CN116745552A - 多层腐蚀体系 - Google Patents
多层腐蚀体系 Download PDFInfo
- Publication number
- CN116745552A CN116745552A CN202180078304.8A CN202180078304A CN116745552A CN 116745552 A CN116745552 A CN 116745552A CN 202180078304 A CN202180078304 A CN 202180078304A CN 116745552 A CN116745552 A CN 116745552A
- Authority
- CN
- China
- Prior art keywords
- nickel
- mil
- electroless nickel
- nickel layer
- layer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 230000007797 corrosion Effects 0.000 title claims description 37
- 238000005260 corrosion Methods 0.000 title claims description 37
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 371
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 184
- 239000000758 substrate Substances 0.000 claims abstract description 88
- 238000000576 coating method Methods 0.000 claims abstract description 56
- 239000011248 coating agent Substances 0.000 claims abstract description 48
- CLDVQCMGOSGNIW-UHFFFAOYSA-N nickel tin Chemical compound [Ni].[Sn] CLDVQCMGOSGNIW-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052782 aluminium Inorganic materials 0.000 claims description 51
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 51
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 35
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 33
- 229910052698 phosphorus Inorganic materials 0.000 claims description 33
- 239000011574 phosphorus Substances 0.000 claims description 33
- 229910000990 Ni alloy Inorganic materials 0.000 claims description 27
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 23
- 238000012360 testing method Methods 0.000 claims description 13
- 238000009713 electroplating Methods 0.000 claims description 11
- 150000003839 salts Chemical class 0.000 claims description 10
- 239000007921 spray Substances 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 6
- 238000003618 dip coating Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000007747 plating Methods 0.000 description 30
- 229910052718 tin Inorganic materials 0.000 description 22
- 239000000243 solution Substances 0.000 description 20
- 239000008139 complexing agent Substances 0.000 description 14
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 12
- 238000011010 flushing procedure Methods 0.000 description 12
- 239000003638 chemical reducing agent Substances 0.000 description 11
- 229910052751 metal Inorganic materials 0.000 description 11
- 239000002184 metal Substances 0.000 description 11
- 230000008569 process Effects 0.000 description 11
- 238000000151 deposition Methods 0.000 description 9
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 8
- 239000002738 chelating agent Substances 0.000 description 7
- 230000008021 deposition Effects 0.000 description 7
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 6
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 6
- 238000011282 treatment Methods 0.000 description 6
- 238000006392 deoxygenation reaction Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 150000002815 nickel Chemical class 0.000 description 5
- 238000005457 optimization Methods 0.000 description 5
- 239000006174 pH buffer Substances 0.000 description 5
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 4
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 4
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 4
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 238000013019 agitation Methods 0.000 description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 4
- 229910001453 nickel ion Inorganic materials 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 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 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 3
- 239000004327 boric acid Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- BJEPYKJPYRNKOW-UHFFFAOYSA-N malic acid Chemical compound OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 3
- KERTUBUCQCSNJU-UHFFFAOYSA-L nickel(2+);disulfamate Chemical compound [Ni+2].NS([O-])(=O)=O.NS([O-])(=O)=O KERTUBUCQCSNJU-UHFFFAOYSA-L 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 2
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 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
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical class NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 2
- 239000004471 Glycine Substances 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 235000004279 alanine Nutrition 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000000872 buffer Substances 0.000 description 2
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000004310 lactic acid Substances 0.000 description 2
- 235000014655 lactic acid Nutrition 0.000 description 2
- 239000001630 malic acid Substances 0.000 description 2
- 235000011090 malic acid Nutrition 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 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
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 2
- -1 organic acid salts Chemical class 0.000 description 2
- 230000000737 periodic effect Effects 0.000 description 2
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 235000019260 propionic acid Nutrition 0.000 description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000001384 succinic acid Substances 0.000 description 2
- IIACRCGMVDHOTQ-UHFFFAOYSA-M sulfamate Chemical compound NS([O-])(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-M 0.000 description 2
- XXSPKSHUSWQAIZ-UHFFFAOYSA-L 36026-88-7 Chemical compound [Ni+2].[O-]P=O.[O-]P=O XXSPKSHUSWQAIZ-UHFFFAOYSA-L 0.000 description 1
- 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 1
- 229910001094 6061 aluminium alloy Inorganic materials 0.000 description 1
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229910000521 B alloy Inorganic materials 0.000 description 1
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical class NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- RGHNJXZEOKUKBD-SQOUGZDYSA-M D-gluconate Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O RGHNJXZEOKUKBD-SQOUGZDYSA-M 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
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- 229940120146 EDTMP Drugs 0.000 description 1
- DBVJJBKOTRCVKF-UHFFFAOYSA-N Etidronic acid Chemical compound OP(=O)(O)C(O)(C)P(O)(O)=O DBVJJBKOTRCVKF-UHFFFAOYSA-N 0.000 description 1
- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 description 1
- KDXKERNSBIXSRK-YFKPBYRVSA-N L-lysine Chemical compound NCCCC[C@H](N)C(O)=O KDXKERNSBIXSRK-YFKPBYRVSA-N 0.000 description 1
- 239000004472 Lysine Substances 0.000 description 1
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 description 1
- 229910006414 SnNi Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 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 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-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
- 230000000996 additive effect Effects 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- GJYJYFHBOBUTBY-UHFFFAOYSA-N alpha-camphorene Chemical compound CC(C)=CCCC(=C)C1CCC(CCC=C(C)C)=CC1 GJYJYFHBOBUTBY-UHFFFAOYSA-N 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 235000003704 aspartic acid Nutrition 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- OQFSQFPPLPISGP-UHFFFAOYSA-N beta-carboxyaspartic acid Natural products OC(=O)C(N)C(C(O)=O)C(O)=O OQFSQFPPLPISGP-UHFFFAOYSA-N 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- QDWJUBJKEHXSMT-UHFFFAOYSA-N boranylidynenickel Chemical compound [Ni]#B QDWJUBJKEHXSMT-UHFFFAOYSA-N 0.000 description 1
- RJTANRZEWTUVMA-UHFFFAOYSA-N boron;n-methylmethanamine Chemical compound [B].CNC RJTANRZEWTUVMA-UHFFFAOYSA-N 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000021615 conjugation Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000002788 crimping Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 150000001991 dicarboxylic acids Chemical class 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- NFDRPXJGHKJRLJ-UHFFFAOYSA-N edtmp Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CCN(CP(O)(O)=O)CP(O)(O)=O NFDRPXJGHKJRLJ-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- XZUAPPXGIFNDRA-UHFFFAOYSA-N ethane-1,2-diamine;hydrate Chemical class O.NCCN XZUAPPXGIFNDRA-UHFFFAOYSA-N 0.000 description 1
- 229940071106 ethylenediaminetetraacetate Drugs 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 description 1
- 229940050410 gluconate Drugs 0.000 description 1
- 239000000174 gluconic acid Substances 0.000 description 1
- 235000012208 gluconic acid Nutrition 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229940049920 malate Drugs 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002763 monocarboxylic acids Chemical class 0.000 description 1
- 229940078494 nickel acetate Drugs 0.000 description 1
- UQPSGBZICXWIAG-UHFFFAOYSA-L nickel(2+);dibromide;trihydrate Chemical compound O.O.O.Br[Ni]Br UQPSGBZICXWIAG-UHFFFAOYSA-L 0.000 description 1
- BFSQJYRFLQUZKX-UHFFFAOYSA-L nickel(ii) iodide Chemical compound I[Ni]I BFSQJYRFLQUZKX-UHFFFAOYSA-L 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- AQSJGOWTSHOLKH-UHFFFAOYSA-N phosphite(3-) Chemical class [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 description 1
- 150000003009 phosphonic acids Chemical class 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229910001380 potassium hypophosphite Inorganic materials 0.000 description 1
- CRGPNLUFHHUKCM-UHFFFAOYSA-M potassium phosphinate Chemical compound [K+].[O-]P=O CRGPNLUFHHUKCM-UHFFFAOYSA-M 0.000 description 1
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 description 1
- 229940074439 potassium sodium tartrate Drugs 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011165 process development Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- YGSDEFSMJLZEOE-UHFFFAOYSA-M salicylate Chemical compound OC1=CC=CC=C1C([O-])=O YGSDEFSMJLZEOE-UHFFFAOYSA-M 0.000 description 1
- 229960001860 salicylate Drugs 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 235000011006 sodium potassium tartrate Nutrition 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 229960001763 zinc sulfate Drugs 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
- 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
-
- 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
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Abstract
本发明公开了一种制品,该制品包括在其表面的至少一部分上具有多层涂层的衬底。该多层涂层包括覆盖表面部分的至少一个化学镀镍层、覆盖化学镀镍层的至少一个电解镍层和覆盖电解镍层的至少一个电解锡‑镍层。
Description
相关申请
本申请要求2020年12月17日提交的美国临时申请63/126,892的优先权,该文献的主题全文以引用方式并入本文
背景技术
化学镀金属涂层用于多种应用中,在该应用中需要保护涂层以改善化学镀金属涂层下面的衬底的性能特征。此类涂层的实用性主要在于该化学镀金属涂层相对于其所设置于上的衬底的增强的物理特性(例如,硬度)。化学镀金属涂层可用于保护制品,否则该制品容易受到使用该制品的环境中存在的化学品的腐蚀。另外,因为化学镀金属涂层从溶液施加到衬底,所以衬底可具有各种形状、尺寸和穿孔,并且仍然实现均匀组成和厚度的涂层。关于化学镀金属涂层的制备和特性的大量信息目前可用,具体地讲在包含镍-磷或镍-硼合金的涂层领域中。
发明内容
本文所述的实施方案涉及包含多层腐蚀体系的制品,并且具体地讲,涉及包含化学镀镍、电解镍和电解锡-镍合金的多层涂层,以及其在改善衬底(诸如锌酸盐涂覆的铝衬底)的耐腐蚀性的方法中的用途。
在一些实施方案中,制品可包括在其表面的至少一部分上具有多层涂层的锌酸盐涂覆的铝衬底。该多层涂层可包括设置或沉积在该锌酸盐涂覆的铝衬底的至少一部分上的至少一个化学镀镍层、覆盖该化学镀镍层的至少一个电解镍层和覆盖该电解镍层的至少一个电解锡-镍层。
在一些实施方案中,多层涂层可具有约0.5密耳至约2.0密耳的厚度并且能够经受至少336小时的中性盐雾腐蚀测试(NSST)而不腐蚀下面的衬底。
在一些实施方案中,化学镀镍层可具有约5重量%至约14重量%的磷含量。在其他实施方案中,化学镀镍层可具有约5重量%至约9重量%的中等磷含量。在其他实施方案中,化学镀镍涂层可具有约10重量%至约14重量%的高磷含量。在其他实施方案中,多层涂层可包括具有第一磷含量(诸如中等磷含量)的第一化学镀镍层,以及具有与第一磷含量不同的第二磷含量(诸如高磷含量)的覆盖的第二化学镀镍层。
在一些实施方案中,化学镀镍层可覆盖锌酸盐涂覆的铝衬底的表面并且是微孔的。化学镀镍层的厚度可为约0.5密耳至约2密耳,例如约1.0密耳。
在其他实施方案中,覆盖化学镀镍层的电解镍层可以是无孔的或基本上无孔的。电解镍层的厚度可以为约0.05密耳至约0.6密耳,例如约0.2密耳。在一些实施方案中,电解镍层的厚度可基本上小于化学镀镍层的厚度,例如,小至少约10%、小至少约20%、小至少约30%、小至少约40%、小至少约50%、小至少约60%、小至少约70%、小至少约80%或小至少约90%。
在一些实施方案中,覆盖电解镍层的电解锡-镍合金层可包含约50重量%至约80重量%的锡,其中余量基本上为镍。例如,电解锡-镍合金可包含约55重量%至约80重量%的锡、约60重量%至约80重量%的锡、约65重量%至约80重量%的锡、约70重量%至约80重量%的锡、或约50重量%至约80重量%的锡,其中余量基本上为镍。在其他实施方案中,电解锡-镍合金可包含约65重量%的锡,其中余量基本上为镍。电解锡-镍合金层的厚度可以为约0.1密耳至约0.6密耳,例如约0.2密耳。
在其他实施方案中,铝衬底可以用锌酸盐浸渍涂层进行锌酸化。
本文所述的其他实施方案涉及在铝衬底上形成多层涂层的方法。该方法可包括在铝衬底的锌酸盐涂覆表面的至少一部分上涂覆和/或沉积至少一个化学镀镍层。然后在化学镀镍的层或顶层上电镀一层镍。随后将锡-镍合金层电镀在电镀的镍层上。
在一些实施方案中,化学镀镍层可具有约5重量%至约9重量%的磷含量。在其他实施方案中,化学镀镍涂层的层可具有约10重量%至约14重量%的磷含量。在其他实施方案中,多层涂层可包括具有第一磷含量的第一化学镀镍层和具有不同于第一磷含量的第二磷含量的覆盖的第二化学镀镍层。
在一些实施方案中,化学镀镍层可覆盖锌酸盐涂覆的铝衬底的表面并且是微孔的。化学镀镍层的厚度可以为约0.5密耳至约2密耳,例如约1.0密耳。
在其他实施方案中,电镀在化学镀镍层上的镍层可以是无孔的或基本上无孔的。电镀镍层的厚度可以是约0.05密耳至约0.6密耳,例如约0.2密耳。在一些实施方案中,电镀镍层的厚度可基本上小于化学镀镍层的厚度。
在一些实施方案中,电镀在电镀镍层上的锡-镍合金层可包含约50重量%至约80重量%的锡,其中余量基本上为镍。例如,电解锡-镍合金可包含约55重量%至约80重量%的锡、约60重量%至约80重量%的锡、约65重量%至约80重量%的锡、约70重量%至约80重量%的锡、或约50重量%至约80重量%的锡,其中余量基本上为镍。在其他实施方案中,电解锡-镍合金可包含约65重量%的锡,其中余量基本上为镍。电解锡-镍合金层的厚度可以是约0.1密耳至约0.6密耳,例如约0.2密耳。
在其他实施方案中,该方法可包括在施加多层涂层之前对铝衬底的表面进行锌酸化。
附图说明
图1是示出根据一个实施方案在锌酸盐涂覆的衬底上形成多层涂层的方法的流程图。
图2(A-B)示出了在涂覆之前的连接器的图像。
图3(A-B)示出了在用多层腐蚀体系涂覆之后的连接器的图像。
图4(A-B)示出了通过优化循环处理的样品连接器上的沉积层的横截面SEM图像。
图5(A-B)示出了在>500小时的NSS室暴露之后六个经处理连接器的光学图像。
图6(A-B)示出了压碎/卷曲的连接器的相对侧的图像。
具体实施方式
在随后的说明书和权利要求书中,将参考多个术语,这些术语将被定义为具有以下含义。
除非上下文另有明确说明,否则单数形式“一个”、“一种”和“该”包括复数指示物。
如本文所用,如本说明书和权利要求书中所用的动词“包含”及其变化形式以其非限制性意义使用,意指包括该词语之后的项目,但不排除未具体提及的项目。本发明可适当地“包含”权利要求中所述的步骤、元素和/或试剂、“由其组成”或“基本上由其组成”。
还应注意,权利要求可被撰写为排除任何任选的元素。因此,该陈述旨在用作使用与表述权利要求元素相关的排他性术语诸如“仅”、“只有”等或使用“否定”限制的前提基础。
“任选的”或“任选地”意指随后描述的事件或情况可能发生或可能不发生,并且该描述包括事件发生的情况和事件不发生的情况。
还应理解的是,术语诸如“顶部”、“底部”、“向外”、“向内”等是为了方便起见的词语,并且不应被解释为限制性术语。此外,每当本发明的特定特征被认为包括一组多个元素中的至少一个以及它们的组合或由其组成时,应当理解该特征可包括该组元素中的任一个或由其组成,所述元素单独被包括或与该组的其他元素中的任一个组合被包括。
如本文在整个说明书和权利要求中所使用的,近似语言可适于修饰任何定量表示,所述定量表示可允许变化而不导致其所涉及的基本功能的改变。因此,由一个或多个术语诸如“约”修饰的值不限于所指定的精确值。术语“约”或“大约”可指相对于参考量、水平、值、数目、频率、百分比、尺寸、大小、量、重量或长度变化多达15%、10%、9%、8%、7%、6%、5%、4%、3%、2%或1%的量、水平、值、数目、频率、百分比、尺寸、大小、量、重量或长度。在一个实施方案中,术语“约”或“大约”指量、水平、值、数目、频率、百分比、尺寸、大小、量、重量或长度的范围关于参考量、水平、值、数目、频率、百分比、尺寸、大小、量、重量或长度相差±15%、±10%、±9%、±8%、±7%、±6%、±5%、±4%、±3%、±2%或±1%。
本文所述的实施方案涉及包含多层腐蚀体系的制品,并且具体地讲,涉及包含化学镀镍、电解镍和电解锡-镍合金的多层涂层,以及其在改善衬底(诸如锌酸盐涂覆的铝衬底)的耐腐蚀性的方法中的用途。该制品可包括在其表面的至少一部分上具有多层涂层的锌酸盐涂覆的铝衬底。该多层涂层可包括至少一个化学镀镍层、覆盖该化学镀镍层的至少一个电解镍层和覆盖该电解镍层的至少一个电解锡-镍层。
可将化学镀镍涂层施加于衬底(诸如锌酸盐涂覆的铝衬底)以改善耐腐蚀性和/或增强衬底的物理特性。典型地,这种化学镀镍涂层是衬底上的最终涂层或饰面,或者使化学镀镍涂覆的衬底经受锡-镍合金的二次沉积以进一步改善涂层和下面衬底的耐腐蚀性。
化学镀镍涂层的耐腐蚀性可使用中性盐雾腐蚀测试(NSST)来测量,其中期望和/或最小耐腐蚀性由化学镀镍涂覆的铝衬底经受336小时的NSST而无任何铝腐蚀的能力来确定。对于其中覆盖涂层的期望厚度为约0.5密耳至约2密耳的铝连接器应用而言,几乎从不利用期望厚度为0.5密耳至约2密耳的化学镀镍沉积物来实现承受336小时的NSST而没有任何铝腐蚀的能力。比约2密耳厚的沉积物趋于产生连接器的公差问题。发现在化学镀镍沉积物上设置附加锡-镍合金沉积物(例如,65% Sn/35% Ni)增强化学镀镍涂覆的铝的耐腐蚀性,使得336小时的NSST规格能够被满足,但发现此类耐腐蚀性正好处于可行性的边缘。
意料不到的是,发现可在化学镀镍沉积物和锡-镍合金沉积物的层之间设置电解镍层,以显著改善涂层的耐腐蚀性,而不使多层涂层的总厚度增加超过铝连接器所期望的约2密耳的厚度。不仅实现了目标336小时的NSST,而且在大于500小时后中断测试,而没有任何沉积或衬底腐蚀或甚至污染的迹象。虽然不希望受理论的束缚,但假定中间电解镍沉积物可最小化或消除化学镀镍层中的孔隙率或微孔性,该孔隙率或微孔性可能允许从表面到铝衬底的直接腐蚀路径。
图1是示出根据本文所述的实施方案,在铝衬底(诸如铝连接器)上形成多层涂层的方法的流程图。该方法可包括通过标准铝预镀清洁和锌酸化处理(诸如双锌酸化处理)来处理铝部件或衬底(诸如铝连接器)。在典型的对铝双锌酸化处理中,首先清洁铝衬底以去除污垢、油脂和油,然后蚀刻以提供适用于粘附铝酸盐涂层的衬底。然后用硝酸对蚀刻的衬底进行去污以去除表面氧化铝,然后通过浸入锌酸盐溶液中对铝衬底进行锌酸化。
锌酸盐溶液通常包含约120g/l至约500g/l的氢氧化钠、约20g/l至约100g/l的氧化锌、约10g/l至约60g/l的盐,诸如酒石酸钾钠或其他络合有机酸盐,诸如葡糖酸盐和水杨酸盐以及添加剂。
通过将铝衬底浸入锌酸盐溶液中形成的锌酸盐层可以是短效涂层,其可以在后续金属镀覆操作中消失。在一些实施方案中,可以使用硝酸将第一锌酸盐层退镀,并且可以通过浸入锌酸盐溶液中将第二锌酸盐层施加到铝衬底上,该第二锌酸盐层可比第一锌层更均匀。
在一些实施方案中,在对铝衬底的表面进行锌酸化之后,可使锌酸盐涂覆的铝衬底的表面与碱性化学触击镀镍液接触以引发用化学镀镍溶液的镍沉积,从而提供具有约0.5密耳至约2密耳(例如,约1.0密耳)的基本上均匀厚度的磷化学镀镍沉积物或层。
在一些实施方案中,化学镀镍层可具有约5重量%至约14重量%的磷含量。在其他实施方案中,化学镀镍层可具有约5重量%至约9重量%的中等磷含量。在其他实施方案中,化学镀镍涂层可具有约10重量%至约14重量%的高磷含量。为清楚起见,高磷化学镀镍包含约10重量%至约14重量%的磷,其中余量为镍,并且中等磷化学镀镍沉积物包含约5重量%至约9重量%的磷,其中余量为镍。
在其他实施方案中,沉积在锌酸盐涂覆的铝衬底上的化学镀镍可包括具有第一磷含量(诸如中等磷含量的第一化学镀镍层),以及具有与第一磷含量不同的第二磷含量(诸如高磷含量)的覆盖的第二化学镀镍层。磷化学镀镍层可具有约0.5密耳至约2密耳(例如,约1.0密耳)的基本上均匀的总厚度或合并厚度
在其他实施方案中,在对铝衬底进行锌酸化之后,可以省略碱性化学触击镀镍,并且可使锌酸盐涂覆的铝衬底与化学镀镍溶液(诸如高磷化学镀镍溶液和/或中等磷化学镀镍溶液)接触,以提供具有约0.5密耳至约2密耳(例如,约1.0密耳)的基本上均匀厚度的高和/或中磷化学镀镍的沉积物或层。
可使用次磷酸盐还原镍浴或溶液在铝衬底的锌酸盐涂覆表面上提供化学镀镍层。应当理解的是,也可以使用利用其他还原剂(例如,硼氢化物、二甲胺硼烷、肼、甲醛)的其他化学镀镍浴。在一些实施方案中,用于在锌酸盐涂覆的铝衬底上形成化学镀镍的层或沉积物的高磷化学镀镍浴和/或中等磷化学镀镍浴可包含Ni、次磷酸还原剂以及任选的络合剂、螯合剂、稳定剂和/或pH缓冲剂中的至少一种。
镍可以以水溶性镍盐的形式在浴中提供。水溶性镍盐可包括可溶于浴中并且可产生预定浓度的水溶液的那些。镍盐可包括例如硫酸镍、氯化镍、溴化镍、碘化镍、乙酸镍、苹果酸镍、次磷酸镍以及它们的组合。水溶性镍盐可单独使用或作为混合物使用。
在一些实施方案中,化学镀镍浴中镍的浓度可为约1g/L至70g/L。在其他实施方案中,化学镀镍浴中的镍浓度可为约4g/L至约6g/L。
在浴中使用的次磷酸还原剂可包括在已知类型的化学镀镍浴中使用的多种次磷酸还原剂中的任一种。在一些实施方案中,次磷酸还原剂可包括例如次磷酸钠、次磷酸钾、次磷酸铵以及它们的组合。
化学镀镍浴中的次磷酸还原剂的浓度可根据相应类型的次磷酸还原剂而不同,并且可调节以改变使用该浴形成的化学镀镍的层或沉积物中的磷浓度。在一些实施方案中,次磷酸还原剂在化学镀镍-磷电镀浴中的浓度可以为约25g/L至约40g/L,例如约30g/L至约35g/L。
在一些实施方案中,化学镀镍-磷电镀浴中可包含络合剂或络合剂的混合物。如本文所用的,络合剂还可包括螯合剂。络合剂和/或螯合剂通常通过与镍离子形成更稳定的镍络合物来阻止镍离子作为不溶性盐(诸如亚磷酸盐)从电镀浴中沉淀,并且提供适度的镍沉淀反应速率。
络合剂和/或螯合剂可以足以络合溶液中存在的镍离子并且进一步增溶在沉积过程中形成的次磷酸盐降解产物的量被包含在浴中。
可使用在已知的化学镀镍浴中使用的多种络合剂。络合剂的具体示例可包括单羧酸,诸如乙醇酸、乳酸、葡糖酸或丙酸;二羧酸,诸如苹果酸、丙二酸、琥珀酸、酒石酸、草酸或己二酸;氨基羧酸,诸如甘氨酸或丙氨酸;乙二胺衍生物,诸如乙二胺四乙酸盐、依地烯醇(N-羟乙基乙二胺-N,N',N'-三乙酸)或乙二胺(N,N,N',N'-四羟乙基乙二胺);膦酸,诸如1-羟基乙烷-1,1-二膦酸、乙二胺四亚甲基膦酸及其水溶性盐。该络合剂可单独使用或组合使用。
例如一些络合剂(诸如乙酸或琥珀酸)也可充当pH缓冲剂,并且此类添加剂组分的适当浓度可在考虑其双官能度之后针对任何镀浴进行优化。
在一些实施方案中,至少一种pH缓冲剂、络合剂或螯合剂可选自乙酸、甲酸、琥珀酸、丙二酸、铵盐、乳酸、苹果酸、柠檬酸、甘氨酸、丙氨酸、乙醇酸、赖氨酸、天冬氨酸、乙二胺四乙酸(EDTA)以及它们的组合。在一些实施方案中,上述pH缓冲剂、络合剂和/或螯合剂中的两种或更多种的混合物可用于本文所述的化学镀镍浴中,其中每种pH缓冲剂、络合剂和/或螯合剂以约1g/l至约75g/l的浓度提供。
除了上述组分之外,化学镀镍浴还可包含具有各种目的添加剂,只要不劣化电镀浴的特性即可。
在锌酸盐涂覆的铝衬底的化学镀镍期间,化学镀镍浴可在约4.5至约5.0的pH下操作或维持在该pH下。在该pH范围的情况下,允许通过次磷酸还原剂进行的还原反应有效地发生,以防止次磷酸还原剂分解、以及防止电镀的沉淀性能劣化和防止电镀浴分解。另外,在该pH范围的情况下,可防止由于还原剂的还原电位过高而导致的电镀浴稳定性降低。
可使用至少一种pH调节剂将pH调节至上述范围。当浴的pH太高时,可通过添加例如酸来进行调节。当浴的pH太低时,可通过添加例如氢氧化铵来调节。
电镀浴的操作pH的稳定性可通过添加各种缓冲化合物诸如乙酸、丙酸、硼酸等来控制,其量高达约30g/l,其中约2g/l至约30g/l的量是典型的。如上所述,一些缓冲化合物诸如乙酸和琥珀酸也可以起到络合剂的作用。
应当理解,具有多层腐蚀体系和/或具有化学镀镍沉积物或层的电镀衬底不限于锌酸盐涂覆的铝衬底,并且包括可用化学镀镍浴电镀以在衬底上提供化学镀镍沉积物或涂层的任何衬底。衬底可以为能够支撑化学镀镍涂层的任何衬底,但通常是化学镀镍涂层对其表现出足够亲和力以在其上形成稳定涂层的材料。衬底可以为无机材料诸如金属,或有机材料诸如塑料,或复合材料例如包含无机填料的有机聚合物。在一个实施方案中,衬底是金属衬底。金属衬底的非限制性示例包含铁、铬、镍、钴、铜、铝、钛等。在另一个实施方案中,衬底包含钢。在一个实施方案中,衬底包含低合金钢,例如低合金碳钢。在另一个实施方案中,衬底是锌酸盐涂覆的铝衬底。
可通过使衬底与电镀浴接触或将衬底浸入电镀浴中并持续在衬底的期望表面上有效形成化学镀镍涂层或沉积物的持续时间来电镀衬底。在一些实施方案中,可在电镀之前清洁或预处理衬底。在电镀期间,该浴可保持在约175℉至约200℉的浴温下。化学镀镍浴与被电镀的衬底接触的持续时间将决定化学镀镍涂层的厚度。典型地,接触时间可在少至约一分钟至几小时或甚至几天的范围内。
在化学镀镍沉积物或涂层的沉积过程中,可采用温和搅拌。温和搅拌可以为,例如,温和空气搅拌、机械搅拌、通过泵送的浴循环、用于滚镀的滚筒的旋转等。也可对化学镀镍浴进行定期或连续的过滤处理以降低其中的污染物含量。在一些实施方案中,还可在周期性或连续的基础上进行浴成分的补充,以将成分的浓度(并且具体地讲镍离子和次磷酸根离子的浓度)以及pH水平维持在期望的限度内。
在衬底(诸如锌酸盐涂覆的铝衬底)上沉积化学镀镍层之后,可任选地冲洗化学镀镍涂覆的铝衬底,然后用镍电镀以提供电解镍层。电解镍的层或沉积物可被称为“微结构镍”。“微结构镍”或微结构镍沉积物可以为无孔或基本上无孔的镍沉积物或层,其由在镍电镀溶液(诸如基于氨基磺酸盐的镍电解质或镍电镀溶液)中电镀化学镀镍涂覆的衬底而产生。
另选地,电解镍或微结构镍层可由硫酸盐/氯化物电解质的组合(通常称为“瓦特浴”)产生,或由产生基本上无孔沉积物的其他产生镍沉积物的电解质产生。典型地,此类浴含有溶解在水中的硫酸镍、氯化镍和硼酸。也可使用所有的氯化物和氟硼酸盐电镀液。这些浴可任选地包含多种众所周知的和常规使用的化合物,诸如流平剂、增白剂等。电解镍沉积物或层可以是无孔的或基本上无孔的,并且具有基本上均匀的厚度,该厚度可以基本上小于约0.05密耳至约0.6密耳(例如,约0.2密耳至约0.3密耳)的厚度。
然后可冲洗化学镀镍和电解镀镍的硫酸锌涂覆的铝衬底,并且可使用常规的锡-镍合金电镀工艺在电解镍层上设置电解锡-镍合金沉积物或层。这些工艺和电镀浴是众所周知的,并且公开于例如美国专利4,033,835、4,049,508、3,887,444、3,772,168和3,940,319中,所有这些专利均以引用方式并入本文。电解锡-镍合金的层或沉积物可包含约50重量%至约80重量%的锡和约20重量%至约50重量%的镍。例如,电解锡-镍合金可包含约55重量%至约80重量%的锡、约60重量%至约80重量%的锡、约65重量%至约80重量%的锡、约70重量%至约80重量%的锡、或约50重量%至约80重量%的锡,其中余量基本上为镍。在其他实施方案中,电解锡-镍合金可包含约65重量%的锡,其中余量基本上为代表原子组成SnNi的镍。电解锡-镍合金层或锡-镍电镀层可具有在中间微结构或电解镍层的顶部上或覆盖该层的约0.1密耳至约0.6密耳(例如,约0.2密耳目标)的基本上均匀的厚度。
有利地,与仅是化学镀镍部件或衬底以及仅具有锡-镍合金电镀顶层而没有中间电解镍层的化学镀镍部件或衬底相比,经处理的部件或衬底(诸如铝部件或衬底)将具有显著改善的耐腐蚀性。在一些实施方案中,该方法和多层涂层可提高铝衬底的耐腐蚀性,使得涂覆有多层涂层的铝衬底可经受至少336小时的NSST、至少360小时的NSST、至少384小时的NSST、至少408小时的NSST、至少432小时的NSST、至少456小时的NSST、至少480小时的NSST、至少500小时的NSST或更长时间。
意料不到的是,在已经含有显著量镍本身的两种合金之间包括薄的微结构镍层,与没有该层的两个层(化学镀镍和电解锡-镍)相比,可具有此类显著的或实质性的(至少约50%、至少约60%、至少约70%、至少约80%或更多)的改善。
以下实施例示出了本发明的处理方法。除非在以下实施例中另有说明,否则在书面说明书和权利要求书中,所有份数和百分比均以重量计,温度以华氏度计,压力为大气压或接近大气压。
实施例
提供约100个小的6061铝连接器的样品组以用于工艺开发(图2A-2B)。目标是开发循环和沉积模型,其中连接器将用化学镀镍沉积物、电解镍沉积物处理,并且最终层是电解锡-镍沉积物。这些连接器将需要展示出它们可承受至少336小时的NSS室暴露而不在试样上观察到铝腐蚀。
为了验证和表征连接器上的最终处理模型的性能,对代表性部件进行横截面研究以突出相对沉积厚度(并且确保满足近似目标厚度)。还对6个电镀连接器的样品组进行NSS腐蚀测试,并且将第8个连接器“卷曲”或压碎,以验证沉积层的足够粘附性。
产生最有希望的结果的处理模型包括优化的预处理循环(本文中概述)、施加碱性镍触击、化学镀镍沉积(约1.0密耳)、氨基磺酸盐电解镍触击(约0.2密耳)、用电解Sn/Ni沉积物涂饰。
处理方法
1.将20加仑化学镀镍浴共混以用于处理(在电镀前老化至约0.5金属周转数(MTO))。
2.在下文列出的处理循环之后,然后在化学镀镍浴中处理部件。
3.该浴经由Ni滴定分析,并将Ni和次磷酸钠的活性保持在约90%至100%。pH维持在约4.8(+/-0.1)。
4.氨基磺酸镍由约3g/L NiCl2、约37.5g/L硼酸、约180g/L氨基磺酸镍组成;pH为约3.9;在约10ASF下在约120℉下操作约30分钟。
5.按照规范要求组成电解锡-镍浴;pH为约4.5至约5.0;在约15ASF下在约155℉下操作约12分钟。
处理循环
1.在PRESOL 5161/5opg./150℉中非蚀刻浸泡清洁5分钟。
2.冲洗
3.用脱氧溶液脱氧5分钟/30%b.v./室温
4.冲洗
5.用38g/L蚀刻溶液(约5盎司/加仑)/在160℉下进行碱性蚀刻90秒。
6.冲洗
7.用脱氧溶液脱氧5分钟/30%b.v./室温
8.冲洗
9.在室温下(例如,约75℉)在50体积/体积%HNO3酸中的附加脱氧
10.冲洗
11.在约75℉下在锌酸盐溶液/25%b.v.中浸渍45秒。
12.冲洗
13.在50体积/体积%硝酸中将锌酸盐退镀45秒
14.冲洗
15.在锌酸盐溶液中浸渍20秒。
16.冲洗
17.按照规范在化学镀镍工艺中碱性冲击约5分钟至约10分钟/90℉
18.浸渍冲洗
19.在190℉下在化学镀镍浴中进行化学镀镍(约1.0密耳厚)
20.冲洗
21.氨基磺酸镍电镀-(在120℉和10ASF下30分钟);0.2密耳厚度
22.冲洗
23.在电解锡-镍浴中进行锡-镍合金电镀(155℉和约15ASF下12分钟);0.2密耳厚度
24.冲洗
25.空气干燥
中性盐雾腐蚀室暴露
对上述样品进行盐雾腐蚀测试。以24小时的间隔检查部件的腐蚀破坏迹象,总共暴露>500小时。腐蚀破坏被定义为红锈的视觉迹象,其将指示基底金属腐蚀(在镀锌部件上,或在Al是与钢相对的衬底之处观察到的“白”锈)。根据ASTM B117标准进行盐雾腐蚀测试。包括测试之前以及测试结束时连接器的光学图像。
表1
结论
在对上文概述的循环的各种迭代和型式进行分析之后,通过最终的优化循环处理多个测试件(总共40个样品)(图3A-3B)。该循环产生的连接器表现出足够的粘附性、均匀的外观、>500小时的NSS腐蚀室暴露而没有失效,并且横截面厚度验证测量结果指示所概述的过程产生了每个单独层的近似目标厚度。
表2-平均横截面厚度测量结果
将通过本报告中概述的优化循环处理的一个代表性连接器横切,其中检查OD和ID表面,并且将沉积层厚度测量结果收集在上表中并求平均值(图4A和图4B)。
中性盐雾腐蚀室测试:
在>500小时的室暴露之后,通过如在报告中概述的优化循环处理的六个代表性连接器未表现出对Al衬底的污染或腐蚀的迹象(图5A-5B)。
定性沉积物粘附性评估:
在通过优化循环处理的代表性连接器的卷曲/压碎之后,在光学检查时,未发现或记录到剥落或不充分的粘附(图6A-6B)。
从本发明的以上描述,本领域技术人员将认识到改善、改变和修改。此类改善、改变和修改在本领域的技术范围内,并且旨在由所附权利要求覆盖。在本申请中引用的所有专利公布和参考文献均全文以引用方式并入本文中。
Claims (21)
1.一种制品,所述制品包括:
铝衬底,所述铝衬底任选地被锌酸盐涂覆,在其表面的至少一部分上具有多层涂层,所述多层涂层包括覆盖所述表面的部分的至少一个化学镀镍层、覆盖所述化学镀镍层的至少一个电解镍层和覆盖所述电解镍层的至少一个电解锡-镍层。
2.根据权利要求1所述的制品,其中所述至少一个化学镀镍层具有约5重量%至约14重量%、优选地约5重量%至约9重量%或约10重量%至约14重量%的磷含量。
3.根据权利要求1或2所述的制品,其中所述至少一个化学镀镍层包括具有不同磷含量的两个化学镀镍层,优选地第一化学镀镍层具有约5重量%至约9重量%的磷含量,并且第二化学镀镍层具有约10重量%至约14重量%的磷含量。
4.根据权利要求1至3中任一项所述的制品,其中所述至少一个化学镀镍层是微孔的并且所述电解镍层是无孔的或基本上无孔的。
5.根据权利要求1至4中任一项所述的制品,其中所述电解锡-镍合金层包含约50重量%至约80重量%的锡,其中余量基本上为镍。
6.根据权利要求1至5中任一项所述的制品,其中所述至少一个化学镀镍层具有约0.5密耳至约2密耳的厚度。
7.根据权利要求1至6中任一项所述的制品,其中所述电解镍层具有约0.05密耳至约0.6密耳的厚度。
8.根据权利要求1至7中任一项所述的制品,其中所述电解锡-镍合金层具有约0.1密耳至约0.6密耳的厚度。
9.根据权利要求1至8中任一项所述的制品,其中所述铝衬底用锌酸盐浸渍涂层锌酸化。
10.根据权利要求1至9中任一项所述的制品,其中所述多层涂层具有约0.5密耳至约2.0密耳的厚度并且能够经受至少336小时的中性盐雾腐蚀测试(NSST)而不腐蚀下面的衬底。
11.一种在衬底上形成多层涂层的方法,所述方法包括:
用至少一个化学镀镍层涂覆所述衬底的表面;
在所述至少一个化学镀镍层上电镀镍层;以及
在所述电镀镍层上电镀锡-镍合金层。
12.根据权利要求11所述的方法,其中所述衬底是任选地被锌酸盐涂覆的铝衬底。
13.根据权利要求11或12所述的方法,其中所述至少一个化学镀镍层具有约5重量%至约14重量%、优选地约5重量%至约9重量%或约10重量%至约14重量%的磷含量。
14.根据权利要求11至13中任一项所述的方法,用具有不同磷含量的两个化学镀镍层涂覆所述衬底的表面,其中第一化学镀镍层具有约5重量%至约9重量%的磷含量,并且第二化学镀镍层具有约10重量%至约14重量%的磷含量。
15.根据权利要求11至14中任一项所述的方法,其中所述至少一个化学镀镍层是微孔的并且所述电镀镍层是无孔的或基本上无孔的。
16.根据权利要求11至15中任一项所述的方法,其中所述电镀锡-镍合金包含约50重量%至约80重量%的锡,其中余量基本上为镍。
17.根据权利要求11至16中任一项所述的方法,其中所述至少一个化学镀镍层具有约0.5密耳至约2密耳的厚度。
18.根据权利要求11至17中任一项所述的方法,其中所述电镀镍层具有约0.05密耳至约0.6密耳的厚度。
19.根据权利要求11至18中任一项所述的方法,其中所述电镀锡-镍合金层具有约0.1密耳至约0.6密耳的厚度。
20.根据权利要求11至19中任一项所述的方法,所述方法还包括在用所述化学镀镍层涂覆所述表面之前对所述铝衬底的表面进行锌酸化。
21.根据权利要求11至20中任一项所述的方法,其中所述多层涂层具有约0.5密耳至约2.0密耳的厚度并且能够经受至少336小时的中性盐雾腐蚀测试(NSST)而不腐蚀下面的衬底。
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