CN113874550B - 层叠体及其制造方法 - Google Patents
层叠体及其制造方法 Download PDFInfo
- Publication number
- CN113874550B CN113874550B CN202080037913.4A CN202080037913A CN113874550B CN 113874550 B CN113874550 B CN 113874550B CN 202080037913 A CN202080037913 A CN 202080037913A CN 113874550 B CN113874550 B CN 113874550B
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- Prior art keywords
- nickel
- gold
- film layer
- plating film
- layer
- Prior art date
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 270
- 238000007747 plating Methods 0.000 claims abstract description 199
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 136
- 229910052751 metal Inorganic materials 0.000 claims abstract description 44
- 239000002184 metal Substances 0.000 claims abstract description 44
- DBJLJFTWODWSOF-UHFFFAOYSA-L nickel(ii) fluoride Chemical compound F[Ni]F DBJLJFTWODWSOF-UHFFFAOYSA-L 0.000 claims abstract description 30
- 239000004065 semiconductor Substances 0.000 claims abstract description 7
- 239000010410 layer Substances 0.000 claims description 142
- 239000010931 gold Substances 0.000 claims description 65
- 229910052737 gold Inorganic materials 0.000 claims description 65
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 59
- 239000011247 coating layer Substances 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 27
- 229910052698 phosphorus Inorganic materials 0.000 claims description 23
- 239000011574 phosphorus Substances 0.000 claims description 23
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 claims description 22
- 239000000758 substrate Substances 0.000 claims description 22
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 19
- 229910001096 P alloy Inorganic materials 0.000 claims description 18
- 239000010935 stainless steel Substances 0.000 claims description 17
- 229910001220 stainless steel Inorganic materials 0.000 claims description 17
- 238000000576 coating method Methods 0.000 claims description 14
- 238000007789 sealing Methods 0.000 claims description 12
- 230000009467 reduction Effects 0.000 claims description 11
- -1 gold ions Chemical class 0.000 claims description 10
- 229910052731 fluorine Inorganic materials 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 238000006467 substitution reaction Methods 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- 229910000838 Al alloy Inorganic materials 0.000 claims description 7
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 7
- 239000011737 fluorine Substances 0.000 claims description 7
- 239000003638 chemical reducing agent Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 1
- 230000007797 corrosion Effects 0.000 abstract description 23
- 238000005260 corrosion Methods 0.000 abstract description 23
- 239000002253 acid Substances 0.000 abstract description 6
- 239000007769 metal material Substances 0.000 abstract description 2
- 238000011282 treatment Methods 0.000 description 28
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 14
- 239000007789 gas Substances 0.000 description 13
- 230000015572 biosynthetic process Effects 0.000 description 12
- 239000011248 coating agent Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 7
- 238000005238 degreasing Methods 0.000 description 5
- 238000005554 pickling Methods 0.000 description 5
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical group [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 4
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 4
- 150000002815 nickel Chemical class 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000004913 activation Effects 0.000 description 3
- 238000007772 electroless plating Methods 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 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 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 2
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 238000003682 fluorination reaction Methods 0.000 description 2
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229940078494 nickel acetate Drugs 0.000 description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 2
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 2
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910001380 potassium hypophosphite Inorganic materials 0.000 description 2
- CRGPNLUFHHUKCM-UHFFFAOYSA-M potassium phosphinate Chemical compound [K+].[O-]P=O CRGPNLUFHHUKCM-UHFFFAOYSA-M 0.000 description 2
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 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 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- RJTANRZEWTUVMA-UHFFFAOYSA-N boron;n-methylmethanamine Chemical compound [B].CNC RJTANRZEWTUVMA-UHFFFAOYSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- ADPOBOOHCUVXGO-UHFFFAOYSA-H dioxido-oxo-sulfanylidene-$l^{6}-sulfane;gold(3+) Chemical compound [Au+3].[Au+3].[O-]S([O-])(=O)=S.[O-]S([O-])(=O)=S.[O-]S([O-])(=O)=S ADPOBOOHCUVXGO-UHFFFAOYSA-H 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001312 dry etching Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 1
- SRCZENKQCOSNAI-UHFFFAOYSA-H gold(3+);trisulfite Chemical compound [Au+3].[Au+3].[O-]S([O-])=O.[O-]S([O-])=O.[O-]S([O-])=O SRCZENKQCOSNAI-UHFFFAOYSA-H 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 1
- 239000004312 hexamethylene tetramine Substances 0.000 description 1
- 229910000042 hydrogen bromide Inorganic materials 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- QKCGXXHCELUCKW-UHFFFAOYSA-N n-[4-[4-(dinaphthalen-2-ylamino)phenyl]phenyl]-n-naphthalen-2-ylnaphthalen-2-amine Chemical compound C1=CC=CC2=CC(N(C=3C=CC(=CC=3)C=3C=CC(=CC=3)N(C=3C=C4C=CC=CC4=CC=3)C=3C=C4C=CC=CC4=CC=3)C3=CC4=CC=CC=C4C=C3)=CC=C21 QKCGXXHCELUCKW-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- CTSLXHKWHWQRSH-UHFFFAOYSA-N oxalyl chloride Substances ClC(=O)C(Cl)=O CTSLXHKWHWQRSH-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- NRTDAKURTMLAFN-UHFFFAOYSA-N potassium;gold(3+);tetracyanide Chemical compound [K+].[Au+3].N#[C-].N#[C-].N#[C-].N#[C-] NRTDAKURTMLAFN-UHFFFAOYSA-N 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 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
- 238000004073 vulcanization Methods 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
- C23C28/321—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer with at least one metal alloy layer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
- B32B15/013—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of an iron alloy or steel, another layer being formed of a metal other than iron or aluminium
-
- 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
- C23C18/42—Coating with noble metals
-
- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/021—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material including at least one metal alloy layer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
- B32B15/017—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of aluminium or an aluminium alloy, another layer being formed of an alloy based on a non ferrous metal other than aluminium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
- B32B15/018—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of a noble metal or a noble metal alloy
-
- 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
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
-
- 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
- C23C18/1646—Characteristics of the product obtained
- C23C18/165—Multilayered product
- C23C18/1651—Two or more layers only obtained by electroless plating
-
- 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
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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
- 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
- C23C18/1692—Heat-treatment
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Abstract
本发明的课题是提供一种可适用于半导体制造装置的构成部件且耐腐蚀性、特别是对酸的耐腐蚀性优异的金属材料。本发明涉及的层叠体具有金属基材、在所述金属基材上形成的第1含镍镀敷被膜层、在所述第1含镍镀敷被膜层形成的镀金被膜层、在所述镀金被膜层上形成的第2含镍镀敷被膜层、以及在所述第2含镍镀敷被膜层上形成的氟化镍被膜层。
Description
技术领域
本发明涉及层叠体及其制造方法。更具体而言，涉及适合作为半导体制造装置等的构成部件的层叠体及其制造方法。
背景技术
以往，在半导体制造工艺中，在干蚀刻工序和制造装置的清洁等中，使用氟、氯化氢、三氯化硼、三氟化氮、三氟化氯、溴化氢等卤素类的反应性和腐蚀性强的特殊气体(以下也称为“腐蚀性气体”)。
但是，上述腐蚀性气体与气氛下的水分反应而水解时，会产生氟化氢、草酸和氯化氢等生成物。上述生成物容易腐蚀使用上述腐蚀性气体时的阀、接头、配管和反应室等构成部件的金属表面，因此成为问题。
迄今为止，为了谋求耐腐蚀性的提高，进行了对金属基材实施镍-磷合金镀敷、形成镍的氟化钝态膜的方法(例如，参照专利文献1～3)，但这些方法有时不充分。
此外，镀层表面的针孔也会成为腐蚀加剧的原因。针孔的产生原因，可以认为是例如通过镀敷反应产生的氢气在形成镀敷被膜时成为气泡而阻碍成膜，或者残留在基材上的杂质(氧化膜、污垢、油分等)在前处理工序中未被除去而阻碍成膜等多种原因。对此，专利文献4中公开了在镀金上形成硬质的合金镀层，能够提高耐磨损性以及防止由气体、水分引起的氧化、硫化等导致的变色、腐蚀的方法。
在先技术文献
专利文献1：日本特许第2954716号公报
专利文献2：日本特许第3094000号公报
专利文献3：日本特开2004-360066号公报
专利文献4：日本特许第2581021号公报
发明内容
发明要解决的课题
根据本发明人的研究，如专利文献1～3所示，在镍-磷合金镀层表面形成镍的氟化钝态膜的方法中，已知会发生以镍-磷合金镀层的针孔为起点的腐蚀，对于盐酸耐腐蚀性有时不充分。另外，在专利文献4的方法中，由于最表面层是合金镀层，因此存在无法显著提高耐腐蚀性的课题。
因此，本发明的课题是提供一种可适用于半导体制造装置的构成部件且耐腐蚀性、特别是对酸的耐腐蚀性优异的金属材料。
用于解决课题的手段
本发明例如涉及以下的[1]～[14]。
[1]一种层叠体，具有金属基材、在所述金属基材上形成的第1含镍镀敷被膜层、在所述第1含镍镀敷被膜层上形成的镀金被膜层、在所述镀金被膜层上形成的第2含镍镀敷被膜层、以及在所述第2含镍镀敷被膜层上形成的氟化镍被膜层。
[2]根据上述[1]记载的层叠体，所述镀金被膜层的针孔被镍单质金属封孔，并且，所述第1含镍镀敷被膜层和第2含镍镀敷被膜层的针孔被金单质金属封孔。
[3]根据上述[1]或[2]记载的层叠体，所述金属基材包含选自不锈钢、铁、铝、铝合金、铜和铜合金中的至少一种金属。
[4]根据上述[1]～[3]中任一项记载的层叠体，在所述金属基材与所述第1含镍镀敷被膜层之间、以及所述镀金被膜层与所述第2含镍镀敷被膜层之间，具有镍触击电镀层。
[5]根据上述[1]～[4]中任一项记载的层叠体，所述第1含镍镀敷被膜层包含磷浓度为8质量％以上且小于10质量％的镍-磷合金镀层，并且，所述第2含镍镀敷被膜层包含磷浓度为10质量％以上且12质量％以下的镍-磷合金镀层。
[6]根据上述[1]～[5]中任一项记载的层叠体，所述镀金被膜层从所述第1含镍镀敷被膜层侧起依次包含置换型镀金被膜层和还原型镀金被膜层。
[7]根据上述[1]～[6]中任一项记载的层叠体，所述氟化镍被膜层的厚度为70nm以上。
[8]一种层叠体的制造方法，包括在金属基材上形成第1含镍镀敷被膜层的工序(A)、在所述第1含镍镀敷被膜层上形成镀金被膜层的工序(B)、在所述镀金被膜层上形成第2含镍镀敷被膜层的工序(C)、以及在所述第2含镍镀敷被膜层上形成氟化镍被膜层的工序(D)。
[9]根据上述[8]记载的层叠体的制造方法，在所述工序(C)与所述工序(D)之间，包括通过将工序(C)中得到的层叠体在温度250℃以上的条件下进行加热处理，从而利用镍单质金属将所述镀金被膜层的针孔封孔，并且，利用金单质金属将所述第1含镍镀敷被膜层和第2含镍镀敷被膜层的针孔封孔的工序(X)。
[10]根据上述[8]或[9]记载的层叠体的制造方法，所述工序(D)在氟气浓度为8体积％以上且温度为250℃以上的气氛下进行。
[11]根据上述[8]～[10]中任一项记载的层叠体的制造方法，在所述工序(A)之前和所述工序(C)之前，包括对金属基材以电流密度为3～20A/dm2的条件实施镍触击电镀处理的工序。
[12]根据上述[8]～[11]中任一项记载的层叠体的制造方法，所述工序(A)包括形成磷浓度为8质量％以上且小于10质量％的镍-磷合金镀层的工序，并且，所述工序(C)包括形成磷浓度为10质量％以上且12质量％以下的镍-磷合金镀层的工序。
[13]根据上述[8]～[12]中任一项记载的层叠体的制造方法，所述工序(B)包括形成置换型镀金被膜层的工序(b1)、和在该工序(b1)之后形成还原型镀金被膜层的工序(b2)。
[14]一种半导体制造装置的构成部件，由上述[1]～[7]中任一项记载的层叠体制成。
发明的效果
根据本发明，能够提供一种耐腐蚀性、特别是对酸的耐腐蚀性优异的层叠体。
附图说明
图1是表示封孔处理前后的层叠体的概略图((a)：封孔处理前，(b)：封孔处理后)。
具体实施方式
以下，对本发明的一个实施方式进行具体说明。
本发明的一个实施方式的层叠体具有金属基材、在所述金属基材上形成的第1含镍镀敷被膜层、在所述第1含镍镀敷被膜层上形成的镀金被膜层、在所述镀金被膜层上形成的第2含镍镀敷被膜层、以及在所述第2含镍镀敷被膜层上形成的氟化镍被膜层。
另外，本发明的一个实施方式的层叠体，优选所述镀金被膜层的针孔被镍单质金属封孔，并且，所述第1和第2含镍镀敷被膜层的针孔被金单质金属封孔。
本发明的一个实施方式的层叠体的制造方法，包括在金属基材上形成第1含镍镀敷被膜层的工序(A)、在所述第1含镍镀敷被膜层上形成镀金被膜层的工序(B)、在所述镀金被膜层上形成第2含镍镀敷被膜层的工序(C)、以及在所述第2含镍镀敷被膜层上形成氟化镍被膜层的工序(D)。
另外，本发明的一个实施方式的层叠体的制造方法，优选在所述工序(C)和所述工序(D)之间，包括通过将工序(C)中得到的层叠体在温度250℃以上和2小时以上的条件下进行加热处理，从而利用镍单质金属将所述镀金被膜层的针孔封孔，并且利用金单质金属将所述第1和第2含镍镀敷被膜层的针孔封孔的工序(X)。
[金属基材]
本发明的一个实施方式中使用的金属基材是至少表面由金属构成的基材。作为所述金属基材，没有特别限定，可举出半导体制造装置的构成部件通常使用的金属，优选为不锈钢、铁、铝、铝合金、铜和铜合金。
所述金属基材，为了使与含镍镀敷被膜层的密合性牢固，作为工序(A)的前处理，可以实施脱脂、酸洗或镍触击电镀处理等与基材相应的处理。镍触击电镀处理是使用含镍镀浴的预镀敷处理，镍触击电镀处理中的电流密度优选为3～20A/dm2，更优选为6～10A/dm2。另外，镍触击电镀处理的时间优选为1分钟以上且5分钟以下。
[第1含镍镀敷被膜层]
第1含镍镀敷被膜层通过工序(A)而形成于所述金属基材上。再者，在对所述金属基材实施镍触击电镀处理的情况下，在金属基材与第1镍镀敷被膜层之间具有镍触击电镀层。
从提高耐腐蚀性的观点出发，含镍镀敷被膜层优选含有磷，优选包含磷浓度为8质量％以上且小于10质量％的镍-磷合金镀层。
在将含镍镀敷被膜层整体设为100质量％时，第1含镍镀敷被膜层中的镍含量优选为80质量％以上，更优选为85～95质量％，特别优选为90～92质量％。通过使镍含量在上述范围，被膜层中的磷的比率增加，能够发挥优异的耐腐蚀性。
＜工序(A)＞
上述第1含镍镀敷被膜层可以使用含有镍盐和作为还原剂的磷化合物的无电解镀(化学镀)浴在金属基材上形成。作为镍盐，例如可举出硫酸镍、氯化镍、乙酸镍、碳酸镍等。作为磷化合物，例如可举出次磷酸钠、次磷酸钾等。
上述第1镍-磷合金镀层的成膜速度优选为20～30μm/h(小时)，更优选为22～25μm/h(小时)。第1含镍镀敷被膜层的膜厚优选为5μm以上，更优选为7～25μm，从不易产生针孔的被膜性能和成本的观点出发，进一步优选为9～20μm。
[镀金被膜层]
镀金被膜层通过工序(B)形成在所述含镍镀敷被膜层上。
在将镀金被膜层整体设为100质量％的情况下，镀金被膜中的金含量优选为90质量％以上，更优选为99质量％以上，特别优选为99.9质量％以上。通过使金含量在上述范围内，本申请发明的层叠体的耐腐蚀性稳定。金含量通过杂质定量法求出，即、用王水溶解镀金，采用原子吸光分析和高频诱导耦合等离子体(ICP)发射光谱分析来测定。
从难以产生针孔的被膜性能和成本的观点出发，镀金被膜的厚度优选为0.1μm～2μm，更优选为0.2～1.5μm，特别优选为0.3～0.8μm。现有技术已知如果加厚贵金属镀敷被膜，则针孔减少，可期待高的耐腐蚀性，但由于价格变高，因此优选设为适当的厚度。
＜工序(B)＞
作为所述镀金被膜层的形成方法，没有特别限定，优选无电解镀金法。在无电解镀金法中，优选在进行置换型镀金之后进行还原型镀金。即、所述工序(B)优选包括形成置换型镀金被膜层的工序(b1)和在该工序(b1)之后形成还原型镀金被膜层的工序(b2)。
在置换型镀金中，镍从镍被膜溶解，并且溶液中的金离子被此时释放的电子还原，从而作为镀金被膜析出。在还原型镀金中，溶液中的金离子被还原剂的氧化反应中释放的电子还原，从而析出镀金被膜。
作为无电解镀金液，例如可举出含有氰化金钾、氯化金、亚硫酸金、硫代硫酸金等的镀浴等，作为还原剂，例如可举出氢氧化钠、二甲胺硼烷、六亚甲基四胺、具有碳原子数为3个以上的烷基和多个氨基的链状多胺等。
置换型镀金优选以50～90℃实施3～7分钟，更优选以65～75℃实施3～7分钟，还原型镀金优选以55～65℃实施7～15分钟，更优选以58～62℃实施7～15分钟，由此可以形成镀金被膜层。
[第2含镍镀敷被膜层]
第2含镍镀敷被膜层通过工序(C)在所述镀金被膜层上形成。再者，在对所述镀金被膜层实施镍触击电镀处理的情况下，在镀金被膜层与第2镀镍被膜层之间具有镍触击电镀层。
从提高耐腐蚀性的观点出发，含镍镀敷被膜层优选含有磷，优选包含磷浓度为10质量％以上且12质量％以下的镍-磷合金镀层。
在将含镍镀敷被膜层整体设为100质量％的情况下，第2含镍镀敷被膜层中的镍含量优选为80质量％以上，更优选为85～95质量％，特别优选为90～92质量％。通过使镍含量在上述范围，被膜层中的磷的比率增加，能够发挥优异的耐腐蚀性。另外，如果使改变了磷浓度的无电解镀镍-磷合金镀敷被膜层叠，则针孔缺陷在不同的位置形成并进行成膜，因此外部干扰难以直接到达基材，能够期待耐腐蚀性提高。
＜工序(C)＞
上述第2含镍镀敷被膜层可以使用包含镍盐和作为还原剂的磷化合物的无电解镀浴在金属基材上形成。作为镍盐，例如可举出硫酸镍、氯化镍、乙酸镍、碳酸镍等。作为磷化合物，例如可举出次磷酸钠、次磷酸钾等。
上述第2镍-磷合金镀层的成膜速度优选为10～15μm/h(小时)，更优选为11～13μm/h(小时)。第2镍-磷合金镀敷被膜的膜厚优选分别为5μm以上，更优选为7～25μm，从不易产生针孔的被膜性能和成本的观点出发，进一步优选为10～20μm。
[封孔处理]
封孔处理是通过利用镍单质金属将上述镀金被膜层封孔，并利用金单质金属将上述第1和第2含镍镀敷被膜层的针孔封孔而进行的。
＜工序(X)＞
在工序(X)中，在所述工序(C)和后述的工序(D)之间，通过对工序(C)中得到的层叠体进行加热处理，金属发生热扩散，利用镍单质金属将上述镀金被膜层的针孔封孔，并且利用金单质金属对所述第1和第2含镍镀敷被膜层的针孔进行封孔处理。金和镍单质的存在可以通过能量色散型X射线分析(EDS)来确认。
加热条件优选为250℃以上且2小时以上，更优选为300～350℃且2～6小时。
[氟化镍被膜层]
氟化镍被膜层形成在上述第2含镍镀敷被膜层上。氟化镍被膜层是钝态被膜。通过在工序(D)中对上述第2含镍镀敷被膜层表面进行氟化处理，在所述含镍镀敷被膜层上形成氟化镍被膜层作为钝态被膜。
氟化镍被膜层的厚度优选为70nm以上，更优选为80～200nm，进一步优选为100～150nm。通过氟化镍被膜层的厚度在上述范围，镀金被膜层与第2含镍镀敷被膜层的密合性提高。
＜工序(D)＞
在工序(D)中，经过上述工序(A)～(C)和根据需要的上述工序(X)，通过利用氟气将上述含镍镀敷被膜层表面氟化，形成氟化镍被膜层。
工序(D)在氟气浓度优选为8体积％以上、更优选为10体积％以上的气氛下进行。成膜温度优选为250℃以上，更优选为300℃以上。另外，氟化处理时间优选为2小时以上。作为伴随氟气的气体，可举出氮气等惰性气体。在本发明的一个实施方式中，通过上述反应条件，可以得到厚膜的由氟化镍构成的氟化钝态膜，根据部件的使用目的，通过调节镍合金镀敷皮膜的厚度、反应温度、反应时间，能够任意地调整氟化镍被膜的膜厚。再者，上述反应温度是指用热电偶测定反应炉内的气体气氛的温度。
实施例
以下，基于实施例对本发明进行更具体的说明，但本发明不限定于这些实施例。层叠体的各层(除氟化镍被膜层以外)的膜厚由重量的增加量、层面积和已知的密度算出。氟化镍被膜层的膜厚通过X射线光电子分光法(XPS)用后述方法算出。
[实施例1]
＜工序(A)＞
对于不锈钢(SUS316L)的表面，作为前处理，实施脱脂、酸洗和镍触击电镀处理。在实施了该镍触击电镀处理的不锈钢的表面，使用无电解镀镍-磷镀敷药剂“ニムデン(商标)NSX”(上村工业(株)制)，在镀敷温度90℃、pH值为4.5～4.8的条件下，以镀敷时间为25分钟，形成了成膜时的磷含量为8质量％以上且小于10质量％的第1含镍镀敷被膜层(膜厚：10μm)。
＜工序(B)＞
依次使用两种无电解镀金液“フラッシュゴールドNC(置换型)”和“セルフゴールドOTK-IT(还原型)”(均为奥野制药工业(株)制)，在工序(A)中形成的第1含镍镀敷被膜层上，依次分别进行置换型镀敷温度70℃下5分钟和还原型镀敷温度60℃下10分钟的处理，形成合计0.6μm厚的镀金被膜层。
＜工序(C)＞
在工序(B)中形成的镀金被膜层的表面上，与工序(A)同样地实施了镍触击电镀处理。在实施了该镍触击电镀处理的镀金被膜层的表面，使用无电解镀镍-磷镀敷药剂“ニムデン(商标)HDX”(上村工业(株)制)，以镀敷时间为50分钟，形成了成膜时的磷含量为10质量％以上且12质量％以下的第2含镍镀敷被膜层(膜厚：10μm)。
＜工序(X)＞
将具有在工序(A)、工序(B)和工序(C)中形成的第1含镍镀敷被膜层、镀金被膜层和第2含镍镀敷被膜层的不锈钢安装在常压气相流通式反应炉的内部，使炉内温度升温至300℃，保持该状态2小时。
加热后，通过能量分散型X射线分析(EDS)对该不锈钢进行分析，确认第1和第2含镍镀敷被膜层的针孔被金单质金属封孔，镀金被膜层的针孔被镍单质金属封孔。
＜工序(D)＞
在工序(X)之后，用氮气置换上述常压气相流通式反应炉内部的大气，接着导入100体积％氧气以将氮气完全置换成氧气，保持该状态12小时。接着，将氧气置换成氮气后，导入10体积％的氟气(剩余的90体积％为氮气)，保持该状态12小时，形成氟化镍被膜层。此外，使氮气流通12小时，使成膜稳定化。对于所得到的最表面层为氟化镍被膜的不锈钢，根据采用X射线光电子分光法(XPS)检测出的F和Ni量比确认了氟化镍的存在。根据F和Ni的溅射时间和已知的溅射速率2.4nm/min(SiO2换算)求出氟化镍被膜的厚度为103nm。
[实施例2]
与实施例1同样地实施工序(A)后，除了将实施例1的工序(B)中金的还原镀敷处理变更为20分钟以外，采用与实施例1同样的方法形成了1.2μm厚的镀金被膜层。然后，与实施例1同样地实施工序(C)、工序(X)和工序(D)。与实施例1同样地求出氟化镍被膜的厚度为103nm。
[实施例3]
代替实施例1中的不锈钢(SUS316L)而使用了铝合金(A5052)，作为前处理，实施了脱脂、活性化处理、酸洗和锌置换处理。然后，采用与实施例1同样的方法实施了工序(A)、工序(B)、工序(C)、工序(X)和工序(D)。与实施例1同样地求出氟化镍被膜的厚度为103nm。再者，所述活性化处理使用酸性氟化铵和硝酸的混合酸作为处理剂，在室温下进行30秒。所述酸洗使用硝酸作为清洗剂，在室温下进行25秒。所述锌置换处理使用锌酸盐浴作为处理剂，在室温下进行25秒。另外，所述酸洗和所述锌置换处理在上述条件下分别各进行2次。
[比较例1]
对于不锈钢(SUS316L)的表面，作为前处理实施了脱脂、酸洗和镍触击电镀处理。在实施了该镍触击电镀处理的不锈钢的表面，使用无电解镀镍-磷镀敷药剂“ニムデン(商标)NSX”(上村工业(株)制)，在镀敷温度为90℃、pH值为4.5～4.8的条件下，以成膜速度为10μm/25分钟，形成了成膜时的磷含量为8质量％以上且小于10质量％的第1含镍镀敷被膜层。接着，使用无电解镀镍-磷镀敷药剂“ニムデン(商标)HDX”(上村工业(株)制)，以成膜速度为10μm/50分钟，形成了成膜时的磷含量为10质量％以上且12质量％以下的第2含镍镀敷被膜层。由此，在实施了镍触击电镀处理的不锈钢上形成总计20μm厚的含镍镀敷被膜层。然后，采用与实施例1同样的方法实施工序(D)，在实施了镍触击电镀处理的不锈钢的表面上形成含镍镀敷被膜层和氟化镍被膜层。
[比较例2]
将比较例1中的金属基材从不锈钢(SUS316L)变更为铝合金(A5052)，作为前处理实施了脱脂、活性化处理、酸洗和锌置换处理后，与比较例1同样地形成无电解镀镍-磷合金镀敷被膜层和氟化镍被膜层。
[比较例3]
在实施例1的基础上仅实施工序(A)、工序(B)和工序(C)，也就是不实施工序(X)和工序(D)，从而在不锈钢上形成了第1含镍镀敷被膜层、镀金被膜层和第2含镍镀敷被膜层。
[评价]
对于上述实施例1～3和比较例1～3中得到的金属基材表面上的被膜，进行了盐酸耐腐蚀试验。评价结果示于表1。
<盐酸耐腐蚀试验>
将长15mm×宽15mm×厚1mm的试验片在25℃浸渍于35质量％盐酸溶液中5小时。基于浸渍前后的质量减少量[mg/dm2]，以下述基准评价盐酸耐腐蚀性。
(评价基准)
A：小于0.1mg/dm2
B：0.1mg/dm2以上且小于3mg/dm2
C：3mg/dm2以上且小于10.0mg/dm2
D：10.0mg/dm2以上
表1
| 实施例1 | 实施例2 | 实施例3 | 比较例1 | 比较例2 | 比较例3 | |
| 金属基材 | SUS | SUS | Al | SUS | Al | SUS |
| 第1含镍镀敷被膜层[μm] | 10 | 10 | 10 | 10 | 10 | 10 |
| 第2含镍镀敷被膜层[μm] | 10 | 10 | 10 | 10 | 10 | 10 |
| 镀金被膜层[μm] | 0.6 | 1.2 | 0.6 | - | - | 0.6 |
| 氟化镍被膜层[μm] | 103 | 103 | 103 | 103 | 103 | - |
| 耐盐酸腐蚀性 | B | A | B | C | C | D |
表1中，SUS表示不锈钢(SUS316L)，Al表示铝合金(A5052)。
附图标记说明
1···金属基材
2···第1含镍镀敷被膜层
3···镀金被膜层
4···第2含镍镀敷被膜层
5···氟化镍被膜层
6···针孔
7···针孔被封孔处理的部位
Claims (9)
1.一种层叠体，具有：
金属基材；
在所述金属基材上形成的第1含镍镀敷被膜层；
在所述第1含镍镀敷被膜层上形成的镀金被膜层；
在所述镀金被膜层上形成的第2含镍镀敷被膜层；以及
在所述第2含镍镀敷被膜层上形成的氟化镍被膜层，
所述金属基材包含选自不锈钢、铁、铝、铝合金、铜和铜合金中的至少一种金属，
在将所述镀金被膜层整体设为100质量%的情况下，所述镀金被膜层中的金含量为90质量%以上，
所述第1含镍镀敷被膜层包含磷浓度为8质量%以上且小于10质量%的镍-磷合金镀层，并且，所述第2含镍镀敷被膜层包含磷浓度为10质量%以上且12质量%以下的镍-磷合金镀层。
2.根据权利要求1所述的层叠体，所述镀金被膜层的针孔被镍单质金属封孔，并且，
所述第1含镍镀敷被膜层和第2含镍镀敷被膜层的针孔被金单质金属封孔。
3.根据权利要求1或2所述的层叠体，在所述金属基材与所述第1含镍镀敷被膜层之间、以及所述镀金被膜层与所述第2含镍镀敷被膜层之间，具有镍触击电镀层，所述镍触击电镀层是使用含镍镀浴的镍触击电镀处理形成的，镍触击电镀处理中的电流密度为3~20A/dm2。
4.根据权利要求1或2所述的层叠体，所述镀金被膜层从所述第1含镍镀敷被膜层侧起依次包含置换型镀金被膜层和还原型镀金被膜层，
所述置换型镀金被膜层是通过以下方法形成的层，即，镍从镍被膜溶解，并且溶液中的金离子被此时释放的电子还原，从而作为镀金被膜析出，所述还原型镀金被膜层是通过以下方法形成的层，即，溶液中的金离子被还原剂的氧化反应中释放的电子还原，从而析出镀金被膜。
5.根据权利要求1或2所述的层叠体，所述氟化镍被膜层的厚度为70nm以上。
6.一种层叠体的制造方法，包括：
在金属基材上形成第1含镍镀敷被膜层的工序A，所述工序A包括形成磷浓度为8质量%以上且小于10质量%的镍-磷合金镀层的工序，所述金属基材包含选自不锈钢、铁、铝、铝合金、铜和铜合金中的至少一种金属；
在所述第1含镍镀敷被膜层上形成镀金被膜层的工序B，所述工序B包括形成置换型镀金被膜层的工序b1和在该工序b1之后形成还原型镀金被膜层的工序b2，在工序b1中，镍从镍被膜溶解，并且溶液中的金离子被此时释放的电子还原，从而作为镀金被膜析出，在工序b2中，溶液中的金离子被还原剂的氧化反应中释放的电子还原，从而析出镀金被膜；
在所述镀金被膜层上形成第2含镍镀敷被膜层的工序C，所述工序C包括形成磷浓度为10质量%以上且12质量%以下的镍-磷合金镀层的工序；以及
在所述第2含镍镀敷被膜层上形成氟化镍被膜层的工序D，所述工序D在氟气浓度为8体积%以上且温度为250℃以上的气氛下进行。
7.根据权利要求6所述的层叠体的制造方法，在所述工序C与所述工序D之间，包括通过将工序C中得到的层叠体在温度250℃以上的条件下进行加热处理，从而利用镍单质金属将所述镀金被膜层的针孔封孔，并且，利用金单质金属将所述第1含镍镀敷被膜层和第2含镍镀敷被膜层的针孔封孔的工序X。
8.根据权利要求6或7所述的层叠体的制造方法，在所述工序A之前和所述工序C之前，包括对金属基材以电流密度为3~20A/dm2的条件实施镍触击电镀处理的工序。
9.一种半导体制造装置的构成部件，由权利要求1~5中任一项所述的层叠体制成。
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