WO2001029280A1 - Deposition of transition metal carbides - Google Patents
Deposition of transition metal carbides Download PDFInfo
- Publication number
- WO2001029280A1 WO2001029280A1 PCT/US2000/028537 US0028537W WO0129280A1 WO 2001029280 A1 WO2001029280 A1 WO 2001029280A1 US 0028537 W US0028537 W US 0028537W WO 0129280 A1 WO0129280 A1 WO 0129280A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- transition metal
- source gas
- compound
- substrate
- carbon
- Prior art date
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- 229910052723 transition metal Inorganic materials 0.000 title claims abstract description 70
- -1 transition metal carbides Chemical class 0.000 title claims description 19
- 230000008021 deposition Effects 0.000 title description 26
- 239000000758 substrate Substances 0.000 claims abstract description 104
- 150000001875 compounds Chemical class 0.000 claims abstract description 90
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 77
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 71
- 238000000034 method Methods 0.000 claims abstract description 71
- 150000003624 transition metals Chemical class 0.000 claims abstract description 63
- 229910052751 metal Inorganic materials 0.000 claims abstract description 62
- 239000002184 metal Substances 0.000 claims abstract description 62
- 239000007789 gas Substances 0.000 claims abstract description 46
- 239000010409 thin film Substances 0.000 claims abstract description 38
- 238000000231 atomic layer deposition Methods 0.000 claims abstract description 37
- 238000000151 deposition Methods 0.000 claims abstract description 34
- 230000004888 barrier function Effects 0.000 claims abstract description 9
- 238000009792 diffusion process Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims description 99
- 230000008569 process Effects 0.000 claims description 33
- 239000006227 byproduct Substances 0.000 claims description 26
- 239000010410 layer Substances 0.000 claims description 21
- 229910052796 boron Inorganic materials 0.000 claims description 20
- 229910052710 silicon Inorganic materials 0.000 claims description 19
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000010703 silicon Substances 0.000 claims description 18
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 17
- 239000011261 inert gas Substances 0.000 claims description 14
- 229910052721 tungsten Inorganic materials 0.000 claims description 14
- 229910052715 tantalum Inorganic materials 0.000 claims description 9
- 239000012808 vapor phase Substances 0.000 claims description 9
- 229910052804 chromium Inorganic materials 0.000 claims description 8
- 229910052735 hafnium Inorganic materials 0.000 claims description 8
- 229910052750 molybdenum Inorganic materials 0.000 claims description 8
- 229910052758 niobium Inorganic materials 0.000 claims description 8
- 229910052719 titanium Inorganic materials 0.000 claims description 8
- 229910052720 vanadium Inorganic materials 0.000 claims description 8
- 229910052726 zirconium Inorganic materials 0.000 claims description 8
- 239000010937 tungsten Substances 0.000 claims description 7
- 229930195733 hydrocarbon Natural products 0.000 claims description 6
- 150000002430 hydrocarbons Chemical class 0.000 claims description 6
- 150000003018 phosphorus compounds Chemical class 0.000 claims description 6
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 6
- 150000001639 boron compounds Chemical class 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 229910001507 metal halide Inorganic materials 0.000 claims description 5
- 239000002356 single layer Substances 0.000 claims description 5
- 150000001721 carbon Chemical group 0.000 claims description 4
- 239000012159 carrier gas Substances 0.000 claims description 4
- 150000003377 silicon compounds Chemical class 0.000 claims description 4
- 239000004215 Carbon black (E152) Substances 0.000 claims description 3
- 230000009977 dual effect Effects 0.000 claims description 3
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 claims description 3
- 150000005309 metal halides Chemical class 0.000 claims description 3
- 238000005260 corrosion Methods 0.000 claims description 2
- 230000007797 corrosion Effects 0.000 claims description 2
- 150000004696 coordination complex Chemical class 0.000 claims 4
- 150000001722 carbon compounds Chemical class 0.000 claims 2
- 239000007809 chemical reaction catalyst Substances 0.000 claims 1
- 239000004020 conductor Substances 0.000 claims 1
- 125000004437 phosphorous atom Chemical group 0.000 claims 1
- 239000011800 void material Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000004065 semiconductor Substances 0.000 abstract description 4
- 238000010926 purge Methods 0.000 description 24
- 239000000126 substance Substances 0.000 description 22
- 239000000463 material Substances 0.000 description 20
- 238000005137 deposition process Methods 0.000 description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- 239000010408 film Substances 0.000 description 14
- 125000000217 alkyl group Chemical group 0.000 description 10
- 150000001247 metal acetylides Chemical class 0.000 description 10
- NXHILIPIEUBEPD-UHFFFAOYSA-H tungsten hexafluoride Chemical compound F[W](F)(F)(F)(F)F NXHILIPIEUBEPD-UHFFFAOYSA-H 0.000 description 10
- 239000000376 reactant Substances 0.000 description 9
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 8
- 229910052698 phosphorus Chemical group 0.000 description 8
- 239000011574 phosphorus Chemical group 0.000 description 8
- 238000005229 chemical vapour deposition Methods 0.000 description 7
- 239000012071 phase Substances 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 7
- 238000009835 boiling Methods 0.000 description 6
- 239000011651 chromium Substances 0.000 description 6
- 239000010955 niobium Substances 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 239000010936 titanium Substances 0.000 description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 5
- 239000002052 molecular layer Substances 0.000 description 5
- 238000009738 saturating Methods 0.000 description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 5
- 229910010271 silicon carbide Inorganic materials 0.000 description 5
- 238000006557 surface reaction Methods 0.000 description 5
- 238000005979 thermal decomposition reaction Methods 0.000 description 5
- 150000003623 transition metal compounds Chemical class 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 238000005240 physical vapour deposition Methods 0.000 description 4
- 125000004429 atom Chemical group 0.000 description 3
- 238000010923 batch production Methods 0.000 description 3
- GZUXJHMPEANEGY-UHFFFAOYSA-N bromomethane Chemical compound BrC GZUXJHMPEANEGY-UHFFFAOYSA-N 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 229910003460 diamond Inorganic materials 0.000 description 3
- 239000010432 diamond Substances 0.000 description 3
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 3
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 description 3
- 150000002894 organic compounds Chemical class 0.000 description 3
- 230000000737 periodic effect Effects 0.000 description 3
- 229910003468 tantalcarbide Inorganic materials 0.000 description 3
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- ILAHWRKJUDSMFH-UHFFFAOYSA-N boron tribromide Chemical compound BrB(Br)Br ILAHWRKJUDSMFH-UHFFFAOYSA-N 0.000 description 2
- RDHPKYGYEGBMSE-UHFFFAOYSA-N bromoethane Chemical compound CCBr RDHPKYGYEGBMSE-UHFFFAOYSA-N 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000002003 electron diffraction Methods 0.000 description 2
- 238000010574 gas phase reaction Methods 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000012212 insulator Substances 0.000 description 2
- INQOMBQAUSQDDS-UHFFFAOYSA-N iodomethane Chemical compound IC INQOMBQAUSQDDS-UHFFFAOYSA-N 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229910052756 noble gas Inorganic materials 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 241000894007 species Species 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- VCZQFJFZMMALHB-UHFFFAOYSA-N tetraethylsilane Chemical compound CC[Si](CC)(CC)CC VCZQFJFZMMALHB-UHFFFAOYSA-N 0.000 description 2
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 2
- LALRXNPLTWZJIJ-UHFFFAOYSA-N triethylborane Chemical compound CCB(CC)CC LALRXNPLTWZJIJ-UHFFFAOYSA-N 0.000 description 2
- RXJKFRMDXUJTEX-UHFFFAOYSA-N triethylphosphine Chemical compound CCP(CC)CC RXJKFRMDXUJTEX-UHFFFAOYSA-N 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- 125000000008 (C1-C10) alkyl group Chemical group 0.000 description 1
- UUFQTNFCRMXOAE-UHFFFAOYSA-N 1-methylmethylene Chemical compound C[CH] UUFQTNFCRMXOAE-UHFFFAOYSA-N 0.000 description 1
- ZRNSSRODJSSVEJ-UHFFFAOYSA-N 2-methylpentacosane Chemical compound CCCCCCCCCCCCCCCCCCCCCCCC(C)C ZRNSSRODJSSVEJ-UHFFFAOYSA-N 0.000 description 1
- 229910015845 BBr3 Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910020667 PBr3 Inorganic materials 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229910003691 SiBr Inorganic materials 0.000 description 1
- 229910004014 SiF4 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910008940 W(CO)6 Inorganic materials 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- PPWPWBNSKBDSPK-UHFFFAOYSA-N [B].[C] Chemical compound [B].[C] PPWPWBNSKBDSPK-UHFFFAOYSA-N 0.000 description 1
- JXBAVRIYDKLCOE-UHFFFAOYSA-N [C].[P] Chemical compound [C].[P] JXBAVRIYDKLCOE-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000001350 alkyl halides Chemical class 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- KKAXNAVSOBXHTE-UHFFFAOYSA-N boranamine Chemical class NB KKAXNAVSOBXHTE-UHFFFAOYSA-N 0.000 description 1
- 229910000085 borane Inorganic materials 0.000 description 1
- 229950005499 carbon tetrachloride Drugs 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- NEHMKBQYUWJMIP-NJFSPNSNSA-N chloro(114C)methane Chemical compound [14CH3]Cl NEHMKBQYUWJMIP-NJFSPNSNSA-N 0.000 description 1
- HRYZWHHZPQKTII-UHFFFAOYSA-N chloroethane Chemical compound CCCl HRYZWHHZPQKTII-UHFFFAOYSA-N 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000001678 elastic recoil detection analysis Methods 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229960003750 ethyl chloride Drugs 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- UHCBBWUQDAVSMS-UHFFFAOYSA-N fluoroethane Chemical compound CCF UHCBBWUQDAVSMS-UHFFFAOYSA-N 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- HVTICUPFWKNHNG-UHFFFAOYSA-N iodoethane Chemical compound CCI HVTICUPFWKNHNG-UHFFFAOYSA-N 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 229910001512 metal fluoride Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 229940102396 methyl bromide Drugs 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- IPNPIHIZVLFAFP-UHFFFAOYSA-N phosphorus tribromide Chemical compound BrP(Br)Br IPNPIHIZVLFAFP-UHFFFAOYSA-N 0.000 description 1
- 238000004375 physisorption Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/38—Nitrides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/20—Deposition of semiconductor materials on a substrate, e.g. epitaxial growth solid phase epitaxy
-
- 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
- C23C16/22—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
- C23C16/32—Carbides
-
- 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
-
- 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
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
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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
- C23C16/44—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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- 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
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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
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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
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- 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
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Definitions
- the present invention relates to the deposition of transition metal carbide thin films. More specifically, the present invention relates to the use of sequential self-saturating surface reactions to form transition metal carbides on various substrates. Description of the Related Art
- Transition metal elements in groups 4 (Ti, Zr, Hf), 5 (V, Nb, Ta) and 6 (Cr, Mo, W) of the periodic table possess several attractive properties. They are relatively inert, have very high melting points, are extremely hard and wear resistant, and have high thermal conductivity and metal-like electrical conductivity. For these reasons, transition metal carbides have been proposed for use as low resistance diffusion barriers in semiconductor fabrication
- metal carbides can have a wide range of compositions. Ordered and disordered carbon deficient forms exist, of which the tungsten carbides W 3 C, W 2 C, WC and WC, merit are examples. In these forms, carbon resides in the interstitial cavities between metal atoms.
- Suggested deposition methods include Chemical Vapor Deposition (CVD), Metal Organic Chemical Vapor Deposition (MOCVD) and Physical Vapor Deposition (PVD).
- CVD Chemical Vapor Deposition
- MOCVD Metal Organic Chemical Vapor Deposition
- PVD Physical Vapor Deposition
- Carbides have been deposited by CVD type processes wherein more than one source chemical is present in the reaction space at the same time.
- a CVD method of depositing tungsten carbide from tungsten hexafluoride, hydrogen and a carbon-containing gas has been described, for example, in international patent application WO 00/47796.
- the carbon-containing gas is initially thermally activated. All of the gaseous source chemicals are present at the same time in the reaction space, resulting in the deposition of nonvolatile tungsten carbide on the substrate.
- a CVD reaction of WF 6 with trimethylamine and H 2 has been disclosed for yielding WC films at 700°C - 800°C and beta- WC, , films at 400°C - 600°C (Nakajima et al., J. Electrochem. Soc. 144:2096-2100 (1997)).
- the H 2 flow rate affects the deposition rate of tungsten carbide.
- One problem with the disclosed process is that the substrate temperature is rather high relative to thermal budgets for state-of-the-art semiconductor fabrication, particularly in metallization stages.
- MOCVD processes utilize organometallic compounds that are thermally decomposed on the substrate or combined with other organic compounds in gas phase and then contacted with the substrate thus breaking the source chemical molecules and forming the final product.
- Tungsten carbide has also been deposited on substrates by the thermal decomposition of organotungsten derivatives of W(CO) 6 at low pressures (Lai et al., Chem. Mater. 7:2284- 2292 (1995)).
- TiC has been deposited in a CVD process by the thermal decomposition of organometallic titanium compounds (Girolami et al., Mater. Res. Soc. Sy p. Proc. 121 :429-438 (1988)).
- U.S. Patent No. 5,916,365 also discloses thermal decomposition of pentadimeth ⁇ l-aminotantalum. In these processes, the source chemical molecules contain both the metal and the carbon. However it's utility on complex, irregular surfaces is not known.
- PVD processes generally deposit along a hne-of-sight.
- One method of depositing tantalum carbide for a diffusion barrier layer by PVD has been described in U.S. Patent No. 5,973,400.
- the tantalum carbide layer was formed by sputtering tantalum or tantalum carbide under N2/CH4/Ar atmosphere.
- Line of sight deposition means that complex substrate contours will have insufficient thin film coverage in shaded areas. Additionally, line of- sight deposition means that low-volatility source material arriving directly from the source to the substrate will likely adhere to the first solid surface that it encounters, thus producing low-conformality coverage.
- a method for depositing a transition metal carbide thin film by an atomic layer deposition (ALD) process.
- ALD atomic layer deposition
- vapor-phase pulses of at least one transition metal source compound and at least one carbon source compound are alternately fed into a reaction space containing a substrate.
- the transition metal source compound preferably comprises a metal source gas selected from the group consisting of Ti, Zr, Hf, V, Nb, Ta, Cr, Mo and W.
- An exemplary transition metal source gas is a metal halide, such as tungsten hexafluonde.
- Exemplary carbon source compounds include boron compounds, silicon compounds and phosphorous compounds. Desirably, in these exemplary source gas compounds, either boron, silicon or phosphorus bond directly to carbon.
- a metal carbide thin film can advantageously form thin diffusion barrier that is conductive and conformal over integrated circuit topography [e.g., dual damascene trenches and vias).
- Figure 1 presents a schematic view of a dual damascene structure and the placement of the metal carbide diffusion barrier.
- Figure 2 presents a flow chart of the metal carbide ALD process.
- an "atomic layer deposition” or “ALD” type process designates a process where the deposition of thin film onto a substrate is based on sequential and alternating self-saturating surface reactions.
- ALD atomic layer deposition
- the principles of ALD are disclosed, e.g., in U.S. Patent Nos. 4,058,430 and 5,71 1 ,81 1 , the disclosures of which are hereby incorporated by reference herein.
- Substrate temperature means a temperature that is maintained in the reaction space during the deposition process.
- Transition metals means elements of groups 3 to 12 of the periodic table of the elements. A preferred subset of the transition metals are those of groups 5 (titanium, zirconium and hafnium), 6 (vanadium, niobium and tantalum) and 7 (chromium, molybdenum and tungsten) of the periodic table of the elements. Metal carbides of these elements contain interstitial carbon and have some of the properties of pure metals.
- Reaction space is used to designate a reactor or reaction chamber in which the conditions can be adjusted so that deposition by ALD is possible.
- transition metal carbide thin films are prepared by a chemical gaseous deposition process.
- the preferred chemical gaseous deposition process is an atomic layer deposition (ALD) type process.
- ALD atomic layer deposition
- a transition metal carbide thin film is grown on a substrate placed in a reaction space at an elevated temperature.
- a substrate is preferably placed in a reaction space and is subjected to sequential, alternately repeated surface reactions of at least two vapor-phase reacta ⁇ ts such that a transition metal carbide thin film grows on the substrate.
- the conditions in the reaction space are adjusted so that no gas phase reactions, i.e., reactions between gaseous reactants, occur.
- a metal source compound and a carbon source compound are alternately fed to the reaction space in gaseous form such that they are not present simultaneously in the gas phase in the reaction space.
- the reactions are preferably self-saturating and self-limiting.
- the vapor-phase pulses of the transition metal source compound and the carbon source compound are alternately and sequentially fed into the reaction space and brought in contact with the surface of the substrate.
- the source compounds are preferably fed into the reaction space with the aid of an inert or noble carrier gas, such as nitrogen or argon.
- the "surface" of the substrate initially comprises the substrate material.
- the substrate has been pretreated in advance, e.g , by contacting it with a chemical for modifying the surface properties thereof.
- Each cycle in the deposition preferably comprises: feeding a vapor phase pulse of a transition metal source compound into the reaction space in an inert carrier gas; removing the surplus transition metal source compound and any gaseous by-products from the reaction space (e.g., by purging with an inert gas); feeding a vapor-phase pulse of a carbon source compound into the reaction space in an inert carrier gas; and removing the surplus carbon source compound and any gaseous by-products from the reaction space (e.g., by purging with an inert gas).
- the cycle may be repeated as many times as desired to produce a transition metal carbide film of the desired thickness.
- the purging time is preferably selected to be long enough to prevent gas phase reactions and to prevent transition metal carbide thin film growth rates higher than one lattice constant of the transition metal carbide per cycle.
- the deposition is carried out at atmospheric pressure. However, it is preferable to carry out the deposition at reduced pressure
- the pressure in the reactor is preferably about 0.01 mbar to 50 bar, and more preferably about 0.1 mbar to 10 mbar.
- the substrate temperature is preferably low enough to prevent thermal decomposition of the gaseous reactants. On the other hand, the substrate temperature is preferably high enough to avoid the physisorption, or condensation of the source materials. Further, the substrate temperature is preferably sufficiently high to provide the activation energy for the surface reaction.
- the temperature of the substrate is preferably about 200°C to 600°C, and more preferably about 250°C to 400°C.
- the most preferable substrate temperature and reaction space pressure will depend on the identity of the reactants and the substrate. if the partial pressure of the gaseous source compound exceeds the condensation limit at the substrate temperature, controlled, layer-by-layer growth of the transition metal carbide film is lost.
- the temperature of the source container is preferably set below the substrate temperature.
- the transition metal source compound is chemisorbed on the substrate surface, forming a surface bound transition metal complex.
- the amount of reactants bound to the surface of the substrate by chemisorption will be determined by the surface itself.
- the reactant molecules will bind to the surface until no more available binding sites remain on the surface, and terminating ligands on the monolayer are non reactive with excess source compound still in the vapor phase. This phenomenon is known as "self saturation".
- the physical size of the reactant molecules may prevent complete coverage of the surface when all of the binding sites are occupied.
- the preferred coverage on the substrate is obtained when no more than a single layer of transition metal source complex is adsorbed per pulsing sequence. Thus, several cycles may be necessary to produce a complete monolayer of transition metal carbide.
- the amount of time available for the self-saturating reactions is limited mostly by economic factors. For example, the required substrate throughput time for economic efficiency will impose a limit on the time available for the self-saturating reactions.
- the substrate may be composed of any material known in the art. Examples include silicon, silica, coated silicon, metals, metal nitrides, metal oxides, porous materials, silicon carbide and silicon nitride. As discussed above, in the preferred embodiment, once a transition metal carbide thin film layer has been deposited by the present method, that layer will form the substrate surface for any subsequent layer.
- the transition metal source compound and the carbon source compound are preferably chosen so that the requirements for sufficient vapor pressure, thermal stability at the substrate temperature and sufficient reactivity of the compounds on the substrate surface are fulfilled.
- Sufficient vapor pressure means that there are enough source compound molecules in the gas phase near the substrate surface to enable self-saturated reactions at the surface.
- Sufficient thermal stability means that the source chemical itself does not form growth-disturbing condensable phases on the substrate or leave harmful levels of impurities on the substrate surface through thermal decomposition.
- the reactants are preferably chosen to avoid uncontrolled condensation of atoms or molecules on the substrate. According to the preferred embodiment of the present invention, a transition metal source material and a carbon source material are required.
- the carbon source material is preferably a boron source compound, a silicon source compound or a phosphorus source compound. However in one embodiment plasma is used and the preferred carbon source material is a hydrocarbon.
- the preferred metal source compounds are transition metal compounds that are volatile at sufficiently low source temperatures. These transition metal compounds preferably comprise a transition metal selected from the group consisting of W, Ti, Zr, Hf, V, Nb, Ta, Cr and Mo. More preferably, the metal source compounds are metal halides, including metal fluorides and metal chlorides. In an illustrated preferred embodiment, the metal source material is tungsten hexafluoride. 2. Boron Source Compounds
- the preferred boron source compounds are boron compounds that comprise at least one carbon atom and that are volatile at temperatures below the substrate temperature. More preferably the boron source materials are boron compounds that have at least one boron-carbon bond in the boron source compound molecule.
- the boron source compound is preferably chosen from the following: Carboranes according to formula I.
- CAH n+I ID Wherein n is an integer from 1 to 10, preferably from 2 to 6, and x is an even integer, preferably 2, 4 or 6.
- Examples of carboranes according to formula I include c/ ⁇ s ⁇ -carboranes (C 2 B n H n , 2 ), /vi/ ⁇ -carboranes (C 2 B n H Community +4 ) and arachno carboxanes (C 2 B n H n+6 ).
- R 3 NBX 3 (II) wherein R is linear or branched C1 to CI O, preferably C1 to C4 alkyl or H, and
- X is linear or branched C1 to CI O, preferably C1 to C4 alkyl, H or halogen.
- Aminoboranes where one or more of the substituents on B is an amino group according to formula III.
- R 2 N (III) Wherein R is linear or branched C1 to C10, preferably C1 to C4 alkyl or substituted or unsubstituted aryl group.
- An example of a suitable aminobora ⁇ e is (CH 3 ) 2 NB(CH 3 ) 2 .
- Alkyl borons or alkyl boranes wherein the alkyl is typically linear or branced C1 to C10 alkyl, preferably C2 to C4 alkyl.
- the alkylboron compounds are especially preferred.
- the boron source material is t ⁇ ethylboron (CH 3 CH 2 ) 3 B.
- the preferred silicon source materials are carbon-containing silicon compounds that are volatile at temperatures below the substrate temperature. More preferably silicon source materials are silicon compounds that have at least one silicon-carbon bond in the silicon source chemical molecule. Even more preferably the silicon source materials are alk ⁇ lsilicon compounds.
- the preferred phosphorous source materials are carbon containing phosphorus compounds that are volatile at temperatures below the substrate temperature. More preferably the phosphorus source materials are phosphorus compounds that have at least one phosphorus-carbon bond in the phosphorus source chemical molecule. Even more preferably the phosphorus source materials are alkylphosphorus compounds.
- Hydrocarbons with a high hydrogen/carbon ratio are preferably used as carbon source chemicals. More preferably, linear or branched alkanes are used as carbon source chemicals.
- the metal source gas and the carbon source gas do not exist in the gas phase in the reaction space at the same time.
- the source chemicals are alternately fed to the reaction space and contacted with the substrate surface, thus providing for ALD type growth of metal carbide on the substrate.
- the by products of the reaction between the surface bound transition metal compound and the carbon source compound are preferably gaseous and thus can easily be removed from the reaction space by varying the reaction space pressure and/or with inert gas flow.
- the carbon source compound leaves some carbon in the metal carbide film and takes halogens away from the substrate surface.
- the carbon source chemical can change the oxidation state of the surface bound transition metal compound molecules.
- Analyses of thin films of the present invention revealed a high metal-to-carbon ratio W 3 C in the carbide thin film. This indicates a partial reduction of tungsten on the surface.
- inert gas flow dilutes the byproducts of the reaction between the carbon source compound and the surface bound transition metal compound until the concentration of the gas phase byproducts is insignificant in the reaction space.
- the carbon source compound leaves carbon in the growing transition metal carbide thin film.
- a transition metal halide is used as a metal source compound
- a halide byproduct may be formed in the reaction with the carbon source compound.
- a boron carbon source is used, a boron halide may be formed as a byproduct.
- Table 1 show that the resulting boron halides are volatile at a preferred substrate temperature, for example 350 °C, and that they will not condense on the substrate surface. The volatility allows them to be removed from the reaction space as described above.
- Boiling point temperatures in Tables 1 to 5 indicate that the vapor pressure of the compound is 1013 mbar (760 torr). However, much lower vapor pressures, down to about 0.01 to 0.1 mbar are sufficient for ALD processes.
- halogenated hydrocarbons have high volatility (Table 2) at a preferred substrate temperature, for example 350 °C.
- Tables 3 and 4 show that byproducts consisting of silicon or phosphorus halides also have high vapor pressure, making it possible to utilize reactive organic silicon and phosphorus compounds as carbon sources for the metal carbide deposition.
- Examples of Commercial Carbon Source Chemicals from Sigma Aldrich Carbon sources that are useful for the metal carbide depositions disclosed herein and that are commercially available include:
- a silicon wafer was loaded into the reaction space of a PulsarTM 2000 reactor, commercially available from ASM Microchemistry O ⁇ of Espoo, Finland, which is designed for ALD processes.
- the reaction space was evacuated with a mechanical vacuum pump. After evacuation the pressure of the reaction space was adjusted to about 5 mbar - 10 mbar (absolute) with flowing nitrogen gas that had a purity of 99.9999%. Then the reaction space was allowed to stabilize at about 350°C.
- Alternating pulses of electronic grade WF 6 and (CH 3 CH 2 ) 3 B were vaporized from external sources, introduced into the reaction space and contacted with the substrate surface. The source compound pulses were separated from each other by purging with flowing nitrogen gas.
- the pulsing cycle consisted of the two source compound pulses and the two nitrogen purges. The pulsing cycle was repeated 167 times.
- the pulsing and purging times of the pulsing cycle were as follows: WF 6 pulse 0.25 s
- the silicon substrate was unloaded from the reactor for inspection and analysis.
- the thin film covered the whole top surface of the substrate and it had a metallic luster and gray color. It had good adhesion to the wafer and was electrically conductive.
- Thin film samples were analyzed with TOF-ERDA (Time-Of- Flight Elastic Recoil Detection Analysis) for elements, with EDS (Electron Diffraction Spectroscopy) for thin film thickness and with four-point probe for sheet resistance. Resistivity was calculated from the thickness and sheet resistance values.
- the thin film samples consisted of tungsten and carbon in an atomic ratio corresponding to W 3 C.
- the thickness of the samples was about 23 nm, indicating that the growth rate of the tungsten carbide film had been about 1.4 A/cycle. This value is below the lattice constant of tungsten carbide, possibly due to the molecular size of the precursors that occupy more of the substrate surface than tungsten and carbon atoms do.
- the resistivity of the film was in the range of 200 micro-ohm-cm.
- the films had only about 1.0 atomic % - 1.5 atomic % of fluorine as an impurity.
- a substrate is placed into a reaction space.
- the reaction space is adjusted to a preferred temperature and the gas atmosphere of the reaction space is adjusted to a preferred pressure.
- a repeatable process sequence consisting of four basic steps is then begun.
- a vapor phase pulse of a transition metal source compound is introduced to the reaction space and contacted with the substrate surface.
- the surplus transition metal source compound and any reaction byproducts are removed from the reaction space by varying the reaction space pressure and/or by inert gas flow.
- a vapor phase pulse of a carbon source compound is introduced to the reaction chamber and contacted with the substrate surface.
- the surplus carbon source compound and any reaction byproducts are removed from the reaction space by varying the reaction space pressure and/or by inert gas flow.
- the process sequence may be repeated until a metal carbide thin film of a specified thickness is obtained.
- the substrate having a thin film is transported from the reaction chamber.
- the carbon source compound may be a boron, silicon or phosphorus carbon source compound.
- a substrate, as shown in Figure 1, having trench 1 and via 2 openings, etch stop layers 3, via insulator 4 and trench insulator 5 is placed in the reaction space of an ALD reactor.
- the reaction space is evacuated to vacuum and the pressure of the reaction space is adjusted to a preferred pressure with an inert gas, preferably nitrogen.
- a preferred pressure is in the range of about 1 mbar to 50 mbar, more preferably about 3 mbar to 10 mbar.
- the temperature of the reaction space is then stabilized at the preferred process temperature.
- the temperature is preferably in the range of 300°C to 425 °C, more preferably in the range of about 325°C to 375 °C, and is most preferably set at about 350°C.
- a transition metal carbide layer 6 is then produced on the substrate by the following cycle: a transition metal source compound is introduced into the reaction space and contacted with the substrate for a first pulse time; surplus transition metal source compound molecules and any byproduct molecules are removed from the reaction space during the first purge time; a carbon source compound is introduced to the reaction space and contacted with the substrate for a second pulse time; surplus carbon source compound molecules and any byproduct molecules are removed from the reaction space during the second purge time.
- the transition metal source compound is preferably selected from the group consisting of Ti, Zr, Hf, V, Nb, Ta, Cr, Mo and W compounds. Metal halide compounds are more preferred.
- the carbon source compound is selected from the group consisting of boron, silicon and phosphorus compounds that contain carbon. Alkyl borons, alkyl silicons and alkyl phosphorus compounds are more preferred.
- inert or noble gas is introduced to the reaction space to dilute the surplus compound and byproduct concentration to an insignificant level by forcing these molecules to enter the pumping line.
- Each pulsing cycle increases the thickness of the film by up to one molecular layer of metal carbide.
- the exact number of the pulsing cycles depends on the application and the desired thickness of the film.
- the transition metal carbide layer may serve as a diffusion barrier.
- the substrate may then be further manipulated, such as by the deposition of a metal seed layer.
- EXAMPLE 4 Coating tools with metal carbide in a batch process It would be beneficial to provide bits for drilling that have an extended useful life. This may be achieved by coating them with a metal carbide. Because the ALD type process of the present invention is not sensitive to the sample geometry, a batch process can be used. Thus, parts to be coated may be relatively small. The ability to use a batch process also decreases the coating costs per part significantly.
- a number of bits are set in a substrate holder that is then loaded into the reaction space of a batch reactor.
- the reaction space is evacuated to vacuum.
- the pressure of the reaction space is adjusted to a preferred pressure with an inert gas, preferably nitrogen.
- a preferred pressure is in the range of about 1 mbar to 50 mbar, more preferably about 3 mbar to 10 mbar.
- the temperature of the reaction space is then stabilized at the preferred process temperature.
- the temperature is preferably in the range of about 300°C to 425°C, more preferably in the range of about 325°C to 375°C, and in the illustrated embodiment is set at about 350°C.
- the transition metal carbide deposition process consists of the following repeatable process steps that form a pulsing cycle: a transition metal source compound is introduced into the reaction space and contacted with the substrates for a first pulse time; surplus transition metal source compound molecules and any byproduct molecules are removed from the reaction space during a first purge time; a carbon source compound is introduced to the reaction space and contacted with the substrates for a second pulse time; surplus carbon source compound molecules and any byproduct molecules are removed from the reaction space during a second purge time.
- the transition metal source compound is preferably selected from the group consisting of Ti, Zr, Hf, V, Nb, Ta, Cr, Mo and W compounds. Metal halide compounds are more preferred.
- the carbon source chemical is selected from the group consisting of volatile boron, silicon and phosphorus compounds that contain carbon. Alkyl borons, alkyl silicons and alkyl phosphorus compounds are more preferred.
- each pulsing cycle increases the thickness of the film by up to one molecular layer of metal carbide. The exact number of the pulsing cycles depends on the application and the desired thickness of the film.
- Metal carbide thin films may serve as a nucleation surface for the growth of diamond thin film.
- Metal carbide thin films are deposited on a substrate by the ALD type process of the present invention. The metal carbide thin film may then be used as a starting layer for the subsequent deposition of diamond thin film on the substrate.
- EXAMPLE 6 Electrical contacts to SiC with the help of ALD metal carbides
- a silicon carbide substrate is provided.
- the substrate surface has enough reactive sites for the nucleation of the first few metal carbide molecular layers.
- the most critical part of the process is the adsorption of the first molecular layer of the ALD source chemical on the silicon carbide surface.
- the deposition process can be started either with the metal source chemical or the carbon source chemical.
- Metal carbide thin films may be used as an intermediate layer on a substrate to improve the adhesion of a subsequent material layer deposited on the substrate.
- the metal carbide thin film is produced according to the deposition process described above.
- a substrate is first placed in the reaction space.
- the pressure of the reaction space is set to a preferred pressure with a vacuum pump and flowing inert gas.
- the temperature of the reaction space is set to a preferred temperature and the deposition process is started.
- the deposition process comprises the following repeatable pulse and purge steps that form the basic deposition cycle: metal source compound is introduced into the reaction chamber and contacted with the substrate for a first pulse time; surplus metal source compound molecules and any byproduct molecules are removed from the reaction space during a first purge time; carbon source compound is introduced into the reaction chamber in the form of plasma radicals and contacted with the substrate for a second pulse time; surplus carbon source compound molecules and any byproduct molecules are removed from the reaction space during a second purge time.
- the maximum deposition rate of the metal carbide thin film that allows for controlled thickness uniformity is one molecular layer per cycle.
- the carbon source compound is preferably an organic compound that contains only carbon and hydrogen.
- the carbon source compound is preferably turned into plasma with UV radiation, electric arc, RF generator or any other method known in the art that is capable of forming plasma from gas atoms or molecules.
- the resulting radicals preferably have a high hydrogen/carbon ratio, thus improving the volatility of these species and decreasing the possibility of obtaining a low-volatility carbon-rich coating on the substrate. Because this embodiment utilizes pulsed plasma, it is preferable to switch off or redirect the plasma source during the metal source compound pulse to avoid uncontrolled deposition of metal on the substrates.
- the cycle may be repeated as many times as necessary to produce a film of the desired thickness. After the deposition process the substrate is unloaded from the reaction space.
- the substrate holder In the case of powders having high area/volume ratio, the substrate holder consists of a length of container having a sinter on both ends.
- the substrate holder may be placed horizontally in the reaction space. In this orientation the substrate holder is filled with substrate powder so that there is no free gas space inside the substrate holder. In this orientation the source compound gases and purging gas preferably go through the powder.
- the substrate holder may alternatively be placed vertically in the reaction space. In this orientation there may be some free gas space left inside the substrate holder so that the substrate powder can float in the gas stream that preferably comes through the bottom sinter and exits through the top sinter.
- Transition metal carbide is deposited on the substrate surface by the ALD type process described above.
- source compound gases are preferably directed through the container holding the powder, thus ensuring that the gas contacts the particles of the powder. Due to the large surface area to be coated the pulse and purge times are preferably extended compared to the values provided for non-powder substrates.
- ALD metal carbides as corrosion protection Bearings are an example of parts that may benefit from a hard, protective outer layer when used in corroding atmospheres.
- a set of bearings is loaded into a perforated substrate holder.
- the holes on the substrate holder have a conical opening at the upper surface of the holder.
- the bearings rest on the bottom of these shallow cones.
- the substrate holder is transported into the reaction space where it is connected to the source gas and inert gas lines.
- the reaction space is evacuated to vacuum.
- the pressure of the reaction chamber is adjusted with flowing inert gas to the preferred processing pressure.
- Inert gas enters the reaction chamber through the holes of the substrate holder and raises the bearings from the bottom of the cones.
- the bearings preferably rotate freely in the flowing nitrogen streams (Bernoulli's principle) and they are not in contact with any solid surface during the deposition process.
- the temperature of the reaction space is adjusted to the preferred deposition temperature.
- the ALD type metal carbide deposition process is started and comprises the following steps: metal source compound is introduced to the reaction space and contacted with the substrates for a first pulse time; surplus metal source compound molecules and any byproduct molecules are removed from the reaction space during a first purge time; carbon source compound is introduced to the reaction space and contacted with the substrates for a second pulse time; surplus carbon source compound molecules and any byproduct molecules are removed from the reaction space during a second purge time.
- Source chemical gases flow through the conical holes of the substrate holder and contact the bearings that are held in the vertical gas streams. The process forms up to a molecular layer of metal carbide per pulsing cycle. After the deposition process, nitrogen flow is slowly decreased until the bearings have returned to the bottom of the cones.
- the substrate holder may be unloaded through a load lock or the pressure of the reaction chamber may be increased to the external room pressure with inert gas and the substrate holder unloaded without the use of a load lock chamber.
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Abstract
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AU10884/01A AU1088401A (en) | 1999-10-15 | 2000-10-16 | Deposition of transition metal carbides |
JP2001532259A JP4965782B2 (en) | 1999-10-15 | 2000-10-16 | Transition metal carbide deposition |
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US15979999P | 1999-10-15 | 1999-10-15 | |
FI19992233 | 1999-10-15 | ||
FI19992235 | 1999-10-15 | ||
FI19992234 | 1999-10-15 | ||
FI992235A FI117943B (en) | 1999-10-15 | 1999-10-15 | Deposition of metal carbide film on substrate, e.g. integrated circuit, involves atomic layer deposition |
US60/159,799 | 1999-10-15 | ||
FI992234A FI117944B (en) | 1999-10-15 | 1999-10-15 | A method for growing transition metal nitride thin films |
FI992233A FI118158B (en) | 1999-10-15 | 1999-10-15 | Process for modifying the starting chemical in an ALD process |
US17694800P | 2000-01-18 | 2000-01-18 | |
US60/176,948 | 2000-01-18 | ||
FI20000564A FI119941B (en) | 1999-10-15 | 2000-03-10 | A process for preparing nanolaminates |
FI20000564 | 2000-03-10 |
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AU1088401A (en) | 2001-04-30 |
KR20020063165A (en) | 2002-08-01 |
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