US20230103643A1 - ADVANCED BARRIER NICKEL OXIDE (BNiO) COATING DEVELOPMENT FOR THE PROCESS CHAMBER COMPONENTS - Google Patents
ADVANCED BARRIER NICKEL OXIDE (BNiO) COATING DEVELOPMENT FOR THE PROCESS CHAMBER COMPONENTS Download PDFInfo
- Publication number
- US20230103643A1 US20230103643A1 US17/449,844 US202117449844A US2023103643A1 US 20230103643 A1 US20230103643 A1 US 20230103643A1 US 202117449844 A US202117449844 A US 202117449844A US 2023103643 A1 US2023103643 A1 US 2023103643A1
- Authority
- US
- United States
- Prior art keywords
- chamber component
- layer
- metal plating
- nickel
- chamber
- 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.)
- Abandoned
Links
- 230000004888 barrier function Effects 0.000 title claims abstract description 93
- 229910000480 nickel oxide Inorganic materials 0.000 title claims abstract description 47
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims description 95
- 238000000576 coating method Methods 0.000 title description 17
- 239000011248 coating agent Substances 0.000 title description 16
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 172
- 229910052751 metal Inorganic materials 0.000 claims abstract description 166
- 239000002184 metal Substances 0.000 claims abstract description 166
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 84
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 58
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 18
- 239000007800 oxidant agent Substances 0.000 claims abstract description 12
- 238000007747 plating Methods 0.000 claims description 76
- 238000011109 contamination Methods 0.000 claims description 50
- 238000012545 processing Methods 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- 239000002253 acid Substances 0.000 claims description 24
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 claims description 17
- 239000008367 deionised water Substances 0.000 claims description 14
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 10
- DBJLJFTWODWSOF-UHFFFAOYSA-L nickel(ii) fluoride Chemical compound F[Ni]F DBJLJFTWODWSOF-UHFFFAOYSA-L 0.000 claims description 10
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 229910000838 Al alloy Inorganic materials 0.000 claims description 6
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 4
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- 239000011574 phosphorus Substances 0.000 claims description 4
- 230000003746 surface roughness Effects 0.000 claims description 3
- GRIMOWUYBQPMQB-UHFFFAOYSA-N O(F)F.[Ni] Chemical compound O(F)F.[Ni] GRIMOWUYBQPMQB-UHFFFAOYSA-N 0.000 claims description 2
- 239000010410 layer Substances 0.000 description 249
- 239000007789 gas Substances 0.000 description 54
- 238000004519 manufacturing process Methods 0.000 description 28
- 210000002381 plasma Anatomy 0.000 description 24
- 239000000758 substrate Substances 0.000 description 23
- 229910052731 fluorine Inorganic materials 0.000 description 21
- 239000011737 fluorine Substances 0.000 description 19
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 17
- 238000004140 cleaning Methods 0.000 description 16
- 238000007254 oxidation reaction Methods 0.000 description 16
- 239000000243 solution Substances 0.000 description 15
- 230000003647 oxidation Effects 0.000 description 13
- 239000002245 particle Substances 0.000 description 12
- 239000000203 mixture Substances 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 9
- 238000007772 electroless plating Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 235000012431 wafers Nutrition 0.000 description 9
- 238000003682 fluorination reaction Methods 0.000 description 7
- 229910052720 vanadium Inorganic materials 0.000 description 7
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000010408 film Substances 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 238000009713 electroplating Methods 0.000 description 5
- GVGCUCJTUSOZKP-UHFFFAOYSA-N nitrogen trifluoride Chemical compound FN(F)F GVGCUCJTUSOZKP-UHFFFAOYSA-N 0.000 description 5
- 230000001590 oxidative effect Effects 0.000 description 5
- 238000000231 atomic layer deposition Methods 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 238000012423 maintenance Methods 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 230000002829 reductive effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- MEIDRGPPJVWRKW-UHFFFAOYSA-N [F].[Ni] Chemical compound [F].[Ni] MEIDRGPPJVWRKW-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000005524 ceramic coating Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 230000001010 compromised effect Effects 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000002845 discoloration Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 229910001512 metal fluoride Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 229910021654 trace metal Inorganic materials 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 1
- -1 Al 6061) Chemical compound 0.000 description 1
- 229910017077 AlFx Inorganic materials 0.000 description 1
- 229910015844 BCl3 Inorganic materials 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- XPDWGBQVDMORPB-UHFFFAOYSA-N Fluoroform Chemical compound FC(F)F XPDWGBQVDMORPB-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 description 1
- 229910003910 SiCl4 Inorganic materials 0.000 description 1
- 229910004014 SiF4 Inorganic materials 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000001427 coherent effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000013500 data storage Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- WMIYKQLTONQJES-UHFFFAOYSA-N hexafluoroethane Chemical compound FC(F)(F)C(F)(F)F WMIYKQLTONQJES-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000000284 resting effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-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
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 description 1
- 238000009279 wet oxidation reaction Methods 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32431—Constructional details of the reactor
- H01J37/32458—Vessel
- H01J37/32477—Vessel characterised by the means for protecting vessels or internal parts, e.g. coatings
- H01J37/32495—Means for protecting the vessel against plasma
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1635—Composition of the substrate
- C23C18/1637—Composition of the substrate metallic substrate
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1635—Composition of the substrate
- C23C18/1639—Substrates other than metallic, e.g. inorganic or organic or non-conductive
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1689—After-treatment
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
-
- 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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
-
- 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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/56—Treatment of aluminium or alloys based thereon
Definitions
- Embodiments of the present disclosure relate, in general, to erosion resistant metal oxide coated chamber components and methods of forming and using such coated chamber components.
- devices are fabricated by a number of manufacturing processes producing structures of an ever-decreasing size. As device geometries shrink, controlling the process uniformity and repeatability of devices becomes much more challenging.
- Various semiconductor manufacturing processes use high temperatures, high energy plasma (such as remote and direct fluorine plasma such as NF 3 , CF 4 , and the like), a mixture of corrosive gases, corrosive cleaning chemistries (e.g., hydrofluoric acid) and combinations thereof. These extreme conditions may result in a reaction between materials of components within the process chamber and the plasma or corrosive gases to form metal fluorides, particles, other trace metal contaminates and high vapor pressure gases (e.g., AlF x ). Such gases may readily sublime and deposit on other components within the chamber. During a subsequent process step, the deposited material may release from the other components as particles and fall onto the wafer causing defects.
- high energy plasma such as remote and direct fluorine plasma such as NF 3 , CF 4 , and the like
- a mixture of corrosive gases e.g., hydrofluoric acid
- corrosive cleaning chemistries e.g., hydrofluoric acid
- gases e
- certain semiconductor processing chamber components include an electroless nickel plated (ENP) surface to reduce these defects.
- ENP electroless nickel plated
- the fluorine-containing layer develops because of contamination during use, thus the fluorine-containing layer can be considered a contamination layer.
- the fluorine-containing layer lessens the lifetime of one or more components of the process chamber and a mean wafers between cleaning (MWBC) metric.
- a chamber component for a processing chamber may include a body; a metal plating on at least one surface of the body, the metal plating comprising nickel; and a barrier layer on the metal plating.
- the barrier layer may include a nickel oxide.
- the metal plating may include nickel and phosphorus.
- the metal plating may include nickel and is free of phosphorous.
- the body includes aluminum, an aluminum alloy, aluminum nitride, alumina, or combinations thereof.
- the metal plating has a thickness of about 20 microns to about 75 microns
- the barrier layer has a thickness of about 2 nm to about 50 nm.
- the barrier layer has an average surface roughness (Ra) of about 2 micro-inches to about 60 micro-inches.
- the chamber component may be a showerhead for a process chamber.
- a method of protecting a chamber component includes forming a metal plating on a body of the chamber component, wherein the metal plating may include nickel, and contacting the metal plating with an oxidizing agent to form a barrier layer on the metal plating, wherein the barrier layer may include nickel oxide.
- the oxidizing agent may include one of at least one of hydrofluoric acid, oxalic acid, or nitric acid.
- the barrier layer may have a thickness from about 2 ⁇ m to about 60 ⁇ m.
- forming the metal plating may include performing electroless metal plating, and wherein the metal plating further comprises phosphorus.
- the body may include an aluminum alloy, aluminum nitride, alumina, or combinations thereof.
- the method may include removing a native oxide from the metal plating prior to forming the barrier layer.
- the method may include after the forming the metal playing, forming a nickel fluoride (NiF2) or nickel oxy-fluoride layer on the metal plating by contacting the metal plating with ammonium fluoride.
- NiF2 nickel fluoride
- nickel oxy-fluoride layer on the metal plating by contacting the metal plating with ammonium fluoride.
- the method may also include placing the chamber component in an acid bath comprising 5-25% hydrofluoric acid and 75-95% water to contact the metal plating with the oxidizing agent; subsequently placing the chamber component in a de-ionized water bath; subsequently placing the chamber component in the acid bath; and subsequently placing the chamber in the di-ionized water bath.
- a method of refurbishing a used chamber component may include removing a contamination layer from a metal plating on the used chamber component using a first acid solution, wherein the metal plating comprises nickel; and subsequently contacting the metal plating with an oxidizing agent to form a barrier layer on the metal plating, wherein the barrier layer comprises nickel oxide.
- the contamination layer may include nickel fluoride.
- the removing the contamination layer may include placing the used chamber component in a first acid bath, subsequently rinsing the used chamber component with deionized water, subsequently drying the used chamber component, subsequently placing the used chamber component in a second acid bath, subsequently rinsing the used chamber component with deionized water, and subsequently drying the used chamber component.
- the oxidizing agent may include at least one of hydrofluoric acid or nitric acid.
- the barrier layer may have a thickness from about 2 ⁇ m to about 60 ⁇ m.
- FIG. 1 A depicts a sectional view of one embodiment of a processing chamber
- FIG. 1 B depicts a sectional view of one embodiment of a showerhead for a processing chamber
- FIG. 2 illustrates one embodiment of a bottom view of a showerhead, in accordance with an embodiment
- FIG. 3 A illustrates a method of forming an advanced barrier oxide layer according to an embodiment
- FIG. 3 B illustrates another method of refurbishing and forming an advanced barrier oxide layer according to another embodiment
- FIG. 4 illustrates an example architecture of a manufacturing system
- FIG. 5 is a flow chart representing a method of forming an advanced barrier oxide layer according to an embodiment
- FIG. 6 is a flow chart representing a method of refurbishing and forming an advanced barrier layer according to another embodiment
- Embodiments disclosed herein describe coated articles, coated chamber components, methods of coating articles and chamber components, methods of reducing or eliminating particles from semiconductor processing chambers, and methods of using coated articles and chamber components and processing chambers containing coated chamber components.
- a metal layer e.g., which may be a metal coating or metal plating
- the metal layer may be a nickel-containing layer (e.g., a pure nickel layer or a layer having nickel as a primary constituent and additionally including other materials such as phosphorous and/or vanadium).
- the barrier layer may be a nickel oxide layer formed under controlled conditions.
- the barrier layer may be added to new chamber components to improve a lifespan of the chamber components and/or to reduce or eliminate a buildup of a contamination layer on the chamber component. Further, to improve the life of the coated articles or coated chamber components (which may be new or used chamber components), they may be treated to remove a contamination layer and to add a barrier layer over a metal layer on the chamber components.
- a metal layer e.g., an ENP comprising nickel
- a metal layer e.g., an ENP comprising nickel
- a native oxide naturally occurs on the metal layer due to exposure to air.
- the native oxide has undesirable properties.
- the native oxide interacts with process gases (e.g., fluorine) to form a contamination layer.
- process gases e.g., fluorine
- the native oxide's interaction with fluorine causes discoloration and forms a black film (contamination layer) over the metal coating that produces particles that can contaminate processed substrates. If a black film/contamination layer is present on a chamber component such as a shower head, there may be a drop in yield for substrates processed by the process chamber that includes the shower head having the contamination layer.
- the chamber component is removed and replaced.
- embodiments improve the surface of chamber components such as showerheads to prevent the formation of the black film/contamination layer over a metal layer of the chamber components. It would be advantageous to have a protective barrier layer to prevent the chemical degradation of the surface metal layer and formation of the black film/contamination layer.
- a chamber component having a protective barrier layer may also degrade and/or become contaminated more slowly than a chamber component lacking the barrier layer, which may cause the chamber component with the barrier layer over the metal layer to have a higher mean wafers between cleaning than a chamber component with a metal layer and lacking the barrier layer.
- the mean wafers between cleaning represents the mean number of wafers that are processed between each cleaning of the chamber component. Such an increased mean wafers between cleaning may be particularly pronounced for chamber components used in chambers that perform processes at higher temperatures of about 200° C. or above.
- chamber components for processing chambers and/or processing chambers containing such chamber components e.g., semiconductor processing chambers
- the chamber components include a chamber component and a metal layer (e.g., a metal plating or a metal coating) on at least one surface of the chamber component.
- the metal layer may include an advanced barrier layer in embodiments.
- a chamber component may include a metal layer on a surface of the substrate.
- the chamber component or portions thereof may be composed of, without limitation, one or more of a metal, for example, aluminum, stainless steel and/or titanium, a ceramic, for example, alumina, silica and/or aluminum nitride, and/or combinations thereof.
- the metal layer may be an electroless metal plating including nickel or an electrolytic metal plating including nickel.
- a chamber component may be plated using an electroless plating process to form an electroless metal plating on one or more surface of the chamber component.
- the electroless metal plating may be a nickel-phosphorous plating.
- the electroless plating process can form a metal plating directly on the surface of the chamber component.
- the chamber component may be plated using an electrolytic metal plating process.
- the electrolytic plating process may form a layer containing nickel, silver and/or gold.
- one or more surface of the chamber component may be coated using a sputtering process, such as a sputtering process that sputters a nickel-containing coating onto the one or more surface of the chamber component.
- the nickel containing coating may include, for example, 98-99 atomic % nickel and 1-2 atomic % vanadium.
- the chamber component when the chamber component is coated with an electroless plating process, the chamber component is placed in a bath that contains nickel and phosphorous.
- the bath may include about 84% nickel and about 16% phosphorous, about 86% nickel and 14% phosphorous, about 88% nickel and about 12% phosphorous, about 90% nickel and about 10% phosphorous, about 92% nickel and about 8% phosphorous, about 94% nickel and about 6% phosphorous, and about 96% nickel and about 4% phosphorous.
- the bath may include about 84-96% nickel and about 4-16% phosphorous.
- the coating is free of phosphorous.
- the plating may be 100% nickel.
- the chamber component is coated with a sputtered nickel.
- the sputtered nickel as understood by one of skill in the art, may include nickel and vanadium. The vanadium may be present in the sputtered nickel in about 1% to about 2%.
- the layer when the chamber component includes a metal layer that is an electroless nickel plating or an electrolytic Ni plating, the layer may be in a thickness from about 20 microns to about 75 microns, from about 25 microns to about 70 microns, from about 30 microns to 60 microns, or from about 35 microns to about 50 microns.
- the metal layer may have a hardness from about 450 HV to about 500 HV.
- the roughness of the metal layer may be less than 50 ⁇ inch in embodiments.
- the thickness of the metal layer formed by electroless plating may be targeted based on the amount of time that the chamber component is in the bath.
- the chamber component may be in the bath for about one minute to about three minutes to form the metal layer having a target thickness.
- a contamination layer may be found on the metal layer.
- the contamination layer may include a combination of nickel, fluorine and/or oxygen.
- the metal layer is a nickel layer that becomes slowly fluorinated over time due to exposure to fluorine-rich chemistries.
- a contamination layer of nickel fluorine and/or nickel oxy-fluorine may be formed on the surface of the metal layer.
- the contamination layer may react to process gases differently than the metal layer, and may cause subtle changes to process chemistries.
- the contamination layer may flake off of the chamber component and/or cause particle contamination on substrates processed in the process chamber in which the chamber component is installed. As a result, periodic maintenance may be performed on chamber components to remove those chamber components that include the contamination layer and to replace the removed chamber components with new chamber components that lack the contamination layer.
- the chamber component includes a barrier layer comprising nickel oxide over a metal layer (e.g., a nickel layer).
- a metal layer e.g., a nickel layer
- the formation of the barrier layer (e.g., the nickel oxide barrier layer) on the metal layer protects the metal layer from attack by process gases, and in particular to attack by fluorine-containing plasmas and other fluorine-containing chemistries.
- the barrier layer may be referred to as a protective layer.
- the nickel oxide barrier layer may be formed using an oxidation process, which may include immersing the chamber component (or a portion thereof that is to have a nickel oxide barrier layer) into a bath containing an oxidation agent (e.g., a bath containing hydrofluoric acid and/or nitric acid with water).
- the chamber component includes generating a nickel fluorination (NiF 2 ) or nickel oxy-fluorination (NiOF) layer after removing the contamination layer and before forming the barrier layer.
- the nickel fluorination or nickel oxy-fluorination layer may be generated by placing the metal plated chamber component in a bath with an ammonium fluoride (NH 4 F) solution.
- the ammonium fluoride solution may have a concertation from about 0.5 M to about 3 M.
- the metal plated chamber component remains in the bath for about 5 minutes to about 60 minutes at a temperature of about 35 to about 45° C. to form a nickel fluorinated or nickel oxy-fluorinated layer.
- Ni is present in an amount of abut 60 wt. % and F is present in an amount of about 40 wt. %.
- a nickel oxy-fluorinated layer is formed, then Ni is present in an amount of about 62 wt. %, F is present in an amount of about 20 wt %, and O is present in an amount of about 17 wt. %.
- the nickel oxide barrier layer may be formed using an oxidation process as described herein.
- preventative maintenances may be reduced by two times up to ten times in embodiments as compared to the number and/or frequency of preventative maintenances performed to service and/or replace chamber components having an exposed nickel layer.
- Some embodiments are descried herein with reference to a showerhead, and are particularly useful for coating chamber components having both high aspect ratio features and regions that are directly exposed to bombardment by a plasma.
- the barrier layer described herein can also be beneficially used on many other chamber components having metal layers that are exposed to plasma, such as chamber components for a plasma etcher (also known as a plasma etch reactor) or other processing chambers including walls, liners, bases, rings, view ports, lids, nozzles, substrate holding frames, electrostatic chucks (ESCs), face plates, selectivity modulation devices (SMDs), plasma sources, pedestals, and so forth.
- a plasma etcher also known as a plasma etch reactor
- ESCs electrostatic chucks
- SMDs selectivity modulation devices
- plated or coated chamber components and other articles that may cause reduced particle contamination when used in a process chamber for plasma rich processes.
- the plated or coated articles discussed herein may also provide reduced particle contamination when used in process chambers for other processes such as non-plasma etchers, non-plasma cleaners, chemical vapor deposition (CVD) chambers, physical vapor deposition (PVD) chambers, and so forth.
- CVD chemical vapor deposition
- PVD physical vapor deposition
- FIG. 1 A is a sectional view of a processing chamber 100 (e.g., a semiconductor processing chamber) having one or more chamber components that include a metal layer and a nickel oxide-containing barrier layer over the metal layer in accordance with embodiments of the present disclosure.
- the processing chamber 100 may be used for processes in which a corrosive plasma environment and/or corrosive chemistry is provided.
- the processing chamber 100 may be a chamber for a plasma etch reactor (also known as a plasma etcher), a plasma cleaner, an atomic layer deposition (ALD) chamber that performs plasma-enhanced ALD, other deposition chambers, and so forth.
- a plasma etch reactor also known as a plasma etcher
- ALD atomic layer deposition
- chamber components that may include a metal layer and a barrier layer over the metal layer are a substrate support assembly 148 , an electrostatic chuck (ESC), a ring (e.g., a process kit ring or single ring), a chamber wall, a base, a showerhead 130 , a gas distribution plate, a liner, a liner kit, a shield, a plasma screen, a flow equalizer, a cooling base, a chamber viewport, a chamber lid, a nozzle, process kit rings, and so on.
- ESC electrostatic chuck
- a ring e.g., a process kit ring or single ring
- a chamber wall e.g., a chamber wall, a base, a showerhead 130 , a gas distribution plate, a liner, a liner kit, a shield, a plasma screen, a flow equalizer, a cooling base, a chamber viewport, a chamber lid, a nozzle, process kit rings, and so on.
- the metal layer is a nickel-containing layer (e.g., 100% nickel or nickel in combination with one or more additional materials such as phosphorous and/or vanadium).
- the barrier layer is a nickel-oxide containing layer (e.g., 100% nickel oxide or nickel oxide with one or more additional materials such as phosphorous and/or vanadium). The metal layer and the barrier layer may be conformal thin films.
- the processing chamber 100 includes a chamber body 102 and a showerhead 130 that enclose an interior volume 106 .
- the showerhead 130 may or may not include a gas distribution plate.
- the showerhead may be a multi-piece showerhead that includes a showerhead base and a showerhead gas distribution plate bonded to the showerhead base.
- the showerhead 130 may be replaced by a lid and a nozzle in some embodiments, or by multiple pie shaped showerhead compartments and plasma generation units in other embodiments.
- the chamber body 102 may be fabricated from aluminum, stainless steel or other suitable material.
- the chamber body 102 generally includes sidewalls 108 and a bottom 110 . Any of the showerhead 130 (or lid and/or nozzle), sidewalls 108 and/or bottom 110 may include the multi-layer plasma resistant coating.
- An outer liner 116 may be disposed adjacent the sidewalls 108 to protect the chamber body 102 .
- the outer liner 116 may be a halogen-containing gas resist material such as Al 2 O 3 or Y 2 O 3 .
- the outer liner 116 may be coated with the multi-layer plasma resistant ceramic coating in some embodiments.
- An exhaust port 126 may be defined in the chamber body 102 , and may couple the interior volume 106 to a pump system 128 .
- the pump system 128 may include one or more pumps and throttle valves utilized to evacuate and regulate the pressure of the interior volume 106 of the processing chamber 100 .
- the showerhead 130 may be supported on the sidewalls 108 of the chamber body 102 and/or on a top portion of the chamber body.
- the showerhead 130 (or lid) may be opened to allow access to the interior volume 106 of the processing chamber 100 , and may provide a seal for the processing chamber 100 while closed.
- a gas panel 158 may be coupled to the processing chamber 100 to provide process and/or cleaning gases to the interior volume 106 through the showerhead 130 or lid and nozzle.
- the showerhead 130 includes multiple gas delivery holes 132 throughout the showerhead 130 .
- the showerhead 130 may be or include aluminum, anodized aluminum, an aluminum alloy (e.g., Al 6061), or an anodized aluminum alloy.
- the showerhead includes a gas distribution plate (GDP) bonded to the showerhead.
- the GDP may be, for example, Si or SiC.
- the GDP may additionally include multiple holes that line up with the holes in the showerhead.
- FIG. 1 B illustrates a zoomed in view of a portion of the showerhead 130 of FIG. 1 A .
- the showerhead 130 is coated by a metal layer 150 and a barrier layer 152 .
- a surface of the showerhead and walls of holes 132 in the showerhead are coated by a thin conformal metal layer 150 .
- the backside of the showerhead 130 and outer side walls of the showerhead may also be coated by the conformal metal layer 150 .
- a non-line of sight deposition technique such as ALD or plating (e.g., electroplating or electroless plating) may be used to deposit or form the metal layer 150 on the surface of the showerhead 130 and on the walls of the holes 132 in the showerhead 130 .
- a line-of-sight deposition technique such as sputtering may be used to form the metal layer.
- the metal layer 150 may be nickel, nickel doped with phosphorous, or nickel doped with vanadium in embodiments.
- a barrier layer 152 covers the metal layer 150 at some or all regions of the surface of the showerhead 130 .
- the barrier layer 152 may be formed using an oxidation process, which may be a dry oxidation process or a wet oxidation process (e.g., by dipping the showerhead 130 into a bath containing an oxidizing agent such as hydrofluoric acid or nitric acid.
- the barrier layer 152 may cover the metal layer on all surfaces of the chamber component, including on the inner walls of holes in the showerhead 130 .
- the barrier layer may be a grown layer and may be conformal and uniform in embodiments.
- the uniform barrier layer may have a difference in thickness of less than about 10% across the surface of the showerhead in embodiments.
- processing gases that may be used to process substrates in the processing chamber 100 include halogen-containing gases, such as C 2 F 6 , SF 6 , SiCl 4 , HBr, NF 3 , CF 4 , CHF 3 , CH 2 F 3 , F, Cl 2 , CCl 4 , BCl 3 and SiF 4 , among others, and other gases such as O 2 , or N 2 O.
- halogen-containing gases such as C 2 F 6 , SF 6 , SiCl 4 , HBr, NF 3 , CF 4 , CHF 3 , CH 2 F 3 , F, Cl 2 , CCl 4 , BCl 3 and SiF 4 , among others, and other gases such as O 2 , or N 2 O.
- carrier gases include N 2 , He, Ar, and other gases inert to process gases (e.g., non-reactive gases).
- the fluorine based gases may cause fluoride deposits to buildup on the holes of standard showerhead
- a substrate support assembly 148 is disposed in the interior volume 106 of the processing chamber 100 below the showerhead 130 .
- the substrate support assembly 148 holds a substrate 144 (e.g., a wafer) during processing.
- the substrate support assembly 148 may include an electrostatic chuck that secures the substrate 144 during processing, a metal cooling plate bonded to the electrostatic chuck, and/or one or more additional components.
- An inner liner may cover a periphery of the substrate support assembly 148 .
- the inner liner may be a halogen-containing gas resist material such as Al 2 O 3 or Y 2 O 3 .
- the substrate support assembly, portions of the substrate support assembly, and/or the inner liner may be coated with the metal layer and barrier layer in some embodiments.
- FIG. 2 illustrates one embodiment of a bottom view of a showerhead 200 .
- the showerhead 200 may have a series of gas conduits 204 (also referred to as holes) arranged concentrically that evenly distribute plasma gasses directly over a substrate or wafer to be etched or processed.
- the showerhead is depicted here having approximately 1100 gas conduits 204 arranged in evenly distributed concentric rings for even distributing of gasses.
- the gas conduits 204 may be configured in alternative geometric configurations on the lower surface 205 of the showerhead (or on a lower surface of a GDP bonded to a showerhead).
- the showerhead may have a square or rectangular configuration having rows and columns of gas conduits 204 .
- the showerhead 200 can have many gas conduits 204 , as depicted, or as few gas conduits as appropriate depending on the type of reactor and/or process utilized.
- some or all gas conduits 204 do not include branches (e.g., each gas conduit may have a single entry point and a single exit point). Additionally, the gas conduits may have various lengths and orientation angles. Gas may be delivered to the gas conduits 204 via one or more gas delivery nozzles. Some gas conduits 204 may receive the gas before other gas conduits 204 (e.g., due to a proximity to a gas delivery nozzle). However, the gas conduits 204 may be configured to deliver gas to a substrate resting beneath the showerhead at approximately the same time based on varying the orientation angles, diameters and/or lengths of the gas conduits 204 , or by using an additional flow equalizer. For example, gas conduits 204 that will receive gas first may be longer and/or have a greater angle (e.g., an angle that is further from 90 degrees) than conduits that will receive gas later.
- a greater angle e.g., an angle that is further from 90 degrees
- a schematic 300 of oxidizing the metal plated coated chamber component is illustrated.
- a metal plated chamber component includes a nickel layer 301 and a bare aluminum body 302 of the chamber component, wherein the nickel layer 301 is on a surface of the bare aluminum body 302 .
- the metal plated chamber component undergoes an oxidation process 305 according to the present disclosure.
- the metal plated chamber component includes a dense barrier layer 303 of nickel oxide on a surface of the nickel layer 301 .
- the barrier layer 303 of NiO may prevent discoloration of the metal layer.
- the barrier layer 303 may also prevent as the chamber component from becoming a source of particles on processed substrates.
- the barrier layer 303 of NiO may also inhibit the reaction of fluorine with nickel in the nickel layer 301 to prevent the formation of a discolored/contaminated layer.
- the barrier layer 303 may prevent a native oxide from forming on the nickel layer 1 .
- the chamber component may be a used chamber component that has been used to perform one or more processes on substrates, where the processes exposed the substrates to a fluorine-rich environment.
- the chamber component may not have been coated with a barrier layer prior to use.
- the chamber component may include a contamination layer over the metal layer 302 .
- the chamber component may be refurbished by removing the contamination layer to expose the metal layer, and then form the barrier layer over the metal layer. A schematic of such embodiment is illustrated in schematic 350 of FIG. 3 B .
- the chamber component includes an aluminum body 302 having a metal layer 301 disposed thereon, and a contamination layer 310 over the metal layer 301 .
- the chamber component may undergo a cleaning process 315 to strip the contamination layer 310 from the metal layer 301 .
- the chamber component having the cleaned metal layer 301 may then be processed using an oxidation process 305 to form barrier layer 303 , as described in more detail in the present disclosure.
- the contamination layer 310 is removed and a barrier layer 303 of dense nickel oxide is present over the metal layer 301 .
- FIG. 4 illustrates an example architecture of a manufacturing system 400 .
- the manufacturing system 400 may be a manufacturing system for applying platings and/or coatings to articles such as chamber components.
- the manufacturing system 400 includes manufacturing machines 401 (e.g., processing equipment) connected to an equipment automation layer 415 .
- the manufacturing machines may include a polisher 402 , one or more wet cleaners 403 , a plating system 404 , a sputtering system 405 , an oxidation system 406 , and/or other machines.
- the manufacturing system 400 may further include one or more computing device 420 connected to the equipment automation layer 415 .
- the manufacturing system 400 may include more or fewer components.
- the manufacturing system 400 may include manually operated (e.g., off-line) manufacturing machines 401 without the equipment automation layer 415 or the computing device 420 .
- Polisher 402 is a machine configured to polish or smoothen the surface of articles such as chamber components for processing chambers.
- Polisher 402 may be, for example, a chemical mechanical planarization (CMP) device or an abrasive polisher.
- CMP chemical mechanical planarization
- a motorized abrasive pad may be used to smoothen the surface of an article.
- a sander may rotate or vibrate the abrasive pad while the abrasive pad is pressed against a surface of the article.
- a roughness achieved by the abrasive pad may depend on an applied pressure, on a vibration or rotation rate and/or on a roughness of the abrasive pad.
- Wet cleaners 403 are cleaning apparatuses that clean articles (e.g., articles) using a wet clean process.
- Wet cleaners 403 include wet baths filled with liquids, in which the substrate is immersed to clean the substrate.
- Wet cleaners 403 may agitate the wet bath using ultrasonic waves during cleaning to improve a cleaning efficacy. This is referred to herein as sonicating the wet bath.
- wet cleaners 403 include a first wet cleaner that contains deionized (DI) water and a second wet cleaner that contains an acid solution.
- the acid solution may be a hydrofluoric acid (HF) solution, a hydrochloric acid (HCl) solution, a nitric acid (HNO 3 ) solution, or combination thereof in embodiments.
- the acid solution may remove surface contaminants from the article and/or may remove an oxide from the surface of the article. Cleaning the article having a metal layer with the acid solution prior to forming a barrier layer over the metal layer may improve a quality of the barrier layer formed over the metal layer.
- an acid solution containing approximately 5 to 15 vol % HF is used to clean chamber components having a nickel layer.
- an acid solution containing approximately 5 to 15 vol % HNO 3 is used to clean articles having a nickel layer.
- the wet cleaners 403 may clean articles at multiple stages during processing. For example, wet cleaners 403 may clean an article after a substrate has been polished, before performing plating (e.g., electroplating), before forming a barrier layer over a metal plating, and so on.
- plating e.g., electroplating
- dry cleaners may be used to clean the articles.
- Dry cleaners may clean articles by applying heat, by applying gas, by applying plasma, and so forth.
- Plating system 404 is a system that performs electroplating (e.g., of Ni) or electroless plating (e.g., of Ni).
- Plating system 404 may be an electroplating system that applies a current to reduce dissolved metal cations so that they form a thin coherent metal coating on the article (e.g., on surfaces of a chamber component such as an aluminum chamber component).
- the article to be plated may be the cathode of a circuit and a metal donor may be the anode of the circuit.
- the article and metal donor may be immersed in an electrolyte containing one or more dissolved metal salts and/or other ions that increase an electrical conductivity of the electrolyte. Metal from the metal donor than plates a surface of the article.
- Electroless plating also known as chemical or auto-catalytic plating, is a non-galvanic plating method that involves several simultaneous reactions in an aqueous solution, which occur without the use of external electrical power. The reaction is accomplished when hydrogen is released by a reducing agent, normally sodium hypophosphite or thiourea, and oxidized, thus producing a negative charge on the surface of the part.
- a reducing agent normally sodium hypophosphite or thiourea
- the equipment automation layer 415 may interconnect some or all of the manufacturing machines 401 with computing devices 420 , with other manufacturing machines, with metrology tools and/or other devices.
- the equipment automation layer 415 may include a network (e.g., a location area network (LAN)), routers, gateways, servers, data stores, and so on.
- Manufacturing machines 401 may connect to the equipment automation layer 415 via a SEMI Equipment Communications Standard/Generic Equipment Model (SECS/GEM) interface, via an Ethernet interface, and/or via other interfaces.
- SECS/GEM SEMI Equipment Communications Standard/Generic Equipment Model
- the equipment automation layer 415 enables process data (e.g., data collected by manufacturing machines 401 during a process run) to be stored in a data store (not shown).
- the computing device 420 connects directly to one or more of the manufacturing machines 401 .
- some or all manufacturing machines 401 include a programmable controller that can load, store and execute process recipes.
- the programmable controller may control temperature settings, gas and/or vacuum settings, time settings, etc. of manufacturing machines 401 .
- the programmable controller may include a main memory (e.g., read-only memory (ROM), flash memory, dynamic random access memory (DRAM), static random access memory (SRAM), etc.), and/or a secondary memory (e.g., a data storage device such as a disk drive).
- the main memory and/or secondary memory may store instructions for performing heat treatment processes described herein.
- the programmable controller may also include a processing device coupled to the main memory and/or secondary memory (e.g., via a bus) to execute the instructions.
- the processing device may be a general-purpose processing device such as a microprocessor, central processing unit, or the like.
- the processing device may also be a special-purpose processing device such as an application specific integrated circuit (ASIC), a field programmable gate array (FPGA), a digital signal processor (DSP), network processor, or the like.
- programmable controller is a programmable logic controller (PLC).
- the manufacturing machines 401 are programmed to execute recipes that will cause the manufacturing machines to polish an article, clean an article, plate an article, form a barrier layer on an article, and so on. In one embodiment, the manufacturing machines 401 are programmed to execute recipes that perform operations of a multi-step process for manufacturing an article having a metal layer and a barrier layer, as described with reference to FIGS. 5 - 6 .
- the computing device 420 may store one or more plating, oxidizing, cleaning and/or polishing recipes 425 that can be downloaded to the manufacturing machines 401 to cause the manufacturing machines 401 to manufacture articles in accordance with embodiments of the present disclosure.
- FIG. 5 is a flow chart representing a method 500 of refurbishing, and forming an advanced barrier oxide layer on, a chamber component according to an embodiment.
- Method 500 may be performed on chamber components having a metal layer (e.g., a metal plating) that has been used to perform one or more cycles of one or more manufacturing processes that expose the chamber component to chemistries that cause formation of a contamination layer on the metal layer.
- the contamination layer may contain oxygen, fluorine and/or one or more process elements.
- the contamination layer may cause particle contamination and/or negatively affect future processes performed in the process chamber in embodiments. Accordingly, in some embodiments of the present disclosure, when a contamination layer is present on the metal plated chamber component, the chamber component is placed in a first bath 502 .
- the first bath may include water and a first acid (e.g., hydrofluoric acid, nitric acid (HNO 3 ), sulfuric acid (H 2 SO 4 ), oxalic acid (HC 2 O 4 ), or ammonium fluoride (NH 4 F)).
- the hydrofluoric acid may be included in an amount from about 5 wt. % to about 15 wt. % in the bath based on the total composition of the first bath.
- the water may be included in an amount from about 85 wt. % to about 95 wt. % in the bath based on the total composition of the bath.
- the first bath includes about 5 wt. % hydrofluoric acid and about 95 wt. % water.
- the first bath may be at a temperature from about 25° C. to about 35° C.
- the used metal plated chamber component may be placed in the first bath for about one minute to about 30 minutes to loosen the contamination layer. After soaking in the first bath, the metal plated chamber may include a loosened contamination layer.
- the metal plated chamber component may then be rinsed (e.g., with deionized water) to remove the loosened contamination layer and dried at block 504 .
- the metal plated chamber component is placed into the first bath or a second bath at block 506 .
- the second bath includes water and an acid (e.g., hydrofluoric acid).
- the acid may be included in an amount from about 5 wt. % to about 15 wt. % in the bath based on the total composition of the first bath or second bath.
- the water may be included in an amount from about 85 wt. % to about 95 wt. % in the bath based on the total composition of the first bath or second bath.
- the second bath includes about 5 wt. % hydrofluoric acid and about 95% water.
- the second bath may be at a temperature from about 25° C. to about 35° C.
- the used metal plated chamber component may be placed in the second bath for about one minute to about 30 minutes, where the remaining contamination layer may be removed. After the second bath, the metal plated chamber component may be rinsed (e.g., with deionized water) and dried 508 .
- the metal plated chamber component may then be polished after removing the contamination layer 510 .
- the metal plated chamber component may be polished using an automatic polisher with different polishing sheets, such as a Scotch-Brite® sheet, or another advanced method to uniformly polish a surface.
- the metal plated coated chamber component may be polished until the surface roughness is about 10 ⁇ in to about 20 ⁇ in in one embodiment.
- the metal plated coated chamber component may undergo an oxidation treatment 512 .
- the oxidation treatment may be performed by placing the metal plated coated chamber component in a third bath.
- the third bath includes water and an acid (e.g., nitric acid (HNO 3 ), sulfuric acid (H 2 SO 4 ), oxalic acid (HC 2 O 4 ), or ammonium fluoride (NH 4 F)).
- the acid may be included in an amount from about 5 wt. % to about 25 wt. % in the bath based on the total composition of the third bath.
- the water may be included in an amount form about 75 wt. % to about 95 wt. % in the bath based on the total composition of the third bath.
- the third bath may include about 5 wt. % hydrofluoric acid and about 95 wt. % water.
- the third bath may be at a temperature from about 25° C.
- the metal plated chamber component may be placed in the third bath for about one minute to about 30 minutes.
- the oxidized metal plated chamber component may be rinsed (e.g., with deionized water), where a nickel oxide layer may be formed on the surface of the metal plating layer.
- the nickel oxide layer may be between about 5 nanometers to about 35 nanometers in one embodiment.
- the metal plated coated chamber component may be a new component, which may be oxidized through a second method 600 .
- FIG. 6 is a flow chart representing a method of forming an advanced barrier layer on a metal plated or metal coated chamber component according to an embodiment.
- the metal plated chamber component is placed in a first bath 602 .
- the first bath may include water and an acid (e.g., hydrofluoric acid).
- the hydrofluoric acid may be included in an amount from about 5 wt. % to about 25 wt. % in the bath based on the total composition of the first bath.
- the water may be included in an amount form about 75 wt. % to about 95 wt.
- the first bath includes about 5 wt. % hydrofluoric acid and about 95 wt. % water.
- the first bath may be at a temperature from about 25° C. to about 35° C.
- the metal plated chamber component may be placed in the first bath for about one minute to about 30 minutes. After the first bath 604 , the metal plated chamber component may be rinsed (e.g., with deionized water) and dried 606 .
- the metal plated chamber component may be treated with an acid (e.g., hydrofluoric acid or nitric acid (HNO 3 )) to oxidize the metal plating layer and form a nickel oxide layer 608 .
- the metal plated coated chamber component may be treated for a time from about one minute to about 30 minutes until a target thickness of the nickel oxide layer is achieved.
- the nickel oxide layer may be between about 5 nanometers to about 30 nanometers in embodiments, such as about 15 nanometers.
- the metal plated coated chamber component is then rinsed with deionized water and dried at block 610 .
- the metal plated coated chamber component may be a new component, having a nickel fluorinated or nickel oxy-fluorinated layer, and oxidizing the chamber component.
- FIG. 7 is a flow chart representing a method of forming an advanced barrier layer on a metal plated or metal coated chamber component having a nickel fluorinated (NiF 2 ) or nickel oxy-fluorinated (NiOF) layer according to an embodiment.
- the chamber component is placed in a first bath and rinsed in steps 702 to 706 , as described in FIG. 6 , steps 602 to 606 .
- the chamber component After rinsing and drying the chamber component, the chamber component is then placed in a second bath including an ammonium fluoride solution 708 to form a nickel fluorine or nickel oxy-fluorine layer.
- the ammonium fluoride solution has a concentration of about 0.5M to about 3 M.
- the chamber component remains in the second bath for about 5 minutes to about 60 minutes, where the second bath is at a temperature of about 35 to 45° C. to form a NiF 2 or NiOF layer.
- the chamber component is then removed from the bath 710 .
- the chamber component is then rinsed and dried in step 712 as described above for step 606 in FIG. 6 .
- the chamber component may be treated with an acid (e.g., hydrofluoric acid or nitric acid (HNO 3 )) to oxidize the metal plating layer 718 and form a nickel oxide layer as described above in steps 512 and 608 in FIGS. 5 and 6 , respectively.
- an acid e.g., hydrofluoric acid or nitric acid (HNO 3 )
- the metal plated chamber component may be oxidized through an in situ method. This method may occur in the same chamber in which the chamber component is being coated with the nickel plated coating or in the chamber in which the part will be used.
- the metal plated chamber component may be treated with a gas and moisture while the chamber component is in the chamber.
- the gas may be selected from the group consisting of NH 3 , NF 3 , HF or H 2 , or a combination thereof.
- the gas may be a combination of NH 3 and NF 3 or NH 3 , NF 3 and HF.
- the gas may be in a concentration from about 5 sccm to about 2000 sccm of total gas.
- the gas reacts with the ambient moisture within the chamber.
- the temperature of the chamber be from about 150° C. to about 220° C.
- the nickel oxide coating layer may have a thickness of about 4 nm to about 50 nm.
- the inventors have found that the lifetime of the part may be more than 10 times that of the original coating that lacks the barrier layer.
- the standard lifetime is about 3000 cycles.
- the lifetime of the part increases almost 10 times more than the standard lifetime of the part, where the lifetime is greater than 10,000 cycles.
- the inventors have found that the oxidation method can be used to coat a new part and for refurbishing an existing part where a contamination layer has formed.
- a showerhead having a nickel plating and a nickel oxide barrier layer on the nickel plating.
- the showerhead was first coated with nickel layer using a metal plating process.
- a natural oxide layer was formed on the nickel plating prior to formation of an intentional nickel oxide layer.
- the natural nickel oxide layer has inferior properties and impedes the formation of a target nickel oxide layer that will reduce particle contamination and improve a lifespan of the chamber component.
- the native nickel oxide layer may have a thickness of about 2 to 3 nm.
- the showerhead then underwent an oxidization treatment in which the showerhead was placed in a bath of 5% (5%-25%) hydrofluoric acid and 95% water at a temperature between 25 to 35° C.
- the showerhead was removed from the bath and rinsed with deionized water.
- a barrier nickel oxide layer was formed over the nickel layer.
- the barrier nickel oxide (NiO) layer on the metal layer had a thickness of from about 6 nm to about 22 nm.
- a showerhead comprising a nickel plating (a nickel ENP) that has been used, where a contamination layer has formed on the showerhead as a result of the use.
- the total thickness of the contamination layer i.e., a fluorinated or oxy-fluorinated layer
- the showerhead was cleaned to remove the contamination layer by placing the showerhead in a first bath of 5% (5%-25%) hydrofluoric acid and 95% water for 40 minutes at 25 to 40° C. The showerhead was then removed from the first bath and rinsed with deionized water and dried. After it was dried, the showerhead was then placed in a second bath of 25% hydrofluoric acid and 75% water for 40 minutes at 25 to 40° C. The showerhead was then removed from the second bath and rinsed again with deionized water and dried.
- the contamination layer was removed from the showerhead as a result of the cleaning.
- the showerhead was then treated and oxidized by placing the showerhead in a bath of 5% hydrofluoric acid to form a barrier layer over the ENP layer.
- a barrier nickel oxide layer was formed on the ENP layer as a result of the treatment and oxidation.
- the barrier nickel oxide (NiO) layer on the ENP coating layer had a combined thickness of about 22 nm.
- An EDS line profile of the barrier NiO layer on the ENP layer showed that nickel was present in the barrier NiO layer and there was no phosphorous in such layer.
- a TEM image and an EDS line profile of an inside of a small hole of the showerhead was also taken, and showed that the barrier layer had a thickness between 6.3 nm to 31.2 nm.
- the barrier layer on the backside of the showerhead was also measured to have a thickness of about 19 to 30 nm. This was also shown in an EDS line profile. This confirms that the barrier nickel oxide layer was formed along the entire showerhead, and was not limited to only the front side of the showerhead.
- a showerhead comprising a nickel plating (a nickel ENP) coating that is treated with ammonium fluoride (NH 4 F) solution having a concentration of 0.5M to 3M to convert a fluorinated (NiF 2 ) or oxidized-fluorinated (NiOF) layer having a thickness of about 6 nm to about 50 nm.
- the showerhead underwent an oxidization treatment in which the showerhead was placed in a bath of 5% (5%-25%) hydrofluoric acid and 95% water at a temperature between 25 to 35° C. to have a NiO thickness of about 6 nm to about 50 nm.
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Abstract
Description
- Embodiments of the present disclosure relate, in general, to erosion resistant metal oxide coated chamber components and methods of forming and using such coated chamber components.
- In the semiconductor industry, devices are fabricated by a number of manufacturing processes producing structures of an ever-decreasing size. As device geometries shrink, controlling the process uniformity and repeatability of devices becomes much more challenging.
- Various semiconductor manufacturing processes use high temperatures, high energy plasma (such as remote and direct fluorine plasma such as NF3, CF4, and the like), a mixture of corrosive gases, corrosive cleaning chemistries (e.g., hydrofluoric acid) and combinations thereof. These extreme conditions may result in a reaction between materials of components within the process chamber and the plasma or corrosive gases to form metal fluorides, particles, other trace metal contaminates and high vapor pressure gases (e.g., AlFx). Such gases may readily sublime and deposit on other components within the chamber. During a subsequent process step, the deposited material may release from the other components as particles and fall onto the wafer causing defects. Additional issues caused by such reactions include deposition rate drift, etch rate drift, compromised film uniformity, and compromised etch uniformity. It is beneficial to reduce these defects with a stable, non-reactive coating on chamber components to limit the sublimation and/or formation of particles and metal contaminants on the chamber components within the chamber.
- Hence, certain semiconductor processing chamber components (e.g., liners, doors, lids, shower heads and so on) include an electroless nickel plated (ENP) surface to reduce these defects. However, the ENP surface has been found to develop a fluorine-containing layer after use in a fluorine-based atmosphere and at higher temperatures of about 150° C. or above. Without being limited to a theory, the fluorine-containing layer develops because of contamination during use, thus the fluorine-containing layer can be considered a contamination layer. Further, after processing a few hundreds of wafers, it has been found that the fluorine-containing layer lessens the lifetime of one or more components of the process chamber and a mean wafers between cleaning (MWBC) metric.
- In some embodiments of the present disclosure, a chamber component for a processing chamber may include a body; a metal plating on at least one surface of the body, the metal plating comprising nickel; and a barrier layer on the metal plating. In some embodiments, the barrier layer may include a nickel oxide. In some embodiments, the metal plating may include nickel and phosphorus. In some embodiments, the metal plating may include nickel and is free of phosphorous. In some embodiments, the body includes aluminum, an aluminum alloy, aluminum nitride, alumina, or combinations thereof. In some embodiments, the metal plating has a thickness of about 20 microns to about 75 microns, and the barrier layer has a thickness of about 2 nm to about 50 nm. In some embodiments, the barrier layer has an average surface roughness (Ra) of about 2 micro-inches to about 60 micro-inches. In some embodiments, the chamber component may be a showerhead for a process chamber.
- In other embodiments of the present disclosure, a method of protecting a chamber component includes forming a metal plating on a body of the chamber component, wherein the metal plating may include nickel, and contacting the metal plating with an oxidizing agent to form a barrier layer on the metal plating, wherein the barrier layer may include nickel oxide. In some embodiments, the oxidizing agent may include one of at least one of hydrofluoric acid, oxalic acid, or nitric acid. In some embodiments, the barrier layer may have a thickness from about 2 μm to about 60 μm. In some embodiments, forming the metal plating may include performing electroless metal plating, and wherein the metal plating further comprises phosphorus. In some embodiments, the body may include an aluminum alloy, aluminum nitride, alumina, or combinations thereof. In some embodiments, the method may include removing a native oxide from the metal plating prior to forming the barrier layer. In some embodiments, the method may include after the forming the metal playing, forming a nickel fluoride (NiF2) or nickel oxy-fluoride layer on the metal plating by contacting the metal plating with ammonium fluoride. In some embodiments, the method may also include placing the chamber component in an acid bath comprising 5-25% hydrofluoric acid and 75-95% water to contact the metal plating with the oxidizing agent; subsequently placing the chamber component in a de-ionized water bath; subsequently placing the chamber component in the acid bath; and subsequently placing the chamber in the di-ionized water bath.
- In another embodiment of the present disclosure, a method of refurbishing a used chamber component may include removing a contamination layer from a metal plating on the used chamber component using a first acid solution, wherein the metal plating comprises nickel; and subsequently contacting the metal plating with an oxidizing agent to form a barrier layer on the metal plating, wherein the barrier layer comprises nickel oxide. In some embodiments, the contamination layer may include nickel fluoride. In some embodiments, the removing the contamination layer may include placing the used chamber component in a first acid bath, subsequently rinsing the used chamber component with deionized water, subsequently drying the used chamber component, subsequently placing the used chamber component in a second acid bath, subsequently rinsing the used chamber component with deionized water, and subsequently drying the used chamber component. In some embodiments, the oxidizing agent may include at least one of hydrofluoric acid or nitric acid. In some embodiments, the barrier layer may have a thickness from about 2 μm to about 60 μm.
- The present invention is illustrated by way of example, and not by way of limitation, in the figures of the accompanying drawings in which like references indicate similar elements. It should be noted that different references to “an” or “one” embodiment in this disclosure are not necessarily to the same embodiment, and such references mean at least one.
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FIG. 1A depicts a sectional view of one embodiment of a processing chamber; -
FIG. 1B depicts a sectional view of one embodiment of a showerhead for a processing chamber; -
FIG. 2 illustrates one embodiment of a bottom view of a showerhead, in accordance with an embodiment; -
FIG. 3A illustrates a method of forming an advanced barrier oxide layer according to an embodiment; -
FIG. 3B illustrates another method of refurbishing and forming an advanced barrier oxide layer according to another embodiment; -
FIG. 4 illustrates an example architecture of a manufacturing system; -
FIG. 5 is a flow chart representing a method of forming an advanced barrier oxide layer according to an embodiment; -
FIG. 6 is a flow chart representing a method of refurbishing and forming an advanced barrier layer according to another embodiment; - Embodiments disclosed herein describe coated articles, coated chamber components, methods of coating articles and chamber components, methods of reducing or eliminating particles from semiconductor processing chambers, and methods of using coated articles and chamber components and processing chambers containing coated chamber components. To reduce reactions between component materials and reactive chemicals and/or plasmas, which form metal fluorides, particles, other trace metal contaminates and/or high vapor pressure gases, a metal layer (e.g., which may be a metal coating or metal plating) with a barrier layer is included. The metal layer may be a nickel-containing layer (e.g., a pure nickel layer or a layer having nickel as a primary constituent and additionally including other materials such as phosphorous and/or vanadium). The barrier layer may be a nickel oxide layer formed under controlled conditions. The barrier layer may be added to new chamber components to improve a lifespan of the chamber components and/or to reduce or eliminate a buildup of a contamination layer on the chamber component. Further, to improve the life of the coated articles or coated chamber components (which may be new or used chamber components), they may be treated to remove a contamination layer and to add a barrier layer over a metal layer on the chamber components.
- It has been found that there is an interaction between fluorine and a metal layer (e.g., an ENP comprising nickel) on chamber components that adds oxides and/or fluorides to the metal layer. A native oxide naturally occurs on the metal layer due to exposure to air. However, the native oxide has undesirable properties. In particular, the native oxide interacts with process gases (e.g., fluorine) to form a contamination layer. The native oxide's interaction with fluorine causes discoloration and forms a black film (contamination layer) over the metal coating that produces particles that can contaminate processed substrates. If a black film/contamination layer is present on a chamber component such as a shower head, there may be a drop in yield for substrates processed by the process chamber that includes the shower head having the contamination layer.
- Further, if there is a black film/contamination layer that forms while the chamber component is in use, the chamber component is removed and replaced.
- Thus, embodiments improve the surface of chamber components such as showerheads to prevent the formation of the black film/contamination layer over a metal layer of the chamber components. It would be advantageous to have a protective barrier layer to prevent the chemical degradation of the surface metal layer and formation of the black film/contamination layer. Such a chamber component having a protective barrier layer may also degrade and/or become contaminated more slowly than a chamber component lacking the barrier layer, which may cause the chamber component with the barrier layer over the metal layer to have a higher mean wafers between cleaning than a chamber component with a metal layer and lacking the barrier layer. The mean wafers between cleaning represents the mean number of wafers that are processed between each cleaning of the chamber component. Such an increased mean wafers between cleaning may be particularly pronounced for chamber components used in chambers that perform processes at higher temperatures of about 200° C. or above.
- In embodiments disclosed herein are chamber components for processing chambers and/or processing chambers containing such chamber components (e.g., semiconductor processing chambers), wherein the chamber components include a chamber component and a metal layer (e.g., a metal plating or a metal coating) on at least one surface of the chamber component. The metal layer may include an advanced barrier layer in embodiments.
- In some embodiments, a chamber component may include a metal layer on a surface of the substrate. The chamber component or portions thereof may be composed of, without limitation, one or more of a metal, for example, aluminum, stainless steel and/or titanium, a ceramic, for example, alumina, silica and/or aluminum nitride, and/or combinations thereof. The metal layer may be an electroless metal plating including nickel or an electrolytic metal plating including nickel.
- In some embodiments, a chamber component may be plated using an electroless plating process to form an electroless metal plating on one or more surface of the chamber component. In embodiments, the electroless metal plating may be a nickel-phosphorous plating. The electroless plating process can form a metal plating directly on the surface of the chamber component. In some embodiments, the chamber component may be plated using an electrolytic metal plating process. For example, the electrolytic plating process may form a layer containing nickel, silver and/or gold. In some embodiments, one or more surface of the chamber component may be coated using a sputtering process, such as a sputtering process that sputters a nickel-containing coating onto the one or more surface of the chamber component. The nickel containing coating may include, for example, 98-99 atomic % nickel and 1-2 atomic % vanadium.
- In some embodiments, when the chamber component is coated with an electroless plating process, the chamber component is placed in a bath that contains nickel and phosphorous. The bath may include about 84% nickel and about 16% phosphorous, about 86% nickel and 14% phosphorous, about 88% nickel and about 12% phosphorous, about 90% nickel and about 10% phosphorous, about 92% nickel and about 8% phosphorous, about 94% nickel and about 6% phosphorous, and about 96% nickel and about 4% phosphorous. For example, the bath may include about 84-96% nickel and about 4-16% phosphorous.
- In some embodiments, when the chamber component is plated with an electrolytic metal plating process, the coating is free of phosphorous. For example, the plating may be 100% nickel. In some embodiments, the chamber component is coated with a sputtered nickel. The sputtered nickel, as understood by one of skill in the art, may include nickel and vanadium. The vanadium may be present in the sputtered nickel in about 1% to about 2%.
- In embodiments, when the chamber component includes a metal layer that is an electroless nickel plating or an electrolytic Ni plating, the layer may be in a thickness from about 20 microns to about 75 microns, from about 25 microns to about 70 microns, from about 30 microns to 60 microns, or from about 35 microns to about 50 microns.
- In some embodiments, the metal layer may have a hardness from about 450 HV to about 500 HV. The roughness of the metal layer may be less than 50 μinch in embodiments.
- The thickness of the metal layer formed by electroless plating may be targeted based on the amount of time that the chamber component is in the bath. The chamber component may be in the bath for about one minute to about three minutes to form the metal layer having a target thickness.
- In some embodiments, a contamination layer may be found on the metal layer. The contamination layer may include a combination of nickel, fluorine and/or oxygen. In embodiments, the metal layer is a nickel layer that becomes slowly fluorinated over time due to exposure to fluorine-rich chemistries. For example, a contamination layer of nickel fluorine and/or nickel oxy-fluorine may be formed on the surface of the metal layer. The contamination layer may react to process gases differently than the metal layer, and may cause subtle changes to process chemistries. Additionally, or alternatively, the contamination layer may flake off of the chamber component and/or cause particle contamination on substrates processed in the process chamber in which the chamber component is installed. As a result, periodic maintenance may be performed on chamber components to remove those chamber components that include the contamination layer and to replace the removed chamber components with new chamber components that lack the contamination layer.
- In embodiments, the chamber component includes a barrier layer comprising nickel oxide over a metal layer (e.g., a nickel layer). In embodiments, the formation of the barrier layer (e.g., the nickel oxide barrier layer) on the metal layer protects the metal layer from attack by process gases, and in particular to attack by fluorine-containing plasmas and other fluorine-containing chemistries. Accordingly, the barrier layer may be referred to as a protective layer. The nickel oxide barrier layer may be formed using an oxidation process, which may include immersing the chamber component (or a portion thereof that is to have a nickel oxide barrier layer) into a bath containing an oxidation agent (e.g., a bath containing hydrofluoric acid and/or nitric acid with water).
- In some embodiments, the chamber component includes generating a nickel fluorination (NiF2) or nickel oxy-fluorination (NiOF) layer after removing the contamination layer and before forming the barrier layer. The nickel fluorination or nickel oxy-fluorination layer may be generated by placing the metal plated chamber component in a bath with an ammonium fluoride (NH4F) solution. The ammonium fluoride solution may have a concertation from about 0.5 M to about 3 M. The metal plated chamber component remains in the bath for about 5 minutes to about 60 minutes at a temperature of about 35 to about 45° C. to form a nickel fluorinated or nickel oxy-fluorinated layer. If a nickel fluorinated layer is formed, then Ni is present in an amount of abut 60 wt. % and F is present in an amount of about 40 wt. %. If a nickel oxy-fluorinated layer is formed, then Ni is present in an amount of about 62 wt. %, F is present in an amount of about 20 wt %, and O is present in an amount of about 17 wt. %. After this nickel fluorination (NiF2) or nickel oxy-fluorination (NiOF) layer is formed then the nickel oxide barrier layer may be formed using an oxidation process as described herein.
- Experimentation has shown that use of the nickel oxide barrier layer over a nickel layer on chamber components increases the serviceable lifetime of the chamber components by ten times. Accordingly, preventative maintenances may be reduced by two times up to ten times in embodiments as compared to the number and/or frequency of preventative maintenances performed to service and/or replace chamber components having an exposed nickel layer.
- Some embodiments are descried herein with reference to a showerhead, and are particularly useful for coating chamber components having both high aspect ratio features and regions that are directly exposed to bombardment by a plasma. However, the barrier layer described herein can also be beneficially used on many other chamber components having metal layers that are exposed to plasma, such as chamber components for a plasma etcher (also known as a plasma etch reactor) or other processing chambers including walls, liners, bases, rings, view ports, lids, nozzles, substrate holding frames, electrostatic chucks (ESCs), face plates, selectivity modulation devices (SMDs), plasma sources, pedestals, and so forth.
- Moreover, embodiments are described herein with reference to plated or coated chamber components and other articles that may cause reduced particle contamination when used in a process chamber for plasma rich processes. However, it should be understood that the plated or coated articles discussed herein may also provide reduced particle contamination when used in process chambers for other processes such as non-plasma etchers, non-plasma cleaners, chemical vapor deposition (CVD) chambers, physical vapor deposition (PVD) chambers, and so forth.
- Referring now to the figures,
FIG. 1A is a sectional view of a processing chamber 100 (e.g., a semiconductor processing chamber) having one or more chamber components that include a metal layer and a nickel oxide-containing barrier layer over the metal layer in accordance with embodiments of the present disclosure. Theprocessing chamber 100 may be used for processes in which a corrosive plasma environment and/or corrosive chemistry is provided. For example, theprocessing chamber 100 may be a chamber for a plasma etch reactor (also known as a plasma etcher), a plasma cleaner, an atomic layer deposition (ALD) chamber that performs plasma-enhanced ALD, other deposition chambers, and so forth. Examples of chamber components that may include a metal layer and a barrier layer over the metal layer are asubstrate support assembly 148, an electrostatic chuck (ESC), a ring (e.g., a process kit ring or single ring), a chamber wall, a base, ashowerhead 130, a gas distribution plate, a liner, a liner kit, a shield, a plasma screen, a flow equalizer, a cooling base, a chamber viewport, a chamber lid, a nozzle, process kit rings, and so on. - In one embodiment, the metal layer is a nickel-containing layer (e.g., 100% nickel or nickel in combination with one or more additional materials such as phosphorous and/or vanadium). In one embodiment, the barrier layer is a nickel-oxide containing layer (e.g., 100% nickel oxide or nickel oxide with one or more additional materials such as phosphorous and/or vanadium). The metal layer and the barrier layer may be conformal thin films.
- In one embodiment, the
processing chamber 100 includes achamber body 102 and ashowerhead 130 that enclose aninterior volume 106. Theshowerhead 130 may or may not include a gas distribution plate. For example, the showerhead may be a multi-piece showerhead that includes a showerhead base and a showerhead gas distribution plate bonded to the showerhead base. Alternatively, theshowerhead 130 may be replaced by a lid and a nozzle in some embodiments, or by multiple pie shaped showerhead compartments and plasma generation units in other embodiments. Thechamber body 102 may be fabricated from aluminum, stainless steel or other suitable material. Thechamber body 102 generally includessidewalls 108 and a bottom 110. Any of the showerhead 130 (or lid and/or nozzle),sidewalls 108 and/orbottom 110 may include the multi-layer plasma resistant coating. - An
outer liner 116 may be disposed adjacent thesidewalls 108 to protect thechamber body 102. Theouter liner 116 may be a halogen-containing gas resist material such as Al2O3 or Y2O3. Theouter liner 116 may be coated with the multi-layer plasma resistant ceramic coating in some embodiments. - An
exhaust port 126 may be defined in thechamber body 102, and may couple theinterior volume 106 to apump system 128. Thepump system 128 may include one or more pumps and throttle valves utilized to evacuate and regulate the pressure of theinterior volume 106 of theprocessing chamber 100. - The
showerhead 130 may be supported on thesidewalls 108 of thechamber body 102 and/or on a top portion of the chamber body. The showerhead 130 (or lid) may be opened to allow access to theinterior volume 106 of theprocessing chamber 100, and may provide a seal for theprocessing chamber 100 while closed. Agas panel 158 may be coupled to theprocessing chamber 100 to provide process and/or cleaning gases to theinterior volume 106 through theshowerhead 130 or lid and nozzle. Theshowerhead 130 includes multiple gas delivery holes 132 throughout theshowerhead 130. Theshowerhead 130 may be or include aluminum, anodized aluminum, an aluminum alloy (e.g., Al 6061), or an anodized aluminum alloy. In some embodiments, the showerhead includes a gas distribution plate (GDP) bonded to the showerhead. The GDP may be, for example, Si or SiC. The GDP may additionally include multiple holes that line up with the holes in the showerhead. -
FIG. 1B illustrates a zoomed in view of a portion of theshowerhead 130 ofFIG. 1A . With reference toFIG. 1B , in embodiments theshowerhead 130 is coated by ametal layer 150 and abarrier layer 152. In particular, in some embodiments a surface of the showerhead and walls ofholes 132 in the showerhead are coated by a thinconformal metal layer 150. Additionally, the backside of theshowerhead 130 and outer side walls of the showerhead may also be coated by theconformal metal layer 150. A non-line of sight deposition technique such as ALD or plating (e.g., electroplating or electroless plating) may be used to deposit or form themetal layer 150 on the surface of theshowerhead 130 and on the walls of theholes 132 in theshowerhead 130. Alternatively, a line-of-sight deposition technique such as sputtering may be used to form the metal layer. Themetal layer 150 may be nickel, nickel doped with phosphorous, or nickel doped with vanadium in embodiments. - A
barrier layer 152 covers themetal layer 150 at some or all regions of the surface of theshowerhead 130. Thebarrier layer 152 may be formed using an oxidation process, which may be a dry oxidation process or a wet oxidation process (e.g., by dipping theshowerhead 130 into a bath containing an oxidizing agent such as hydrofluoric acid or nitric acid. Thebarrier layer 152 may cover the metal layer on all surfaces of the chamber component, including on the inner walls of holes in theshowerhead 130. The barrier layer may be a grown layer and may be conformal and uniform in embodiments. The uniform barrier layer may have a difference in thickness of less than about 10% across the surface of the showerhead in embodiments. - Examples of processing gases that may be used to process substrates in the
processing chamber 100 include halogen-containing gases, such as C2F6, SF6, SiCl4, HBr, NF3, CF4, CHF3, CH2F3, F, Cl2, CCl4, BCl3 and SiF4, among others, and other gases such as O2, or N2O. Examples of carrier gases include N2, He, Ar, and other gases inert to process gases (e.g., non-reactive gases). The fluorine based gases may cause fluoride deposits to buildup on the holes of standard showerheads and/or a contamination layer to form on the holes of the showerheads. However, theholes 132 ofshowerhead 130 may be resistant to such fluoride buildup due to thebarrier layer 152. - Referring back to
FIG. 1A , asubstrate support assembly 148 is disposed in theinterior volume 106 of theprocessing chamber 100 below theshowerhead 130. Thesubstrate support assembly 148 holds a substrate 144 (e.g., a wafer) during processing. Thesubstrate support assembly 148 may include an electrostatic chuck that secures thesubstrate 144 during processing, a metal cooling plate bonded to the electrostatic chuck, and/or one or more additional components. An inner liner may cover a periphery of thesubstrate support assembly 148. The inner liner may be a halogen-containing gas resist material such as Al2O3 or Y2O3. The substrate support assembly, portions of the substrate support assembly, and/or the inner liner may be coated with the metal layer and barrier layer in some embodiments. -
FIG. 2 illustrates one embodiment of a bottom view of ashowerhead 200. Theshowerhead 200 may have a series of gas conduits 204 (also referred to as holes) arranged concentrically that evenly distribute plasma gasses directly over a substrate or wafer to be etched or processed. The showerhead is depicted here having approximately 1100gas conduits 204 arranged in evenly distributed concentric rings for even distributing of gasses. In another embodiment, thegas conduits 204 may be configured in alternative geometric configurations on thelower surface 205 of the showerhead (or on a lower surface of a GDP bonded to a showerhead). For example, the showerhead may have a square or rectangular configuration having rows and columns ofgas conduits 204. It is to be understood that other shapes (e.g., triangle, pentagon, etc.) may be implemented and coated with a ceramic coating (e.g., an HPM coating) as described above. Theshowerhead 200 can havemany gas conduits 204, as depicted, or as few gas conduits as appropriate depending on the type of reactor and/or process utilized. - In one embodiment, some or all
gas conduits 204 do not include branches (e.g., each gas conduit may have a single entry point and a single exit point). Additionally, the gas conduits may have various lengths and orientation angles. Gas may be delivered to thegas conduits 204 via one or more gas delivery nozzles. Somegas conduits 204 may receive the gas before other gas conduits 204 (e.g., due to a proximity to a gas delivery nozzle). However, thegas conduits 204 may be configured to deliver gas to a substrate resting beneath the showerhead at approximately the same time based on varying the orientation angles, diameters and/or lengths of thegas conduits 204, or by using an additional flow equalizer. For example,gas conduits 204 that will receive gas first may be longer and/or have a greater angle (e.g., an angle that is further from 90 degrees) than conduits that will receive gas later. - As can be seen in
FIG. 3A , a schematic 300 of oxidizing the metal plated coated chamber component is illustrated. InFIG. 3A , a metal plated chamber component includes anickel layer 301 and abare aluminum body 302 of the chamber component, wherein thenickel layer 301 is on a surface of thebare aluminum body 302. The metal plated chamber component undergoes anoxidation process 305 according to the present disclosure. After being oxidized, the metal plated chamber component includes adense barrier layer 303 of nickel oxide on a surface of thenickel layer 301. Thebarrier layer 303 of NiO may prevent discoloration of the metal layer. Thebarrier layer 303 may also prevent as the chamber component from becoming a source of particles on processed substrates. Thebarrier layer 303 of NiO may also inhibit the reaction of fluorine with nickel in thenickel layer 301 to prevent the formation of a discolored/contaminated layer. - Further, the
barrier layer 303 may prevent a native oxide from forming on the nickel layer 1. - In some embodiments, the chamber component may be a used chamber component that has been used to perform one or more processes on substrates, where the processes exposed the substrates to a fluorine-rich environment. The chamber component may not have been coated with a barrier layer prior to use. Accordingly, the chamber component may include a contamination layer over the
metal layer 302. In some embodiments, the chamber component may be refurbished by removing the contamination layer to expose the metal layer, and then form the barrier layer over the metal layer. A schematic of such embodiment is illustrated inschematic 350 ofFIG. 3B . - In
FIG. 3B , the chamber component includes analuminum body 302 having ametal layer 301 disposed thereon, and acontamination layer 310 over themetal layer 301. The chamber component may undergo acleaning process 315 to strip thecontamination layer 310 from themetal layer 301. The chamber component having the cleanedmetal layer 301 may then be processed using anoxidation process 305 to formbarrier layer 303, as described in more detail in the present disclosure. After cleaning and oxidization, thecontamination layer 310 is removed and abarrier layer 303 of dense nickel oxide is present over themetal layer 301. -
FIG. 4 illustrates an example architecture of amanufacturing system 400. Themanufacturing system 400 may be a manufacturing system for applying platings and/or coatings to articles such as chamber components. In one embodiment, themanufacturing system 400 includes manufacturing machines 401 (e.g., processing equipment) connected to anequipment automation layer 415. The manufacturing machines may include apolisher 402, one or morewet cleaners 403, aplating system 404, asputtering system 405, anoxidation system 406, and/or other machines. Themanufacturing system 400 may further include one ormore computing device 420 connected to theequipment automation layer 415. In alternative embodiments, themanufacturing system 400 may include more or fewer components. For example, themanufacturing system 400 may include manually operated (e.g., off-line)manufacturing machines 401 without theequipment automation layer 415 or thecomputing device 420. -
Polisher 402 is a machine configured to polish or smoothen the surface of articles such as chamber components for processing chambers.Polisher 402 may be, for example, a chemical mechanical planarization (CMP) device or an abrasive polisher. For example, a motorized abrasive pad may be used to smoothen the surface of an article. A sander may rotate or vibrate the abrasive pad while the abrasive pad is pressed against a surface of the article. A roughness achieved by the abrasive pad may depend on an applied pressure, on a vibration or rotation rate and/or on a roughness of the abrasive pad. -
Wet cleaners 403 are cleaning apparatuses that clean articles (e.g., articles) using a wet clean process.Wet cleaners 403 include wet baths filled with liquids, in which the substrate is immersed to clean the substrate.Wet cleaners 403 may agitate the wet bath using ultrasonic waves during cleaning to improve a cleaning efficacy. This is referred to herein as sonicating the wet bath. - In some embodiments,
wet cleaners 403 include a first wet cleaner that contains deionized (DI) water and a second wet cleaner that contains an acid solution. The acid solution may be a hydrofluoric acid (HF) solution, a hydrochloric acid (HCl) solution, a nitric acid (HNO3) solution, or combination thereof in embodiments. The acid solution may remove surface contaminants from the article and/or may remove an oxide from the surface of the article. Cleaning the article having a metal layer with the acid solution prior to forming a barrier layer over the metal layer may improve a quality of the barrier layer formed over the metal layer. In one embodiment, an acid solution containing approximately 5 to 15 vol % HF is used to clean chamber components having a nickel layer. In one embodiment, an acid solution containing approximately 5 to 15 vol % HNO3 is used to clean articles having a nickel layer. - The
wet cleaners 403 may clean articles at multiple stages during processing. For example,wet cleaners 403 may clean an article after a substrate has been polished, before performing plating (e.g., electroplating), before forming a barrier layer over a metal plating, and so on. - In other embodiments, alternative types of cleaners such as dry cleaners may be used to clean the articles. Dry cleaners may clean articles by applying heat, by applying gas, by applying plasma, and so forth.
-
Plating system 404 is a system that performs electroplating (e.g., of Ni) or electroless plating (e.g., of Ni).Plating system 404 may be an electroplating system that applies a current to reduce dissolved metal cations so that they form a thin coherent metal coating on the article (e.g., on surfaces of a chamber component such as an aluminum chamber component). Specifically, the article to be plated may be the cathode of a circuit and a metal donor may be the anode of the circuit. The article and metal donor may be immersed in an electrolyte containing one or more dissolved metal salts and/or other ions that increase an electrical conductivity of the electrolyte. Metal from the metal donor than plates a surface of the article. - Another type of plating system that may be used is an electroless plating system that performs electroless plating. Electroless plating, also known as chemical or auto-catalytic plating, is a non-galvanic plating method that involves several simultaneous reactions in an aqueous solution, which occur without the use of external electrical power. The reaction is accomplished when hydrogen is released by a reducing agent, normally sodium hypophosphite or thiourea, and oxidized, thus producing a negative charge on the surface of the part.
- The
equipment automation layer 415 may interconnect some or all of themanufacturing machines 401 withcomputing devices 420, with other manufacturing machines, with metrology tools and/or other devices. Theequipment automation layer 415 may include a network (e.g., a location area network (LAN)), routers, gateways, servers, data stores, and so on.Manufacturing machines 401 may connect to theequipment automation layer 415 via a SEMI Equipment Communications Standard/Generic Equipment Model (SECS/GEM) interface, via an Ethernet interface, and/or via other interfaces. In one embodiment, theequipment automation layer 415 enables process data (e.g., data collected bymanufacturing machines 401 during a process run) to be stored in a data store (not shown). In an alternative embodiment, thecomputing device 420 connects directly to one or more of themanufacturing machines 401. - In one embodiment, some or all
manufacturing machines 401 include a programmable controller that can load, store and execute process recipes. The programmable controller may control temperature settings, gas and/or vacuum settings, time settings, etc. ofmanufacturing machines 401. The programmable controller may include a main memory (e.g., read-only memory (ROM), flash memory, dynamic random access memory (DRAM), static random access memory (SRAM), etc.), and/or a secondary memory (e.g., a data storage device such as a disk drive). The main memory and/or secondary memory may store instructions for performing heat treatment processes described herein. - The programmable controller may also include a processing device coupled to the main memory and/or secondary memory (e.g., via a bus) to execute the instructions. The processing device may be a general-purpose processing device such as a microprocessor, central processing unit, or the like. The processing device may also be a special-purpose processing device such as an application specific integrated circuit (ASIC), a field programmable gate array (FPGA), a digital signal processor (DSP), network processor, or the like. In one embodiment, programmable controller is a programmable logic controller (PLC).
- In one embodiment, the
manufacturing machines 401 are programmed to execute recipes that will cause the manufacturing machines to polish an article, clean an article, plate an article, form a barrier layer on an article, and so on. In one embodiment, themanufacturing machines 401 are programmed to execute recipes that perform operations of a multi-step process for manufacturing an article having a metal layer and a barrier layer, as described with reference toFIGS. 5-6 . Thecomputing device 420 may store one or more plating, oxidizing, cleaning and/or polishingrecipes 425 that can be downloaded to themanufacturing machines 401 to cause themanufacturing machines 401 to manufacture articles in accordance with embodiments of the present disclosure. -
FIG. 5 is a flow chart representing amethod 500 of refurbishing, and forming an advanced barrier oxide layer on, a chamber component according to an embodiment.Method 500 may be performed on chamber components having a metal layer (e.g., a metal plating) that has been used to perform one or more cycles of one or more manufacturing processes that expose the chamber component to chemistries that cause formation of a contamination layer on the metal layer. The contamination layer may contain oxygen, fluorine and/or one or more process elements. The contamination layer may cause particle contamination and/or negatively affect future processes performed in the process chamber in embodiments. Accordingly, in some embodiments of the present disclosure, when a contamination layer is present on the metal plated chamber component, the chamber component is placed in afirst bath 502. The first bath may include water and a first acid (e.g., hydrofluoric acid, nitric acid (HNO3), sulfuric acid (H2SO4), oxalic acid (HC2O4), or ammonium fluoride (NH4F)). The hydrofluoric acid may be included in an amount from about 5 wt. % to about 15 wt. % in the bath based on the total composition of the first bath. The water may be included in an amount from about 85 wt. % to about 95 wt. % in the bath based on the total composition of the bath. In some embodiments, the first bath includes about 5 wt. % hydrofluoric acid and about 95 wt. % water. The first bath may be at a temperature from about 25° C. to about 35° C. The used metal plated chamber component may be placed in the first bath for about one minute to about 30 minutes to loosen the contamination layer. After soaking in the first bath, the metal plated chamber may include a loosened contamination layer. The metal plated chamber component may then be rinsed (e.g., with deionized water) to remove the loosened contamination layer and dried atblock 504. - Subsequently, the metal plated chamber component is placed into the first bath or a second bath at
block 506. The second bath includes water and an acid (e.g., hydrofluoric acid). The acid may be included in an amount from about 5 wt. % to about 15 wt. % in the bath based on the total composition of the first bath or second bath. The water may be included in an amount from about 85 wt. % to about 95 wt. % in the bath based on the total composition of the first bath or second bath. In some embodiments, the second bath includes about 5 wt. % hydrofluoric acid and about 95% water. The second bath may be at a temperature from about 25° C. to about 35° C. The used metal plated chamber component may be placed in the second bath for about one minute to about 30 minutes, where the remaining contamination layer may be removed. After the second bath, the metal plated chamber component may be rinsed (e.g., with deionized water) and dried 508. - The metal plated chamber component may then be polished after removing the
contamination layer 510. The metal plated chamber component may be polished using an automatic polisher with different polishing sheets, such as a Scotch-Brite® sheet, or another advanced method to uniformly polish a surface. The metal plated coated chamber component may be polished until the surface roughness is about 10 μin to about 20 μin in one embodiment. After polishing, the metal plated coated chamber component may undergo anoxidation treatment 512. The oxidation treatment may be performed by placing the metal plated coated chamber component in a third bath. The third bath includes water and an acid (e.g., nitric acid (HNO3), sulfuric acid (H2SO4), oxalic acid (HC2O4), or ammonium fluoride (NH4F)). The acid may be included in an amount from about 5 wt. % to about 25 wt. % in the bath based on the total composition of the third bath. The water may be included in an amount form about 75 wt. % to about 95 wt. % in the bath based on the total composition of the third bath. In some embodiments, the third bath may include about 5 wt. % hydrofluoric acid and about 95 wt. % water. The third bath may be at a temperature from about 25° C. to about 35° C. The metal plated chamber component may be placed in the third bath for about one minute to about 30 minutes. The oxidized metal plated chamber component may be rinsed (e.g., with deionized water), where a nickel oxide layer may be formed on the surface of the metal plating layer. The nickel oxide layer may be between about 5 nanometers to about 35 nanometers in one embodiment. - In another embodiment, the metal plated coated chamber component may be a new component, which may be oxidized through a
second method 600.FIG. 6 is a flow chart representing a method of forming an advanced barrier layer on a metal plated or metal coated chamber component according to an embodiment. In thesecond method 600, the metal plated chamber component is placed in afirst bath 602. The first bath may include water and an acid (e.g., hydrofluoric acid). The hydrofluoric acid may be included in an amount from about 5 wt. % to about 25 wt. % in the bath based on the total composition of the first bath. The water may be included in an amount form about 75 wt. % to about 95 wt. % in the bath based on the total composition of the bath. In some embodiments, the first bath includes about 5 wt. % hydrofluoric acid and about 95 wt. % water. The first bath may be at a temperature from about 25° C. to about 35° C. The metal plated chamber component may be placed in the first bath for about one minute to about 30 minutes. After thefirst bath 604, the metal plated chamber component may be rinsed (e.g., with deionized water) and dried 606. - Once dried, the metal plated chamber component may be treated with an acid (e.g., hydrofluoric acid or nitric acid (HNO3)) to oxidize the metal plating layer and form a
nickel oxide layer 608. The metal plated coated chamber component may be treated for a time from about one minute to about 30 minutes until a target thickness of the nickel oxide layer is achieved. The nickel oxide layer may be between about 5 nanometers to about 30 nanometers in embodiments, such as about 15 nanometers. The metal plated coated chamber component is then rinsed with deionized water and dried atblock 610. - In another embodiment, the metal plated coated chamber component may be a new component, having a nickel fluorinated or nickel oxy-fluorinated layer, and oxidizing the chamber component.
FIG. 7 is a flow chart representing a method of forming an advanced barrier layer on a metal plated or metal coated chamber component having a nickel fluorinated (NiF2) or nickel oxy-fluorinated (NiOF) layer according to an embodiment. The chamber component is placed in a first bath and rinsed insteps 702 to 706, as described inFIG. 6 ,steps 602 to 606. After rinsing and drying the chamber component, the chamber component is then placed in a second bath including anammonium fluoride solution 708 to form a nickel fluorine or nickel oxy-fluorine layer. The ammonium fluoride solution has a concentration of about 0.5M to about 3 M. The chamber component remains in the second bath for about 5 minutes to about 60 minutes, where the second bath is at a temperature of about 35 to 45° C. to form a NiF2 or NiOF layer. The chamber component is then removed from thebath 710. The chamber component is then rinsed and dried instep 712 as described above forstep 606 inFIG. 6 . After formation of the NiF2 or NiOF layer, the chamber component may be treated with an acid (e.g., hydrofluoric acid or nitric acid (HNO3)) to oxidize themetal plating layer 718 and form a nickel oxide layer as described above insteps FIGS. 5 and 6 , respectively. - In another embodiment, the metal plated chamber component may be oxidized through an in situ method. This method may occur in the same chamber in which the chamber component is being coated with the nickel plated coating or in the chamber in which the part will be used. In a first step of the in situ method, the metal plated chamber component may be treated with a gas and moisture while the chamber component is in the chamber. The gas may be selected from the group consisting of NH3, NF3, HF or H2, or a combination thereof. In some embodiments, the gas may be a combination of NH3 and NF3 or NH3, NF3 and HF. The gas may be in a concentration from about 5 sccm to about 2000 sccm of total gas. The gas reacts with the ambient moisture within the chamber. The temperature of the chamber be from about 150° C. to about 220° C. The nickel oxide coating layer may have a thickness of about 4 nm to about 50 nm.
- By treating the part with an oxidation treatment to form a barrier layer as described herein, the inventors have found that the lifetime of the part may be more than 10 times that of the original coating that lacks the barrier layer. When an ENP coated layer chamber component is used, the standard lifetime is about 3000 cycles. When a barrier nickel oxide layer is present on the ENP coated layer, the lifetime of the part increases almost 10 times more than the standard lifetime of the part, where the lifetime is greater than 10,000 cycles.
- Further, the inventors have found that the oxidation method can be used to coat a new part and for refurbishing an existing part where a contamination layer has formed.
- The following examples are set forth to assist in understanding the disclosure and should not be construed as specifically limiting the disclosure described and claimed herein. Such variations of the disclosure, including the substitution of all equivalents now known or later developed, which would be within the purview of those skilled in the art, and changes in formulation or minor changes in experimental design, are to be considered to fall within the scope of the disclosure incorporated herein.
- Exemplified herein is a showerhead having a nickel plating and a nickel oxide barrier layer on the nickel plating. The showerhead was first coated with nickel layer using a metal plating process. A natural oxide layer was formed on the nickel plating prior to formation of an intentional nickel oxide layer. The natural nickel oxide layer has inferior properties and impedes the formation of a target nickel oxide layer that will reduce particle contamination and improve a lifespan of the chamber component. The native nickel oxide layer may have a thickness of about 2 to 3 nm. The showerhead then underwent an oxidization treatment in which the showerhead was placed in a bath of 5% (5%-25%) hydrofluoric acid and 95% water at a temperature between 25 to 35° C. After 40 minutes, the showerhead was removed from the bath and rinsed with deionized water. A barrier nickel oxide layer was formed over the nickel layer. The barrier nickel oxide (NiO) layer on the metal layer had a thickness of from about 6 nm to about 22 nm.
- Exemplified herein is a showerhead comprising a nickel plating (a nickel ENP) that has been used, where a contamination layer has formed on the showerhead as a result of the use. The total thickness of the contamination layer (i.e., a fluorinated or oxy-fluorinated layer) was greater than 5 to 200 nm.
- The showerhead was cleaned to remove the contamination layer by placing the showerhead in a first bath of 5% (5%-25%) hydrofluoric acid and 95% water for 40 minutes at 25 to 40° C. The showerhead was then removed from the first bath and rinsed with deionized water and dried. After it was dried, the showerhead was then placed in a second bath of 25% hydrofluoric acid and 75% water for 40 minutes at 25 to 40° C. The showerhead was then removed from the second bath and rinsed again with deionized water and dried.
- The contamination layer was removed from the showerhead as a result of the cleaning. The showerhead was then treated and oxidized by placing the showerhead in a bath of 5% hydrofluoric acid to form a barrier layer over the ENP layer. A barrier nickel oxide layer was formed on the ENP layer as a result of the treatment and oxidation. The barrier nickel oxide (NiO) layer on the ENP coating layer had a combined thickness of about 22 nm. An EDS line profile of the barrier NiO layer on the ENP layer showed that nickel was present in the barrier NiO layer and there was no phosphorous in such layer. A TEM image and an EDS line profile of an inside of a small hole of the showerhead was also taken, and showed that the barrier layer had a thickness between 6.3 nm to 31.2 nm.
- The barrier layer on the backside of the showerhead was also measured to have a thickness of about 19 to 30 nm. This was also shown in an EDS line profile. This confirms that the barrier nickel oxide layer was formed along the entire showerhead, and was not limited to only the front side of the showerhead.
- Exemplified herein is a showerhead comprising a nickel plating (a nickel ENP) coating that is treated with ammonium fluoride (NH4F) solution having a concentration of 0.5M to 3M to convert a fluorinated (NiF2) or oxidized-fluorinated (NiOF) layer having a thickness of about 6 nm to about 50 nm. The showerhead underwent an oxidization treatment in which the showerhead was placed in a bath of 5% (5%-25%) hydrofluoric acid and 95% water at a temperature between 25 to 35° C. to have a NiO thickness of about 6 nm to about 50 nm.
- SEM images were also taken of the barrier layer on the ENP coated showerhead. From the SEM images, the weight percent of C, O, P and Ni were calculated and are presented in Table 1. It is noted that P comes from the ENP layer.
-
TABLE 1 Element Weight % Atomic % C K 12.62 35.92 O K 4.08 8.72 P K 13.16 14.52 Ni K 70.14 40.84 Totals 100.00 - The preceding description sets forth numerous specific details such as examples of specific systems, components, methods, and so forth, in order to provide a good understanding of several embodiments of the present invention. It will be apparent to one skilled in the art, however, that at least some embodiments of the present invention may be practiced without these specific details. In other instances, well-known components or methods are not described in detail or are presented in simple block diagram format in order to avoid unnecessarily obscuring the present invention. Thus, the specific details set forth are merely exemplary. Particular implementations may vary from these exemplary details and still be contemplated to be within the scope of the present invention.
- Reference throughout this specification to “one embodiment” or “an embodiment” means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment. Thus, the appearances of the phrase “in one embodiment” or “in an embodiment” in various places throughout this specification are not necessarily all referring to the same embodiment. In addition, the term “or” is intended to mean an inclusive “or” rather than an exclusive “or.” When the term “about” or “approximately” is used herein, this is intended to mean that the nominal value presented is precise within ±10%.
- Although the operations of the methods herein are shown and described in a particular order, the order of the operations of each method may be altered so that certain operations may be performed in an inverse order or so that certain operation may be performed, at least in part, concurrently with other operations. In another embodiment, instructions or sub-operations of distinct operations may be in an intermittent and/or alternating manner.
- It is to be understood that the above description is intended to be illustrative, and not restrictive. Many other embodiments will be apparent to those of skill in the art upon reading and understanding the above description. The scope of the invention should, therefore, be determined with reference to the appended claims, along with the full scope of equivalents to which such claims are entitled.
Claims (20)
Priority Applications (5)
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US17/449,844 US20230103643A1 (en) | 2021-10-04 | 2021-10-04 | ADVANCED BARRIER NICKEL OXIDE (BNiO) COATING DEVELOPMENT FOR THE PROCESS CHAMBER COMPONENTS |
PCT/US2022/045268 WO2023059502A1 (en) | 2021-10-04 | 2022-09-29 | Advanced barrier nickel oxide (bnio) coating development for the process chamber components |
KR1020247002952A KR20240068623A (en) | 2021-10-04 | 2022-09-29 | Development of advanced barrier nickel oxide (BNIO) coatings for process chamber components |
CN202280056329.2A CN117813670A (en) | 2021-10-04 | 2022-09-29 | Advanced barrier nickel oxide (BNiO) coating formation for process chamber components |
TW111137635A TW202340528A (en) | 2021-10-04 | 2022-10-04 | Advanced barrier nickel oxide (bnio) coating development for the process chamber components |
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US17/449,844 US20230103643A1 (en) | 2021-10-04 | 2021-10-04 | ADVANCED BARRIER NICKEL OXIDE (BNiO) COATING DEVELOPMENT FOR THE PROCESS CHAMBER COMPONENTS |
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US20230103643A1 true US20230103643A1 (en) | 2023-04-06 |
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US17/449,844 Abandoned US20230103643A1 (en) | 2021-10-04 | 2021-10-04 | ADVANCED BARRIER NICKEL OXIDE (BNiO) COATING DEVELOPMENT FOR THE PROCESS CHAMBER COMPONENTS |
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KR (1) | KR20240068623A (en) |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5952718A (en) * | 1996-02-23 | 1999-09-14 | Matsushita Electric Industrial Co., Ltd. | Semiconductor devices having protruding contacts |
JP2003342752A (en) * | 2002-05-21 | 2003-12-03 | Mitsubishi Heavy Ind Ltd | Heat resistant and corrosion resistant member for vacuum use, vacuum apparatus having parts obtained by using the same member and coating method therefor |
US20110101076A1 (en) * | 2009-10-30 | 2011-05-05 | Nhk Spring Co ., Ltd. | Reflow bonding method and method of manufacturing head suspension |
US20150110965A1 (en) * | 2012-06-04 | 2015-04-23 | Atotech Deutschland Gmbh | Plating bath for electroless deposition of nickel layers |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
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JP4770239B2 (en) * | 2005-03-31 | 2011-09-14 | 大日本印刷株式会社 | Method for producing metal oxide film |
JP5975747B2 (en) * | 2012-06-12 | 2016-08-23 | 太陽誘電ケミカルテクノロジー株式会社 | Vacuum chamber components |
US11932938B2 (en) * | 2019-08-01 | 2024-03-19 | Applied Materials, Inc. | Corrosion resistant film on a chamber component and methods of depositing thereof |
-
2021
- 2021-10-04 US US17/449,844 patent/US20230103643A1/en not_active Abandoned
-
2022
- 2022-09-29 KR KR1020247002952A patent/KR20240068623A/en active Search and Examination
- 2022-09-29 CN CN202280056329.2A patent/CN117813670A/en active Pending
- 2022-09-29 WO PCT/US2022/045268 patent/WO2023059502A1/en active Application Filing
- 2022-10-04 TW TW111137635A patent/TW202340528A/en unknown
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5952718A (en) * | 1996-02-23 | 1999-09-14 | Matsushita Electric Industrial Co., Ltd. | Semiconductor devices having protruding contacts |
JP2003342752A (en) * | 2002-05-21 | 2003-12-03 | Mitsubishi Heavy Ind Ltd | Heat resistant and corrosion resistant member for vacuum use, vacuum apparatus having parts obtained by using the same member and coating method therefor |
US20110101076A1 (en) * | 2009-10-30 | 2011-05-05 | Nhk Spring Co ., Ltd. | Reflow bonding method and method of manufacturing head suspension |
US20150110965A1 (en) * | 2012-06-04 | 2015-04-23 | Atotech Deutschland Gmbh | Plating bath for electroless deposition of nickel layers |
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