JP5814155B2 - 金属アミジナートを用いる原子層の析出 - Google Patents
金属アミジナートを用いる原子層の析出 Download PDFInfo
- Publication number
- JP5814155B2 JP5814155B2 JP2012033846A JP2012033846A JP5814155B2 JP 5814155 B2 JP5814155 B2 JP 5814155B2 JP 2012033846 A JP2012033846 A JP 2012033846A JP 2012033846 A JP2012033846 A JP 2012033846A JP 5814155 B2 JP5814155 B2 JP 5814155B2
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- JP
- Japan
- Prior art keywords
- metal
- vapor
- substrate
- amidinate
- precursor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 101
- 239000002184 metal Substances 0.000 title claims abstract description 101
- 238000000231 atomic layer deposition Methods 0.000 title description 30
- 239000000758 substrate Substances 0.000 claims abstract description 76
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000001257 hydrogen Substances 0.000 claims abstract description 22
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 22
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 15
- 150000004767 nitrides Chemical class 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 56
- 150000001875 compounds Chemical class 0.000 claims description 36
- 239000010409 thin film Substances 0.000 claims description 32
- 239000007789 gas Substances 0.000 claims description 21
- 239000010408 film Substances 0.000 claims description 17
- 125000003709 fluoroalkyl group Chemical group 0.000 claims description 7
- 125000003342 alkenyl group Chemical group 0.000 claims description 6
- 125000000304 alkynyl group Chemical group 0.000 claims description 6
- 125000004665 trialkylsilyl group Chemical group 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 150000002431 hydrogen Chemical class 0.000 claims description 5
- 229910044991 metal oxide Inorganic materials 0.000 claims description 5
- 150000004706 metal oxides Chemical class 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims 3
- 229910052733 gallium Inorganic materials 0.000 claims 3
- 229910052738 indium Inorganic materials 0.000 claims 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims 3
- 238000005121 nitriding Methods 0.000 claims 1
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 98
- 239000010949 copper Substances 0.000 abstract description 49
- 229910017052 cobalt Inorganic materials 0.000 abstract description 43
- 239000010941 cobalt Substances 0.000 abstract description 43
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract description 39
- 229910052802 copper Inorganic materials 0.000 abstract description 38
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 36
- 238000006243 chemical reaction Methods 0.000 abstract description 26
- VMQMZMRVKUZKQL-UHFFFAOYSA-N Cu+ Chemical compound [Cu+] VMQMZMRVKUZKQL-UHFFFAOYSA-N 0.000 abstract description 7
- 150000002739 metals Chemical class 0.000 abstract description 7
- 238000004377 microelectronic Methods 0.000 abstract description 5
- 229910021529 ammonia Inorganic materials 0.000 abstract description 4
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 abstract description 3
- 238000003860 storage Methods 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 description 64
- 238000000151 deposition Methods 0.000 description 50
- 239000010410 layer Substances 0.000 description 40
- 230000008021 deposition Effects 0.000 description 39
- 239000000376 reactant Substances 0.000 description 31
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 25
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 24
- 238000000859 sublimation Methods 0.000 description 21
- 230000008022 sublimation Effects 0.000 description 21
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 20
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 18
- 239000000243 solution Substances 0.000 description 18
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 16
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical group [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 16
- 230000008018 melting Effects 0.000 description 16
- 238000002844 melting Methods 0.000 description 16
- 239000007787 solid Substances 0.000 description 16
- 239000012159 carrier gas Substances 0.000 description 15
- 239000007788 liquid Substances 0.000 description 15
- 239000011148 porous material Substances 0.000 description 15
- 229910052746 lanthanum Inorganic materials 0.000 description 13
- 239000007983 Tris buffer Substances 0.000 description 12
- 125000000217 alkyl group Chemical group 0.000 description 12
- 230000015572 biosynthetic process Effects 0.000 description 12
- 239000013078 crystal Substances 0.000 description 12
- -1 iron metals Chemical class 0.000 description 12
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 12
- 238000003786 synthesis reaction Methods 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 11
- 239000000203 mixture Substances 0.000 description 11
- 239000012691 Cu precursor Substances 0.000 description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 10
- 125000004429 atom Chemical group 0.000 description 10
- 239000000539 dimer Substances 0.000 description 10
- 229910052742 iron Inorganic materials 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- 229910052710 silicon Inorganic materials 0.000 description 10
- 239000010703 silicon Substances 0.000 description 10
- 239000010936 titanium Substances 0.000 description 10
- 150000001409 amidines Chemical class 0.000 description 9
- 230000008901 benefit Effects 0.000 description 9
- 238000001704 evaporation Methods 0.000 description 9
- 239000011572 manganese Substances 0.000 description 9
- 229910052759 nickel Inorganic materials 0.000 description 9
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 9
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 8
- 230000008020 evaporation Effects 0.000 description 8
- 229910052744 lithium Inorganic materials 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 6
- 239000000178 monomer Substances 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 229910052707 ruthenium Inorganic materials 0.000 description 6
- 238000006557 surface reaction Methods 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- BDNKZNFMNDZQMI-UHFFFAOYSA-N 1,3-diisopropylcarbodiimide Chemical compound CC(C)N=C=NC(C)C BDNKZNFMNDZQMI-UHFFFAOYSA-N 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 239000002035 hexane extract Substances 0.000 description 5
- 239000011777 magnesium Substances 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- 239000011541 reaction mixture Substances 0.000 description 5
- 239000013638 trimer Substances 0.000 description 5
- 229910052720 vanadium Inorganic materials 0.000 description 5
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 4
- 239000012692 Fe precursor Substances 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- 230000004888 barrier function Effects 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 4
- 229910052804 chromium Inorganic materials 0.000 description 4
- 239000011651 chromium Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- 239000012705 liquid precursor Substances 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- DVSDBMFJEQPWNO-UHFFFAOYSA-N methyllithium Chemical compound C[Li] DVSDBMFJEQPWNO-UHFFFAOYSA-N 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- 238000005001 rutherford backscattering spectroscopy Methods 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 239000011343 solid material Substances 0.000 description 4
- WJKHJLXJJJATHN-UHFFFAOYSA-N triflic anhydride Chemical compound FC(F)(F)S(=O)(=O)OS(=O)(=O)C(F)(F)F WJKHJLXJJJATHN-UHFFFAOYSA-N 0.000 description 4
- MONVAZUNBHXPRN-UHFFFAOYSA-N 3-methylpentanimidamide Chemical compound CCC(C)CC(N)=N MONVAZUNBHXPRN-UHFFFAOYSA-N 0.000 description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 150000001408 amides Chemical class 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 3
- 150000001718 carbodiimides Chemical class 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 150000001868 cobalt Chemical class 0.000 description 3
- 229910000428 cobalt oxide Inorganic materials 0.000 description 3
- BKFAZDGHFACXKY-UHFFFAOYSA-N cobalt(II) bis(acetylacetonate) Chemical compound [Co+2].CC(=O)[CH-]C(C)=O.CC(=O)[CH-]C(C)=O BKFAZDGHFACXKY-UHFFFAOYSA-N 0.000 description 3
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical group [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000006870 function Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- WGJJZRVGLPOKQT-UHFFFAOYSA-K lanthanum(3+);trifluoromethanesulfonate Chemical compound [La+3].[O-]S(=O)(=O)C(F)(F)F.[O-]S(=O)(=O)C(F)(F)F.[O-]S(=O)(=O)C(F)(F)F WGJJZRVGLPOKQT-UHFFFAOYSA-K 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [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 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052758 niobium Inorganic materials 0.000 description 3
- 239000010955 niobium Substances 0.000 description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 229910052715 tantalum Inorganic materials 0.000 description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- 238000009834 vaporization Methods 0.000 description 3
- 230000008016 vaporization Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 description 2
- 239000005749 Copper compound Substances 0.000 description 2
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 2
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 2
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical group CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 description 2
- 229910052777 Praseodymium Inorganic materials 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000012790 adhesive layer Substances 0.000 description 2
- 239000003570 air Substances 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 229910000416 bismuth oxide Inorganic materials 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 150000001869 cobalt compounds Chemical class 0.000 description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 150000001880 copper compounds Chemical class 0.000 description 2
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- 238000002716 delivery method Methods 0.000 description 2
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 239000005350 fused silica glass Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 150000007975 iminium salts Chemical class 0.000 description 2
- 229910052741 iridium Inorganic materials 0.000 description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-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
- 150000002604 lanthanum compounds Chemical class 0.000 description 2
- CZMAIROVPAYCMU-UHFFFAOYSA-N lanthanum(3+) Chemical compound [La+3] CZMAIROVPAYCMU-UHFFFAOYSA-N 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- VASIZKWUTCETSD-UHFFFAOYSA-N manganese(II) oxide Inorganic materials [Mn]=O VASIZKWUTCETSD-UHFFFAOYSA-N 0.000 description 2
- 150000002736 metal compounds Chemical class 0.000 description 2
- 229910001507 metal halide Inorganic materials 0.000 description 2
- 150000005309 metal halides Chemical class 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- IDVWLLCLTVBSCS-UHFFFAOYSA-N n,n'-ditert-butylmethanediimine Chemical compound CC(C)(C)N=C=NC(C)(C)C IDVWLLCLTVBSCS-UHFFFAOYSA-N 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- BHRZNVHARXXAHW-UHFFFAOYSA-N sec-butylamine Chemical compound CCC(C)N BHRZNVHARXXAHW-UHFFFAOYSA-N 0.000 description 2
- 125000005353 silylalkyl group Chemical group 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical compound CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 description 2
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 2
- 239000003039 volatile agent Substances 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000283153 Cetacea Species 0.000 description 1
- 229910021589 Copper(I) bromide Inorganic materials 0.000 description 1
- 229910020676 Co—N Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 101100007427 Manduca sexta COVA gene Proteins 0.000 description 1
- 101100386623 Mus musculus Amd2 gene Proteins 0.000 description 1
- 101100496858 Mus musculus Colec12 gene Proteins 0.000 description 1
- 229910014291 N—Cu Inorganic materials 0.000 description 1
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- FKFRDPYOIGLUHT-UHFFFAOYSA-N [Co+]C Chemical compound [Co+]C FKFRDPYOIGLUHT-UHFFFAOYSA-N 0.000 description 1
- 230000001464 adherent effect Effects 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 125000005210 alkyl ammonium group Chemical group 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000012080 ambient air Substances 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000003877 atomic layer epitaxy Methods 0.000 description 1
- QCLQZCOGUCNIOC-UHFFFAOYSA-N azanylidynelanthanum Chemical compound [La]#N QCLQZCOGUCNIOC-UHFFFAOYSA-N 0.000 description 1
- IVHJCRXBQPGLOV-UHFFFAOYSA-N azanylidynetungsten Chemical compound [W]#N IVHJCRXBQPGLOV-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 description 1
- ODWXUNBKCRECNW-UHFFFAOYSA-M bromocopper(1+) Chemical compound Br[Cu+] ODWXUNBKCRECNW-UHFFFAOYSA-M 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
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 150000008280 chlorinated hydrocarbons Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- 239000013058 crude material Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000004508 fractional distillation Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 229910021397 glassy carbon Inorganic materials 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
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- IGHXQFUXKMLEAW-UHFFFAOYSA-N iron(2+) oxygen(2-) Chemical compound [O-2].[Fe+2].[Fe+2].[O-2] IGHXQFUXKMLEAW-UHFFFAOYSA-N 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- QPRFPZGRQQKMEX-UHFFFAOYSA-N lanthanum(2+) Chemical compound [La+2] QPRFPZGRQQKMEX-UHFFFAOYSA-N 0.000 description 1
- UBJFKNSINUCEAL-UHFFFAOYSA-N lithium;2-methylpropane Chemical compound [Li+].C[C-](C)C UBJFKNSINUCEAL-UHFFFAOYSA-N 0.000 description 1
- QWDJLDTYWNBUKE-UHFFFAOYSA-L magnesium bicarbonate Chemical compound [Mg+2].OC([O-])=O.OC([O-])=O QWDJLDTYWNBUKE-UHFFFAOYSA-L 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- OZOAXHQNOFIFGD-UHFFFAOYSA-N manganese(2+) oxygen(2-) Chemical compound [O-2].[O-2].[Mn+2].[Mn+2] OZOAXHQNOFIFGD-UHFFFAOYSA-N 0.000 description 1
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical compound [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000015654 memory Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- AUHZEENZYGFFBQ-UHFFFAOYSA-N mesitylene Substances CC1=CC(C)=CC(C)=C1 AUHZEENZYGFFBQ-UHFFFAOYSA-N 0.000 description 1
- 125000001827 mesitylenyl group Chemical group [H]C1=C(C(*)=C(C([H])=C1C([H])([H])[H])C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 150000004681 metal hydrides Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 238000002663 nebulization Methods 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 238000001953 recrystallisation Methods 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
- 150000003839 salts Chemical class 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- ITMCEJHCFYSIIV-UHFFFAOYSA-M triflate Chemical compound [O-]S(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-M 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000002424 x-ray crystallography Methods 0.000 description 1
- 239000008096 xylene Substances 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
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- 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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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
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-
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C257/00—Compounds containing carboxyl groups, the doubly-bound oxygen atom of a carboxyl group being replaced by a doubly-bound nitrogen atom, this nitrogen atom not being further bound to an oxygen atom, e.g. imino-ethers, amidines
- C07C257/10—Compounds containing carboxyl groups, the doubly-bound oxygen atom of a carboxyl group being replaced by a doubly-bound nitrogen atom, this nitrogen atom not being further bound to an oxygen atom, e.g. imino-ethers, amidines with replacement of the other oxygen atom of the carboxyl group by nitrogen atoms, e.g. amidines
- C07C257/14—Compounds containing carboxyl groups, the doubly-bound oxygen atom of a carboxyl group being replaced by a doubly-bound nitrogen atom, this nitrogen atom not being further bound to an oxygen atom, e.g. imino-ethers, amidines with replacement of the other oxygen atom of the carboxyl group by nitrogen atoms, e.g. amidines having carbon atoms of amidino groups bound to acyclic carbon atoms
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- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F19/00—Metal compounds according to more than one of main groups C07F1/00 - C07F17/00
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- 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
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/403—Oxides of aluminium, magnesium or beryllium
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/406—Oxides of iron group metals
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- 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]
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45553—Atomic layer deposition [ALD] characterized by the use of precursors specially adapted for ALD
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Description
n=(Peq−Pdep)(V/RT1)
に従うということを仮定して概算できる。式中、Rは、気体定数である。また、この数式は、チューブ90からのキャリアガスは、バルブ70が開放されて先駆物質蒸気が解放される短い時間中には、当該バルブを通してチェンバー60に入らないということを仮定している。仮に、バルブ70が開放されている時間中に、キャリアガスと先駆物質の蒸気との混合が起こるとすると、そのときは、多量の先駆物質蒸気の投与量が最大値:
n=(Peq)(V/RT1)
となるまで送出されてしまう。仮に、チェンバー60内の残留先駆物質の蒸気の全てがキャリアガスと置換されてしまうとすると、比較的高い蒸気圧(Pew>>Pdep)をもつ先駆物質の場合には、これら二つの先駆体物質量の投与量の概算値には、通常、大きな差異はない。
n=(Peq/Ptot)(Ptot−Pdep)(V/RT1’)
から推定することができる。式中、Vは、チェンバー11内の蒸気空間31の容積であり、そしてT1’は、オーブン41によって保持される温度である。オーブン81は、凝縮を避けるため、T1’より十分高い温度T2’に維持されている。仮に、チューブ91からのキャリアガスが、バルブ71の開放中に当該容積に入り込むと、そのときは、この推定値よりも幾分多い一回分の投与量が送出されることとなる。当該容積Vを十分に大きくすることによって、表面反応を最大値まで進めるに足るような、確実に多量な先駆物質の一回分の投与量が送出されてもよい。仮に、蒸気圧Peqが低いため、所要の容積Vが実行不能な程度に成る程大きくなるならば、そのときは、一回分の他の反応体の投与量を送出する前に、容積Vからの付加的な複数回分の投与量が送出されてもよい。
メチルリチウムのエーテル溶液(エーテル34mL中1.6モル、0.054モル)を、−30℃下で、100mLの1,3−ジイソプロピルカルボジイミド(6.9g、0.055モル)エーテル溶液に滴下して加えた。この混合物を室温まで暖め、4時間攪拌した。次いで、得られた無色溶液を、50mLの臭化銅(7.8g、0.054モル)溶液に添加した。この反応混合物を、光を排除した下で12時間攪拌した。次いで、減圧下で全ての揮発物を除き、得られた固体をヘキサン(100mL)で抽出した。このヘキサン抽出物をガラスフリット上のセライトパッドを通過させて濾過して、淡黄色の溶液を得た。炉液を濃縮し、それを−30℃に冷却したところ、9.5gの無色の結晶を生成物(83%)として得た。昇華:50ミリトール下で70℃。1H NMR(C6D6、25℃):1.16(d,12H)、1.65(s,3H)、3.40(m,2H)。C16H34N4Cu2の計算値:C,46.92、H,8.37、N,13.68。実測値:C,46.95、H,8.20、N,13.78。
[Cu(iPr−AMD)]2結晶を、X線結晶学によって構造決定した。図2に示す[Cu(iPr−AMD)]2は、アミジナート配位子がμ,η1:η1様に銅金属原子を橋架けしている固体状態の二量体である。その平均Cu−Nの距離は、1.860(1)Åである。Cu−N−C−N−Cuの5員環の形状は、結晶構造的に中心に対して対称である平面状である。
この化合物を、溶媒としてエーテルとTHFの1:1の混合物を用いたことを除いて、 [Cu(iPr−AMD)]2に関して記載したと同様な方法で得た。−30℃下で、ヘキサン中で再結晶したところ、暗緑色の結晶を生成物(77%)として得た。昇華:50ミリトール下で40℃。融点:72℃。C16H34N4Coの計算値:C,56.29、H,10.04、N,16.41。実測値:C,54.31、H,9.69、N,15.95。
図3に示されるCo(iPr−AMD)2は、歪んだ四面体位置におけるそれぞれのコバルト原子の近傍に配位した2個のアミジナート配位子をもつ単量体である。その平均Co−Nの距離は、2.012(8)Åである。Co−N−C−Nの4員環は、強制鏡面をもつ平面である。
この化合物を、1,3−ジイソプロピルカルボジイミドの代わりに1,3−ジ−t−ブチルカルボジイミドを用いて、実施例2における([Co(iPr−AMD)2])と同様な方法で得た。暗青色の結晶(84%)。昇華:50ミリトール下で45℃。融点:90℃。C20H42N4Coの計算値:C,60.43、H,10.65、N,14.09。実測値:C,58.86、H,10.33、N,14.28。
CoCl2の代わりにLaCl3(THF)2を用いて、[Co(iPr−AMD)2]に関して上記したと同様な手順にしたがって、灰色がかった白色の固体を、粗原料の固体材料を昇華した生成物として得た。昇華:40ミリトール下で80℃。1H NMR(C6D6、25℃):1.20(d,36H)、1.67(s,18H)、3.46(m,6H)。C24H51N6Laの計算値:C,51.24、H,9.14、N,14.94。実測値:C,51.23、H,8.22、N,14.57。
LaCl3(THF)2を用いることを除いて、[Co(iPr−AMD)2]に関して上記したと同様な手順にしたがって、灰色がかった白色固体を、粗原料の固体材料を昇華した生成物として得た。無色の結晶(80%)。昇華:50ミリトール下で120℃。融点:140℃。1H NMR(C6D6、25℃):1.33(br,21H)、4.26(m,6H)。C33H75N6Laの計算値:C,57.04、H,10.88、N,12.09。実測値:C,58.50、H,10.19、N,11.89。
FeCl2を用いたことを除いて、[Co(iPr−AMD)2]に関して上記したと同様な手順にしたがって、黄緑色の固体[Fe(iPr−AMD)2]2を、そのヘキサン抽出から溶媒を蒸発させた生成物として得た。昇華:50ミリトール下で70℃。融点:110℃。
1,3−ジイソプロピルカルボジイミドに代えて1,3−ジ−t−ブチルカルボジイミドを用いたことを除いて、[Fe(iPr−AMD)2]2に関して上記したと同様な手順にしたがって、白色の結晶(77%)を得た。昇華:60ミリトール下で55℃。融点:107℃。C20H42N4Feの計算値:C,60.90、H,10.73、N,14.20。実測値:C,59.55、H,10.77、N,13.86。
NiCl2を用いたことを除いて、[Co(iPr−AMD)2]に関して実施例2に記載したと同様な手順にしたがい、かつ当該反応混合物を一晩還流して、褐色の固体[Ni(iPr−AMD)2]2を、そのヘキサン抽出物から溶媒を蒸発させた生成物として得た。褐色の結晶(70%)。昇華:70ミリトール下で35℃。融点:55℃。C16H34N4Niの計算値:C,56.34、H,10.05、N,16.42。実測値:C,55.22、H,10.19、N,16.12。
MnCl2を用いたことを除いて、[Co(iPr−AMD)2]に関して記載したと同様な手順にしたがい、固体[Mn(iPr−AMD)2]2を、そのヘキサン抽出物から溶媒を蒸発させた生成物として得た。黄緑色の結晶(79%)。昇華:50ミリトール下で65℃。C32H68N8Mn2の計算値:C,56.96、H,10.16、N,16.61。実測値:C,57.33、H,9.58、N,16.19。
1,3−ジイソプロピルカルボジイミドに代えて1,3−ジ−t−ブチルカルボジイミドを用いたことを除いて、[Mn(iPr−AMD)2]に関して上記したと同様な手順にしたがって、淡黄色の結晶(87%)を得た。昇華:60ミリトール下で55℃。融点:100℃。
LaCl3(THF)2の代わりにTiCl3を用いたことを除いて、[La(iPr−AMD)3]に関して上記したと同様な手順にしたがって、[Ti(iPr−AMD)3]を、そのヘキサン抽出物から溶媒を蒸発させた生成物として得た。褐色の結晶(70%)。昇華:50ミリトール下で70℃。C24H51N6Tiの計算値:C,61.13、H,10.90、N,17.82。実測値:C,60.22、H,10.35、N,17.14。
TiCl3の代わりにVCl3を用いたことを除いて、[Ti(iPr−AMD)3]に関して上記したと同様な手順にしたがって、[V(iPr−AMD)3]を、そのヘキサン抽出物から溶媒を蒸発させた生成物として得た。赤褐色の粉体(80%)。昇華:45ミリトール下で70℃。
これら二種の化合物は、[Cu(iPr−AMD)]に関して記載したと同様な方法で同時に調製して、二量体と三量体の1:1の混合物として得た。無色の結晶(90%)。昇華:40ミリトール下で80℃。融点:95℃。1H NMR(C6D6、25℃):1.10(d,二量体)、1.21(d,三量体)、1.74(s,三量体)、1.76(s,二量体)、3.52(m,二量体及び三量体に係るピークは明瞭に分解されない)。[C8H17N2Ag]xの計算値:C,38.57、H,6.88、N,11.25。実測値:C,38.62、H,6.76、N,11.34。
図1の装置を用いて、銅材料を析出させた。銅(I)N,N’−ジイソプロピルアセトアミジナートの二量体を、蒸気容積125cm3をもつステンレス鋼製の容器11内に置いて、85℃に加熱した。その温度では、約0.15トールの蒸気圧を有する。1.0ミクロモルの投与量の銅先駆物質を、窒素のキャリアガスを用いて10トールまでチェンバーを加圧することによって導入した。水素を、ガスクロマトグラフの試料採取バルブを用いて1.4ミリモルの投与量で導入した。基板130とチェンバー110の加熱壁の面積の合計は、約103cm2となった。よって、銅先駆物質の1回分の投与量は1×10-9モル/cm2で、水素の1回分の投与量は1.4×10-6モル/cm2であった。その「暴露」は、析出領域における先駆物質の蒸気の分圧とこの蒸気が基板表面の所定の位置で接触する時間との積として定義される。当該銅先駆物質に対する基板の暴露は、2.3×104ラングミュア/作業周期で、水素に対するそれの暴露は3.4×107ラングミュア/作業周期であった。
両反応体の複数回分の投与量を2倍にしたことを除いて、実施例14を繰り返した。薄膜の厚さ及びその特性は、実施例14のそれと不変であった。この結果は、その表面反応が自己制御的であることを示している。
500回の作業周期に代えて1000回の作業周期を用いたことを除いて、実施例14を繰り返した。2倍量の材料が析出した。この結果は、それぞれの自己制御的反応が、再度開始するための他の反応に必要な条件を再生していること、および基板表面での開始反応又は核生長に、実質的な遅れが全くないことを示している。
基板温度を180℃〜300℃の範囲内で変えたことを除いて、実施例14を繰り返した。作業周期当たりの厚さが図6に示されるように温度と共に変化したことを除いては、同様な結果が得られた。基板温度が180℃以下では、銅の析出は全く観察されなかった。この観察によると、反応チェンバーの壁の温度が180℃以下でかつ先駆物質の露点以上に保持されるならば、当該壁には望ましくない銅の析出物は残留しないことを教示している。
銅先駆物質に代えて75℃に保持されたコバルトビス(N,N’−ジイソプロピルアセトアミジナート)を用い、かつ基板温度を300℃に上げたことを除いて、実施例14を繰り返した。析出チェンバー内に、内径20μmを有する溶融シリカ製の毛管と共に、先に二酸化珪素で次いで窒化タングステンで被覆したシリコン基板を配置した。各回の作業周期では、コバルト先駆物質の一回分の投与量は4×10-9モル/cm2であり、水素の一回分の投与量は9×10-7モル/cm2であった。コバルト先駆物質に対する基板の暴露は、1×105ラングミュア/作業周期で、水素に対するそれの暴露は、2×107ラングミュア/作業周期であった。
基板温度を250℃〜350℃の範囲内で変えたことを除いて、実施例18を繰り返した。作業周期当たりの厚さが図7に示されるように温度と共に変化したことを除いては、同様な結果が得られた。基板温度が250℃以下では、コバルトの析出は全く観察されなかった。この観察によると、反応チェンバーの壁の温度が250℃以下でかつ先駆物質の露点以上に保持されるならば、当該壁には望ましくないコバルトの析出物は残留しないことを教示している。
先に二酸化珪素上に被覆された窒化タングステン(WN)層、WN/SiO2/Si上に、実施例14と実施例18における作業を交互に繰り返した。多層構造Cu/Co/WN/SiO2をもつ平滑な、付着性薄膜が得られた。次いで、この多層構造の表面に接着テープを接着した。当該テープを引き剥がしたときに、接着力の喪失は全く観察されなかった。
水素ガスを水蒸気に代えたことを除いて、実施例18を繰り返した。略CoOの組成をもつ酸化コバルトの均一で、平滑な層が析出した。
銅先駆物質に代えて75℃に保持されたニッケルビス(N,N’−ジイソプロピルアセトアミジナート)を用い、かつ基板温度を280℃に上げたことを除いて、実施例14を繰り返した。析出チェンバー内に、先に二酸化珪素で次いで窒化タングステンで被覆したシリコン基板を配置した。各回の作業周期では、ニッケル先駆物質の一回分の投与量は4×10-9モル/cm2であり、水素の一回分の投与量は8×10-7モル/cm2であった。ニッケル先駆物質に対する基板の暴露は、3×104ラングミュア/作業周期で、水素に対するそれの暴露は、7×106ラングミュア/作業周期であった。
当該基板をラザフォード後方散乱分光分析法で調べたところ、5×1016原子/cm2厚、即ち8×10-8モル/cm2厚の新鮮なニッケル金属からなる薄膜を有していることが判明した。
銅先駆物質に代えて75℃に保持された鉄ビス(N,N’−ジ−t−ブチルアセトアミジナート)を用い、かつ基板温度を280℃に上げたことを除いて、実施例14を繰り返した。析出チェンバー内に、先に二酸化珪素で次いで窒化タングステンで被覆したシリコン基板を配置した。各回の作業周期では、鉄先駆物質の一回分の投与量は4×10-9モル/cm2であり、水素の一回分の投与量は4×10-6モル/cm2であった。鉄先駆物質に対する基板の暴露は、8×104ラングミュア/作業周期で、水素に対するそれの暴露は、4×107ラングミュア/作業周期であった。
当該基板をラザフォード後方散乱分光分析法で調べたところ、5×1016原子/cm2厚、即ち8×10-8モル/cm2厚の新鮮な鉄金属からなる薄膜を有していることが判明した。
コバルトビス(N,N’−ジイソプロピルアセトアミジナート)に代えて85℃に保持された鉄ビス(N,N’−ジ−t−ブチルアセトアミジナート)([Fe(iBu-AMD)2])を用いて、実施例21を繰り返した。各回の作業周期では、鉄先駆物質の一回分の投与量は4×10-9モル/cm2であり、水蒸気の一回分の投与量は8×10-8モル/cm2であった。鉄先駆物質に対する基板の暴露は、8×104ラングミュア/作業周期で、水蒸気に対するそれの暴露は、7×105ラングミュア/作業周期であった。略FeOの組成をもつ酸化鉄の均一で、平滑な層が250℃に加熱された基板上に析出した。
コバルトトリス(N,N’−ジイソプロピルアセトアミジナート)に代えて120℃に保持されたランタントリス(N,N’−ジイソプロピルアセトアミジナート)([La(iBu-AMD)3])を用いて、実施例21を繰り返した。50回の作業周期のそれぞれでは、ランタン先駆物質の一回分の投与量は4×10-9モル/cm2であり、水蒸気の一回分の投与量は8×10-8モル/cm2であった。ランタン先駆物質に対する基板の暴露は、3×104ラングミュア/作業周期で、水蒸気に対するそれの暴露は、7×105ラングミュア/作業周期であった。略La2O3の組成をもち、約5nm厚の酸化ランタンの均一で、平滑な層が300℃に加熱された基板上に析出した。
実施例25を、16回の作業周期の酸化ランタンを析出させるために繰り返した。次いで、当該分野の周知技術にしたがい、トリメチルアルミニウム蒸気と水蒸気の交互の複数回の投与量を用いて、6回の作業周期の酸化アルミニウムをALDによって析出させた。このパターン(16La2O3+6Al2O3)の作業周期を5回繰り返した。約10nm厚の均一で、平滑な層が、300℃に加熱された基体上に析出した。当該層は、略LaAlO3の平均組成を有していた。この材料から作られたコンデンサーは、約18の誘電率を有し、1ボルトの印加電圧下で、非常に低い約5×10−8アンペア/cm2の漏れ電流しか生じなかった。
実施例26で達成した厚さの均一性についての我々の解釈によれば、その酸化アルミニウム層が、下方の酸化ランタン層への水の拡散を防止するバリアとして作用しているということである。
コバルトビス(N,N’−ジイソプロピルアセトアミジナート)に代えて75℃に保持されたマンガンビス(N,N’−ジ−t−ブチルアセトアミジナート)([Mn(iBu-AMD)2])を用いて、実施例21を繰り返した。各回の作業周期では、マグネシウム先駆物質の一回分の投与量は4×10-9モル/cm2であり、水蒸気の一回分の投与量は8×10-8モル/cm2であった。マンガン先駆物質に対する基板の暴露は、3×104ラングミュア/作業周期で、水蒸気に対するそれの暴露は、6×105ラングミュア/作業周期であった。略MnOの組成をもつ酸化マンガン(II)の均一で、平滑な層が、約0.1nm/作業周期の析出速度で、250℃に加熱された基板上に析出した。
実施例21で用いたコバルトビス(N,N’−ジイソプロピルアセトアミジナート)に代えて、実施例3に記載したそれと同様な手順によって調製された、80℃に保持されたマグネシウムビス(N,N’−ジ−t−ブチルアセトアミジナート)([Mg(iBu-AMD)2])を用いて、実施例21を繰り返した。各回の作業周期では、マグネシウム先駆物質の一回分の投与量は3×10-9モル/cm2であり、水蒸気の一回分の投与量は6×10-8モル/cm2であった。マグネシウム先駆物質に対する基板の暴露は、3×104ラングミュア/作業周期で、水蒸気に対するそれの暴露は、5×105ラングミュア/作業周期であった。略MgOの組成をもつ酸化マグネシウムの均一で、平滑な層が、0.08nm/作業周期の析出速度で、250℃に加熱された基板上に析出した。
1当量の乾燥第二ブチルアミン、1当量の乾燥アセトニトリル及び0.02当量のランタントリフレート、触媒を、還流冷却器付シュレンクフラスコに投入した。反応混合物を3日間還流させながら、乾燥窒素を、還流カラムを通して通気ビンからフラスコ中にゆっくりと通過させた。次いで、過剰の反応体を真空下に取り除き、残留液を蒸留により精製して、第二ブチルアセトアミジンを得た。1H NMR(C6D6、25℃):δ1.49(m,4H)、δ1.38(s,3H)、δ1.11(d,J=6Hz,6H)、δ0.90(t,J=8Hz,6H)。
無水塩化コバルト(II)、CoCl2を、乾燥箱内のシュレンクフラスコ中に秤量装填した。実施例29で作製した2当量のリチウムN,N’−ジ−sec−ブチルアセトアミジナート溶液を、等容量の乾燥THFと共に添加した。反応混合物を一晩攪拌し、次いで揮発物を室温下、真空中で取り除いた。当該固体を乾燥ヘキサンに溶解し、濾過して、真空中、室温下で濾液からヘキサンを除いたところ、粗収率82%のコバルトビス(N,N’−ジ−sec−ブチルアセトアミジナート)を得た。この液体を蒸留(60ミリトール下で55℃)により精製した。
実施例30の手順を、塩化コバルトと実施例29で調製した1当量のリチウムN,N’−ジ−sec−ブチルアセトアミジナートとに代えて、1当量の塩化銅(I)、CuClを用いて実施した。[Cu(sec−Bu−AMD)]2を、実施例30の手順で単離した。昇華:50ミリトール下で55℃。融点:77℃。[Cu(sec−Bu−AMD)]2は、銅のALD用の先駆物質として、それが蒸発に用いられる温度(約100℃)下で液体であり、その結果、固体先駆物質の昇華により得られるよりも一層再生可能な蒸気の送出が得られるという点で利点を有する。
1当量の三塩化ビスマス、BiCl3、及び3当量のリチウムN,N’−ジ−t−ブチルアセトアミジナート(1,3−ジ−t−ブチルカルボジイミドとメチルリチウムとの反応によって得られる)を、THF中で一晩還流した。THFを蒸発した後、乾燥ヘキサンで抽出し、濾過して、濾液からヘキサンを抽出し、粗生成物を昇華(80ミリトール下で70℃)によって単離した。融点:95℃。p−キシレン溶液中での凝固点降下法による二量体。
実施例32で用いたそれと同様な手順にしたがって、ストロンチウムビス(N,N’−ジ−t−ブチルアセトアミジナート)を得た。粗生成物を、昇華(90ミリトール下で130℃)によって生成した。
実施例25と同様な手順にしたがって、酸化ビスマス、Bi2O3の薄膜を、85℃でビスマストリス(N,N’−ジ−t−ブチルアセトアミジナート)を含む蒸発源から、200℃の温度下で基板上に析出させた。当該薄膜の厚さは、約0.03nm/作業周期であった。
実施例11と同様な手順にしたがって、ルテニウムトリス(N,N’−ジイソプロピルアセトアミジナート)([Ru(iPr−AMD)3])を、低収率で得た。
実施例14を、銅先駆物質のみを用い、かつ水素ガスを用いないで繰り返した。基板表面に析出された薄膜は、全く観察されなかった。
実施例18を、コバルト先駆物質のみを用い、かつ水素を用いないで繰り返した。基板表面に析出された薄膜は、全く観察されなかった。
Claims (5)
- 加熱基板を一種以上の揮発性金属アミジナート化合物又はそのオリゴマーの蒸気に、次いで、還元性ガス又は蒸気に交互に暴露して、当該基板表面に金属皮膜を形成させることを含んでなる、金属を含む薄膜の形成方法であって、
前記揮発性金属アミジナート化合物が、以下の一般式で表される化合物からなる群より選ばれる方法。
(1)下記一般式の揮発性金属(III)アミジナート化合物:
- 前記還元性ガスが水素である、請求項1に記載の方法。
- 加熱基板を一種以上の揮発性金属アミジナート化合物又はそのオリゴマーの蒸気に、次いで、アンモニアガス又は蒸気に交互に暴露して、当該基板表面に金属窒化物皮膜を形成させることを含んでなる、金属窒化物を含む薄膜の形成方法であって、
前記揮発性金属アミジナート化合物が、以下の一般式で表される化合物からなる群より選ばれる方法。
(1)下記一般式の揮発性金属(III)アミジナート化合物:
- 加熱基板を一種以上の揮発性金属アミジナート化合物又はそのオリゴマーの蒸気に、次いで、酸素含有ガス又は蒸気に交互に暴露して、当該基板表面に金属酸化物皮膜を形成させることを含んでなる、金属酸化物を含む薄膜の形成方法であって、
前記揮発性金属アミジナート化合物が、以下の一般式で表される化合物からなる群より選ばれる方法。
(1)下記一般式の揮発性金属(III)アミジナート化合物:
- 前記酸素含有ガスが水蒸気である、請求項4に記載の方法。
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