銅（II）、雙（1-（三級丁基亞胺基）-2,3-二甲基丁-2-醇）鎳（II）、雙（1-（三級丁基亞胺基）-2,3-二甲基丁-2-醇）鈷（II）、雙（1-（三級丁基亞胺基）-2,3-二甲基丁-2-醇）鐵（II）、雙（1-（三級丁基亞胺基）-2,3-二甲基丁-2-醇）銅（II）、雙（3-（（三級丁基亞胺基）甲基）-2,2,4,4-四甲基戊-3-醇）錳（II）、雙（3-（（三級丁基亞胺基）甲基）-2,2,4,4-四甲基戊-3-醇）銅（II）、雙（3-（異丙基亞胺基）-2-甲基丁-2-醇）鈷（II）、雙（3-（異丙基亞胺基）-2-甲基丁-2-醇）鐵（II）、雙（3-（異丙基亞胺基）-2-甲基丁-2-醇）錳（II）、雙（3-（異丙基亞胺基）-2-甲基丁-2-醇）鉻（II）、雙（3-（2,2-二甲基亞肼基）-2-甲基丁-2-醇）鎳（II）、雙（3-（2,2-二甲基亞肼基）-2-甲基丁-2-醇）鈷（II）、雙（3-（2,2-二甲基亞肼基）-2-甲基丁-2-醇）鐵（II）、雙（3-（2,2-二甲基亞肼基）-2-甲基丁-2-醇）錳（II）、雙（3-（2,2-二甲基亞肼基）-2-甲基丁-2-醇）chrolium（II），雙（3-（2,2-二甲基亞肼基）-2-甲基丁-2-醇）銅（II）。
在一些實施例中，不含鹵素之金屬前驅物不包括所需金屬（例如Co、Ni、Cu）以外的其他金屬原子。在一些實施例中，不含鹵素之金屬前驅物中之金屬具有0的氧化態。在一些實施例中，不含鹵素之金屬前驅物中的金屬具有+I的氧化態。在一些實施例中，不含鹵素之金屬前驅物中的金屬具有+III的氧化態。在一些實施例中，不含鹵素之金屬前驅物中之金屬的氧化態具有+II的氧化態。在一些實施例中，氧化態為在室溫下前驅物中金屬的氧化態。氧化態可在不同條件中改變，諸如在不同壓力、溫度及/或大氣中，還有當在該等不同條件與不同表面材料接觸時。在一些實施例中，不含鹵素之金屬前驅物不包括鹵化物，諸如F、Cl、Br或I。在一些實施例中，不含鹵素之金屬前驅物包括碳、氫及氮和可選地氧。
在一些實施例中，不含鹵素之金屬前驅物可包括，例如，Cu（dmap）
2或銅（I）N,N’-二異丙基乙脒。在一些實施例中，銅前驅物可選自由銅β二酮酸鹽化合物、銅β二酮亞胺基化合物、銅胺基醇鹽化合物，如Cu（dmae）
2、Cu（deap）
2或Cu（dmamb）
2、銅脒鹽化合物，如Cu（sBu-amd）]
2、銅環戊二烯基化合物、羰基銅化合物及上述組合組成之群組。在一些實施例中，使用X(acac)y或X(thd)y化合物，其中X為銅、y通常但非絕對為2或3以及thd為2,2,6,6-四甲基-3,5-庚烷二酮酸。在一些實施例中，不含鹵素之金屬前驅物為乙酸銅（II），[Cu（HMDS）]
4或Cu（nhc）HMDS（1,3-二異丙基-咪唑啉-2-亞基銅六甲基二矽氮化物）或Cu-β-二酮亞胺基，如Cu（dki）VTMS（dki＝二酮亞胺）。
在一些實施例中，不含鹵素之金屬前驅物可為，例如，雙（4-N-乙基胺基-3-戊烯-2-N-乙基亞胺基）鎳（II）。在一些實施例中，鎳前驅物可選自由鎳β二酮酸鹽化合物、鎳β二酮亞胺基化合物、鎳胺基醇鹽化合物、鎳脒鹽化合物、鎳環戊二烯基化合物、鎳羰基化合物及上述之組合組成之群組。在一些實施例中，使用X(acac)y或X(thd)y化合物，其中X為鎳、y通常但非絕對為2或3、以及thd為2,2,6,6-四甲基-3,5-庚烷二酮酸。
在一些實施例中，Co前驅物為Coβ-二酮亞胺基化合物。在一些實施例中，Co前驅物為Co酮亞胺鹽化合物。在一些實施例中，Co前驅物為Co脒鹽化合物。在一些實施例中，Co前驅物為Coβ-二酮酸鹽化合物。在一些實施例中，Co前驅物含有至少一個酮亞胺配位體或其衍生物。在一些實施例中，Co前驅物含有至少一個脒配位體或其衍生物。在一些實施例中，Co前驅物含有至少一個酮酸鹽或其衍生物。在一些實施例中，Co前驅物為Co
2(CO)
8、CCTBA、CoCp
2、Co(Cp-amd)、Co(Cp(CO)
2)、tBu-AllylCo(CO)
3或Co(HMDS)
2。
舉具體範例而言，第一氣相反應物可以是或包含金屬鹵化物TMPDA化合物，其中金屬例如為Ni或Co，鹵化物例如為Cl或I，以及TMPDA為N,N,N’,N’，-四甲基-1,3-丙二胺—例如，NiCl
2(TMPDA)及CoCl
2(TMPDA)及/或金屬鹵化物TMEDA化合物，其中金屬例如為Ni或Co，鹵化物例如為Cl或I，以及TMEDA為N,N,N’,N’-四甲基-1,2-乙二胺，諸如CoCl
2(TMEDA)及NiCl
2(TMEDA)。金屬氫化物，諸如丙烷，可用作第一氣相反應物（例如，用於氫化物-氫化物型反應）。
可用於方法100中的第二氣相反應物可包含含金屬的有機化合物、有機金屬或金屬有機化合物。例如，第二氣相反應物可包含選自由具有R-M-H（例如R
(X-n)-M
X-H
n）式子的化合物組成之群組的化合物，其中R為有機基且M為金屬，以與第一金屬物種反應而形成含金屬的材料。根據各種範例，X為M的正式氧化態而n的範圍可以是從1到5。舉具體範例而言，M可以是或包含Ge、Ga、In、Sn、As、Sb、Pb及Bi。或者，M可包含Al。例如，M可包含Ge、Ga、In及/或Sn。R可以是或包含有或沒有額外的予體官能基之烷基或環戊二烯基、醯胺基、烷氧基、脒基、胍基、亞胺基、羧根基、β-二酮基、β-酮亞胺基、丙二酸、β-二酮亞胺基。示範烷基可獨立地選自C1-C10、C1-C8、C1-C7、C1-C6或C1-C5烷基。在某些情況中，第二氣相反應物（例如R-M-H化合物）可以是金屬還原劑。圖6繪示三丁基金屬氫化物之具體第二氣相反應物範例，其中M可例如為本文中所提到的任何金屬—例如氫化三丁基鍺（TBGH）。
如本文中所述的由金屬間化合物構成、基本上由金屬間化合物組成或由金屬間化合物組成的金屬間膜，諸如Co
3Sn
2或Ni
3Sn
2可呈現具有超過500 Oe的高矯頑磁力值的磁滯。取決於膜厚度及/或化學計量，這種膜的電阻率值（還有根據方法200所形成的膜）的範圍可以是從約10至約10
6µΩcm、從約20至約10
4µΩcm或從約50至約1000 µΩcm，例如，80至180 µΩcm。並且，根據方法100所形成之Ni
3Sn
2薄膜呈現金屬間晶體結構及高純度。範例金屬間化合物及膜可用於各種應用中，包含，例如，磁阻裝置、超導裝置、作為催化劑、作為能量（例如氫）貯存等等。
圖2繪示根據本發明的至少一個實施例的另一個循環沉積方法200。方法200可用來沉積含金屬的材料，以例如形成包含含有金屬的材料、基本上由含有金屬的材料組成或由含有金屬的材料組成的膜或層。含金屬的材料可包含任何上述金屬間化合物，還有本文中所述的其他含金屬的化合物。當膜（例如經由方法100或200所形成）基本上由或由金屬間化合物組成時，膜可呈現本文中所述的優異性質。然而，除非另有所指，膜、方法、結構、裝置及系統不限於金屬間化合物。
方法200從步驟210開始，其可與步驟110相同或類似。例如，反應室內的溫度及壓力可與步驟110中提出的相同或類似。
方法200可進至步驟220，其包含提供第一氣相反應物，諸如上述第一氣相反應物的任何者。此步驟可在與先前連同步驟210所提到之相同的壓力及溫度。脈衝時間或將第一氣相反應物提供至反應室的時間可以是介於約0.01秒及約60秒之間、介於約0.05秒及約10秒之間或介於約0.1秒及約5秒之間。於步驟220期間，第一氣相反應物之流速可以少於2000 sccm、少於1000 sccm、少於500 sccm、少於200 sccm或甚至少於100 sccm，或可以是從約1至約5000 sccm、從約5至約2000 sccm或從約10至約1000 sccm的範圍內。
在提供第一氣相反應物之步驟220後，可從反應室藉由清除/泵送程序（步驟225）移除任何多餘的第一氣相反應物及任何反應副產物。在步驟225期間清除氣體的流動可以少於2000 sccm、少於1000 sccm、少於500 sccm、少於200 sccm或甚至少於100 sccm，或可以是從約1至約5000 sccm、從約5至約2000 sccm或從約10至約1000 sccm的範圍內。雖未分別繪示，步驟225可視為步驟220的一部分。
方法200可進至步驟230，其包含提供包括具有R-M-H通式的化合物之第二氣相反應物，其中R為有機基且M為金屬，以與第一金屬物種(例如在基板表面上)反應而形成含金屬的材料。具有R-M-H通式的化合物可與上述的相同。脈衝時間或將第二氣相反應物提供至反應室的時間可以是介於約0.01秒及約60秒之間、介於約0.05秒及約10秒之間或介於約0.1秒及約5秒之間。於步驟230期間，第二氣相反應物之流速可以少於2000 sccm、少於1000 sccm、少於500 sccm、少於200 sccm或甚至少於100 sccm，或可以是從約1至約5000 sccm、從約5至約2000 sccm或從約10至約1000 sccm的範圍內。
如圖2中所示，當第二氣相反應物與基板表面上的物種反應時，形成含金屬的材料—例如包括含金屬的材料、基本上由含金屬的材料組成或由含金屬的材料組成的膜。
在步驟230後，可從反應室藉由清除/泵送程序（步驟245）移除任何多餘的第二氣相反應物及任何反應副產物。清除氣體的流速可與先前步驟225中所提到的相同。此外，雖未分別繪示，步驟245可視為步驟230的一部分。
可以和先前連同圖1所述之步驟120-145的相同或類似方式重複步驟220-245。例如，可重複這些步驟直到將含金屬材料之所要的膜厚度或量沉積於基板上為止。
步驟220中所用的第一氣相反應物可以是或包含本文中所述的任何第一氣相反應物且/或步驟230中所用的第二氣相反應物可以是或包含本文中所述的任何第二氣相反應物。如上所提出，第一氣相反應物及第二氣相反應物可包含相同或不同的材料。例如，藉由將第一氣相反應物，諸如GeCl
2（二㗁烷）或某些其他Ge前驅物與R
3GeH，可形成元素Ge膜。此外，使用R
3GeH有其益處，因為R
3GeH呈現相對低的毒性及相對高的穩定性。可類似地形成其他元素膜（或多金屬膜）。含金屬材料可具有合金、混合物、金屬間材料或元素金屬的形成。
舉具體範例而言，使用方法200所沉積的含金屬材料可包含M-Ge、M-Ga及/或M-In之一或多者，其中M選自由Ni及Co所組成的群組。根據這些範例的示範實施例，第一氣相反應物包含金屬鹵化物—例如，一相應金屬鹵化物的二胺加成物，諸如金屬鹵化物TMPDA化合物，如上所述，且第二氣相反應物包含具有本文中所述之R-M-H通式的化合物。在形成M-Ge、M-Ga及/或M-In含金屬膜之沉積製程期間的溫度可以是介於從約150 °C至約250 °C之間、介於從約160 °C至約200 °C之間或介於第一及第二反應物的昇華溫度和分解溫度之間。可在無任何退火處理、在少於400 °C溫度及/或僅使用第一氣相反應物、第二氣相反應物及可選的清除步驟下形成含金屬材料。令人驚訝和出乎意料地，根據方法100及200所形成的示範含金屬材料膜，尤其是上述的M-Ge、M-Ga及/或M-In膜，是相對純的，其中污染物（例如非金屬材料）少於1 at.%，以及任何鹵化物污染物可少於0.1 at.%。吾人認為本文中所述的第一及第二氣相反應物經歷快速且完整（或幾乎完整）的反應，藉此在任何所形成的材料中留下相對低的污染物。由於其高純度的關係，本文中所述的示範材料及膜可呈現低電阻率，這使得這些材料適合用於微電子裝置中的低電阻接觸層。例如，本文中所述的M-Ge、M-Ga及/或M-In材料可呈現低電阻，且因此可用作電子裝置結構中的接觸層。
如上所提及，取決於膜厚度及/或化學計量，根據方法200所形成的膜之電阻率值，諸如金屬鍺膜，諸如Ni
xGe
y及Co
xGe
y，可以是介於從約10至約10
6µΩcm之間、介於從約20至約10
4µΩcm之間或介於從約50至約1000 µΩcm之間，例如，80至180µΩcm。
根據本發明的一些實施例，方法100及/或方法200可包含原子層沉積（ALD）。ALD是基於自限反應，藉此使用反應物之依序且交替的脈衝來於每個沉積循環沉積約一個原子(或分子)單層的材料。通常選擇沉積條件及反應物，以提供自飽和反應，使得一種反應物之吸附層留下不與同一種反應物之氣相反應物反應的表面終止(surface termination)。接著使基板與一種不同的反應物接觸，此不同的反應物與先前終止反應，以便能夠持續沉積。因此，交替脈衝的每個循環通常留下不超過約一個單層的所要材料。然而，如上文所提及，在一或多個ALD循環中，可沉積超過一個單層的材料，例如在不管製程之交替性質如何發生一些氣相反應時。
在一些實施例中，使用循環沉積製程以在基板上形成含金屬膜且該循環沉積製程可為ALD類型製程。在一些實施例中，循環沉積可以是混合式ALD/CVD或循環式CVD製程。例如，在一些實施例中，ALD製程之生長速率相較於CVD製程可能是較低的。一種增加生長速率之方法可以是在比ALD製程中通常使用之溫度更高的基板溫度下操作，從而導致化學氣相沉積製程，但是仍利用前驅物的依序引入。這樣的製程可以稱為循環式CVD。
可在ALD或CVD沉積系統中執行本文中所述的循環沉積製程。舉例來說，在一些實施例中，方法可包含將基板加熱至介於大約80°C與大約150°C之間的溫度，或甚至將基板加熱至介於大約80°C與大約120°C之間的溫度，或介於大約150°C與大約250°C之間的溫度，或介於大約160°C與大約200°C之間的溫度。當然，任何給定的循環沉積製程(諸如，就ALD反應而言)之適宜溫度窗將取決於所涉及的表面終止及反應物物種。在此，溫度取決於所使用的前驅物而有所不同且通常係約700℃或低於約700℃。在一些實施例中，對於氣相沉積製程，沉積溫度通常係約100℃或高於約100℃，在一些實施例中，沉積溫度係介於約100℃與約300℃之間，以及在一些實施例中，沉積溫度係介於約120℃與約200℃之間。在一些實施例中，沉積溫度係低於約500℃或低於約400℃或低於約350℃或低於約300℃。在一些實例中，沉積溫度可係低於約300℃或低於約200℃或低於約100℃。在一些實例中，沉積溫度可係高於約20℃或高於約50℃或高於約75℃。在本發明之一些實施例中，沉積溫度(亦即，在沉積期間之基板的溫度)係與先前連同方法100及200所述之相同或不同的溫度。
如圖1及2中所繪示，循環製程，包含ALD製程，可包含清除步驟，諸如上述清除步驟125、145、225及245。在該等步驟期間所用的清除氣體可包含一或多個惰性氣體，諸如氬（Ar）或氮（N
2），以防止或減輕反應物之間、製程步驟之間的氣相反應，以便能有自我飽和的表面反應。然而，在一些實施例中，基板可額外或替代地被移動（例如至另一個反應室），以分別接觸第一氣相反應物及第二氣相反應物。因此，不須在相同的反應室中執行步驟120/130及/或步驟220/230。另外或替代地，可使用真空泵來協助清除。
應明瞭在本發明之一些實施例中，提供第一氣相反應物及提供第二氣相反應物之順序可為使基板先與第二氣相反應物接觸並接著與第一氣相反應物接觸。換言之，可顛倒步驟120、130和220、230。此外，在一些實施例中，循環沉積製程可包括在使基板與第二氣相反應物接觸一或多次之前，使基板與第一氣相反應物接觸一次或多次，並且類似地，可以替代地包括在使基板與第一氣相反應物接觸一次或多次之前，使基板與第二氣相反應物接觸一或多次。
本發明之至少一些實施例（如方法100及/或方法200）可包括非電漿反應物，例如，第一及第二氣相反應物實質上沒有離子化反應性物種。在一些實施例中，第一及第二氣相反應物實質上沒有離子化反應性物種、激發物種或自由基物種。例如，第一氣相反應物及第二氣相反應物皆可以包括非電漿反應物，以防止對底層基板的離子化損壞及由此所產生的相關缺陷。當底層基板包含易碎之製造的或至少部分製造的半導體裝置結構時，非電漿反應物的使用可能是特別有用的，因為高能電漿物種可能造成裝置性能特性的損害及/或惡化。
雖未顯示在圖2中，在本發明之一些實施例中，本發明的示範方法可包括額外的製程步驟，其包括使基板與包括還原劑之第三氣相反應物接觸。在一些實施例中，還原劑可包括氫（H
2）、氫（H
2）電漿、氨（NH
3）、氨（NH
3）電漿、肼（N
2H
4）、矽烷（SiH
4）、二矽烷（Si
2H
6）、三矽烷（Si
3H
8）、鍺烷（GeH
4）、二鍺烷（Ge
2H
6）、硼烷（BH
3）、二硼烷（B
2H
6）、三級丁基肼（C
4H
12N
2）、硒反應物、硼反應物、磷反應物、硫反應物、有機反應物（如醇、醛或羧酸）或氫反應物的至少一者。在本發明的一些實施例中，本發明的示範沉積方法可包括使基板與為還原劑之第二氣相反應物接觸（而無任何額外的前驅物/反應物接觸步驟）。如上所提及，根據至少一些範例，無須任何還原劑或還原反應（除了第二反應物）來形成所要的材料，諸如金屬間材料。
若使用的話，可在示範循環沉積方法中的許多製程階段將包含還原劑之第三氣相反應物引入至反應腔室中並與基板接觸。在本發明之一些實施例中，可與第一氣相反應物分開地及/或與第二氣相反應物分開地將還原劑引入至反應腔室中並與基板接觸。例如，可在使基板接觸第一氣相反應物之前、在使基板與第一氣相反應物接觸後以及在使基板與第二氣相反應物接觸前及/或在使基板與第二氣相反應物接觸後，將還原劑引入至反應腔室中並與基板接觸。在本發明之一些實施例中，可與第一氣相反應物同時地及/或與第二氣相反應物同時地將還原劑引入至反應室中並接觸基板。舉例來說，還原劑及第一氣相反應物可共同流入至反應室中並同時地接觸基板，且/或還原劑及第二氣相反應物可共同流入至反應室中並同時地接觸基板。
在一些實施例中，含金屬材料及/或金屬間化合物之生長速率為從約0.005 Å/循環至約5 Å/循環、從約0.01 Å/循環至約2.0 Å/循環。在一些實施例中，含金屬材料及/或金屬間化合物之生長速率大於約0.05 Å/循環、大於約0.1 Å/循環、大於約0.15 Å/循環、大於約0.20 Å/循環、大於約0.25 Å/循環或大於約0.3 Å/循環。在一些實施例中，含金屬材料及/或金屬間化合物之生長速率係小於約2.0 Å/循環、小於約1.0 Å/循環、小於約0.75 Å/循環、小於約0.5 Å/循環或小於約0.2 Å/循環。在本發明的一些實施例中，含金屬材料及/或金屬間化合物之生長速率可為大約0.4 Å/循環或約0.9 Å/循環。舉具體範例而言，當使用NiCl
2(TMPDA)作為第一氣相反應物時，在Co
3Sn
2的情況中，觀察到在約170-200 °C之沉積溫度下範圍在約0.7及1.3Å/循環之間的生長速率，而在Ni
3Sn
2的情況中，觀察到在約160 °C下約1.3Å/循環之生長速率。在Ni
xGe
y膜的情況中，當使用NiCl
2(TMPDA)作為第一氣相反應物時，在約157-200 °C之沉積溫度下生長速率在約0.18及1.3Å/循環的範圍之間。
圖3繪示包含基板302及一層或膜304的結構300。結構300可以是或包含已部分製造的裝置結構。如上所提及，基板302可包含塊體材料，諸如塊體半導體材料，及形成於其上及/或其中的層。膜302可包含金屬間化合物或含金屬材料，諸如根據本文中所述之實施例所沉積的金屬間化合物或含金屬材料。在一些實施例中，膜304可以在低於約100奈米、低於約60奈米、低於約50奈米、低於約40奈米、低於約30奈米、低於約25奈米、低於約20奈米、於約15奈米、低於約10奈米、低於約5奈米或更低的厚度下成連續的。本文所提及之連續性可以是實體連續性或電連續性。在一些實施例中，膜304為實體連續時的厚度可能不同於膜為電連續時的厚度，並且膜304為電連續時的厚度可能不同於膜為實體連續時的厚度。
在一些實施例中，根據本文所述之一些實施例所沉積的金屬間及/或含金屬膜（例如膜304）可以具有從約20奈米至約100奈米的厚度。在一些實施例中，根據本文所述之一些實施例所沉積的金屬間及/或含金屬膜可以具有從約20奈米至約60奈米之厚度。在一些實施例中，根據本文所述之一些實施例所沉積的金屬間及/或含金屬膜可以具有大於約20奈米、大於約30奈米、大於約40奈米、大於約50奈米、大於約60奈米、大於約100奈米、大於約250奈米或大於約500奈米之厚度。在一些實施例中，根據本文所述之一些實施例所沉積的金屬間及/或含金屬膜可以具有小於約50奈米、小於約30奈米、小於約20奈米、小於約15奈米、小於約10奈米、小於約5奈米、小於約3奈米、小於約2奈米或甚至小於約1奈米之厚度。
在本發明之一些實施例中，金屬間及/或含金屬膜可以沉積在三維結構(例如，包括高高寬比特徵之非平面基板)上。在一些實施例中，在具有大於約2、大於約5、大於約10、大於約25、大於約50或甚至大於約100的高寬比(高度/寬度)之結構中，金屬間及/或含金屬膜之階梯覆蓋率(step coverage)可以等於或大於約50%、大於約80%、大於約90%、大於約95%、大於約98%或大於約99%或更大。
金屬間及/或含金屬材料或其相應的膜包括本文中所述的第一金屬及第二金屬。舉具體範例而言，第一金屬可包含Ni、Co、Pt或本文中所提及的任何其他第一金屬，且第二金屬可包含Ge、Ga、In、Sn、As、Sb、Pb及Bi(例如，Ge、Ga、In、Sn)，或本文中所提及的任何其他第二金屬，包含Al。在一些情況中，第一金屬不包含Al。示範金屬間及/或含金屬化合物包含（六角形）Co
3Sn
2或Ni
3Sn
2及非晶質或晶質Ni
xGe
y，諸如（例如，斜方）Ni
2Ge、（例如，單斜）Ni
5Ge
3、N
19Ge
12及/或NiGe。金屬間及/或含金屬化合物亦可具有其他化學計量或其他晶體結構，其可藉由例如熱處理或藉由調諧沉積條件而獲得。其他示範金屬間及/或含金屬材料包括n-Sb、Pt-In、Pt-Sn、Pt-Ir、Pd-Pt、Ru-Pt、Ru、Co、Co-W、Ru-Mn、Cu-Mn及Co-Pt的化合物。示範金屬間及/或含金屬材料之其他具體範例包含Ni、Co、Cu及/或Pt和Ge、Ga、In、Sn、As、Sb、Pb、Al及Bi之一或多者。在一些情況中，包含金屬間及/或含金屬材料的膜不包含Al、Ga及/或In和過渡金屬。
在本發明的一些實施例中金屬間及/或含金屬材料及/或包含上述之膜，如本文中所述，可包括少於約5原子％氧、少於約2原子％氧、少於約1原子％氧或少於約0.5原子％氧。在其他實施例中，化合物、材料或膜可包括少於約5原子%氫、少於約2原子%氫、少於約1原子%氫或甚至少於約0.5原子%氫。在又其他實施例中，化合物、材料或膜可包含少於約5原子%碳、少於約2原子%碳、少於約1原子%碳或甚至少於約0.5原子%碳。在再其他實施例中，化合物、材料或膜可包含少於約5原子%鹵化物物種、少於約2原子%鹵化物物種、少於約1原子%鹵化物物種、少於約0.5原子%鹵化物物種或甚至少於約0.1原子%鹵化物物種。此外，物種（非所要的金屬之物種）之總污染可少於約5原子%物種、少於約2原子%物種或少於約1原子%物種。在一些實施例中，可利用飛行時間彈性回彈檢測分析（ToF-ERDA）來確定金屬間化合物、含金屬材料及包含上述之膜的原子%組成。
能夠用來沉積含金屬膜的反應器可用來形成本文中所述的金屬間化合物、含金屬材料及膜。這樣的反應器包含ALD反應器，還有配備有用以提供反應物之適當設備及手段的CVD反應器。根據一些實施例，可使用熱壁交叉流動式反應器。根據一些實施例，可以使用其他交叉流動式、批次式、小型批次式或空間式ALD反應器。
可使用之合適反應器的實例包含市售單基板(或單晶圓)沉積設備，諸如可購自美國亞利桑那州（Arizona）菲尼克斯（Phoenix）之ASM America,Inc.及荷蘭阿爾梅勒（Almere）之ASM Europe B.V.之Pulsar®反應器(諸如Pulsar® 2000及Pulsar® 3000及Pulsar® XP ALD)以及EmerALD® XP及EmerALD® 反應器。其他市售反應器包括來自ASM Japan K.K(日本東京)商品名為Eagle® XP 及XP8之彼等反應器。在一些實施例中，反應器為空間式ALD反應器，其中基板在加工期間移動或旋轉。
在本發明之一些實施例中，可使用批次式反應器。合適批次式反應器包括(但不限於)購自ASM Europe B.V (荷蘭阿爾梅勒)之商品名為A400及A412 PLUS的Advance® 400系列反應器。在一些實施例中，晶圓在處理期間旋轉。在其他實施例中，批次式反應器包括構造成容納10或更少基板（例如，半導體晶圓）、8或更少基板、6或更少基板、4或更少基板或2或更少基板的小型批次式反應器。在其中使用批次式反應器的一些實施例中，晶圓間之不均勻度係小於3% (1σ)、小於2%、小於1%或甚至小於0.5%。
本文所述之沉積製程可以視情況在連接至集束型製程設備(cluster tool)的反應器或反應室中進行。在集束型製程設備中，因為每個反應室專用於一種類型的製程，所以每個模組中之反應室的溫度可維持恆定，其相較於在每次運轉前將基板加熱至製程溫度的反應器可改善生產量。此外，在集束型製程設備中，可減少將反應室泵至基板間所要的製程壓力位準之時間。在本發明之一些實施例中，沉積製程可以在包括有多個反應室之集束型製程設備中進行，其中可以使用每個個別反應室，以使基板暴露於個別的前驅物氣體，並且基板可以在不同的反應室之間輸送，以便暴露於多種前驅物氣體，基板的輸送係在受控環境下進行，以防止基板的氧化/污染。在本發明之一些實施例中，沉積製程可以在包括多個反應室之集束型製程設備中進行，其中每個個別反應室可以構造成將基板加熱至不同的沉積溫度。
獨立式反應器可配備有裝載鎖定部(load-lock)。在那個情況下，在每次運轉之間沒有必要冷卻反應空間。
圖5繪示根據本發明之至少一實施例之反應器系統500。反應器系統500可用來，例如，執行本文中所述的循環沉積（例如ALD）方法及/或形成本文中所述的膜、化合物及/或材料。
在所繪示之範例中，反應器系統500包括可選之基板處置系統502、反應室504、氣體分佈系統506及設置於反應室504與基板處置系統502之間之可選的壁508。系統500亦可包含第一氣相反應物源512、第二氣相反應物源514及排氣源510。雖然繪有兩個氣體源512、514，但反應器系統500可包含任何適宜數目的反應物氣體源。舉例來說，示範反應器系統可包含至少兩個反應物氣體來源（例如，包含變成第一或第二氣相反應物的化合物之來源）和可選地一或多個載氣及/或清除氣體來源516。反應器系統500亦包含在處理期間保持一或多個基板520的基座518。
反應器系統500可包含任何適宜數目的反應室104及基板處置系統502。舉例來說，反應器系統500之反應室504包括交叉流熱壁磊晶反應室。包含水平流動反應器之一示範反應器系統可得自ASM之系統。
應注意到圖5為反應器系統500的簡化示意版本，且不含有每一個元件，諸如，但不限於，可用於反應器系統500中的閥、電連結、質量流控制器、密封件及氣體導管。
在本發明的一些實施例中，一或多個反應器來源容器522、524與反應室504經過導管或其他適當的手段526、528流體連通，且可進一步耦合至設置在反應器來源容器522、524與反應室504之間的氣體分佈系統506。氣體分佈系統506可包含，例如，歧管、閥控制系統、質量流控制系統及/或控制源自反應物來源容器522或524的氣態反應物之其他機制。反應物來源容器522、524可夠造成儲存含金屬化合物（例如金屬有機化合物或有機金屬化合物），其分別為或其在加熱後分別變成第一氣相反應物及第二氣相反應物。在一些實施例中，反應物來源容器522、524可包括石英材料，其可對除存在來源容器522、524內之個別的第一及第二反應物為實質上化學惰性。在本發明的替代實施例中，反應物來源容器522、524由抗腐蝕金屬或合金製造而成，諸如，例如，哈氏合金（Hastelloy）、蒙耐合金（Monel）或其組合。
在本發明一些實施例中，反應物來源容器522、524可進一步包括一或多個加熱單元526、528，其構造成將儲存在反應物來源容器522、524中的化合物加熱到所要的溫度。在一些實施例中，該一或多個加熱單元可用來將化合物加熱到大約大於0°C、大約大於20°C、大約大於100°C、大約大於150°C、大約大於200°C、大約大於200°C、大約大於300°C或甚至大約大於400°C的溫度。在一些實施例中，一或多個加熱單元526、528可構造成將儲存在反應物來源容器522、524中的化合物加熱到大約25°C至大約200°C、大約25°C至大約300°C或大約25°C至大約400°C的溫度。舉具體範例來說，當氣相反應物包含Bu
3SnH或Bu
3GeH時，溫度可在從約20°C至約40°C的範圍之間或約30°C；當反應物包含CoCl
2(TMEDA)時，溫度可在從約150°C至約190°C的範圍之間或約170°C；當反應物包含NiCl
2(TMPDA)時，溫度可在從約140°C至約180°C的範圍之間或約157°C；且當反應物包含Ni(dmap)
2時，溫度可在從約50°C至約70°C的範圍之間或約62°C。
在一些實施例中，與反應物來源容器522、524關聯的一或多個加熱單元526、528構造成將化合物從固體轉換成液體或氣體，以形成第一氣相反應物或第二氣相反應物。在一些實施例中，分別與反應物來源容器522、524關聯的一或多個加熱單元526、528可用來控制儲存在反應物來源容器522、524中之反應物的粘性。在一些實施例中，與反應物來源容器522、524關聯的一或多個加熱單元526、528可構造成控制由儲存在反應物來源容器522、524中之反應物所產生的蒸氣壓。在本發明的一些實施例中，化合物可在大於25°C、大於50°C或甚至大於100°C的溫度具有大於0.01 mbar的蒸氣壓。在本發明的一些實施例中，化合物可在小於350°C、小於250°C、小於200°C或甚至小於150°C的溫度具有大於0.01 mbar的蒸氣壓。在本發明的一些實施例中，化合物可在大於25°C或甚至大於100°C的溫度具有大於0.1 mbar的蒸氣壓。在本發明的一些實施例中，化合物可在小於400°C、小於200°C或甚至小於100°C的溫度具有大於0.1 mbar的蒸氣壓。在本發明的一些實施例中，化合物可在大於25°C或甚至大於100°C的溫度具有大於1 mbar的蒸氣壓。例如，可將化合物加熱到大於150°C的溫度，產生大於0.001 mbar的蒸氣壓。
在本發明的一些實施例中，蒸氣通道530可連接到反應物來源容器522（及/或反應物來源容器524），使一或多個載氣（例如，來自來源516或另一個來源）可從載氣儲存容器經由蒸氣通道530輸送到反應物來源容器522。在一些實施例中，質量流控制器（未圖示）可放置在蒸氣通道530上並設置在反應物來源容器522附近。例如，質量流控制器可校準成控制進入反應物來源容器522之載氣的質量流量，藉此得以更好的控制從反應物來源容器522出來進到反應室504之反應物蒸氣的後續的流動。
在一些實施例中，載氣（例如，氫、氮、氦、氬或其任何混合物）可流過化合物的一暴露表面，藉此從化合物中提取一部分蒸氣，並連同載氣一起輸送化合物（現在是第一或第二氣相反應物）到反應室504。在本發明的替代實施例中，可使載氣「起泡」通過化合物，例如藉由可選的蒸氣通道（未圖示），藉此攪拌並提取一部分含金屬化合物，並經由氣體導管526輸送含金屬化合物蒸氣（現在是第一或第二氣相反應物）到反應室504。
在本發明的一些實施例中，反應器系統500亦可包括提供電子電路及機械組件以選擇性地操作閥、歧管、泵及與反應器系統500關聯之其他設備的系統操作及控制機構532。這種電路和化合物操作以從各個反應物來源容器522、524及清除氣體容器534引入反應物、清除氣體及/或載氣。系統操作及控制機構532亦可控制氣體脈衝順序之時間安排、基板及/或反應室之溫度及反應室之壓力和提供反應器系統500之恰當操作所必需之各種其他操作。操作及控制機構532可包含控制軟體及電力式或氣動式控制閥，以控制反應物、載氣及/或清除氣體進入及離開反應室504之流動。操作及控制機構532可包含執行特定任務之模組，諸如，軟體及/或硬體組件(例如，FPGA或ASIC)。模組可以有利地構造成存在於系統操作及控制機構532的可定址儲存媒體上且構造成用於執行一或多個程序。
可以有反應器系統的各種其他構造，包含不同數量及種類的反應物來源及清除氣體來源。再者，可以有可用於實現將氣體選擇性地饋送至反應室504中之目標的閥、導管、反應物來源、清除氣體來源之多種配置。
範例
下列範例闡述根據本發明之示範實施例的特定製程、膜及結構。這些範例為例示性且並非意圖限制本發明之範疇。
1. 一種用於沉積金屬間化合物的循環沉積製程，該循環沉積方法包括下列步驟：
提供包括第一金屬的第一氣相反應物至反應室以與基板的表面反應而形成第一金屬物種；以及
提供包括第二金屬之第二氣相反應物至反應室以與該第一金屬物種反應，藉此形金屬間化合物。
2. 如範例1的循環沉積製程，進一步包括重複提供第一氣相反應物及提供第二氣相反應物之步驟直到達到所要膜厚度為止。
3. 如範例1的循環沉積製程，進一步包括一或多個清除步驟，其中清除步驟的至少一者在提供第一氣相反應物的步驟之後以及在提供第二氣相反應物的步驟之前發生。
4. 如範例1的循環沉積製程，其中循環沉積製程包括原子層沉積製程。
5. 如範例1的循環沉積製程，其中循環沉積製程包括循環化學氣相沉積製程。
6. 如範例1的循環沉積製程，其中在提供第一氣相反應物及提供第二氣相反應物的步驟期間反應室內的溫度為大於0°C及小於600°C、小於500°C、小於400°C、小於300°C或小於250°C，或在約20°C至約700°C之間、在約50°C至約500°C之間，或在約50°C至約400°C之間、在約75°C至約300°C之間或在約100°C至約250°C之間。
7. 如範例1的循環沉積製程，其中第二氣相反應物包括含金屬有機化合物。
8. 如範例1的循環沉積製程，其中第二氣相反應物選自由具有R-M-H之通式的化合物組成之群組，其中R為有機基而M為金屬。
9. 如範例1的循環沉積製程，其中第二金屬選自由Ge、Ga、In、Sn、Al、As、Sb、Pb及Bi所組成之群組。
10. 如範例1的循環沉積製程，其中第二金屬選自由Ge、Ga、In及Sn所組成之群組。
11. 如範例1的循環沉積製程，其中第二金屬包括Ge。
12. 如範例1的循環沉積製程，其中第二金屬包括Ga。
13. 如範例1的循環沉積製程，其中第二金屬包括In。
14. 如範例8的循環沉積製程，其中由具有R-M-H之通式的化合物組成的群組具有R
(X-n)-M
X-H
n之式子，其中X為金屬的正式氧化態而n為1至5。
15. 如範例8及14的任何者之循環沉積製程，其中R包括烷基或其他有機基。
16. 如範例8及14的任何者之循環沉積製程，其中R獨立地選自由C1-C10烷基所組成之群組。
17. 如範例8及14的任何者之循環沉積製程，其中R為有或沒有額外的予體官能基之環戊二烯基、醯胺基、烷氧基、脒基（amidinato）、胍基（guanidinato）、亞胺基（imido）、羧根基、β-二酮基（β-diketonato）、β-酮亞胺基（β-ketoiminato）、丙二酸、β-二酮亞胺基（β-diketiminato）。
18. 如範例1之循環沉積製程，其中第二氣相反應物包含金屬還原劑。
19. 如範例1之循環沉積製程，其中第一金屬選自由IUPAC第13-15族金屬所組成之群組。
20. 如範例1之循環沉積製程，其中第一金屬選自由第3-6族金屬所組成之群組。
21. 如範例1之循環沉積製程，其中第一金屬選自由第7-12族金屬所組成之群組。
22. 如範例1之循環沉積製程，其中第一金屬選自由鑭系元素所組成之群組。
23. 如範例1之循環沉積製程，其中第一金屬選自由第8-11族金屬所組成之群組。
24. 如範例1之循環沉積製程，其中第一金屬選自由第13-15族金屬所組成之群組。
25. 如範例1之循環沉積製程，其中第一氣相反應物選自由金屬鹵化物所組成之群組。
26. 如範例1之循環沉積製程，其中第一氣相反應物包括M(dmap)
x（dmap＝二甲基胺基-2-丙醇），其中M為金屬。
27. 如範例1之循環沉積製程，其中第一氣相反應物選自由金屬氫化物所組成之群組。
28. 如範例1之循環沉積製程，其中第一氣相反應物包括一相應金屬鹵化物的二胺加成物。
29. 如範例1之循環沉積製程，其中第一氣相反應物包括金屬鹵化物化合物，其包括含雙牙氮的加成物配位子。
30. 如範例29之循環沉積製程，其中加成物配位子包含兩個氮原子，且其中氮原子之各者與至少一個碳原子鍵合。
31. 如範例1之循環沉積製程，其中第一氣相反應物包括氯化鈷（TMEDA）和氯化鎳（TMPDA）的至少一者。
32. 如範例1之循環沉積製程，其中第二氣相反應物包括TBTH及TBGH的一之多者。
33. 如範例1之循環沉積製程，其中金屬間化合物不包含Al、Ga及/或In和過渡金屬。
34. 一種用於形成含金屬材料之循環沉積製程，該循環沉積製程包括：
提供包括第一金屬的第一氣相前驅物至反應室以形成第一金屬物種；以及
提供包括具有R-M-H之通式的化合物之第二氣相反應物，其中R為有機基而M為金屬，以與第一金屬物種反應，藉此形成含金屬材料。
35. 如範例34之循環沉積製程，其中第一金屬與第二金屬相同。
36. 如範例34之循環沉積製程，其中含金屬材料包括元素金屬。
37. 如範例1或34之循環沉積製程，其中含金屬材料包括例如In及Ge或其他第一及/或第二金屬的混合物。
38. 如範例34之循環沉積製程，進一步包括重複提供第一氣相反應物及提供第二氣相反應物之步驟直到達到所要膜厚度為止。
39. 如範例34之循環沉積製程，進一步包括一或多個清除步驟，其中清除步驟的至少一者在提供第一氣相反應物的步驟之後以及在提供第二氣相反應物的步驟之前發生。
40. 如範例34之循環沉積製程，其中循環沉積製程包括原子層沉積。
41. 如範例34之循環沉積製程，其中循環沉積製程包括循環化學氣相沉積。
42. 如範例34之循環沉積製程，其中在提供第一氣相反應物及提供第二氣相反應物的步驟期間反應室內的溫度為大於0°C及小於600°C、小於500°C、小於400°C、小於300°C或小於250°C，或在約20°C至約700°C之間、在約50°C至約500°C之間，或在約50°C至約400°C之間、在約75°C至約300°C之間或在約100°C至約250°C之間。
43. 如範例34之循環沉積製程，其中第二金屬選自由Ge、Ga、In、Sn、Al、As、Sb、Pb及Bi所組成之群組。
44. 如範例34的循環沉積製程，其中第二金屬選自由Ge、Ga、In及Sn所組成之群組。
45. 如範例34的循環沉積製程，其中第二金屬包括Ge。
46. 如範例34的循環沉積製程，其中第二金屬包括In。
47. 如範例34的循環沉積製程，其中第二金屬包括Ga。
48. 如範例34的循環沉積製程，其中含金屬材料包括元素金屬、金屬混合物、合金及金屬間化合物之一或多者。
49. 如範例34的循環沉積製程，其中含金屬材料為金屬型、導電型、非導電型、半導電型、超導型、催化型、鐵磁型和磁阻型之一或多者。
50. 如範例34的循環沉積製程，其中具有R-M-H之通式的化合物具有R
(X-n)-M
X-H
n之式子，其中X為金屬的正式氧化態而n為1至5。
51. 如範例34的任何者之循環沉積製程，其中R包括烷基或其他有機基。
52. 如範例34之循環沉積製程，其中R獨立地選自由C1-C10烷基所組成之群組。
53. 如範例34-52的任何者之循環沉積製程，其中R為有或沒有額外的予體官能基之環戊二烯基、醯胺基、烷氧基、脒基、胍基、亞胺基、羧根基、β-二酮基、β-酮亞胺基、丙二酸、β-二酮亞胺基。
54. 如範例34之循環沉積製程，其中第二氣相反應物包含金屬還原劑。
55. 如範例34之循環沉積製程，其中第一金屬選自由IUPAC第13-15族金屬所組成之群組。
56. 如範例34之循環沉積製程，其中第一金屬選自由第3-6族金屬所組成之群組。
57. 如範例34之循環沉積製程，其中第一金屬選自由第7-12族金屬所組成之群組。
58. 如範例34之循環沉積製程，其中第一金屬選自由鑭系元素所組成之群組。
59. 如範例34之循環沉積製程，其中第一金屬選自由第8-11族金屬所組成之群組。
60. 如範例34之循環沉積製程，其中第一金屬選自由第13-15族金屬所組成之群組。
61. 如範例34之循環沉積製程，其中第一氣相反應物選自由金屬鹵化物所組成之群組。
62. 如範例34之循環沉積製程，其中第一氣相反應物包括M(dmap)
x（dmap＝二甲基胺基-2-丙醇），其中M為金屬。
63. 如範例34之循環沉積製程，其中第一氣相反應物選自由金屬氫化物所組成之群組。
64. 如範例34之循環沉積製程，其中第一氣相反應物包括一相應金屬鹵化物的二胺加成物。
65. 如範例34之循環沉積製程，其中第一氣相反應物包括金屬鹵化物化合物，其包括含雙牙氮的加成物配位子。
66. 如範例65之循環沉積製程，其中加成物配位子包含兩個氮原子，且其中氮原子之各者與至少一個碳原子鍵合。
67. 如範例34之循環沉積製程，其中第一氣相反應物包括氯化鈷（TMEDA）和氯化鎳（TMPDA）的至少一者。
68. 如範例34之循環沉積製程，其中第二氣相反應物包括TBTH及TBGH的一或多者。
69. 一種根據範例1-33的任何者之循環沉積製程所形成的膜。
70. 如範例69之膜，其中該膜為金屬型、導電型、半導電型或非導電型。
71. 如範例69之膜，其中該膜為超導型。
72. 如範例69之膜，其中該膜為磁阻型。
73. 如範例69之膜，其中該膜為鐵磁型。
74. 如範例69之膜，其中該膜為催化劑。
75. 一種根據範例34-68的任何者之循環沉積製程所形成的膜。
76. 如範例75之膜，其中該膜包括金屬混合物、合金及金屬間化合物之一或多者。
77. 一種包含根據範例69-76之一或多者之膜的裝置結構。
上述揭露內容之示範實施例並沒有限制本發明的範圍，因為這些實施例僅為本發明之實施例之範例，本發明的範圍由所附申請專利範圍及其合法等效者來界定。任何等效實施例意欲在本發明的範圍內。更確切地來說，除本文中所示及所述者之外，本發明之各種修改(諸如，所述元件之替代有用的組合)對於熟悉該項技藝者來說可根據描述而變得顯而易見。這樣的修改及實施例同樣意欲落在所附申請專利範圍之範圍內。
100:循環沉積方法
110:步驟
120:步驟
125:步驟
130:步驟
140:步驟
145:步驟
150:決定閘
160:步驟
200:循環沉積方法
210:步驟
220:步驟
225:步驟
230:步驟
240:步驟
245:步驟
250:決定閘
260:步驟
300:結構
302:基板
304:膜
500:反應器系統
502:基板處置系統
504:反應室
506:氣體分佈系統
508:壁
510:排氣源
512:第一氣相反應物源
514:第二氣相反應物源
516:清除氣體來源
518:基座
520:基板
522:反應器來源容器
524:反應器來源容器
526:導管/加熱單元
528:導管/加熱單元
530:蒸氣通道
532:系統操作及控制機構
534:清除氣體容器
在說明書結尾部分中具體指出並清楚主張本發明之標的。然而，可藉由在連同圖式考量之下參照詳細說明及申請專利範圍來最佳得到本發明之更完整了解，其中類似的標號表示類似的元件，以及其中：
［圖1］繪示根據本發明之至少一個實施例的示範循環沉積方法之流程；
［圖2］繪示根據本發明之至少一個實施例的示範循環沉積方法之另一個流程；
［圖3］繪示包含根據本發明之至少一個實施例所沉積之含金屬膜之示範裝置結構的示意圖；
［圖4］繪示在根據本發明之至少一個實施例的循環沉積製程中所使用的金屬鹵化物化合物之範例；
［圖5］繪示根據本發明之至少一個實施例的示範反應器系統的示意圖；以及
［圖6］繪示根據本發明之至少一個實施例的示範第二氣相反應物。
應理解，圖式中之元件係為簡單及清楚起見而繪示且未必按比例繪製。舉例而言，圖中一些元件的尺寸可能相對於其他元件放大以有助於改進對本發明的所示實施例的理解。
100:循環沉積方法
110:步驟
120:步驟
125:步驟
130:步驟
140:步驟
145:步驟
150:決定閘
160:步驟
Claims (18)
- 一種用於形成含金屬材料之循環沉積製程，該循環沉積製程包括： 從與一反應室流體連通的一第一氣相反應物源容器提供一第一氣相前驅物至該反應室以形成一第一金屬物種，該第一氣相前驅物包括具有下列式子的一金屬化合物：（加成物） n-M-X a，其中每個加成物為加成物形成配位子，其中M為包含第3族-第12族金屬的一第一金屬，n為1至4，X為鹵化物或其他配位子，且a為1至4；以及 提供包括具有R-M-H之通式的一化合物之一第二氣相反應物，其中R為一有機基而M為一第二金屬，以與該第一金屬物種反應，藉此形成該含金屬材料。
- 如請求項1之循環沉積製程，其中該第一金屬及該第二金屬相同。
- 如請求項1之循環沉積製程，其中該第一金屬為鈷（Co）、銅（Cu）或鎳（Ni）。
- 如請求項1之循環沉積製程，其中該第二金屬選自由Ge、Ga、In及Sn所組成之群組。
- 如請求項1之循環沉積製程，其中該第二金屬包括Ge。
- 如請求項1之循環沉積製程，其中該第二金屬包括In。
- 如請求項1之循環沉積製程，其中該第二金屬包括Ga。
- 如請求項1之循環沉積製程，其中具有R-M-H之通式的該化合物具有R (X-n)-M X-H n之式子，其中X為金屬的正式氧化態而n為1至5，且其中R包括一烷基或其他有機基。
- 如請求項1之循環沉積製程，其中R獨立選自由C1-C10烷基所組成之群組。
- 如請求項1之循環沉積製程，其中R為有或沒有額外的予體官能基之環戊二烯基、醯胺基、烷氧基、脒基、胍基、亞胺基、羧根基、β-二酮基、β-酮亞胺基、丙二酸、β-二酮亞胺基。
- 如請求項1之循環沉積製程，其中該含金屬材料包括Co 3Sn 2、Ni 3Sn 2、Ni 2Ge、Ni 5Ge 3、Ni 19Ge 12或NiGe。
- 如請求項1之循環沉積製程，其中該第一金屬選自由第8-11族金屬所組成之群組。
- 如請求項1之循環沉積製程，其中該第一金屬為一過渡金屬，且其中該些加成物形成配位子透過氮原子、磷原子、氧原子或硫原子中的至少一者與該過渡金屬配位。
- 如請求項1之循環沉積製程，其中該第二氣相反應物包括三丁基金屬氫化物。
- 如請求項1之循環沉積製程，其中該第一氣相反應物包括一金屬鹵化物化合物，其包括包含多牙氮（multidentate nitrogen）的加成物配位子。
- 如請求項15之循環沉積製程，其中該加成物配位子包含兩個氮原子，且其中氮原子之各者與至少一個碳原子鍵合。
- 如請求項1之循環沉積製程，其中該第一氣相反應物包括氯化鈷（TMEDA）和氯化鎳（TMPDA）的至少一者。
- 如請求項17之循環沉積製程，其中該第二氣相反應物包括TBTH及TBGH的一或多者。
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-
2019
- 2019-06-21 JP JP2020570520A patent/JP2021529254A/ja active Pending
- 2019-06-21 TW TW112143596A patent/TW202409324A/zh unknown
- 2019-06-21 WO PCT/IB2019/000805 patent/WO2020002995A1/en active Application Filing
- 2019-06-21 TW TW108121806A patent/TWI819010B/zh active
- 2019-06-21 US US17/254,111 patent/US11492703B2/en active Active
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- 2019-06-21 KR KR1020207035951A patent/KR20210024462A/ko not_active Application Discontinuation
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2022
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| TW202012678A (zh) | 2020-04-01 |
| KR20210024462A (ko) | 2021-03-05 |
| TWI819010B (zh) | 2023-10-21 |
| US20210317576A1 (en) | 2021-10-14 |
| JP2021529254A (ja) | 2021-10-28 |
| CN112292478A (zh) | 2021-01-29 |
| US11492703B2 (en) | 2022-11-08 |
| WO2020002995A1 (en) | 2020-01-02 |
| US11814715B2 (en) | 2023-11-14 |
| US20220389583A1 (en) | 2022-12-08 |
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