WO1999050476A1 - Substrat pourvu d'un placage a base de nickel et son procede de preparation - Google Patents
Substrat pourvu d'un placage a base de nickel et son procede de preparation Download PDFInfo
- Publication number
- WO1999050476A1 WO1999050476A1 PCT/JP1999/001352 JP9901352W WO9950476A1 WO 1999050476 A1 WO1999050476 A1 WO 1999050476A1 JP 9901352 W JP9901352 W JP 9901352W WO 9950476 A1 WO9950476 A1 WO 9950476A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- electroless
- based plating
- substrate
- glass substrate
- film
- Prior art date
Links
- 239000000758 substrate Substances 0.000 title claims abstract description 156
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 136
- 238000007747 plating Methods 0.000 title claims abstract description 129
- 238000000034 method Methods 0.000 title claims description 26
- 229910052759 nickel Inorganic materials 0.000 title abstract description 5
- 239000011521 glass Substances 0.000 claims abstract description 85
- 239000011248 coating agent Substances 0.000 claims description 13
- 238000000576 coating method Methods 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 239000003638 chemical reducing agent Substances 0.000 claims description 9
- 229910052717 sulfur Inorganic materials 0.000 claims description 9
- 239000002241 glass-ceramic Substances 0.000 claims description 8
- 150000007524 organic acids Chemical class 0.000 claims description 8
- 239000000919 ceramic Substances 0.000 claims description 7
- 150000002815 nickel Chemical class 0.000 claims description 7
- 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
- 229910018605 Ni—Zn Inorganic materials 0.000 claims description 5
- 229910052787 antimony Inorganic materials 0.000 claims description 5
- 229910052785 arsenic Inorganic materials 0.000 claims description 5
- 229910052791 calcium Inorganic materials 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 229910052711 selenium Inorganic materials 0.000 claims description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 4
- 229910052738 indium Inorganic materials 0.000 claims description 4
- 229910052763 palladium Inorganic materials 0.000 claims description 4
- IIACRCGMVDHOTQ-UHFFFAOYSA-M sulfamate Chemical compound NS([O-])(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-M 0.000 claims description 4
- 229910052718 tin Inorganic materials 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052745 lead Inorganic materials 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 229940095064 tartrate Drugs 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 235000005985 organic acids Nutrition 0.000 claims description 2
- 239000002023 wood Substances 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims 2
- 229910052793 cadmium Inorganic materials 0.000 claims 1
- 229910052721 tungsten Inorganic materials 0.000 claims 1
- 239000000243 solution Substances 0.000 description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
- 239000011701 zinc Substances 0.000 description 17
- 239000010410 layer Substances 0.000 description 16
- 229910052751 metal Inorganic materials 0.000 description 11
- 239000002184 metal Substances 0.000 description 11
- 230000003746 surface roughness Effects 0.000 description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 7
- 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 6
- 229910018104 Ni-P Inorganic materials 0.000 description 6
- 229910018536 Ni—P Inorganic materials 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 6
- JIAARYAFYJHUJI-UHFFFAOYSA-L Zinc chloride Inorganic materials [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 5
- 238000007772 electroless plating Methods 0.000 description 5
- 239000002736 nonionic surfactant Substances 0.000 description 5
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 description 4
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 4
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- 239000001119 stannous chloride Substances 0.000 description 4
- 235000011150 stannous chloride Nutrition 0.000 description 4
- 239000004246 zinc acetate Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000011241 protective layer Substances 0.000 description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 2
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 2
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 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
- 238000007796 conventional method Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 229940046892 lead acetate Drugs 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 2
- 239000001632 sodium acetate Substances 0.000 description 2
- 235000017281 sodium acetate Nutrition 0.000 description 2
- 239000001509 sodium citrate Substances 0.000 description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 239000011975 tartaric acid Substances 0.000 description 2
- 235000002906 tartaric acid Nutrition 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 239000011592 zinc chloride Substances 0.000 description 2
- 235000005074 zinc chloride Nutrition 0.000 description 2
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 description 2
- 229960001763 zinc sulfate Drugs 0.000 description 2
- VRGNUPCISFMPEM-ZVGUSBNCSA-L zinc;(2r,3r)-2,3-dihydroxybutanedioate Chemical compound [Zn+2].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O VRGNUPCISFMPEM-ZVGUSBNCSA-L 0.000 description 2
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 description 1
- SYQQWGGBOQFINV-FBWHQHKGSA-N 4-[2-[(2s,8s,9s,10r,13r,14s,17r)-10,13-dimethyl-17-[(2r)-6-methylheptan-2-yl]-3-oxo-1,2,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-2-yl]ethoxy]-4-oxobutanoic acid Chemical compound C1CC2=CC(=O)[C@H](CCOC(=O)CCC(O)=O)C[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 SYQQWGGBOQFINV-FBWHQHKGSA-N 0.000 description 1
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 1
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 description 1
- JVTAAEKCZFNVCJ-UHFFFAOYSA-M Lactate Chemical compound CC(O)C([O-])=O JVTAAEKCZFNVCJ-UHFFFAOYSA-M 0.000 description 1
- 229910052764 Mendelevium Inorganic materials 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 241000274582 Pycnanthus angolensis Species 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- YXVFQADLFFNVDS-UHFFFAOYSA-N diammonium citrate Chemical compound [NH4+].[NH4+].[O-]C(=O)CC(O)(C(=O)O)CC([O-])=O YXVFQADLFFNVDS-UHFFFAOYSA-N 0.000 description 1
- YPTUAQWMBNZZRN-UHFFFAOYSA-N dimethylaminoboron Chemical compound [B]N(C)C YPTUAQWMBNZZRN-UHFFFAOYSA-N 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000000174 gluconic acid Substances 0.000 description 1
- 235000012208 gluconic acid Nutrition 0.000 description 1
- 229930195712 glutamate Natural products 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- BORTXUKGEOWSPS-UHFFFAOYSA-N n-dimethylboranylmethanamine Chemical compound CNB(C)C BORTXUKGEOWSPS-UHFFFAOYSA-N 0.000 description 1
- 229940078494 nickel acetate Drugs 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 239000011556 non-electrolytic solution Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000011087 paperboard Substances 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- IIACRCGMVDHOTQ-UHFFFAOYSA-N sulfamic acid Chemical class NS(O)(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-N 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- DDFYFBUWEBINLX-UHFFFAOYSA-M tetramethylammonium bromide Chemical compound [Br-].C[N+](C)(C)C DDFYFBUWEBINLX-UHFFFAOYSA-M 0.000 description 1
- FAKFSJNVVCGEEI-UHFFFAOYSA-J tin(4+);disulfate Chemical compound [Sn+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O FAKFSJNVVCGEEI-UHFFFAOYSA-J 0.000 description 1
- 239000005341 toughened glass Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- 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
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
Definitions
- Ni-based plating substrate Ni-based plating substrate and its manufacturing method
- the present invention provides an electroless Ni-based film having good adhesion as a base polar metal film on a glass substrate made of glass, glass ceramics or ceramics, particularly on a glass substrate for a memory medium such as a hard disk.
- the present invention relates to a technique for forming a tack film.
- a substrate (memory) for a storage element of a magnetic memory device such as a memory disk, a fixed hard disk, an optical disk, a magneto-optical disk, and a magnetic disk (hereinafter, these are collectively referred to as a memory medium).
- A1 disk substrates are widely used as media substrates.
- a memory medium is manufactured by forming a memory layer by a sputtering method or the like on a disk-shaped memory medium substrate. Therefore, it is necessary that the surface of the memory medium substrate is composed of a multi-layered polar metal. Therefore, when a memory medium is manufactured using a glass substrate for a memory medium, a metal film having a polarity (hereinafter, referred to as a base polar metal film) is formed on the glass substrate in advance.
- the base polar metal film is required to have good adhesion to the glass substrate, to have a thermal expansion coefficient close to that of the glass substrate, and to be able to improve the recording density. ing.
- a glass substrate as a substrate for a memory medium is used. It is conceivable to use an electroless plating method to form the underlying polar metal film on the substrate. For example, a glass substrate is immersed in a stannous chloride solution to perform Pd activation treatment, washed with water, and then poured into a known electroless Ni-based plating solution to easily add N 2 to the surface of the substrate.
- i-type coating film Pure Ni film, Ni-P film containing P, Ni-B film containing B
- This Ni-based plating film can be deposited very easily when the substrate surface is roughened.
- the Ni-based plating film obtained by such an electroless plating method has extremely low adhesion strength to a glass substrate, and is difficult to use industrially.
- the present invention has been made to solve the problems of the prior art described above, and an electroless Ni-based plating film is formed on a glass substrate, especially a glass substrate for a memory medium, with good adhesion and low cost.
- the purpose is to be formed by Disclosure of the invention
- the present inventors have found that the above object can be achieved by including Zn in the electroless Ni-based plating film, and have completed the present invention.
- the present invention is characterized in that in an Ni-based plating substrate in which an electroless Ni-based plating film is formed on a glass substrate, the electroless Ni-based plating film contains Zn. Provide a Ni-based plating substrate.
- the present invention provides a method for producing an Ni-based plating substrate in which an electroless Ni-based plating film is formed on a glass substrate, the method comprising a nickel salt, an organic acid and a reducing agent;
- the glass substrate is electroless Ni-plated with an electroless Ni-based plating liquid containing 0.01 mg / L to 20 g of ZL.
- a production method characterized by forming an electroless Ni-based plating film.
- the present invention also provides an electroless Ni-based plating solution for forming an electroless Ni-based plating film on a glass substrate, comprising a nickel salt, an organic acid and a reducing agent, To provide an electroless Ni-based plating solution containing 0.01 mg / L to 20 g ZL.
- the present invention provides a memory medium comprising a glass substrate on which an electroless Ni-based plating film is formed, and a memory layer formed on the electroless Ni-based plating film.
- a memory medium characterized in that the i-type plating film contains Zn.
- Ni-based plating substrate of the present invention will be described in detail.
- the Ni-based plating substrate of the present invention is a glass substrate on which an electroless Ni-based plating film containing Zn is formed with good adhesion.
- a glass substrate for use in the present invention, a glass (crystallized glass (e.g. S i O 2 - L i 0 2 - M g O- P 2 0 5 based glass), tempered glass (e.g. Soviet one da-lime glass substrate made of L i ⁇ 2 based glass or the like) or sera mission-box (A l 2 ⁇ 3, etc.) -) and the like), glass ceramic box (S i ⁇ 2 - A 1 2 0 3 based glass, S i O 2 There is no limitation on the surface roughness, and those having various uses can be used.
- crystalstallized glass e.g. S i O 2 - L i 0 2 - M g O- P 2 0 5 based glass
- tempered glass e.g. Soviet one da-lime glass substrate made of L i ⁇ 2 based glass or the like
- sera mission-box A l 2 ⁇ 3, etc.
- glass ceramic box S i ⁇ 2 - A
- Such a crystallized glass substrate is useful as a glass substrate for memory media such as hard disks.
- Z contained in the electroless Ni-based plating film is n includes those in an ionic state such as Zn or Zn2 + , ZnO, and Zn ( ⁇ H) 2 .
- the plating film becomes brittle, it is preferably 3% by weight or less, more preferably 0.00001 to 3% by weight.
- the electroless Ni-based plating film may be a Ni—Zn coating composed of Ni and Zn or an electroless Ni-based plating film containing other elements. included.
- a Ni—Zn—P film further containing P, a Ni—Zn—B film further containing B, and the like can be preferably mentioned.
- the electroless Ni-based plating film may have, if necessary, Si, Tl, Mo, Ti, Pb, Sn, Fe, S, Bi, Cd, Md.
- One or more elements selected from n, Mg, W, Cu, Pd, In, Sb, Se, As, Ca, and Co may be further contained.
- the concentration when these are contained can be appropriately determined according to the type of element to be contained, the purpose of use of the metal-based plating substrate, and the like.
- the thickness of the electroless 1-based paint film is preferably 0.0001 / x m to 2 O m from the viewpoint of adhesion to the glass substrate.
- the Ni-based plating substrate of the present invention as described above contains a nickel salt, an organic acid, and a reducing agent, and further contains Zn at 0.1 mg / L to 20 g / L.
- the glass substrate can be easily manufactured by subjecting the glass substrate to the electroless Ni plating treatment using the electroless Ni plating solution.
- the nickel salts include acetate, formate, oxalate and the like. Preference is given to acid salts, sulphamate salts, sulphates, chlorides, borofluorides and the like. Further, the concentration in the plating solution is preferably 0.1 to 100 g ZL, particularly preferably 1 to 5 g ZL, as Ni 2 + .
- the organic acid linoleic acid, succinic acid, citric acid, lactic acid, tartaric acid, oxalic acid, formic acid, glycolic acid, gluconic acid, adipic acid, EDTA, NTA, glutamate and the like are preferable.
- the concentration of the organic acid in the plating solution is preferably 1 to 100 g ZL, particularly preferably 5 to 30 g ZL.
- the reducing agent depends on the type of electroless Ni coating film to be formed (for example, Ni—Zn coating, Ni—Zn—P coating, or Ni—Zn—B coating). And select as appropriate. For example, when forming a Ni—Zn film, formalin, formic acid, oxalic acid and the like are preferable, and when a Ni—Zn—P film is formed, hypophosphorous acid, phosphorous acid, or these are preferable. preferably salts of, n i- Z n - when forming the B film, DMA B (dimethyl aminoborane), n a BH 4, KBH 4, TMAB (trimethyl aminoborane) or the like are preferable.
- DMA B dimethyl aminoborane
- n a BH 4, KBH 4, TMAB trimethyl aminoborane
- the concentration of the reducing agent in the electroless Ni-based plating solution is preferably 1 to 100 gZL, particularly 3 to 20 g when hypophosphorous acid or phosphite is used as the reducing agent. ZL is preferred.
- the salt simultaneously serves as a source of Ni and hypophosphorous acid.
- the use amount of Ni hypophosphite is preferably 1 to 50 g / L, more preferably 5 to 30 g / L.
- Zn is a characteristic component of the electroless Ni-based plating solution of the present invention, and inorganic salts such as zinc sulfate, chloride and sulfamate, and organic salts such as tartaric acid, acetic acid and lactate. It is preferably supplied as an acid salt. Of these, zinc sulfate, chloride, sulfamate, acetate and tartrate are preferred.
- the concentration of Zn in the electroless Ni-based plating solution is from 0.01 mg / L 20 g / L, preferably 0.3 mg / L to 3 g / L. If the amount is less than 0.01 mg ZL, the adhesion between the electroless Ni-based plating film and the glass substrate is reduced. If the amount exceeds 20 g ZL, the electroless Ni-based plating film tends to become brittle.
- the electroless Ni-based plating solution contains, in addition to the above-mentioned nickel salts, organic acids, reducing agents and Zn, if necessary, Si, Tl, Mo, Ti, Pb, Sn, One or two selected from Fe, S, Bi, Cd, Mn, Mg, W, Cu, Pd, In, Sb, Se, As, Ca, and Co
- the above elements can be contained.
- the concentration when these are contained can be appropriately determined according to the kind of element to be contained, the purpose of use of the Ni-based plating substrate, and the like. For example, when tin sulfate is contained, it is preferable to contain 0.1 to 0.5 g ZL.
- the pH of the electroless Ni-based plating solution is preferably adjusted to 3 to 12, and particularly preferably 3.5 to 9.0.
- the method of performing electroless plating on a glass substrate using the electroless Ni-based plating solution of the present invention can be performed according to a known electroless Ni plating method.
- a glass substrate is first immersed in a stannous chloride solution, washed with water, then immersed in a palladium chloride solution to perform a Pd activation treatment, washed with water, and electroless Ni-based plating solution.
- the temperature of the plating solution is preferably room temperature to 95 ° C, particularly preferably 40 to 80 ° C.
- the electroless Ni-based plating liquid of the present invention is preferably used when an electroless Ni-based plating film is formed on a glass substrate for a memory medium such as a glass substrate for a hard disk.
- a glass substrate for a memory medium such as a glass substrate for a hard disk.
- General other than glass substrates for memory media It can also be preferably used when forming an electroless Ni-based plating film showing good adhesion to a glass substrate for use.
- a memory medium can be obtained by forming a conventionally known memory layer on the electroless N1-based plating film.
- a known magnetic material ⁇ one F e 2 ⁇ 3, C o - C r alloy
- Ru may be mentioned preferably a magnetic memory layers were RiNarumaku by the sputtering evening method.
- Such memory layer further, can be appropriately form a lubricating layer made of coercive Mamoruso or carbon or the like consisting of S i ⁇ 2, S i C, and the like.
- a Zn-containing electroless Ni-based plating film (for example, 0.3 to 1. ⁇ thick) on a glass substrate is known.
- the memory layer After performing the mechanical texturing (Mechanica 1 texturing), the memory layer may be laminated.
- the Zn-containing electroless Ni-based plating film (for example, 0.5 to 2.0 im thick) was slightly polished for the purpose of removing nodule pits. After performing the mechanical texturing, the memory layer may be laminated.
- the Zn-containing electroless Ni-based plating film was replaced with a Ni strike film for ensuring the adhesion between the glass substrate and the conventional general electroless Ni-based plating film for A1 substrates. It can be used as a wood layer. In this case, it is possible to suppress a change in the manufacturing process of the conventional memory medium.
- a commercially available disk-shaped crystallized glass substrate for hard disks with a diameter of 2.5 inch, a thickness of 0.635 mm and a surface roughness (Ra) of 2-3 A was used. Then, an electroless Ni plating treatment was performed as follows, and a 0.5 (500 OA) thick Ni-Zn-P film was formed on the surface.
- the glass substrate was washed with a cleaning solution containing a nonionic surfactant (2 g / L), and then washed with water. Subsequently, the mixture was immersed in a sensitizer solution composed of stannous chloride (2 g L) and 36% HC1 (20 m1 / L) at 50 ° C for 3 minutes, and washed with water.
- a sensitizer solution composed of stannous chloride (2 g L) and 36% HC1 (20 m1 / L) at 50 ° C for 3 minutes, and washed with water.
- an electroless Ni consisting of nickel sulfate (10 g / L), citric acid (20 g ZL), sodium hypophosphite (10 g ZL), and zinc acetate (0.5 g / L).
- a system-based plating solution pH 5.0 was prepared, heated to 70 ° C, and the activated glass substrate was poured into the solution for 20 minutes.
- An i plating process was performed to form a 0.5 izm thick Ni—Zn—P film to obtain a memory medium substrate.
- the adhesion of the Ni—Zn—P film was evaluated. That is, after the memory medium substrate was heated at 150 ° C. for 120 minutes, a grid test (100 squares of 1 mm square was produced with a cutter knife) using an adhesive tape was performed according to a conventional method. Was. As a result, the non-peeled piece / test piece was 100 Z 100, and no peeling occurred.
- the Ni-Zn-P film (unpolished) formed on the glass substrate is coated on the Ni-Zn-P film of the memory medium substrate according to the conventional method.
- 0- 3 T orr at 0. 2 ITI thickness ⁇ over F e 2 0 3 force, Ranaru
- the magnetic memory layers are laminated to form a memory medium by stacking 1 m thick S 1 ⁇ 2 under a pressure of 1 0- 3 T orr as a protective layer.
- the obtained memory medium did not have poor adhesion between the magnetic memory layer and the glass substrate, and the recording density increased 150 times as compared with the memory medium formed from the conventional A1 disk substrate.
- An electroless Ni plating process was performed on a glass substrate in the same manner as in Example 1 except that Zn 2 + was not added to the electroless Ni plating solution at all.
- OA A thick electroless Ni-based plating film was formed to fabricate a substrate for memory media.
- the obtained memory medium substrate was subjected to a grid test in the same manner as in Example 1. As a result, the non-peeled test piece was 0 Z 100, and no adhesion was obtained.
- a glass substrate was subjected to ultrasonic cleaning at 30 ° C. for 10 minutes using a cleaning solution containing a nonionic surfactant (1 g L).
- a cleaning solution containing a nonionic surfactant (1 g L) After washing with water, the plate was immersed in a sensitizer solution containing stannous borofluoride (3 g L) and borofluoric acid (10 g L) at 50 ° C. for 3 minutes, and washed with water.
- stannous borofluoride 3 g L
- borofluoric acid 10 g L
- it was immersed in an active liquid composed of palladium chloride (0.1g / L) and 36% HC1 (10m1 / L) at 50 ° C for 3 minutes and washed with water.
- Ni-based plating solution consisting of (1 / L) was prepared, heated to 80 ° C, and the above-mentioned glass substrate was placed therein.
- An electroless Ni plating treatment was performed to form a 5 / m-thick Ni—Zn—P film to obtain a memory medium substrate.
- the obtained memory medium substrate was washed with water and dried, and the components of the Ni—Zn—P film were analyzed. As a result, it was found that Ni 93 wt%, P 7 wt%, and ZnO.l wt% there were.
- the Ni-Zn-P film (unpolished) formed on the glass substrate is coated on the Ni_Zn_P film of the memory medium substrate by the sputtering method (10 _ 3 T orr) as a magnetic memory layer of 2 Paiiota thickness 0. in ⁇ - at F e 2 ⁇ 3 was laminated, the spa Tsu evening method of carbon 3 m thickness 0.5 as a protective layer to al By stacking, a memory medium was manufactured. As a result, there was no poor adhesion between the magnetic memory layer and the glass substrate, and the recording density was increased by a factor of 100 compared to a conventional memory medium formed from an A1 disk substrate.
- An electroless Ni plating treatment was performed on a glass substrate in the same manner as in Example 2 except that zinc tartrate was not added to the electroless Ni plating solution at all, and a surface of 511 m thick electroless Ni plating was applied to the surface.
- a plating film was formed to produce a memory medium substrate.
- the obtained memory medium substrate was subjected to a grid test in the same manner as in Example 1. As a result, the non-peeled test piece was 0100, and no adhesion was obtained.
- a glass Ceramic substrates using cleaning fluid consisting of a non-ionic surfactant (2 g ZL) and Arai ⁇ then formulated from S n C 1 2, P d C 1 2 and HC 1 It was immersed in a so-called Kya list solution (Pd2 + (0.1 g / L), Sn2 + (0.2 g / L)) at 40 ° C for 5 minutes and washed with water.
- an electroless material consisting of nickel chloride (S g ZL), diammonium citrate (10 g / L), sodium hypophosphite (3 g ZL), and zinc chloride (0.5 g ZL)
- a Ni-based plating solution pH 5.0
- a non-electrolytic solution was prepared by introducing a glass-ceramic substrate treated with a catalyst.
- a Ni plating process was performed to form a 0.1 lm (l OOOA) thick Ni-Zn-P film, thereby obtaining a memory medium substrate.
- An electroless Ni plating treatment was performed on the glass ceramic substrate in the same manner as in Example 3 except that zinc chloride was not added to the electroless Ni-based plating solution at all. Form a Ni-based plating film and use it as a substrate for memory media. Was prepared.
- a cleaning fluid consisting of a non-ionic surfactant (1 g / L), subjected to ultrasonic cleaning, S n C 1 2 (0. 2 g ZL), 3 6 % HC 1 immersed in (3 ml / L) consisting of Senses evening I the one-part 3 0 ° C for 5 minutes, washed with water, P d C 1 2 (0 . 0 5 g Bruno L), 3 6% HC 1 (10 ml / L) of the active solution was immersed at 30 ° C. for 5 minutes and washed with water.
- a cleaning fluid consisting of a non-ionic surfactant (1 g / L), subjected to ultrasonic cleaning, S n C 1 2 (0. 2 g ZL), 3 6 % HC 1 immersed in (3 ml / L) consisting of Senses evening I the one-part 3 0 ° C for 5 minutes, washed with water, P d C 1 2 (0 . 0 5 g
- Ni-based plating solution (pH 4.0), which was heated to a solution temperature of 70, Electroless Ni plating is performed by putting a ceramics substrate that has been treated with a synthesizer into the Ni-Zn-P coating with a thickness of 0.4 Atm (400 A). Thus, a substrate for a memory medium was obtained.
- Comparative Example 4 Except that no zinc acetate was added to the electroless Ni-based plating solution, the electroless Ni plating process was applied to the ceramic (alumina) substrate for the hard disk in the same manner as in Example 4, and the surface was treated with a 0.1 ⁇ m-thick aluminum plate. A 4 tm thick electroless Ni-based plating film was formed to produce a substrate for memory media.
- the obtained memory medium substrate was subjected to a grid test in the same manner as in Example 1. As a result, the non-peeled test piece was 0 Z100, and no adhesion was obtained.
- the glass substrate was washed with a cleaning solution containing a nonionic surfactant (2 gZL), and then washed with water. Then, add a solution of stannous chloride (2 g / L) and 36% HC1 (SOmlZL)
- an electroless Ni-based system consisting of nickel sulfate (10 gZL), citric acid (20 gZL), sodium hypophosphite (10 g / L), and zinc acetate (0.5 g / L)
- a plating solution pH 5.0
- Ni plating treatment was performed to form a Ni-Zn-P coating having a thickness of 0 as a Ni strike plating coating.
- Ni—P-based plating solution (pH 4.0) was prepared, heated to 70 ° C, and charged with the glass substrate described above. Electrolytic Ni plating was performed to form a Ni—P film having a thickness of ⁇ ⁇ . Thus, a substrate for a memory medium was obtained.
- a memory medium was obtained by forming a magnetic memory layer and a protective layer in the same manner as in Example 1.
- the obtained memory medium has no adhesion failure between the glass substrate and the Ni-P film and between the Ni-P film and the magnetic memory layer, and is a memory medium formed from a conventional A1 disk substrate.
- the recording density was dramatically improved as compared with. Industrial applicability
- an electroless Ni-based paint film can be formed on a glass substrate having an arbitrary surface roughness with good adhesion. Therefore, the electroless Ni-based plating film as the underlying polar metal film can be formed on the glass substrate for the memory medium at low cost by the electroless Ni plating process. Even when the surface of the glass substrate is a mirror surface, it can be formed with good adhesion. For this reason, a so-called glass hard disk obtained by applying the Ni-based plating substrate of the present invention to a glass substrate for a hard disk is superior in impact resistance and thinner than a conventional aluminum hard disk. High rigidity and hardness, excellent smoothness, and high-speed rotation (for example, 700 rpm or more) are possible, so that the flying height of the magnetic head can be reduced. The recording density is improved.
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Abstract
L'invention porte sur un substrat de verre destiné à un support mémoire et pourvu d'un film de revêtement à base de nickel dans lequel est incorporé Zn de façon à renforcer le contact entre ledit film de revêtement et le substrat de verre.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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JP10/107008 | 1998-04-01 | ||
JP10700898 | 1998-04-01 |
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WO1999050476A1 true WO1999050476A1 (fr) | 1999-10-07 |
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PCT/JP1999/001352 WO1999050476A1 (fr) | 1998-04-01 | 1999-03-18 | Substrat pourvu d'un placage a base de nickel et son procede de preparation |
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WO (1) | WO1999050476A1 (fr) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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EP3650579A4 (fr) * | 2017-06-28 | 2021-10-13 | Kojima Chemicals Co. Ltd. | Solution d'amorçage au nickel autocatalytique et procédé de formation d'un film de nickelage |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS56136966A (en) * | 1980-03-31 | 1981-10-26 | Hitachi Ltd | Electroless plating method |
JPH0997417A (ja) * | 1995-09-29 | 1997-04-08 | Kao Corp | 磁気記録媒体 |
JPH1074318A (ja) * | 1996-06-03 | 1998-03-17 | Komag Inc | 磁気ディスク用支持体の製造方法 |
-
1999
- 1999-03-18 WO PCT/JP1999/001352 patent/WO1999050476A1/fr active Application Filing
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS56136966A (en) * | 1980-03-31 | 1981-10-26 | Hitachi Ltd | Electroless plating method |
JPH0997417A (ja) * | 1995-09-29 | 1997-04-08 | Kao Corp | 磁気記録媒体 |
JPH1074318A (ja) * | 1996-06-03 | 1998-03-17 | Komag Inc | 磁気ディスク用支持体の製造方法 |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP3650579A4 (fr) * | 2017-06-28 | 2021-10-13 | Kojima Chemicals Co. Ltd. | Solution d'amorçage au nickel autocatalytique et procédé de formation d'un film de nickelage |
EP4086368A1 (fr) * | 2017-06-28 | 2022-11-09 | Kojima Chemicals Co. Ltd. | Solution d'amorçage au nickel autocatalytique et procédé de formation de film de nickel |
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