US20170253955A1 - Yttrium-based sprayed coating and making method - Google Patents
Yttrium-based sprayed coating and making method Download PDFInfo
- Publication number
- US20170253955A1 US20170253955A1 US15/600,953 US201715600953A US2017253955A1 US 20170253955 A1 US20170253955 A1 US 20170253955A1 US 201715600953 A US201715600953 A US 201715600953A US 2017253955 A1 US2017253955 A1 US 2017253955A1
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- United States
- Prior art keywords
- acid
- yttrium
- coating
- particles
- base
- Prior art date
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- 238000000576 coating method Methods 0.000 title claims abstract description 84
- 239000011248 coating agent Substances 0.000 title claims abstract description 76
- 238000000034 method Methods 0.000 title claims description 16
- 229910052727 yttrium Inorganic materials 0.000 title 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 title 1
- 239000002245 particle Substances 0.000 claims abstract description 55
- 238000004140 cleaning Methods 0.000 claims abstract description 35
- 239000007788 liquid Substances 0.000 claims abstract description 15
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000005507 spraying Methods 0.000 claims abstract description 12
- 150000007524 organic acids Chemical class 0.000 claims abstract description 11
- 229940105963 yttrium fluoride Drugs 0.000 claims abstract description 11
- RBORBHYCVONNJH-UHFFFAOYSA-K yttrium(iii) fluoride Chemical compound F[Y](F)F RBORBHYCVONNJH-UHFFFAOYSA-K 0.000 claims abstract description 11
- CHBIYWIUHAZZNR-UHFFFAOYSA-N [Y].FOF Chemical compound [Y].FOF CHBIYWIUHAZZNR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 150000007522 mineralic acids Chemical class 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 14
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 150000001261 hydroxy acids Chemical class 0.000 claims description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 6
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 5
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 5
- 239000007921 spray Substances 0.000 claims description 5
- 235000002906 tartaric acid Nutrition 0.000 claims description 5
- 239000011975 tartaric acid Substances 0.000 claims description 5
- 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 4
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- 239000004310 lactic acid Substances 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 3
- 239000011976 maleic acid Substances 0.000 claims description 3
- 229940098779 methanesulfonic acid Drugs 0.000 claims description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 2
- 239000000758 substrate Substances 0.000 abstract description 17
- 238000005530 etching Methods 0.000 abstract description 12
- 238000005260 corrosion Methods 0.000 abstract description 7
- 230000007797 corrosion Effects 0.000 abstract description 7
- 238000004901 spalling Methods 0.000 abstract description 6
- 229910052736 halogen Inorganic materials 0.000 abstract 1
- 150000002367 halogens Chemical class 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 16
- 238000010410 dusting Methods 0.000 description 9
- 239000007789 gas Substances 0.000 description 9
- 229910052786 argon Inorganic materials 0.000 description 8
- 238000004090 dissolution Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 238000005389 semiconductor device fabrication Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000007750 plasma spraying Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 238000007751 thermal spraying Methods 0.000 description 4
- 229910021642 ultra pure water Inorganic materials 0.000 description 4
- 239000012498 ultrapure water Substances 0.000 description 4
- 150000001735 carboxylic acids Chemical class 0.000 description 3
- 239000012459 cleaning agent Substances 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 230000000873 masking effect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 229910015844 BCl3 Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910020323 ClF3 Inorganic materials 0.000 description 1
- XPDWGBQVDMORPB-UHFFFAOYSA-N Fluoroform Chemical compound FC(F)F XPDWGBQVDMORPB-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- -1 lactic acid Chemical compound 0.000 description 1
- 238000000386 microscopy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 239000011236 particulate material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 description 1
- JOHWNGGYGAVMGU-UHFFFAOYSA-N trifluorochlorine Chemical compound FCl(F)F JOHWNGGYGAVMGU-UHFFFAOYSA-N 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000010290 vacuum plasma spraying Methods 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
-
- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/06—Metallic material
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
-
- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
- C23C4/11—Oxides
-
- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/134—Plasma spraying
-
- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/18—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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/18—After-treatment
- C23C4/185—Separation of the coating from the substrate
-
- 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
Definitions
- This invention relates to an yttrium-base sprayed coating formed by thermally spraying yttrium oxide, yttrium fluoride and/or yttrium oxyfluoride, which is suited as a low dusting coating on parts and articles used in a corrosive plasma atmosphere as encountered in a semiconductor device fabrication process.
- Typical corrosive halogen-base gases are fluorine-base gases such as SF 6 , CF 4 , CHF 3 , ClF 3 and HF and chlorine-base gases such as Cl 2 , BCl 3 and HCl.
- the equipment used for such treatment typically includes parts or components having corrosion resistant coatings on their surface. For example, parts or components having coatings formed by spraying yttrium oxide (Patent Document 1) and yttrium fluoride (Patent Documents 2 and 3) to the surface of metallic aluminum and aluminum oxide ceramic substrates are known to be fully corrosion resistant and used in practice.
- yttrium-base particles may spall off the surface of yttrium-base coatings on the parts during etching treatment and fall onto silicon wafers to interfere with the etching treatment. This causes to reduce the manufacture yield of semiconductor devices. There is a tendency that the number of yttrium-base particles spalling off the yttrium-base coating surface is high at the early stage of etching treatment and decreases with the lapse of etching time.
- Patent Documents 4 and 5 relating to the spraying technology are also incorporated herein by reference.
- Patent Document 1 JP 4006596 (U.S. Pat. No. 6,852,433)
- Patent Document 2 JP 3523222 (U.S. Pat. No. 6,685,991)
- Patent Document 3 JP-A 2011-514933 (US 20090214825)
- Patent Document 4 JP-A 2008-133528 (U.S. Pat. No. 8,349,450)
- Patent Document 5 JP 4591722 (US 20130122218)
- An object of the invention is to provide an yttrium-base sprayed coating which is formed by thermally spraying one or more compounds selected from among yttrium oxide, yttrium fluoride, and yttrium oxyfluoride, capable of substantially preventing yttrium-base particles from spalling off the coating surface during etching or similar treatment, and thus suited for use as a low dusting coating on parts or articles used in a corrosive plasma atmosphere during the semiconductor device fabrication process.
- a particulate material is melted in a plasma flame into droplets, after which droplets deposit and solidify on a substrate to form a coating. If the size of material particles is too small, some particles may not enter the flame, but deposit on the coating in the unmelted state. Also, once particles are melted, sometimes droplets may burst on the coating into finer droplets, which will deposit on the coating as finer particles.
- Patent Document 5 proposes physical removal of sticky particles (i.e., particles which are not removable by ultrapure water cleaning or ultrasonic cleaning) by polishing or blasting. However, physical removal such as polishing is not so effective because the treatment itself generates fine particles.
- an improved yttrium-base sprayed coating is obtained by thermally spraying one or more compounds selected from among yttrium oxide, yttrium fluoride, and yttrium oxyfluoride to form a coating of 10 to 500 ⁇ m thick, and chemically cleaning the coating with a cleaning liquid in the form of an aqueous solution of organic acid or inorganic acid or a mixture thereof for effectively removing yttrium-base particles anchored to the coating surface until the population of particles having a size of up to 300 nm becomes no more than 5 particles/mm 2 of the coating surface.
- the resulting yttrium-base sprayed coating prevents yttrium-base particles from spalling off to cause a failure during subsequent etching treatment, it is suitable for use as a low dusting coating on parts and articles used in a corrosive plasma atmosphere in the semiconductor device fabrication process.
- the invention provides an yttrium-base sprayed coating comprising one or more compounds selected from the group consisting of yttrium oxide, yttrium fluoride, and yttrium oxyfluoride and having a thickness of 10 to 500 ⁇ m, wherein particles with a size of up to 300 nm are present on a coating surface in a population of no more than 5 particles per square millimeters.
- the yttrium-base sprayed coating has a thickness of 80 to 400 ⁇ m.
- the yttrium-base sprayed coating is sprayed onto a surface of a substrate of metallic aluminum, aluminum oxide or metallic silicon.
- the invention provides a method for preparing a yttrium-base sprayed coating, comprising the steps of thermally spraying a particulate spray material comprising at least one compound selected from the group consisting of yttrium oxide, yttrium fluoride, and yttrium oxyfluoride to form a yttrium-base sprayed coating having a thickness of 10 to 500 ⁇ m and chemically cleaning a surface of the coating with a cleaning liquid which is an organic acid aqueous solution, inorganic acid aqueous solution or organic acid/inorganic acid aqueous solution until a population of particles with a size of up to 300 nm is no more than 5 particles per square millimeters of the coating surface.
- a cleaning liquid which is an organic acid aqueous solution, inorganic acid aqueous solution or organic acid/inorganic acid aqueous solution until a population of particles with a size of up to 300 nm is no more than 5 particles per square millimeter
- the cleaning liquid is preferably an aqueous solution of an acid selected from the group consisting of a monofunctional carboxylic acid, difunctional carboxylic acid, trifunctional carboxylic acid, hydroxy acid, sulfonic acid, nitric acid, sulfuric acid, carbonic acid, hydrofluoric acid, and acidic ammonium fluoride or a mixture thereof.
- the monofunctional carboxylic acid is formic acid or acetic acid
- the difunctional carboxylic acid is maleic acid, tartaric acid or phthalic acid
- the trifunctional carboxylic acid is citric acid
- the hydroxy acid is lactic acid
- the sulfonic acid is methanesulfonic acid.
- the chemical cleaning step includes immersing the yttrium-base sprayed coating in the cleaning liquid to dissolve the coating to a depth of at least 0.01 ⁇ m from its surface for thereby removing particles with a size of up to 300 nm on the coating surface.
- the yttrium-base sprayed coating of the invention exhibits high corrosion resistance during treatment in a corrosive halogen-base gas plasma atmosphere, and prevents dusting as a result of yttrium-base particles spalling off during etching or similar treatment in the semiconductor device fabrication process, which is effective for improving the fabrication yield of semiconductor devices.
- the yttrium-base sprayed coating is thus suitable for use as a low dusting coating on parts and articles which are exposed to a corrosive plasma atmosphere.
- FIGS. 1, 2, 3 and 4 are SEM images of the surface of yttrium-base sprayed coatings in Examples 1, 2, 3 and 4, respectively.
- FIGS. 5 and 6 are SEM images of the surface of yttrium-base sprayed coatings in Comparative Examples 1 and 2, respectively.
- the yttrium-base sprayed coating of the invention is formed by thermally spraying one or more compounds selected from among yttrium oxide, yttrium fluoride, and yttrium oxyfluoride.
- Thermal spraying to a substrate is desirably atmospheric plasma spraying or vacuum plasma spraying.
- the plasma gas used herein may be nitrogen/hydrogen, argon/hydrogen, argon/helium, argon/nitrogen, argon alone, or nitrogen gas alone, but not limited thereto.
- the substrate subject to thermal spraying include, but are not limited to, substrates of stainless steel, aluminum, nickel, chromium, zinc, and alloys thereof, metal silicon, aluminum oxide, aluminum nitride, silicon nitride, silicon carbide, and quartz glass when parts or components of the semiconductor fabrication equipment are contemplated.
- the conditions under which yttrium oxide, yttrium fluoride or yttrium oxyfluoride is thermally sprayed are not particularly limited.
- the thermal spraying conditions may be determined as appropriate depending on the identity of substrate, the particle size and composition of spray material, and a particular application of the resulting sprayed component.
- an yttrium oxide coating when an yttrium oxide coating is formed on a metal aluminum substrate, it may be deposited by argon/hydrogen atmospheric plasma spraying using yttrium oxide powder having an average particle size D50 of about 20 ⁇ m and a gas mixture of 40 L/min of argon and 5 L/min of hydrogen.
- the thermal spraying conditions including a spray distance, current value and voltage value may be determined as appropriate depending on a particular application of the sprayed component.
- the feed rates of argon and hydrogen gases may be suitably adjusted.
- the sprayed coating i.e., yttrium-base sprayed coating should have a thickness of 10 to 500 ⁇ m.
- a coating of less than 10 ⁇ m thick may be less corrosion resistant or allow the substrate surface to be partly exposed in the cleaning step to be described below.
- a coating of more than 500 ⁇ m thick may simply add to the cost because no further improvement in corrosion resistance is expectable.
- the thickness of the coating is preferably 80 to 400 ⁇ m, more preferably 100 to 400 ⁇ m, and even more preferably 100 to 300 ⁇ m.
- the surface of the yttrium-base sprayed coating is then cleaned with a preselected cleaning liquid to remove yttrium-base particles anchored thereto until the population (or number) of yttrium-base particles with a size of up to 300 nm becomes no more than 5 particles/square millimeters (mm 2 ) of the coating surface. It is, of course, most preferred that the population of yttrium-base particles with a size of up to 300 nm on the coating surface be 0. As long as the population is no more than 5 particles/mm 2 , dusting to such an extent as to invite a substantial loss of production yield does not occur during etching treatment in the semiconductor device fabrication process.
- the “size” of yttrium-base particles refers to the maximum diameter of individual particles measured by microscopy under a scanning electron microscope (SEM) or the like. As seen from the images of FIGS. 5 and 6 , no or only a few particles with a size in excess of 300 nm are present on the sprayed coating surface. Removal of particles with a size of up to 300 nm means removal of substantially all inhibitory particles.
- the cleaning liquid is an aqueous solution of organic acid, aqueous solution of inorganic acid or aqueous solution of mixed organic and inorganic acids.
- the organic acid is not particularly limited as long as it is water-soluble.
- Suitable organic acids include, but are not limited to, monofunctional carboxylic acids such as formic acid and acetic acid, difunctional carboxylic acids such as maleic acid, tartaric acid and phthalic acid, trifunctional carboxylic acids such as citric acid, hydroxy acids such as lactic acid, and sulfonic acids such as methanesulfonic acid. Inter alia, tartaric acid and citric acid are preferred because they are edible, nontoxic and easy to handle.
- the inorganic acid is not particularly limited as long as it is water-soluble. Suitable inorganic acids include nitric acid, sulfuric acid, carbonic acid, hydrofluoric acid, and acidic ammonium fluoride.
- the cleaning technique is not particularly limited.
- a part or component in the form of a substrate having the yttrium-base sprayed coating formed on its surface is wholly immersed in the cleaning liquid because this technique is effective and efficient.
- the area of the substrate that should avoid corrosion with acid is desirably masked with resin tape or sheet when a strong acid is used for cleaning. Cleaning without masking is possible when a weak organic acid is used for cleaning, for example, a carboxylic acid or hydroxy acid such as phthalic acid, tartaric acid or citric acid.
- a buffer solution based on a combination of acid and salt may be used as the cleaning liquid.
- the yttrium-base sprayed coating is chemically cleaned with the cleaning liquid to dissolve a thin layer from the coating surface for removing particles with a size of up to 300 nm which become a source of dusting.
- the dissolution depth is preferably at least 0.01 ⁇ m from the original coating surface. Although the upper limit of dissolution depth is not critical, the dissolution depth is preferably up to 20 ⁇ m. More preferably the dissolution depth is 1 to 20 ⁇ m from the coating surface. A dissolution depth of less than 0.01 ⁇ m may be insufficient to remove particles with a size of up to 300 nm and fail to reach a population of no more than 5 particles/mm 2 . A dissolution depth in excess of 20 ⁇ m may simply make the coating thinner without further improvements in particle removal.
- the coating is rinsed with ultrapure water to thoroughly remove the acid and dried in vacuum or under atmospheric pressure.
- yttrium-base particles having a size of up to 300 nm on the coating surface are detectable. According to the invention, yttrium-base particles are removed from the coating surface by the cleaning step until the population of particles reaches no more than 5 particles/mm 2 of the surface.
- An yttrium-base sprayed coating was obtained by thermally spraying the coating material shown in Table 1 onto a surface of a substrate of the material shown in Table 1, immersing the coated substrate in a cleaning liquid, which was an aqueous solution of the cleaning agent shown in Table 1, to clean the coating surface, thoroughly rinsing with ultrapure water, and vacuum drying.
- the surface of the yttrium-base coating thus obtained was observed under SEM, and yttrium-base particles having a size of up to 300 nm on the surface were inspected and counted.
- the results are shown in Table 1 and SEM images are shown in FIGS. 1 to 6 .
- the yttrium-base sprayed coating was formed by atmospheric plasma spraying using a gas mixture of 40 L/min of argon and 8 L/min of hydrogen.
- Example Comparative Example 1 2 3 4 1 2 Spray material Y 2 O 3 Y 2 O 3 + YF 3 YF 3 YOF Y 2 O 3 YF 3 Coating thickness, 200 300 100 200 200 200 ⁇ m Substrate material Al Al 2 O 3 Si Al Al Al Al Cleaning Cleaning agent tartaric citric hydrofluoric lactic no no conditions acid acid acid + acid cleaning cleaning acidic ammonium fluoride Concentration, 2 1 0.05 + 0.1 2 — — mol/L Temperature, 30 50 30 50 — — ° C.
- the yttrium-base sprayed coatings in Examples 1 to 4 bear no particles on their surface whereas numerous particles are on the yttrium-base sprayed coatings in Comparative Examples 1 and 2 which omit cleaning with an aqueous solution of acid or cleaning agent. It is readily presumed that these particles cause dust generation during etching treatment.
- dusting as a result of yttrium-base particles spalling off during etching treatment in a semiconductor device fabrication process is substantially prevented. This will eventually improve the fabrication yield of semiconductor devices.
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Abstract
Description
- This application is a divisional of U.S. application Ser. No. 15/220,652 filed on Jul. 27, 2016, which is based upon and claims the benefit of priority of the non-provisional application which claims priority under 35 U.S.C. §119(a) on Patent Application No. 2015-151568 filed in Japan on Jul. 31, 2015, the entire contents of which are incorporated herein by reference.
- This invention relates to an yttrium-base sprayed coating formed by thermally spraying yttrium oxide, yttrium fluoride and/or yttrium oxyfluoride, which is suited as a low dusting coating on parts and articles used in a corrosive plasma atmosphere as encountered in a semiconductor device fabrication process.
- In the prior art process for manufacturing semiconductor devices, treatment is often carried out in a corrosive halogen-base gas plasma atmosphere. Typical corrosive halogen-base gases are fluorine-base gases such as SF6, CF4, CHF3, ClF3 and HF and chlorine-base gases such as Cl2, BCl3 and HCl. The equipment used for such treatment typically includes parts or components having corrosion resistant coatings on their surface. For example, parts or components having coatings formed by spraying yttrium oxide (Patent Document 1) and yttrium fluoride (Patent Documents 2 and 3) to the surface of metallic aluminum and aluminum oxide ceramic substrates are known to be fully corrosion resistant and used in practice.
- As the current semiconductor technology aims at higher integration, the size of interconnections is approaching to 20 nm or less. In the device fabrication process, yttrium-base particles may spall off the surface of yttrium-base coatings on the parts during etching treatment and fall onto silicon wafers to interfere with the etching treatment. This causes to reduce the manufacture yield of semiconductor devices. There is a tendency that the number of yttrium-base particles spalling off the yttrium-base coating surface is high at the early stage of etching treatment and decreases with the lapse of etching time. Patent Documents 4 and 5 relating to the spraying technology are also incorporated herein by reference.
- Patent Document 1: JP 4006596 (U.S. Pat. No. 6,852,433)
- Patent Document 2: JP 3523222 (U.S. Pat. No. 6,685,991)
- Patent Document 3: JP-A 2011-514933 (US 20090214825)
- Patent Document 4: JP-A 2008-133528 (U.S. Pat. No. 8,349,450)
- Patent Document 5: JP 4591722 (US 20130122218)
- An object of the invention is to provide an yttrium-base sprayed coating which is formed by thermally spraying one or more compounds selected from among yttrium oxide, yttrium fluoride, and yttrium oxyfluoride, capable of substantially preventing yttrium-base particles from spalling off the coating surface during etching or similar treatment, and thus suited for use as a low dusting coating on parts or articles used in a corrosive plasma atmosphere during the semiconductor device fabrication process.
- When a coating of yttrium oxide, yttrium fluoride or yttrium oxyfluoride is formed by plasma spraying, a particulate material is melted in a plasma flame into droplets, after which droplets deposit and solidify on a substrate to form a coating. If the size of material particles is too small, some particles may not enter the flame, but deposit on the coating in the unmelted state. Also, once particles are melted, sometimes droplets may burst on the coating into finer droplets, which will deposit on the coating as finer particles. Such fine (unmelted or burst) particles which deposit on the coating surface in the course of spraying are covered with the following droplets and thus integrated into a dense coating, whereas foreign particles which deposit on the coating surface near the end of spraying remain bonded as such. It is difficult to remove the bonded particles by ultrapure water cleaning, ultrasonic cleaning or the like. If fine particles spall off during etching treatment, they become a source of dusting. Patent Document 5 proposes physical removal of sticky particles (i.e., particles which are not removable by ultrapure water cleaning or ultrasonic cleaning) by polishing or blasting. However, physical removal such as polishing is not so effective because the treatment itself generates fine particles.
- The inventors have found that an improved yttrium-base sprayed coating is obtained by thermally spraying one or more compounds selected from among yttrium oxide, yttrium fluoride, and yttrium oxyfluoride to form a coating of 10 to 500 μm thick, and chemically cleaning the coating with a cleaning liquid in the form of an aqueous solution of organic acid or inorganic acid or a mixture thereof for effectively removing yttrium-base particles anchored to the coating surface until the population of particles having a size of up to 300 nm becomes no more than 5 particles/mm2 of the coating surface. Since the resulting yttrium-base sprayed coating prevents yttrium-base particles from spalling off to cause a failure during subsequent etching treatment, it is suitable for use as a low dusting coating on parts and articles used in a corrosive plasma atmosphere in the semiconductor device fabrication process.
- In one aspect, the invention provides an yttrium-base sprayed coating comprising one or more compounds selected from the group consisting of yttrium oxide, yttrium fluoride, and yttrium oxyfluoride and having a thickness of 10 to 500 μm, wherein particles with a size of up to 300 nm are present on a coating surface in a population of no more than 5 particles per square millimeters.
- Preferably the yttrium-base sprayed coating has a thickness of 80 to 400 μm.
- Typically the yttrium-base sprayed coating is sprayed onto a surface of a substrate of metallic aluminum, aluminum oxide or metallic silicon.
- In another aspect, the invention provides a method for preparing a yttrium-base sprayed coating, comprising the steps of thermally spraying a particulate spray material comprising at least one compound selected from the group consisting of yttrium oxide, yttrium fluoride, and yttrium oxyfluoride to form a yttrium-base sprayed coating having a thickness of 10 to 500 μm and chemically cleaning a surface of the coating with a cleaning liquid which is an organic acid aqueous solution, inorganic acid aqueous solution or organic acid/inorganic acid aqueous solution until a population of particles with a size of up to 300 nm is no more than 5 particles per square millimeters of the coating surface.
- The cleaning liquid is preferably an aqueous solution of an acid selected from the group consisting of a monofunctional carboxylic acid, difunctional carboxylic acid, trifunctional carboxylic acid, hydroxy acid, sulfonic acid, nitric acid, sulfuric acid, carbonic acid, hydrofluoric acid, and acidic ammonium fluoride or a mixture thereof. Typically, the monofunctional carboxylic acid is formic acid or acetic acid, the difunctional carboxylic acid is maleic acid, tartaric acid or phthalic acid, the trifunctional carboxylic acid is citric acid, the hydroxy acid is lactic acid, and the sulfonic acid is methanesulfonic acid.
- In a preferred embodiment, the chemical cleaning step includes immersing the yttrium-base sprayed coating in the cleaning liquid to dissolve the coating to a depth of at least 0.01 μm from its surface for thereby removing particles with a size of up to 300 nm on the coating surface.
- The yttrium-base sprayed coating of the invention exhibits high corrosion resistance during treatment in a corrosive halogen-base gas plasma atmosphere, and prevents dusting as a result of yttrium-base particles spalling off during etching or similar treatment in the semiconductor device fabrication process, which is effective for improving the fabrication yield of semiconductor devices. The yttrium-base sprayed coating is thus suitable for use as a low dusting coating on parts and articles which are exposed to a corrosive plasma atmosphere.
-
FIGS. 1, 2, 3 and 4 are SEM images of the surface of yttrium-base sprayed coatings in Examples 1, 2, 3 and 4, respectively. -
FIGS. 5 and 6 are SEM images of the surface of yttrium-base sprayed coatings in Comparative Examples 1 and 2, respectively. - The yttrium-base sprayed coating of the invention is formed by thermally spraying one or more compounds selected from among yttrium oxide, yttrium fluoride, and yttrium oxyfluoride.
- Thermal spraying to a substrate is desirably atmospheric plasma spraying or vacuum plasma spraying. The plasma gas used herein may be nitrogen/hydrogen, argon/hydrogen, argon/helium, argon/nitrogen, argon alone, or nitrogen gas alone, but not limited thereto. Examples of the substrate subject to thermal spraying include, but are not limited to, substrates of stainless steel, aluminum, nickel, chromium, zinc, and alloys thereof, metal silicon, aluminum oxide, aluminum nitride, silicon nitride, silicon carbide, and quartz glass when parts or components of the semiconductor fabrication equipment are contemplated. The conditions under which yttrium oxide, yttrium fluoride or yttrium oxyfluoride is thermally sprayed are not particularly limited. The thermal spraying conditions may be determined as appropriate depending on the identity of substrate, the particle size and composition of spray material, and a particular application of the resulting sprayed component.
- For example, when an yttrium oxide coating is formed on a metal aluminum substrate, it may be deposited by argon/hydrogen atmospheric plasma spraying using yttrium oxide powder having an average particle size D50 of about 20 μm and a gas mixture of 40 L/min of argon and 5 L/min of hydrogen. The thermal spraying conditions including a spray distance, current value and voltage value may be determined as appropriate depending on a particular application of the sprayed component. Likewise, the feed rates of argon and hydrogen gases may be suitably adjusted.
- The sprayed coating, i.e., yttrium-base sprayed coating should have a thickness of 10 to 500 μm. A coating of less than 10 μm thick may be less corrosion resistant or allow the substrate surface to be partly exposed in the cleaning step to be described below. A coating of more than 500 μm thick may simply add to the cost because no further improvement in corrosion resistance is expectable. The thickness of the coating is preferably 80 to 400 μm, more preferably 100 to 400 μm, and even more preferably 100 to 300 μm.
- According to the invention, the surface of the yttrium-base sprayed coating is then cleaned with a preselected cleaning liquid to remove yttrium-base particles anchored thereto until the population (or number) of yttrium-base particles with a size of up to 300 nm becomes no more than 5 particles/square millimeters (mm2) of the coating surface. It is, of course, most preferred that the population of yttrium-base particles with a size of up to 300 nm on the coating surface be 0. As long as the population is no more than 5 particles/mm2, dusting to such an extent as to invite a substantial loss of production yield does not occur during etching treatment in the semiconductor device fabrication process. As used herein, the “size” of yttrium-base particles refers to the maximum diameter of individual particles measured by microscopy under a scanning electron microscope (SEM) or the like. As seen from the images of
FIGS. 5 and 6 , no or only a few particles with a size in excess of 300 nm are present on the sprayed coating surface. Removal of particles with a size of up to 300 nm means removal of substantially all inhibitory particles. - The cleaning liquid is an aqueous solution of organic acid, aqueous solution of inorganic acid or aqueous solution of mixed organic and inorganic acids. The organic acid is not particularly limited as long as it is water-soluble. Suitable organic acids include, but are not limited to, monofunctional carboxylic acids such as formic acid and acetic acid, difunctional carboxylic acids such as maleic acid, tartaric acid and phthalic acid, trifunctional carboxylic acids such as citric acid, hydroxy acids such as lactic acid, and sulfonic acids such as methanesulfonic acid. Inter alia, tartaric acid and citric acid are preferred because they are edible, nontoxic and easy to handle. The inorganic acid is not particularly limited as long as it is water-soluble. Suitable inorganic acids include nitric acid, sulfuric acid, carbonic acid, hydrofluoric acid, and acidic ammonium fluoride.
- The cleaning technique is not particularly limited. Preferably, a part or component in the form of a substrate having the yttrium-base sprayed coating formed on its surface is wholly immersed in the cleaning liquid because this technique is effective and efficient. For those substrates of metallic aluminum and silicon which are readily dissolved in acid, the area of the substrate that should avoid corrosion with acid is desirably masked with resin tape or sheet when a strong acid is used for cleaning. Cleaning without masking is possible when a weak organic acid is used for cleaning, for example, a carboxylic acid or hydroxy acid such as phthalic acid, tartaric acid or citric acid. For those substrates of quart glass or Al2O3 ceramics which are acid resistant, cleaning without masking is possible even with a strong acid solution such as nitric acid. In some cases, a buffer solution based on a combination of acid and salt may be used as the cleaning liquid.
- The yttrium-base sprayed coating is chemically cleaned with the cleaning liquid to dissolve a thin layer from the coating surface for removing particles with a size of up to 300 nm which become a source of dusting. The dissolution depth is preferably at least 0.01 μm from the original coating surface. Although the upper limit of dissolution depth is not critical, the dissolution depth is preferably up to 20 μm. More preferably the dissolution depth is 1 to 20 μm from the coating surface. A dissolution depth of less than 0.01 μm may be insufficient to remove particles with a size of up to 300 nm and fail to reach a population of no more than 5 particles/mm2. A dissolution depth in excess of 20 μm may simply make the coating thinner without further improvements in particle removal.
- After cleaning, the coating is rinsed with ultrapure water to thoroughly remove the acid and dried in vacuum or under atmospheric pressure.
- When a secondary electron image (magnification ×10,000 or more) of the dry coating surface is observed under SEM, yttrium-base particles having a size of up to 300 nm on the coating surface are detectable. According to the invention, yttrium-base particles are removed from the coating surface by the cleaning step until the population of particles reaches no more than 5 particles/mm2 of the surface.
- Examples are given below by way of illustration and not by way of limitation.
- An yttrium-base sprayed coating was obtained by thermally spraying the coating material shown in Table 1 onto a surface of a substrate of the material shown in Table 1, immersing the coated substrate in a cleaning liquid, which was an aqueous solution of the cleaning agent shown in Table 1, to clean the coating surface, thoroughly rinsing with ultrapure water, and vacuum drying. The surface of the yttrium-base coating thus obtained was observed under SEM, and yttrium-base particles having a size of up to 300 nm on the surface were inspected and counted. The results are shown in Table 1 and SEM images are shown in
FIGS. 1 to 6 . Notably, the yttrium-base sprayed coating was formed by atmospheric plasma spraying using a gas mixture of 40 L/min of argon and 8 L/min of hydrogen. -
TABLE 1 Example Comparative Example 1 2 3 4 1 2 Spray material Y2O3 Y2O3 + YF3 YF3 YOF Y2O3 YF3 Coating thickness, 200 300 100 200 200 200 μm Substrate material Al Al2O3 Si Al Al Al Cleaning Cleaning agent tartaric citric hydrofluoric lactic no no conditions acid acid acid + acid cleaning cleaning acidic ammonium fluoride Concentration, 2 1 0.05 + 0.1 2 — — mol/L Temperature, 30 50 30 50 — — ° C. Time, hr 4 12 0.5 12 — — Dissolution 2 20 2 10 — — depth, μm Particle population 0 0 0 0 numerous numerous on surface (particles/mm2) SEM image FIG. 1 FIG. 2 FIG. 3 FIG. 4 FIG. 5 FIG. 6 - As is evident from Table 1 and
FIGS. 1 to 6 , the yttrium-base sprayed coatings in Examples 1 to 4 bear no particles on their surface whereas numerous particles are on the yttrium-base sprayed coatings in Comparative Examples 1 and 2 which omit cleaning with an aqueous solution of acid or cleaning agent. It is readily presumed that these particles cause dust generation during etching treatment. When parts or components having yttrium-base sprayed coatings of Examples 1 to 4 deposited thereon are used, dusting as a result of yttrium-base particles spalling off during etching treatment in a semiconductor device fabrication process is substantially prevented. This will eventually improve the fabrication yield of semiconductor devices. - Japanese Patent Application No. 2015-151568 is incorporated herein by reference.
- Although some preferred embodiments have been described, many modifications and variations may be made thereto in light of the above teachings. It is therefore to be understood that the invention may be practiced otherwise than as specifically described without departing from the scope of the appended claims.
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US20180327892A1 (en) * | 2017-05-10 | 2018-11-15 | Applied Materials, Inc. | Metal oxy-flouride films for chamber components |
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JPS523222B1 (en) | 1971-07-29 | 1977-01-26 | ||
JPS523222A (en) | 1975-06-24 | 1977-01-11 | Hiraki Takehara | Sound adsorbing wall body |
JPS636596A (en) | 1986-06-26 | 1988-01-12 | 富士通株式会社 | Driving of matrix display panel |
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JP3523222B2 (en) | 2000-07-31 | 2004-04-26 | 信越化学工業株式会社 | Thermal spray material and method of manufacturing the same |
JP4006596B2 (en) | 2002-07-19 | 2007-11-14 | 信越化学工業株式会社 | Rare earth oxide sprayed member and powder for spraying |
EP1524682B1 (en) * | 2003-10-17 | 2011-10-05 | Tosoh Corporation | Component for vacuum apparatus, production method thereof and apparatus using the same |
US7494723B2 (en) * | 2005-07-29 | 2009-02-24 | Tocalo Co., Ltd. | Y2O3 spray-coated member and production method thereof |
JP4643478B2 (en) * | 2006-03-20 | 2011-03-02 | トーカロ株式会社 | Manufacturing method of ceramic covering member for semiconductor processing equipment |
JP5159204B2 (en) | 2006-10-31 | 2013-03-06 | 株式会社フジミインコーポレーテッド | Thermal spray powder, thermal spray coating formation method, plasma resistant member, and plasma processing chamber |
JP4952257B2 (en) * | 2007-01-11 | 2012-06-13 | 東ソー株式会社 | Cleaning composition for semiconductor manufacturing apparatus member and cleaning method using the same |
US8114473B2 (en) * | 2007-04-27 | 2012-02-14 | Toto Ltd. | Composite structure and production method thereof |
JP4591722B2 (en) * | 2008-01-24 | 2010-12-01 | 信越化学工業株式会社 | Manufacturing method of ceramic sprayed member |
US20090214825A1 (en) | 2008-02-26 | 2009-08-27 | Applied Materials, Inc. | Ceramic coating comprising yttrium which is resistant to a reducing plasma |
CN102296263B (en) * | 2010-06-25 | 2013-04-24 | 中国科学院微电子研究所 | Modification treatment method for inner surface of plasma etching process chamber |
JP5521184B2 (en) * | 2012-01-17 | 2014-06-11 | トーカロ株式会社 | Method for producing fluoride spray coating coated member |
US8734907B2 (en) * | 2012-02-02 | 2014-05-27 | Sematech, Inc. | Coating of shield surfaces in deposition systems |
US20150140906A1 (en) * | 2012-04-27 | 2015-05-21 | Fujimi Incorporated | Cleaning agent for alloy material, and method for producing alloy material |
JP5939084B2 (en) * | 2012-08-22 | 2016-06-22 | 信越化学工業株式会社 | Method for producing rare earth element oxyfluoride powder sprayed material |
US20160254125A1 (en) * | 2015-02-27 | 2016-09-01 | Lam Research Corporation | Method for coating surfaces |
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CN106399896A (en) | 2017-02-15 |
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KR20170015236A (en) | 2017-02-08 |
CN116695048A (en) | 2023-09-05 |
US20170029628A1 (en) | 2017-02-02 |
JP6500681B2 (en) | 2019-04-17 |
TWI687548B (en) | 2020-03-11 |
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