CN113737160A - 一种化学镀黑镍液 - Google Patents
一种化学镀黑镍液 Download PDFInfo
- Publication number
- CN113737160A CN113737160A CN202110823961.2A CN202110823961A CN113737160A CN 113737160 A CN113737160 A CN 113737160A CN 202110823961 A CN202110823961 A CN 202110823961A CN 113737160 A CN113737160 A CN 113737160A
- Authority
- CN
- China
- Prior art keywords
- plating solution
- nickel plating
- acid
- black nickel
- nickel
- 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
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 142
- 238000007747 plating Methods 0.000 title claims abstract description 82
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 69
- 239000000126 substance Substances 0.000 title claims abstract description 47
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 8
- 239000008139 complexing agent Substances 0.000 claims abstract description 8
- 229910001453 nickel ion Inorganic materials 0.000 claims abstract description 8
- 239000003381 stabilizer Substances 0.000 claims abstract description 8
- 239000006172 buffering agent Substances 0.000 claims abstract description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 12
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 7
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 7
- 229960001763 zinc sulfate Drugs 0.000 claims description 7
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 6
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 6
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 5
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 5
- -1 nitrogen-containing compound Chemical class 0.000 claims description 5
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 4
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 4
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 4
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 claims description 4
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- RJTANRZEWTUVMA-UHFFFAOYSA-N boron;n-methylmethanamine Chemical compound [B].CNC RJTANRZEWTUVMA-UHFFFAOYSA-N 0.000 claims description 4
- HHLFWLYXYJOTON-UHFFFAOYSA-N glyoxylic acid Chemical compound OC(=O)C=O HHLFWLYXYJOTON-UHFFFAOYSA-N 0.000 claims description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 4
- 150000002815 nickel Chemical class 0.000 claims description 4
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims description 4
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims description 4
- 150000003751 zinc Chemical class 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 4
- 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 claims description 3
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 claims description 3
- 239000004471 Glycine Substances 0.000 claims description 3
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 claims description 3
- 229940116357 potassium thiocyanate Drugs 0.000 claims description 3
- 235000019260 propionic acid Nutrition 0.000 claims description 3
- 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 claims description 3
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 3
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 3
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 3
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N thiocyanic acid Chemical compound SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 claims description 3
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 3
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 2
- UPPLJLAHMKABPR-UHFFFAOYSA-H 2-hydroxypropane-1,2,3-tricarboxylate;nickel(2+) Chemical compound [Ni+2].[Ni+2].[Ni+2].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O UPPLJLAHMKABPR-UHFFFAOYSA-H 0.000 claims description 2
- 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 2
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims 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 claims description 2
- FZWLAAWBMGSTSO-UHFFFAOYSA-N Thiazole Chemical compound C1=CSC=N1 FZWLAAWBMGSTSO-UHFFFAOYSA-N 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 2
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 2
- FAPDDOBMIUGHIN-UHFFFAOYSA-K antimony trichloride Chemical compound Cl[Sb](Cl)Cl FAPDDOBMIUGHIN-UHFFFAOYSA-K 0.000 claims description 2
- 229910000380 bismuth sulfate Inorganic materials 0.000 claims description 2
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 2
- 229960004106 citric acid Drugs 0.000 claims description 2
- 235000015165 citric acid Nutrition 0.000 claims description 2
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 claims description 2
- 235000018417 cysteine Nutrition 0.000 claims description 2
- BEQZMQXCOWIHRY-UHFFFAOYSA-H dibismuth;trisulfate Chemical compound [Bi+3].[Bi+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BEQZMQXCOWIHRY-UHFFFAOYSA-H 0.000 claims description 2
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 2
- 239000004310 lactic acid Substances 0.000 claims description 2
- 235000014655 lactic acid Nutrition 0.000 claims description 2
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 claims description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 2
- 239000011976 maleic acid Substances 0.000 claims description 2
- 239000001630 malic acid Substances 0.000 claims description 2
- 235000011090 malic acid Nutrition 0.000 claims description 2
- 229940012189 methyl orange Drugs 0.000 claims description 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims description 2
- 229940078494 nickel acetate Drugs 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- KERTUBUCQCSNJU-UHFFFAOYSA-L nickel(2+);disulfamate Chemical compound [Ni+2].NS([O-])(=O)=O.NS([O-])(=O)=O KERTUBUCQCSNJU-UHFFFAOYSA-L 0.000 claims description 2
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001380 potassium hypophosphite Inorganic materials 0.000 claims description 2
- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 claims description 2
- 239000001230 potassium iodate Substances 0.000 claims description 2
- 235000006666 potassium iodate Nutrition 0.000 claims description 2
- 229940093930 potassium iodate Drugs 0.000 claims description 2
- 235000007715 potassium iodide Nutrition 0.000 claims description 2
- CRGPNLUFHHUKCM-UHFFFAOYSA-M potassium phosphinate Chemical compound [K+].[O-]P=O CRGPNLUFHHUKCM-UHFFFAOYSA-M 0.000 claims description 2
- 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 claims description 2
- IIQJBVZYLIIMND-UHFFFAOYSA-J potassium;antimony(3+);2,3-dihydroxybutanedioate Chemical compound [K+].[Sb+3].[O-]C(=O)C(O)C(O)C([O-])=O.[O-]C(=O)C(O)C(O)C([O-])=O IIQJBVZYLIIMND-UHFFFAOYSA-J 0.000 claims description 2
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 claims description 2
- 229940081974 saccharin Drugs 0.000 claims description 2
- 235000019204 saccharin Nutrition 0.000 claims description 2
- 239000000901 saccharin and its Na,K and Ca salt Substances 0.000 claims description 2
- 229960004889 salicylic acid Drugs 0.000 claims description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 2
- 239000012279 sodium borohydride Substances 0.000 claims description 2
- 239000001509 sodium citrate Substances 0.000 claims description 2
- 235000011006 sodium potassium tartrate Nutrition 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 claims description 2
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 claims description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 2
- 229940038773 trisodium citrate Drugs 0.000 claims description 2
- 235000019263 trisodium citrate Nutrition 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 229910052783 alkali metal Inorganic materials 0.000 claims 1
- 150000001340 alkali metals Chemical class 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000001476 sodium potassium tartrate Substances 0.000 claims 1
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 3
- 230000008021 deposition Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 17
- 239000000758 substrate Substances 0.000 description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- 238000004140 cleaning Methods 0.000 description 11
- 238000001514 detection method Methods 0.000 description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 9
- 229910052802 copper Inorganic materials 0.000 description 9
- 239000010949 copper Substances 0.000 description 9
- 229920003023 plastic Polymers 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 230000004913 activation Effects 0.000 description 7
- 229910052742 iron Inorganic materials 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 238000000151 deposition Methods 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005238 degreasing Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 229910052755 nonmetal Inorganic materials 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 2
- 239000005695 Ammonium acetate Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- JVTAAEKCZFNVCJ-REOHCLBHSA-N L-lactic acid Chemical compound C[C@H](O)C(O)=O JVTAAEKCZFNVCJ-REOHCLBHSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 235000011054 acetic acid Nutrition 0.000 description 2
- 229940043376 ammonium acetate Drugs 0.000 description 2
- 235000019257 ammonium acetate Nutrition 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 235000017281 sodium acetate Nutrition 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- BDKLKNJTMLIAFE-UHFFFAOYSA-N 2-(3-fluorophenyl)-1,3-oxazole-4-carbaldehyde Chemical compound FC1=CC=CC(C=2OC=C(C=O)N=2)=C1 BDKLKNJTMLIAFE-UHFFFAOYSA-N 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical compound [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 description 1
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 235000010338 boric acid Nutrition 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 229940116298 l- malic acid Drugs 0.000 description 1
- 229960000448 lactic acid Drugs 0.000 description 1
- 229940046892 lead acetate Drugs 0.000 description 1
- 229940099690 malic acid Drugs 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 229940074439 potassium sodium tartrate Drugs 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 238000006748 scratching Methods 0.000 description 1
- 230000002393 scratching effect Effects 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 229940087562 sodium acetate trihydrate Drugs 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 229960001367 tartaric acid 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
- 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
-
- 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
本发明涉及化学镀液技术领域，特别涉及一种化学镀黑镍液，包括如下按浓度计的组分：0.5～20g/L镍离子，0.1～10g/L锌离子，1～100g/L络合剂，1～60g/L还原剂，1～50g/L缓冲剂，0.1×10‑3～1g/L稳定剂，0.1×10‑3～5g/L发黑剂。通过所述化学镀黑镍液所形成的黑镍镀层为深黑镀层，并且沉积速度最高可达到12μm/hr以上，具有表面平整，结晶细腻且抗氧化能力强的优点。
Description
技术领域
本发明涉及化学镀液技术领域，特别涉及一种化学镀黑镍液。
背景技术
在仪器、仪表、光学、电子等行业中，需要在零件表面镀黑膜，以降低零件反光率和改变其热性能。
常规的镀黑膜的方法主要包括三种：镍层化学发黑法、化学镀黑镍法和电镀黑镍法。
其中，镍层化学发黑法主要基于镍层氧化发黑的原理，其所形成的黑膜具有硬度低、容易刮花和脱落等的问题；而化学镀黑镍法和电镀黑镍法可有效解决前述问题，但是电镀黑镍法具有工艺复杂，效率低，人工成本高，难以保证在异形件或小型件表面形成均匀的镀层，其品质也难以得到保证等问题；而化学镀黑镍法可有效避免前述问题，但是现有的化学镀黑镍液产品种类少。目前市售的化学镀黑镍液只能在亮镍或白镍的镀层表面沉积厚度不足1μm的黑镍镀层。所以开发一种稳定，可连续沉积黑色镀层的化学黑镍液非常必要。
发明内容
为了克服上述现有技术的缺陷，本发明所要解决的技术问题是：解决现有的化学镀黑镍液无法在基体表面连续稳定沉积任意厚度黑镍镀层的问题。
为了解决上述技术问题，本发明采用的技术方案为：一种化学镀黑镍液，包括如下按浓度计的组分：
0.5～20g/L镍离子，0.1～10g/L锌离子，1～100g/L络合剂，1～60g/L还原剂，1～50g/L缓冲剂，0.1×10-3～1g/L稳定剂，0.1×10-3～5g/L发黑剂。
本发明的有益效果在于：本发明所提供的化学镀黑镍液可适用于在金属或非金属基材表面直接沉积黑镍镀层，并且黑镍镀层在30min内的沉积厚度可达到6.5μm；同时，本发明所提供的化学镀黑镍液品质稳定、环境友好，所形成的黑镍镀层的镀层厚度可随化学镀时间的延长而逐渐增厚，具有表面平整，结晶细腻且抗氧化能力强的优点。
具体实施方式
为详细说明本发明的技术内容、所实现目的及效果，以下结合实施方式予以说明。
一种化学镀黑镍液，以在金属或非金属基材表面连续沉积黑色镍镀层，包括如下按浓度计的组分：
0.5～20g/L镍离子，0.1～10g/L锌离子，1～100g/L络合剂，1～60g/L还原剂，1～50g/L缓冲剂，0.1×10-3～1g/L稳定剂，0.1×10-3～5g/L发黑剂。
优选的，所述化学镀黑镍液由如下按浓度计的组分构成：
3～8g/L镍离子，0.1～5g/L锌离子，10～60g/L络合剂，1～40g/L还原剂，1～30g/L缓冲剂，5×10-3～1×10-2g/L稳定剂，0.1×10-3～1g/L发黑剂。
进一步的，所述络合剂包括但不限于苹果酸、丁二酸、丙酸、马来酸、水杨酸、甘氨酸、三乙醇胺、乙二胺四乙酸、乙二胺四乙酸二钠、乙二胺四乙酸四钠、乳酸、酒石酸、酒石酸钾钠、柠檬酸、柠檬酸三钠中至少两种的复合。
进一步的，所述稳定剂包括但不限于硫脲、碘化钾、碘酸钾、硫代硫酸钠、硫氰酸、硝酸铅、乙酸铅、硝酸铋、硫酸铋、氯化锑、酒石酸锑钾和二氧化碲中至少一种。
进一步的，所述镍离子由可溶性镍盐提供，所述可溶性镍盐为硫酸镍、氯化镍、氨基磺酸镍、乙酸镍和柠檬酸镍中的至少一种。
进一步的，所述锌离子由锌盐提供，所述锌盐为硫酸锌、氯化锌、氧化锌、硝酸锌、硫酸锌中的至少一种。
进一步的，所述发黑剂为含氮化合物，所述含氮化合物为硫脲及其衍生物、硫氰酸钾，巯基乙酸，半胱氨酸，糖精，联吡啶，噻唑，甲基橙，萘中的至少一种。
可选的，所述发黑剂还可包括可溶性金属硫酸盐、亚硫酸盐以及磺酸盐，优选为硫代硫酸钠、亚硫酸钠。
进一步的，所述还原剂为次磷酸钠、次磷酸钾、乙醛酸、二甲基胺硼烷、硼氢化钠、硼氢化钾、肼中的至少一种。
进一步的，所述缓冲剂为乙酸、乙酸钠、乙酸铵、碳酸钠、硼酸中的一种。
实施例一
一种化学镀黑镍液，由如下表1中按浓度计的组分构成：
表1
| 硫酸镍 | 30g/L |
| 硫酸锌 | 2g/L |
| 苹果酸 | 27g/L |
| 丁二酸 | 16g/L |
| 乙酸铵 | 7g/L |
| 二甲基胺硼烷 | 3g/L |
| 硫脲 | 2×10<sup>-3</sup>g/L |
| 半胱氨酸 | 5×10<sup>-1</sup>g/L |
| 镀液pH | 7.5 |
| 温度 | 75℃ |
实施例二
一种化学镀黑镍液，由如下表2中按浓度计的组分构成：
表2
实施例三
一种化学镀黑镍液，由如下表3中按浓度计的组分构成：
表3
| 硫酸镍 | 28g/L |
| 硫酸锌 | 8g/L |
| 甘氨酸 | 8g/L |
| 柠檬酸钠 | 27g/L |
| 乙酸 | 10g/L |
| 次磷酸钠 | 30g/L |
| 硝酸铋 | 8×10<sup>-3</sup>g/L |
| 硫氰酸钾 | 8×10<sup>-3</sup>g/L |
| 镀液pH | 8.0 |
| 温度 | 83℃ |
实施例四
一种化学镀黑镍液，由如下表4中按浓度计的组分构成：
表4
实施例五
一种化学镀黑镍液，由如下表5中按浓度计的组分构成：
表5
| 硫酸镍 | 27g/L |
| 硫酸锌 | 6g/L |
| 乳酸 | 12g/L |
| 丙酸 | 10g/L |
| 三水合乙酸钠 | 18g/L |
| 二甲基胺硼烷 | 2g/L |
| 硫脲 | 2×10<sup>-3</sup>g/L |
| 联吡啶 | 5×10<sup>-3</sup>g/L |
| 镀液pH | 9.5 |
| 温度 | 85℃ |
检测例一
利用实施例一所提供的化学镀黑镍液对铁基材表面进行化学镀黑镍镀层，具体为：
第一步，对铁基材表面进行碱性除油；
第二步，对铁基材表面进行第一次纯水清洗；
第三步，对清洗完成的铁基材表面进行酸活化，酸活化采用的试剂为：硫酸或盐酸；
第四步，对酸活化后的铁基材表面进行第二次纯水清洗；
第五步，将清洗干净的铁基材浸泡在化学镀黑镍液中，在75℃工作温度下进行化学镀；
第六步，化学镀30min后取出铁基材并清洗烘干，得到均匀一致的深黑色镀层，利用X-Ray测试镀层厚度为6.3μm。
检测例二
利用实施例二所提供的化学镀黑镍液对铜基材表面进行化学镀黑镍镀层，具体为：
第一步，对铜基材表面进行碱性化学除油；
第二步，对铜基材表面进行第一次纯水清洗；
第三步，对清洗后的铜基材表面进行抛光处理；
第四步，对抛光后的铜基材表明进行第二次纯水清洗；
第五步，对清洗后的铜基材表面进行Pd活化；
第六步，对Pd活化后的铜基材表面进行第三次清水清洗；
第七步，将清洗干净的铜基材浸泡在化学镀黑镍液中，在85℃的工作温度下进行化学镀；
第八步，化学镀30min后取出铜基材并清洗烘干，得到均匀一致的深黑色镀层，利用X-Ray测试镀层厚度为5.2μm。
检测例三
利用实施例三所提供的化学镀黑镍液对塑料基材表面进行化学镀黑镍镀层，具体为：
第一步，对ABS塑料基材表面进行碱性化学除油；
第二步，对塑料基材表面进行化学粗化(高锰酸钾20g/L+浓硫酸100g/L)；
第三步，对化学粗化后的塑料基材表面进行第一次纯水清洗；
第四步，对清洗后的塑料基材表面进行Pd活化；
第五步，对Pd活化后的塑料基材表面进行第二次纯水清洗；
第六步；对清洗后的塑料基材表面进行Pd还原；
第七步，对Pd还原后的塑料基材表面进行第三次纯水清洗；
第八步，将清洗干净的塑料基材浸泡在化学镀黑镍液中，在83℃的工作温度下进行化学镀；
第九步，化学镀30min后取出塑料基材并清洗烘干，得到均匀一致的深黑色镀层，利用X-Ray测试镀层厚度为5.4μm。
对比例一
与实施例一及检测例一的区别在于：检测例一所用采用的基材在实施例四黑镍溶液中浸泡30min后取出后清洗并烘干，利用X-Ray测得黑镍镀层的厚度为6.5um。
对比例二
与实施例二及检测例二的区别在于：检测例二所用采用的基材在实施例五黑镍溶液中浸泡30min后取出后清洗并烘干，利用X-Ray测得黑镍镀层的厚度为5.8um。
对比例三
与实施例三及检测例三的区别在于：检测例三所用采用的基材在实施例一黑镍溶液中浸泡30min后取出后清洗并烘干，利用X-Ray测得黑镍镀层的厚度为5.5um。
需要说明的是，在本文中，Pd活化为在基材表面吸附催化剂Pd离子；Pd还原为将吸附在基材表面的Pd离子还原为Pd原子。
综上所述，本发明所提供的化学镀黑镍液，可适用于在金属或非金属基材表面直接沉积黑镍镀层，并且黑镍镀层在30min内的沉积厚度最高可达到6.5μm；同时，本发明所提供的化学镀黑镍液品质稳定、环境友好，所形成的黑镍镀层的镀层厚度可随化学镀时间的延长而逐渐增厚，具有表面平整，结晶细腻且抗氧化能力强的优点。
以上所述仅为本发明的实施例，并非因此限制本发明的专利范围，凡是利用本发明说明书内容所作的等同变换，或直接或间接运用在相关的技术领域，均同理包括在本发明的专利保护范围内。
Claims (9)
1.一种化学镀黑镍液，其特征在于，包括如下按浓度计的组分：
0.5～20g/L镍离子，0.1～10g/L锌离子，1～100g/L络合剂，1～60g/L还原剂，1～50g/L缓冲剂，0.1×10-3～1g/L稳定剂，0.1×10-3～5g/L发黑剂。
2.根据权利要求1所述化学镀黑镍液，其特征在于，包括如下按浓度计的组分：
3～8g/L镍离子，0.1～5g/L锌离子，10～60g/L络合剂，1～40g/L还原剂，1～30g/L缓冲剂，5×10-3～1×10-2g/L稳定剂，0.1×10-3～1g/L发黑剂。
3.根据权利要求1所述化学镀黑镍液，其特征在于，所述络合剂为苹果酸、丁二酸、丙酸、马来酸、水杨酸、甘氨酸、三乙醇胺、乙二胺四乙酸、乙二胺四乙酸二钠、乙二胺四乙酸四钠、乳酸、酒石酸、酒石酸钾钠、柠檬酸、柠檬酸三钠中的至少两种。
4.根据权利要求3所述化学镀黑镍液，其特征在于，所述碱金属为钠和/或钾。
5.根据权利要求1所述化学镀黑镍液，其特征在于，所述稳定剂为硫脲、碘化钾、碘酸钾、硫代硫酸钠、硫氰酸、硝酸铅、硝酸铋、硫酸铋、氯化锑、酒石酸锑钾和二氧化碲中至少一种。
6.根据权利要求1所述化学镀黑镍液，其特征在于，所述镍离子由可溶性镍盐提供，所述可溶性镍盐为硫酸镍、氯化镍、氨基磺酸镍、乙酸镍和柠檬酸镍中的至少一种。
7.根据权利要求1所述化学镀黑镍液，其特征在于，所述锌离子由锌盐提供，所述锌盐为硫酸锌、氯化锌、氧化锌、硝酸锌、硫酸锌中的至少一种。
8.根据权利要求1所述化学镀黑镍液，其特征在于，所述发黑剂为含氮化合物，所述含氮化合物为硫脲及其衍生物、硫氰酸钾，巯基乙酸，半胱氨酸，糖精，联吡啶，噻唑，甲基橙，萘中的至少一种。
9.根据权利要求1所述化学镀黑镍液，其特征在于，所述还原剂为次磷酸钠、次磷酸钾、乙醛酸、二甲基胺硼烷、硼氢化钠、硼氢化钾、肼中的至少一种。
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