CN109576718A - A kind of process of surface treatment of rolled copper foil - Google Patents
A kind of process of surface treatment of rolled copper foil Download PDFInfo
- Publication number
- CN109576718A CN109576718A CN201910077181.0A CN201910077181A CN109576718A CN 109576718 A CN109576718 A CN 109576718A CN 201910077181 A CN201910077181 A CN 201910077181A CN 109576718 A CN109576718 A CN 109576718A
- Authority
- CN
- China
- Prior art keywords
- copper foil
- rolled copper
- solution
- sodium
- surface treatment
- 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.)
- Granted
Links
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 338
- 239000011889 copper foil Substances 0.000 title claims abstract description 328
- 238000000034 method Methods 0.000 title claims abstract description 44
- 238000004381 surface treatment Methods 0.000 title claims abstract description 29
- 238000007747 plating Methods 0.000 claims abstract description 77
- 238000004140 cleaning Methods 0.000 claims abstract description 60
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 58
- 238000007788 roughening Methods 0.000 claims abstract description 58
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 52
- 238000002161 passivation Methods 0.000 claims abstract description 45
- 229910000858 La alloy Inorganic materials 0.000 claims abstract description 37
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 35
- 239000010937 tungsten Substances 0.000 claims abstract description 35
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 90
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 73
- 238000009713 electroplating Methods 0.000 claims description 57
- 239000007788 liquid Substances 0.000 claims description 56
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 46
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 34
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 32
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 27
- 238000012545 processing Methods 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 21
- 230000001476 alcoholic effect Effects 0.000 claims description 19
- DOARWPHSJVUWFT-UHFFFAOYSA-N lanthanum nickel Chemical compound [Ni].[La] DOARWPHSJVUWFT-UHFFFAOYSA-N 0.000 claims description 19
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 claims description 16
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims description 16
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims description 16
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 16
- 239000004202 carbamide Substances 0.000 claims description 16
- FPNCFEPWJLGURZ-UHFFFAOYSA-L iron(2+);sulfite Chemical compound [Fe+2].[O-]S([O-])=O FPNCFEPWJLGURZ-UHFFFAOYSA-L 0.000 claims description 16
- 239000000787 lecithin Substances 0.000 claims description 16
- 235000010445 lecithin Nutrition 0.000 claims description 16
- 229940067606 lecithin Drugs 0.000 claims description 16
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 16
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 16
- DITXJPASYXFQAS-UHFFFAOYSA-N nickel;sulfamic acid Chemical compound [Ni].NS(O)(=O)=O DITXJPASYXFQAS-UHFFFAOYSA-N 0.000 claims description 16
- 239000000467 phytic acid Substances 0.000 claims description 16
- 235000002949 phytic acid Nutrition 0.000 claims description 16
- 229940068041 phytic acid Drugs 0.000 claims description 16
- 239000001509 sodium citrate Substances 0.000 claims description 16
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical group O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 16
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical group [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 16
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 16
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 16
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 16
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 15
- -1 alkyl phenol Chemical compound 0.000 claims description 13
- 229910001297 Zn alloy Inorganic materials 0.000 claims description 12
- XZLXGTUBUCMRCH-UHFFFAOYSA-N tungsten zinc Chemical compound [Zn].[W] XZLXGTUBUCMRCH-UHFFFAOYSA-N 0.000 claims description 12
- 239000011888 foil Substances 0.000 claims description 11
- 238000005096 rolling process Methods 0.000 claims description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- 239000003945 anionic surfactant Substances 0.000 claims description 10
- 239000002736 nonionic surfactant Substances 0.000 claims description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 9
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 9
- 239000004327 boric acid Substances 0.000 claims description 9
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 9
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 9
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 9
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims description 9
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 8
- 239000003381 stabilizer Substances 0.000 claims description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- 150000002191 fatty alcohols Chemical group 0.000 claims description 6
- 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 description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 4
- 239000000194 fatty acid Substances 0.000 claims description 4
- 229930195729 fatty acid Natural products 0.000 claims description 4
- 150000004665 fatty acids Chemical class 0.000 claims description 4
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 4
- 235000011152 sodium sulphate Nutrition 0.000 claims description 4
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 claims description 4
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 3
- 244000060011 Cocos nucifera Species 0.000 claims description 3
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 claims description 3
- 125000005456 glyceride group Chemical group 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims description 3
- 239000004299 sodium benzoate Substances 0.000 claims description 3
- 235000010234 sodium benzoate Nutrition 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- 239000011574 phosphorus Substances 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 235000010288 sodium nitrite Nutrition 0.000 claims description 2
- 230000003213 activating effect Effects 0.000 claims 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims 1
- 125000000129 anionic group Chemical group 0.000 claims 1
- 239000000571 coke Substances 0.000 claims 1
- 229910000077 silane Inorganic materials 0.000 claims 1
- 239000001488 sodium phosphate Substances 0.000 claims 1
- 229910000162 sodium phosphate Inorganic materials 0.000 claims 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims 1
- 230000007797 corrosion Effects 0.000 abstract description 29
- 238000005260 corrosion Methods 0.000 abstract description 29
- 230000003746 surface roughness Effects 0.000 abstract description 15
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052785 arsenic Inorganic materials 0.000 abstract description 4
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052804 chromium Inorganic materials 0.000 abstract description 4
- 239000011651 chromium Substances 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000002274 desiccant Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 36
- 239000000758 substrate Substances 0.000 description 28
- 239000000203 mixture Substances 0.000 description 23
- 238000003756 stirring Methods 0.000 description 23
- 230000000052 comparative effect Effects 0.000 description 19
- 150000003839 salts Chemical class 0.000 description 15
- 238000003618 dip coating Methods 0.000 description 14
- 235000013399 edible fruits Nutrition 0.000 description 14
- 229910052746 lanthanum Inorganic materials 0.000 description 14
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 14
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 14
- 239000002253 acid Substances 0.000 description 10
- 229910052802 copper Inorganic materials 0.000 description 9
- 239000010949 copper Substances 0.000 description 9
- 238000007711 solidification Methods 0.000 description 9
- 230000008023 solidification Effects 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- 238000005660 chlorination reaction Methods 0.000 description 8
- 235000019441 ethanol Nutrition 0.000 description 8
- 206010028980 Neoplasm Diseases 0.000 description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 7
- 239000005864 Sulphur Substances 0.000 description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 7
- 239000006210 lotion Substances 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 238000011084 recovery Methods 0.000 description 7
- 230000002787 reinforcement Effects 0.000 description 7
- 239000010936 titanium Substances 0.000 description 7
- 229910052719 titanium Inorganic materials 0.000 description 7
- 238000005406 washing Methods 0.000 description 7
- 238000007596 consolidation process Methods 0.000 description 6
- 229960004756 ethanol Drugs 0.000 description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 5
- 239000000460 chlorine Substances 0.000 description 5
- 229910052801 chlorine Inorganic materials 0.000 description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 5
- 238000013401 experimental design Methods 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- 238000005476 soldering Methods 0.000 description 3
- 229910000990 Ni alloy Inorganic materials 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 150000007942 carboxylates Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- QELJHCBNGDEXLD-UHFFFAOYSA-N nickel zinc Chemical compound [Ni].[Zn] QELJHCBNGDEXLD-UHFFFAOYSA-N 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000004439 roughness measurement Methods 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- MOMKYJPSVWEWPM-UHFFFAOYSA-N 4-(chloromethyl)-2-(4-methylphenyl)-1,3-thiazole Chemical compound C1=CC(C)=CC=C1C1=NC(CCl)=CS1 MOMKYJPSVWEWPM-UHFFFAOYSA-N 0.000 description 1
- 241001163841 Albugo ipomoeae-panduratae Species 0.000 description 1
- 229910021555 Chromium Chloride Inorganic materials 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000003490 calendering Methods 0.000 description 1
- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical compound [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- HIRWGWMTAVZIPF-UHFFFAOYSA-N nickel;sulfuric acid Chemical compound [Ni].OS(O)(=O)=O HIRWGWMTAVZIPF-UHFFFAOYSA-N 0.000 description 1
- GQPLMRYTRLFLPF-UHFFFAOYSA-N nitrous oxide Inorganic materials [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000007719 peel strength test Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 229940005657 pyrophosphoric acid Drugs 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000011775 sodium fluoride Substances 0.000 description 1
- 235000013024 sodium fluoride Nutrition 0.000 description 1
- 235000019983 sodium metaphosphate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/10—Other heavy metals
- C23G1/103—Other heavy metals copper or alloys of copper
-
- 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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/07—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
- C23C22/08—Orthophosphates
- C23C22/10—Orthophosphates containing oxidants
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/38—Pretreatment of metallic surfaces to be electroplated of refractory metals or nickel
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/06—Wires; Strips; Foils
- C25D7/0614—Strips or foils
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
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Abstract
The present invention relates to the technical field of producing of copper foil, more particularly to a kind of process of surface treatment of rolled copper foil, the characteristics of present invention is according to rolled copper foil, improvement is optimized in the every process being surface-treated to it, whole process does not introduce the harmful elements such as chromium, arsenic, environmental protection completely meets European Union ROHS regulation；Through over cleaning, roughening for the first time, not only surface roughness is low for the rolled copper foil that solidify, secondary roughening, secondary curing, nickel plating lanthanum alloy refractory layer, plate tungsten kirsite refractory layer, obtained after the processes such as passivation, drying and silane coupling agent are handled for the first time, and there is excellent heat resistance, corrosion resistance and higher peel strength, it can satisfy industrial requirements at the higher level.
Description
Technical field
The present invention relates to the technical field of producing of copper foil, in particular to a kind of process of surface treatment of rolled copper foil.
Background technique
Copper foil is one of the important materials for manufacturing printed circuit board, and the quality of copper foil has weight to the performance of printed circuit board
The influence wanted.According to the difference of production technology, copper foil mainly has electrolytic copper foil and rolled copper foil two types, and rolled copper foil is than electricity
Solving copper foil has better bending performance, therefore is more suitable in the application of flexible print wiring board.
Then copper foil can be just applied in circuit board before use, usually need first press to form copper-clad plate with resin substrate,
To ensure to have between copper foil and substrate enough binding forces, and there are the spies such as centainly heat-resisting, corrosion-resistant and anti-oxidant
Property, ensure the performance of printed circuit board, copper foil is required to by surface treatment before pressing.Currently, the surface treatment work of copper foil
Skill mainly includes that oil removing, roughening, solidification, plating refractory layer, plating are anti-oxidation etc..But it is prepared using traditional surface treatment process of copper foil
Not only peel strength is small for the copper foil come, heat-resisting, poor corrosion resistance, and can introduce the harmful elements such as chromium, arsenic, inadequate ring
It protects, does not meet the ROHS regulation of European Union.
Summary of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the invention proposes a kind of process of surface treatment of rolled copper foil, no
Only without the harmful elements such as chromium, arsenic, completely environmental protection, meet European Union ROHS regulation, and surface roughness is low, with excellent resistance to
Hot, corrosion resistance and higher peel strength, meet industrial requirements at the higher level.
To achieve the goals above, the technical scheme adopted by the invention is that:
A kind of process of surface treatment of rolled copper foil, comprising the following steps:
S1, cleaning: rolled copper foil being immersed in cleaning solution and is cleaned, and cleans three with 50~80 DEG C of hot water after taking-up
It is secondary, it dries spare；
The cleaning solution is by following weight percent at being grouped as:
15-20% anionic surfactant, 10-15% nonionic surfactant, 8-12% sulfuric acid, 1-3% solubilising
Agent, 1-3% builder and 47-65% pure water；
S2, it is roughened for the first time: coarsening solution is added into electroplating rectifier, is 15~20A/dm in current density2, temperature be
12-18S is electroplated to rolled copper foil under the conditions of 30-40 DEG C；
The coarsening solution includes 15-25g/L copper sulphate, 60~80g/L sulfuric acid, 3-5g/L iron sulfite and 1-3g/L sulfuric acid
Nickel；
S3, solidify for the first time: solidify liquid being added into electroplating rectifier, be 15~20A/dm in current density2, temperature be
8-15S is electroplated to rolled copper foil under the conditions of 45-55 DEG C；
The solidify liquid includes 60-70g/L copper sulphate, 90~100g/L sulfuric acid and 2-3g/L lecithin；
S4, secondary roughening: coarsening solution described in first time roughening step is added into electroplating rectifier, in current density
For 8~12A/dm2, temperature be 20-30 DEG C under the conditions of to rolled copper foil be electroplated 7-10S；
S5, secondary curing: solidify liquid described in first time curing schedule is added into electroplating rectifier, in current density
For 12~15A/dm2, temperature be 35-40 DEG C under the conditions of to rolled copper foil be electroplated 5-10S；
S6, nickel plating lanthanum alloy: nickel lanthanum alloy plating solution being added into electroplating rectifier, is 10~20A/dm in current density2、
30-50S is electroplated to rolled copper foil under the conditions of being 50-65 DEG C in temperature；
The nickel lanthanum alloy plating solution includes 35-45g/L nickel sulfamic acid, 20-30g/L lanthanum chloride, 3-5g/L urea and 2-
The PH of plating solution is adjusted to 3-6 with citric acid by 3g/L stabilizer；
S7, plating tungsten kirsite: tungsten zinc alloy bath being added into electroplating rectifier, is 5~10A/dm in current density2、
15-25S is electroplated to rolled copper foil under the conditions of being 40-50 DEG C in temperature；
The tungsten zinc alloy bath includes 20-30g/L sodium tungstate, 10-15g/L zinc nitrate, 1-2g/L dodecyl sulphate
PH is adjusted to 3-5 with boric acid solution by sodium and 2-3g/L stabilizer；
S8, passivation: passivating solution is first heated to 40-50 DEG C, then rolled copper foil is immersed in passivating solution and is passivated 25-
35s；
The passivating solution includes 6-10g/L titanium trichloride, 8-12g/L phytic acid, 8-15mL/L hydrogen peroxide, 10-18g/L six
The PH of passivating solution is adjusted to 1-3 with nitric acid by sodium metaphosphate；
S9, drying: the rolled copper foil after passivation is placed in 50-60 DEG C of baking oven and dries 8-10h；
S10, silane coupling agent processing:, then will drying first with the silane coupling agent alcoholic solution of dehydrated alcohol configuration 3-5%
Rolling aluminum foil afterwards is impregnated in silane coupling agent alcoholic solution, is taken out after 10-15s, solid under the conditions of finally placing it in 70-80 DEG C
Change 1-3h, the facing operation of rolled copper foil can be completed.
Preferably, in the S1 step, rolled copper foil is immersed in cleaning solution in three times and is cleaned, impregnated every time
1-2min is both needed to be cleaned with 50~80 DEG C of hot water three times after impregnating every time.
Preferably, the anionic surfactant is neopelex, odium stearate, laruyl alcohol, vinethene
With any one in glyceride.
Preferably, the nonionic surfactant be fatty alcohol polyoxyethylene ether, cocoanut fatty acid diethanolamide,
Any one in alkyl phenol polyoxyethylene ether and polyoxyethylene carboxylate.
Preferably, the solubilizer is any one in ethyl alcohol, isopropanol and butanol.
Preferably, the builder is potassium pyrophosphate, sodium nitrite, sodium benzoate, any one in sodium sulphate.
Preferably, the stabilizer in the S6 step is sodium pyrophosphate.
Preferably, the stabilizer in the S7 step is sodium citrate.
Preferably, before the passivation of the S9 step, the rolled copper foil after plating tungsten kirsite is immersed in 45-55 DEG C of temperature
It is cleaned three times in water.
Preferably, the silane coupling agent is silane coupling agent kh550.
Compared with prior art, the beneficial effects of the present invention are:
The process of surface treatment of a kind of rolled copper foil proposed by the present invention, to the basic work of the items of rolled copper foil surface treatment
Skill process is optimized, and entire technique includes cleaning, roughening twice, solidification twice, nickel plating lanthanum alloy, plates tungsten kirsite, is blunt
The processes such as change, drying and silane coupling agent processing, while also to cleaning solution, coarsening solution, solidify liquid, electroplate liquid (nickel lanthanum alloy
Plating solution and tungsten zinc alloy bath) and the optimization that is formulated of the ingredients such as passivating solution, the surface of the rolled copper foil made
Planarization is preferable, and roughness is low；In the present invention, by being roughened twice and curing process twice, copper foil surface can be made to be formed
Well-set roughening knurl, promote its in conjunction with copper foil matrix it is stronger, meanwhile, and due to coat on surfaces of the copper foil
Silane coupling agent can with resin substrate and calendering copper case occur chemical bonding effect, thus further increase rolled copper foil and print
Binding force between making sheet substrate；The Passivation Treatment process of passivating solution can make the surface for prolonging copper foil form one layer of passivating film, both
It can effectively avoid the problem that rolled copper foil changes colour in heat zone compacting, and rolled copper foil and air, moisture can be prevented
It directly contacts and corruption discoloration occurs, to improve its corrosion resistance；Further, since contour containing nickel, tungsten in electroplate liquid
After warm element, these elements coateds and copper foil surface, the heat resistance of rolled copper foil can be made to be greatly improved；It is whole
For, entire technical process does not introduce the harmful elements such as chromium, arsenic, completely environmental protection, meets European Union ROHS regulation；To sum up, lead to
Not only surface roughness is low for obtained rolled copper foil after crossing present invention process processing, but also has excellent heat resistance, corrosion-resistant
Property and higher peel strength, can satisfy industrial requirements at the higher level.
Specific embodiment
Specific embodiments of the present invention will be further explained below.It should be noted that for these implementations
The explanation of mode is used to help understand the present invention, but and does not constitute a limitation of the invention.In addition, invention described below
Technical characteristic involved in each embodiment can be combined with each other as long as they do not conflict with each other.
Embodiment 1:
A kind of process of surface treatment of rolled copper foil, comprising the following steps:
S1, cleaning: rolled copper foil being immersed in cleaning solution and is cleaned, and is cleaned three times after taking-up with 50 DEG C of hot water,
It dries spare；When rolled copper foil has just rolled, surface is more smooth, it is therefore desirable to which the greasy dirt and oxide layer for removing its surface make
Its surface recovery activity, for guarantee rolled copper foil surface clean it is clean, rolled copper foil is immersed in three times in cleaning solution into
Row cleaning, impregnates 1min every time, is both needed to be cleaned with 50 DEG C of hot water three times after impregnating every time；
For the greasy dirt and oxide layer for effectively removing rolled copper foil surface, cleaning solution is optimized in the present embodiment, this is clear
Washing lotion is by following weight percent at being grouped as:
15% neopelex, 10% fatty alcohol polyoxyethylene ether, 8% sulfuric acid, 1% ethyl alcohol, 1% potassium pyrophosphate
With 65% pure water；
Anionic surfactant, nonionic surfactant and sulfuric acid etc. are carried out reasonable compatibility by the cleaning solution, are made
Its greasy dirt and oxide layer that can remove rolled copper foil surface simultaneously, cleaning efficiency are high；
S2, it is roughened for the first time: coarsening solution is added into electroplating rectifier, is 15A/dm in current density2, temperature be 30 DEG C
Under the conditions of to rolled copper foil be electroplated 18S；
Roughening is to improve surface area of the rolled copper foil in conjunction with substrate, in turn to generate copper tumor on rolled copper foil surface
Reinforce the binding force between rolled copper foil and substrate, for the effect for improving roughening, coarsening solution is optimized in the present embodiment, should
Coarsening solution includes 15g/L copper sulphate, 60g/L sulfuric acid, 3g/L iron sulfite and 1g/L nickel sulfate, when configuration, by copper sulphate, sulphur
Acid, iron sulfite and nickel sulfate sequentially add in pure water according to said ratio, and stir and evenly mix；
S3, solidify for the first time: solidify liquid being added into electroplating rectifier, be 15A/dm in current density2, temperature be 45 DEG C
Under the conditions of to rolled copper foil be electroplated 15S；
Solidification plays reinforcement effect to roughening structure, firm foundation is provided for subsequent processing, to improve cured effect
Solidify liquid is optimized in fruit, the present embodiment, which includes 60g/L copper sulphate, 90g/L sulfuric acid and 2g/L lecithin,
When configuration, copper sulphate, sulfuric acid and lecithin are sequentially added in pure water according to said ratio, and is stirred and evenly mixed；
S4, secondary roughening: coarsening solution described in first time roughening step is added into electroplating rectifier, in current density
For 8A/dm2, temperature be 20 DEG C under the conditions of to rolled copper foil be electroplated 10S, it is secondary be roughened improve rolled copper foil roughening effect
Fruit substantially increases its binding force between substrate；
S5, secondary curing: solidify liquid described in first time curing schedule is added into electroplating rectifier, in current density
For 12A/dm2, temperature be 35 DEG C under the conditions of to rolled copper foil be electroplated 10S, secondary curing be for secondary roughening structure carry out
Consolidation process；
S6, nickel plating lanthanum alloy: nickel lanthanum alloy plating solution being added into electroplating rectifier, is 10A/dm in current density2, temperature
50S, nickel and lanthanum are electroplated to rolled copper foil under the conditions of being 50 DEG C and form nickel by the surface that induced codeposition acts on rolled copper foil
Lanthanum alloy refractory layer improves the heat resistance and high temperature peel strength of copper foil；
For the heat resistance for improving copper foil, resistance to hot-dip coating is optimized in the present embodiment, the nickel lanthanum alloy plating solution packet
35g/L nickel sulfamic acid, 20g/L lanthanum chloride, 3g/L urea and 2g/L sodium pyrophosphate are included, when configuration, by nickel sulfamic acid, chlorination
Lanthanum, urea and sodium pyrophosphate sequentially add in pure water according to said ratio, and stir and evenly mix, then with citric acid by the PH of plating solution
It is adjusted to 3；
S7, plating tungsten kirsite: tungsten zinc alloy bath being added into electroplating rectifier, is 5A/dm in current density2, temperature
25S, using sodium tungstate as main salt, salt supplemented by zinc nitrate, in the surface shape of rolled copper foil are electroplated to rolled copper foil under the conditions of being 40 DEG C
At the second refractory layer, i.e. plating tungsten refractory layer, the heat resistance and high temperature peel strength of copper foil are further increased；
For the heat resistance for improving copper foil, the second resistance to hot-dip coating is optimized in the present embodiment, the tungsten kirsite plating
Liquid includes 20g/L sodium tungstate, 10g/L zinc nitrate, 1g/L lauryl sodium sulfate and 2g/L sodium citrate, when configuration, by wolframic acid
Sodium, zinc nitrate, lauryl sodium sulfate and sodium citrate sequentially add in pure water according to said ratio, and stir and evenly mix, then
PH is adjusted to 3 with boric acid solution；
S8, passivation: for the heat resistant coating for removing rolled copper foil excess surface, avoiding its influence to subsequent processing process,
Rolled copper foil after plating tungsten kirsite is immersed in 45 DEG C of warm water before passivation and cleans three times by the present embodiment, then will passivation
Liquid is heated to 40 DEG C, and finally rolled copper foil is immersed in passivating solution and is passivated 35s；
Passivation is to form one layer of fine and close oxidation-resistant film on the surface of rolled copper foil, connects rolled copper foil directly with air
Touching, improves its corrosion resistance, and for the inoxidizability for improving rolled copper foil, passivating solution is optimized in the present embodiment, this is blunt
Changing liquid includes 6g/L titanium trichloride, 8g/L phytic acid, 8mL/L hydrogen peroxide, 10g/L calgon, when configuration, by tri-chlorination
Titanium, phytic acid, hydrogen peroxide and calgon sequentially add in pure water according to said ratio, and stir and evenly mix, and then use nitric acid
The PH of passivating solution is adjusted to 1；
S9, drying: the rolled copper foil after passivation is placed in 50 DEG C of baking ovens and dries 10h；
S10, silane coupling agent processing: first with the silane coupling agent alcoholic solution of dehydrated alcohol configuration 3%, the silane coupling agent
Using silane coupling agent kh550, then the rolling aluminum foil after drying is impregnated in silane coupling agent alcoholic solution, is taken out after 15s,
Solidify 3h under the conditions of finally placing it in 70 DEG C, the facing operation of rolled copper foil can be completed, silane coupling agent handles work
Sequence can be further improved the corrosion resistance of rolled copper foil.
Embodiment 2:
A kind of process of surface treatment of rolled copper foil, comprising the following steps:
S1, cleaning: rolled copper foil being immersed in cleaning solution and is cleaned, and is cleaned three times after taking-up with 65 DEG C of hot water,
It dries spare；When rolled copper foil has just rolled, surface is more smooth, it is therefore desirable to which the greasy dirt and oxide layer for removing its surface make
Its surface recovery activity, for guarantee rolled copper foil surface clean it is clean, rolled copper foil is immersed in three times in cleaning solution into
Row cleaning, impregnates 1.5min every time, is both needed to be cleaned with 65 DEG C of hot water three times after impregnating every time；
For the greasy dirt and oxide layer for effectively removing rolled copper foil surface, cleaning solution is optimized in the present embodiment, this is clear
Washing lotion is by following weight percent at being grouped as:
18% neopelex, 12.5% fatty alcohol polyoxyethylene ether, 10% sulfuric acid, 2% ethyl alcohol, 2% burnt phosphorus
Sour potassium and 55.5% pure water；
Anionic surfactant, nonionic surfactant and sulfuric acid etc. are carried out reasonable compatibility by the cleaning solution, are made
Its greasy dirt and oxide layer that can remove rolled copper foil surface simultaneously, cleaning efficiency are high；
S2, it is roughened for the first time: coarsening solution is added into electroplating rectifier, is 18A/dm in current density2, temperature be 35 DEG C
Under the conditions of to rolled copper foil be electroplated 15S；
Roughening is to improve surface area of the rolled copper foil in conjunction with substrate, in turn to generate copper tumor on rolled copper foil surface
Reinforce the binding force between rolled copper foil and substrate, for the effect for improving roughening, coarsening solution is optimized in the present embodiment, should
Coarsening solution includes 20g/L copper sulphate, 70g/L sulfuric acid, 4g/L iron sulfite and 2g/L nickel sulfate, when configuration, by copper sulphate, sulphur
Acid, iron sulfite and nickel sulfate sequentially add in pure water according to said ratio, and stir and evenly mix；
S3, solidify for the first time: solidify liquid being added into electroplating rectifier, be 18A/dm in current density2, temperature be 50 DEG C
Under the conditions of to rolled copper foil be electroplated 12S；
Solidification plays reinforcement effect to roughening structure, firm foundation is provided for subsequent processing, to improve cured effect
Solidify liquid is optimized in fruit, the present embodiment, which includes 65g/L copper sulphate, 95g/L sulfuric acid and 2.5g/L lecithin
When configuration, copper sulphate, sulfuric acid and lecithin are sequentially added in pure water according to said ratio, and is stirred and evenly mixed for rouge；
S4, secondary roughening: coarsening solution described in first time roughening step is added into electroplating rectifier, in current density
For 10A/dm2, temperature be 25 DEG C under the conditions of to rolled copper foil be electroplated 8.5S, it is secondary be roughened improve rolled copper foil roughening effect
Fruit substantially increases its binding force between substrate；
S5, secondary curing: solidify liquid described in first time curing schedule is added into electroplating rectifier, in current density
For 13.5A/dm2, temperature be 38 DEG C under the conditions of to rolled copper foil be electroplated 7.5S, secondary curing be for secondary roughening structure into
Row consolidation process；
S6, nickel plating lanthanum alloy: nickel lanthanum alloy plating solution being added into electroplating rectifier, is 15A/dm in current density2, temperature
40S, nickel and lanthanum are electroplated to rolled copper foil under the conditions of being 58 DEG C and form nickel by the surface that induced codeposition acts on rolled copper foil
Lanthanum alloy refractory layer improves the heat resistance and high temperature peel strength of copper foil；
For the heat resistance for improving copper foil, resistance to hot-dip coating is optimized in the present embodiment, the nickel lanthanum alloy plating solution packet
40g/L nickel sulfamic acid, 25g/L lanthanum chloride, 4g/L urea and 2.5g/L sodium pyrophosphate are included, when configuration, by nickel sulfamic acid, chlorine
Change lanthanum, urea and sodium pyrophosphate sequentially add in pure water according to said ratio, and stir and evenly mix, then with citric acid by plating solution
PH is adjusted to 4.5；
S7, plating tungsten kirsite: tungsten zinc alloy bath being added into electroplating rectifier, is 8A/dm in current density2, temperature
20S, using sodium tungstate as main salt, salt supplemented by zinc nitrate, in the surface shape of rolled copper foil are electroplated to rolled copper foil under the conditions of being 45 DEG C
At the second refractory layer, i.e. plating tungsten refractory layer, the heat resistance and high temperature peel strength of copper foil are further increased；
For the heat resistance for improving copper foil, the second resistance to hot-dip coating is optimized in the present embodiment, the tungsten kirsite plating
Liquid includes 25g/L sodium tungstate, 12.5g/L zinc nitrate, 1.5g/L lauryl sodium sulfate and 2.5g/L sodium citrate, when configuration,
Sodium tungstate, zinc nitrate, lauryl sodium sulfate and sodium citrate are sequentially added in pure water according to said ratio, and stirred mixed
It is even, PH is then adjusted to 4 with boric acid solution；
S8, passivation: for the heat resistant coating for removing rolled copper foil excess surface, avoiding its influence to subsequent processing process,
Rolled copper foil after plating tungsten kirsite is immersed in 50 DEG C of warm water before passivation and cleans three times by the present embodiment, then will passivation
Liquid is heated to 45 DEG C, and finally rolled copper foil is immersed in passivating solution and is passivated 30s；
Passivation is to form one layer of fine and close oxidation-resistant film on the surface of rolled copper foil, connects rolled copper foil directly with air
Touching, improves its corrosion resistance, and for the inoxidizability for improving rolled copper foil, passivating solution is optimized in the present embodiment, this is blunt
Changing liquid includes 8g/L titanium trichloride, 10g/L phytic acid, 12mL/L hydrogen peroxide, 14g/L calgon, when configuration, by tri-chlorination
Titanium, phytic acid, hydrogen peroxide and calgon sequentially add in pure water according to said ratio, and stir and evenly mix, and then use nitric acid
The PH of passivating solution is adjusted to 2；
S9, drying: the rolled copper foil after passivation is placed in 55 DEG C of baking ovens and dries 9h；
S10, silane coupling agent processing: first with the silane coupling agent alcoholic solution of dehydrated alcohol configuration 4%, the silane coupling agent
Using silane coupling agent kh550, then the rolling aluminum foil after drying is impregnated in silane coupling agent alcoholic solution, is taken out after 12s,
Solidify 2h under the conditions of finally placing it in 75 DEG C, the facing operation of rolled copper foil can be completed, silane coupling agent handles work
Sequence can be further improved the corrosion resistance of rolled copper foil.
Embodiment 3:
A kind of process of surface treatment of rolled copper foil, comprising the following steps:
S1, cleaning: rolled copper foil being immersed in cleaning solution and is cleaned, and is cleaned three times after taking-up with 80 DEG C of hot water,
It dries spare；When rolled copper foil has just rolled, surface is more smooth, it is therefore desirable to which the greasy dirt and oxide layer for removing its surface make
Its surface recovery activity, for guarantee rolled copper foil surface clean it is clean, rolled copper foil is immersed in three times in cleaning solution into
Row cleaning, impregnates 2min every time, is both needed to be cleaned with 80 DEG C of hot water three times after impregnating every time；
For the greasy dirt and oxide layer for effectively removing rolled copper foil surface, cleaning solution is optimized in the present embodiment, this is clear
Washing lotion is by following weight percent at being grouped as:
20% neopelex, 15% fatty alcohol polyoxyethylene ether, 12% sulfuric acid, 3% ethyl alcohol, 3% pyrophosphoric acid
Potassium and 47% pure water；
Anionic surfactant, nonionic surfactant and sulfuric acid etc. are carried out reasonable compatibility by the cleaning solution, are made
Its greasy dirt and oxide layer that can remove rolled copper foil surface simultaneously, cleaning efficiency are high；
S2, it is roughened for the first time: coarsening solution is added into electroplating rectifier, is 20A/dm in current density2, temperature be 40 DEG C
Under the conditions of to rolled copper foil be electroplated 12S；
Roughening is to improve surface area of the rolled copper foil in conjunction with substrate, in turn to generate copper tumor on rolled copper foil surface
Reinforce the binding force between rolled copper foil and substrate, for the effect for improving roughening, coarsening solution is optimized in the present embodiment, should
Coarsening solution includes 25g/L copper sulphate, 80g/L sulfuric acid, 5g/L iron sulfite and 3g/L nickel sulfate, when configuration, by copper sulphate, sulphur
Acid, iron sulfite and nickel sulfate sequentially add in pure water according to said ratio, and stir and evenly mix；
S3, solidify for the first time: solidify liquid being added into electroplating rectifier, be 20A/dm in current density2, temperature be 55 DEG C
Under the conditions of to rolled copper foil be electroplated 8S；
Solidification plays reinforcement effect to roughening structure, firm foundation is provided for subsequent processing, to improve cured effect
Solidify liquid is optimized in fruit, the present embodiment, which includes 70g/L copper sulphate, 100g/L sulfuric acid and 3g/L lecithin,
When configuration, copper sulphate, sulfuric acid and lecithin are sequentially added in pure water according to said ratio, and is stirred and evenly mixed；
S4, secondary roughening: coarsening solution described in first time roughening step is added into electroplating rectifier, in current density
For 12A/dm2, temperature be 30 DEG C under the conditions of to rolled copper foil be electroplated 7S, it is secondary be roughened improve rolled copper foil roughening effect
Fruit substantially increases its binding force between substrate；
S5, secondary curing: solidify liquid described in first time curing schedule is added into electroplating rectifier, in current density
For 15A/dm2, temperature 5S is electroplated to rolled copper foil under the conditions of being 40 DEG C, secondary curing is added for the structure of secondary roughening
Gu processing；
S6, nickel plating lanthanum alloy: nickel lanthanum alloy plating solution being added into electroplating rectifier, is 20A/dm in current density2, temperature
30S, nickel and lanthanum are electroplated to rolled copper foil under the conditions of being 65 DEG C and form nickel by the surface that induced codeposition acts on rolled copper foil
Lanthanum alloy refractory layer improves the heat resistance and high temperature peel strength of copper foil；
For the heat resistance for improving copper foil, resistance to hot-dip coating is optimized in the present embodiment, the nickel lanthanum alloy plating solution packet
45g/L nickel sulfamic acid, 30g/L lanthanum chloride, 5g/L urea and 3g/L sodium pyrophosphate are included, when configuration, by nickel sulfamic acid, chlorination
Lanthanum, urea and sodium pyrophosphate sequentially add in pure water according to said ratio, and stir and evenly mix, then with citric acid by the PH of plating solution
It is adjusted to 6；
S7, plating tungsten kirsite: tungsten zinc alloy bath being added into electroplating rectifier, is 10A/dm in current density2, temperature
25S, using sodium tungstate as main salt, salt supplemented by zinc nitrate, in the surface shape of rolled copper foil are electroplated to rolled copper foil under the conditions of being 50 DEG C
At the second refractory layer, i.e. plating tungsten refractory layer, the heat resistance and high temperature peel strength of copper foil are further increased；
For the heat resistance for improving copper foil, the second resistance to hot-dip coating is optimized in the present embodiment, the tungsten kirsite plating
Liquid includes 30g/L sodium tungstate, 15g/L zinc nitrate, 2g/L lauryl sodium sulfate and 3g/L sodium citrate, when configuration, by wolframic acid
Sodium, zinc nitrate, lauryl sodium sulfate and sodium citrate sequentially add in pure water according to said ratio, and stir and evenly mix, then
PH is adjusted to 5 with boric acid solution；
S8, passivation: for the heat resistant coating for removing rolled copper foil excess surface, avoiding its influence to subsequent processing process,
Rolled copper foil after plating tungsten kirsite is immersed in 55 DEG C of warm water before passivation and cleans three times by the present embodiment, then will passivation
Liquid is heated to 50 DEG C, and finally rolled copper foil is immersed in passivating solution and is passivated 25s；
Passivation is to form one layer of fine and close oxidation-resistant film on the surface of rolled copper foil, connects rolled copper foil directly with air
Touching, improves its corrosion resistance, and for the inoxidizability for improving rolled copper foil, passivating solution is optimized in the present embodiment, this is blunt
Changing liquid includes 10g/L titanium trichloride, 12g/L phytic acid, 15mL/L hydrogen peroxide, 18g/L calgon, when configuration, by trichlorine
Change titanium, phytic acid, hydrogen peroxide and calgon to sequentially add in pure water according to said ratio, and stir and evenly mix, then uses nitre
The PH of passivating solution is adjusted to 3 by acid；
S9, drying: the rolled copper foil after passivation is placed in 60 DEG C of baking ovens and dries 8h；
S10, silane coupling agent processing: first with the silane coupling agent alcoholic solution of dehydrated alcohol configuration 5%, the silane coupling agent
Using silane coupling agent kh550, then the rolling aluminum foil after drying is impregnated in silane coupling agent alcoholic solution, is taken out after 10s,
Solidify 1h under the conditions of finally placing it in 80 DEG C, the facing operation of rolled copper foil can be completed, silane coupling agent handles work
Sequence can be further improved the corrosion resistance of rolled copper foil.
Embodiment 4:
A kind of process of surface treatment of rolled copper foil, comprising the following steps:
S1, cleaning: rolled copper foil being immersed in cleaning solution and is cleaned, and is cleaned three times after taking-up with 65 DEG C of hot water,
It dries spare；When rolled copper foil has just rolled, surface is more smooth, it is therefore desirable to which the greasy dirt and oxide layer for removing its surface make
Its surface recovery activity, for guarantee rolled copper foil surface clean it is clean, rolled copper foil is immersed in three times in cleaning solution into
Row cleaning, impregnates 1.5min every time, is both needed to be cleaned with 65 DEG C of hot water three times after impregnating every time；
For the greasy dirt and oxide layer for effectively removing rolled copper foil surface, cleaning solution is optimized in the present embodiment, this is clear
Washing lotion is by following weight percent at being grouped as:
18% odium stearate, 12.5% cocoanut fatty acid diethanolamide, 10% sulfuric acid, 2% isopropanol, 2% nitrous
Sour sodium and 55.5% pure water；
Anionic surfactant, nonionic surfactant and sulfuric acid etc. are carried out reasonable compatibility by the cleaning solution, are made
Its greasy dirt and oxide layer that can remove rolled copper foil surface simultaneously, cleaning efficiency are high；
S2, it is roughened for the first time: coarsening solution is added into electroplating rectifier, is 18A/dm in current density2, temperature be 35 DEG C
Under the conditions of to rolled copper foil be electroplated 15S；
Roughening is to improve surface area of the rolled copper foil in conjunction with substrate, in turn to generate copper tumor on rolled copper foil surface
Reinforce the binding force between rolled copper foil and substrate, for the effect for improving roughening, coarsening solution is optimized in the present embodiment, should
Coarsening solution includes 20g/L copper sulphate, 70g/L sulfuric acid, 4g/L iron sulfite and 2g/L nickel sulfate, when configuration, by copper sulphate, sulphur
Acid, iron sulfite and nickel sulfate sequentially add in pure water according to said ratio, and stir and evenly mix；
S3, solidify for the first time: solidify liquid being added into electroplating rectifier, be 18A/dm in current density2, temperature be 50 DEG C
Under the conditions of to rolled copper foil be electroplated 12S；
Solidification plays reinforcement effect to roughening structure, firm foundation is provided for subsequent processing, to improve cured effect
Solidify liquid is optimized in fruit, the present embodiment, which includes 65g/L copper sulphate, 95g/L sulfuric acid and 2.5g/L lecithin
When configuration, copper sulphate, sulfuric acid and lecithin are sequentially added in pure water according to said ratio, and is stirred and evenly mixed for rouge；
S4, secondary roughening: coarsening solution described in first time roughening step is added into electroplating rectifier, in current density
For 10A/dm2, temperature be 25 DEG C under the conditions of to rolled copper foil be electroplated 8.5S, it is secondary be roughened improve rolled copper foil roughening effect
Fruit substantially increases its binding force between substrate；
S5, secondary curing: solidify liquid described in first time curing schedule is added into electroplating rectifier, in current density
For 13.5A/dm2, temperature be 38 DEG C under the conditions of to rolled copper foil be electroplated 7.5S, secondary curing be for secondary roughening structure into
Row consolidation process；
S6, nickel plating lanthanum alloy: nickel lanthanum alloy plating solution being added into electroplating rectifier, is 15A/dm in current density2, temperature
40S, nickel and lanthanum are electroplated to rolled copper foil under the conditions of being 58 DEG C and form nickel by the surface that induced codeposition acts on rolled copper foil
Lanthanum alloy refractory layer improves the heat resistance and high temperature peel strength of copper foil；
For the heat resistance for improving copper foil, resistance to hot-dip coating is optimized in the present embodiment, the nickel lanthanum alloy plating solution packet
40g/L nickel sulfamic acid, 25g/L lanthanum chloride, 4g/L urea and 2.5g/L sodium pyrophosphate are included, when configuration, by nickel sulfamic acid, chlorine
Change lanthanum, urea and sodium pyrophosphate sequentially add in pure water according to said ratio, and stir and evenly mix, then with citric acid by plating solution
PH is adjusted to 4.5；
S7, plating tungsten kirsite: tungsten zinc alloy bath being added into electroplating rectifier, is 8A/dm in current density2, temperature
20S, using sodium tungstate as main salt, salt supplemented by zinc nitrate, in the surface shape of rolled copper foil are electroplated to rolled copper foil under the conditions of being 45 DEG C
At the second refractory layer, i.e. plating tungsten refractory layer, the heat resistance and high temperature peel strength of copper foil are further increased；
For the heat resistance for improving copper foil, the second resistance to hot-dip coating is optimized in the present embodiment, the tungsten kirsite plating
Liquid includes 25g/L sodium tungstate, 12.5g/L zinc nitrate, 1.5g/L lauryl sodium sulfate and 2.5g/L sodium citrate, when configuration,
Sodium tungstate, zinc nitrate, lauryl sodium sulfate and sodium citrate are sequentially added in pure water according to said ratio, and stirred mixed
It is even, PH is then adjusted to 4 with boric acid solution；
S8, passivation: for the heat resistant coating for removing rolled copper foil excess surface, avoiding its influence to subsequent processing process,
Rolled copper foil after plating tungsten kirsite is immersed in 50 DEG C of warm water before passivation and cleans three times by the present embodiment, then will passivation
Liquid is heated to 45 DEG C, and finally rolled copper foil is immersed in passivating solution and is passivated 30s；
Passivation is to form one layer of fine and close oxidation-resistant film on the surface of rolled copper foil, connects rolled copper foil directly with air
Touching, improves its corrosion resistance, and for the inoxidizability for improving rolled copper foil, passivating solution is optimized in the present embodiment, this is blunt
Changing liquid includes 8g/L titanium trichloride, 10g/L phytic acid, 12mL/L hydrogen peroxide, 14g/L calgon, when configuration, by tri-chlorination
Titanium, phytic acid, hydrogen peroxide and calgon sequentially add in pure water according to said ratio, and stir and evenly mix, and then use nitric acid
The PH of passivating solution is adjusted to 2；
S9, drying: the rolled copper foil after passivation is placed in 55 DEG C of baking ovens and dries 9h；
S10, silane coupling agent processing: first with the silane coupling agent alcoholic solution of dehydrated alcohol configuration 4%, the silane coupling agent
Using silane coupling agent kh550, then the rolling aluminum foil after drying is impregnated in silane coupling agent alcoholic solution, is taken out after 12s,
Solidify 2h under the conditions of finally placing it in 75 DEG C, the facing operation of rolled copper foil can be completed, silane coupling agent handles work
Sequence can be further improved the corrosion resistance of rolled copper foil.
Embodiment 5:
A kind of process of surface treatment of rolled copper foil, comprising the following steps:
S1, cleaning: rolled copper foil being immersed in cleaning solution and is cleaned, and is cleaned three times after taking-up with 65 DEG C of hot water,
It dries spare；When rolled copper foil has just rolled, surface is more smooth, it is therefore desirable to which the greasy dirt and oxide layer for removing its surface make
Its surface recovery activity, for guarantee rolled copper foil surface clean it is clean, rolled copper foil is immersed in three times in cleaning solution into
Row cleaning, impregnates 1.5min every time, is both needed to be cleaned with 65 DEG C of hot water three times after impregnating every time；
For the greasy dirt and oxide layer for effectively removing rolled copper foil surface, cleaning solution is optimized in the present embodiment, this is clear
Washing lotion is by following weight percent at being grouped as:
18% laruyl alcohol, 12.5% alkyl phenol polyoxyethylene ether, 10% sulfuric acid, 2% butanol, 2% sodium benzoate and
55.5% pure water；
Anionic surfactant, nonionic surfactant and sulfuric acid etc. are carried out reasonable compatibility by the cleaning solution, are made
Its greasy dirt and oxide layer that can remove rolled copper foil surface simultaneously, cleaning efficiency are high；
S2, it is roughened for the first time: coarsening solution is added into electroplating rectifier, is 18A/dm in current density2, temperature be 35 DEG C
Under the conditions of to rolled copper foil be electroplated 15S；
Roughening is to improve surface area of the rolled copper foil in conjunction with substrate, in turn to generate copper tumor on rolled copper foil surface
Reinforce the binding force between rolled copper foil and substrate, for the effect for improving roughening, coarsening solution is optimized in the present embodiment, should
Coarsening solution includes 20g/L copper sulphate, 70g/L sulfuric acid, 4g/L iron sulfite and 2g/L nickel sulfate, when configuration, by copper sulphate, sulphur
Acid, iron sulfite and nickel sulfate sequentially add in pure water according to said ratio, and stir and evenly mix；
S3, solidify for the first time: solidify liquid being added into electroplating rectifier, be 18A/dm in current density2, temperature be 50 DEG C
Under the conditions of to rolled copper foil be electroplated 12S；
Solidification plays reinforcement effect to roughening structure, firm foundation is provided for subsequent processing, to improve cured effect
Solidify liquid is optimized in fruit, the present embodiment, which includes 65g/L copper sulphate, 95g/L sulfuric acid and 2.5g/L lecithin
When configuration, copper sulphate, sulfuric acid and lecithin are sequentially added in pure water according to said ratio, and is stirred and evenly mixed for rouge；
S4, secondary roughening: coarsening solution described in first time roughening step is added into electroplating rectifier, in current density
For 10A/dm2, temperature be 25 DEG C under the conditions of to rolled copper foil be electroplated 8.5S, it is secondary be roughened improve rolled copper foil roughening effect
Fruit substantially increases its binding force between substrate；
S5, secondary curing: solidify liquid described in first time curing schedule is added into electroplating rectifier, in current density
For 13.5A/dm2, temperature be 38 DEG C under the conditions of to rolled copper foil be electroplated 7.5S, secondary curing be for secondary roughening structure into
Row consolidation process；
S6, nickel plating lanthanum alloy: nickel lanthanum alloy plating solution being added into electroplating rectifier, is 15A/dm in current density2, temperature
40S, nickel and lanthanum are electroplated to rolled copper foil under the conditions of being 58 DEG C and form nickel by the surface that induced codeposition acts on rolled copper foil
Lanthanum alloy refractory layer improves the heat resistance and high temperature peel strength of copper foil；
For the heat resistance for improving copper foil, resistance to hot-dip coating is optimized in the present embodiment, the nickel lanthanum alloy plating solution packet
40g/L nickel sulfamic acid, 25g/L lanthanum chloride, 4g/L urea and 2.5g/L sodium pyrophosphate are included, when configuration, by nickel sulfamic acid, chlorine
Change lanthanum, urea and sodium pyrophosphate sequentially add in pure water according to said ratio, and stir and evenly mix, then with citric acid by plating solution
PH is adjusted to 4.5；
S7, plating tungsten kirsite: tungsten zinc alloy bath being added into electroplating rectifier, is 8A/dm in current density2, temperature
20S, using sodium tungstate as main salt, salt supplemented by zinc nitrate, in the surface shape of rolled copper foil are electroplated to rolled copper foil under the conditions of being 45 DEG C
At the second refractory layer, i.e. plating tungsten refractory layer, the heat resistance and high temperature peel strength of copper foil are further increased；
For the heat resistance for improving copper foil, the second resistance to hot-dip coating is optimized in the present embodiment, the tungsten kirsite plating
Liquid includes 25g/L sodium tungstate, 12.5g/L zinc nitrate, 1.5g/L lauryl sodium sulfate and 2.5g/L sodium citrate, when configuration,
Sodium tungstate, zinc nitrate, lauryl sodium sulfate and sodium citrate are sequentially added in pure water according to said ratio, and stirred mixed
It is even, PH is then adjusted to 4 with boric acid solution；
S8, passivation: for the heat resistant coating for removing rolled copper foil excess surface, avoiding its influence to subsequent processing process,
Rolled copper foil after plating tungsten kirsite is immersed in 50 DEG C of warm water before passivation and cleans three times by the present embodiment, then will passivation
Liquid is heated to 45 DEG C, and finally rolled copper foil is immersed in passivating solution and is passivated 30s；
Passivation is to form one layer of fine and close oxidation-resistant film on the surface of rolled copper foil, connects rolled copper foil directly with air
Touching, improves its corrosion resistance, and for the inoxidizability for improving rolled copper foil, passivating solution is optimized in the present embodiment, this is blunt
Changing liquid includes 8g/L titanium trichloride, 10g/L phytic acid, 12mL/L hydrogen peroxide, 14g/L calgon, when configuration, by tri-chlorination
Titanium, phytic acid, hydrogen peroxide and calgon sequentially add in pure water according to said ratio, and stir and evenly mix, and then use nitric acid
The PH of passivating solution is adjusted to 2；
S9, drying: the rolled copper foil after passivation is placed in 55 DEG C of baking ovens and dries 9h；
S10, silane coupling agent processing: first with the silane coupling agent alcoholic solution of dehydrated alcohol configuration 4%, the silane coupling agent
Using silane coupling agent kh550, then the rolling aluminum foil after drying is impregnated in silane coupling agent alcoholic solution, is taken out after 12s,
Solidify 2h under the conditions of finally placing it in 75 DEG C, the facing operation of rolled copper foil can be completed, silane coupling agent handles work
Sequence can be further improved the corrosion resistance of rolled copper foil.
Embodiment 6:
A kind of process of surface treatment of rolled copper foil, comprising the following steps:
S1, cleaning: rolled copper foil being immersed in cleaning solution and is cleaned, and is cleaned three times after taking-up with 65 DEG C of hot water,
It dries spare；When rolled copper foil has just rolled, surface is more smooth, it is therefore desirable to which the greasy dirt and oxide layer for removing its surface make
Its surface recovery activity, for guarantee rolled copper foil surface clean it is clean, rolled copper foil is immersed in three times in cleaning solution into
Row cleaning, impregnates 1.5min every time, is both needed to be cleaned with 65 DEG C of hot water three times after impregnating every time；
For the greasy dirt and oxide layer for effectively removing rolled copper foil surface, cleaning solution is optimized in the present embodiment, this is clear
Washing lotion is by following weight percent at being grouped as:
18% vinethene, 12.5% polyoxyethylene carboxylate, 10% sulfuric acid, 2% ethyl alcohol, 2% sodium sulphate and 55.5%
Pure water；
Anionic surfactant, nonionic surfactant and sulfuric acid etc. are carried out reasonable compatibility by the cleaning solution, are made
Its greasy dirt and oxide layer that can remove rolled copper foil surface simultaneously, cleaning efficiency are high；
S2, it is roughened for the first time: coarsening solution is added into electroplating rectifier, is 18A/dm in current density2, temperature be 35 DEG C
Under the conditions of to rolled copper foil be electroplated 15S；
Roughening is to improve surface area of the rolled copper foil in conjunction with substrate, in turn to generate copper tumor on rolled copper foil surface
Reinforce the binding force between rolled copper foil and substrate, for the effect for improving roughening, coarsening solution is optimized in the present embodiment, should
Coarsening solution includes 20g/L copper sulphate, 70g/L sulfuric acid, 4g/L iron sulfite and 2g/L nickel sulfate, when configuration, by copper sulphate, sulphur
Acid, iron sulfite and nickel sulfate sequentially add in pure water according to said ratio, and stir and evenly mix；
S3, solidify for the first time: solidify liquid being added into electroplating rectifier, be 18A/dm in current density2, temperature be 50 DEG C
Under the conditions of to rolled copper foil be electroplated 12S；
Solidification plays reinforcement effect to roughening structure, firm foundation is provided for subsequent processing, to improve cured effect
Solidify liquid is optimized in fruit, the present embodiment, which includes 65g/L copper sulphate, 95g/L sulfuric acid and 2.5g/L lecithin
When configuration, copper sulphate, sulfuric acid and lecithin are sequentially added in pure water according to said ratio, and is stirred and evenly mixed for rouge；
S4, secondary roughening: coarsening solution described in first time roughening step is added into electroplating rectifier, in current density
For 10A/dm2, temperature be 25 DEG C under the conditions of to rolled copper foil be electroplated 8.5S, it is secondary be roughened improve rolled copper foil roughening effect
Fruit substantially increases its binding force between substrate；
S5, secondary curing: solidify liquid described in first time curing schedule is added into electroplating rectifier, in current density
For 13.5A/dm2, temperature be 38 DEG C under the conditions of to rolled copper foil be electroplated 7.5S, secondary curing be for secondary roughening structure into
Row consolidation process；
S6, nickel plating lanthanum alloy: nickel lanthanum alloy plating solution being added into electroplating rectifier, is 15A/dm in current density2, temperature
40S, nickel and lanthanum are electroplated to rolled copper foil under the conditions of being 58 DEG C and form nickel by the surface that induced codeposition acts on rolled copper foil
Lanthanum alloy refractory layer improves the heat resistance and high temperature peel strength of copper foil；
For the heat resistance for improving copper foil, resistance to hot-dip coating is optimized in the present embodiment, the nickel lanthanum alloy plating solution packet
40g/L nickel sulfamic acid, 25g/L lanthanum chloride, 4g/L urea and 2.5g/L sodium pyrophosphate are included, when configuration, by nickel sulfamic acid, chlorine
Change lanthanum, urea and sodium pyrophosphate sequentially add in pure water according to said ratio, and stir and evenly mix, then with citric acid by plating solution
PH is adjusted to 4.5；
S7, plating tungsten kirsite: tungsten zinc alloy bath being added into electroplating rectifier, is 8A/dm in current density2, temperature
20S, using sodium tungstate as main salt, salt supplemented by zinc nitrate, in the surface shape of rolled copper foil are electroplated to rolled copper foil under the conditions of being 45 DEG C
At the second refractory layer, i.e. plating tungsten refractory layer, the heat resistance and high temperature peel strength of copper foil are further increased；
For the heat resistance for improving copper foil, the second resistance to hot-dip coating is optimized in the present embodiment, the tungsten kirsite plating
Liquid includes 25g/L sodium tungstate, 12.5g/L zinc nitrate, 1.5g/L lauryl sodium sulfate and 2.5g/L sodium citrate, when configuration,
Sodium tungstate, zinc nitrate, lauryl sodium sulfate and sodium citrate are sequentially added in pure water according to said ratio, and stirred mixed
It is even, PH is then adjusted to 4 with boric acid solution；
S8, passivation: for the heat resistant coating for removing rolled copper foil excess surface, avoiding its influence to subsequent processing process,
Rolled copper foil after plating tungsten kirsite is immersed in 50 DEG C of warm water before passivation and cleans three times by the present embodiment, then will passivation
Liquid is heated to 45 DEG C, and finally rolled copper foil is immersed in passivating solution and is passivated 30s；
Passivation is to form one layer of fine and close oxidation-resistant film on the surface of rolled copper foil, connects rolled copper foil directly with air
Touching, improves its corrosion resistance, and for the inoxidizability for improving rolled copper foil, passivating solution is optimized in the present embodiment, this is blunt
Changing liquid includes 8g/L titanium trichloride, 10g/L phytic acid, 12mL/L hydrogen peroxide, 14g/L calgon, when configuration, by tri-chlorination
Titanium, phytic acid, hydrogen peroxide and calgon sequentially add in pure water according to said ratio, and stir and evenly mix, and then use nitric acid
The PH of passivating solution is adjusted to 2；
S9, drying: the rolled copper foil after passivation is placed in 55 DEG C of baking ovens and dries 9h；
S10, silane coupling agent processing: first with the silane coupling agent alcoholic solution of dehydrated alcohol configuration 4%, the silane coupling agent
Using silane coupling agent kh550, then the rolling aluminum foil after drying is impregnated in silane coupling agent alcoholic solution, is taken out after 12s,
Solidify 2h under the conditions of finally placing it in 75 DEG C, the facing operation of rolled copper foil can be completed, silane coupling agent handles work
Sequence can be further improved the corrosion resistance of rolled copper foil.
Embodiment 7:
A kind of process of surface treatment of rolled copper foil, comprising the following steps:
S1, cleaning: rolled copper foil being immersed in cleaning solution and is cleaned, and is cleaned three times after taking-up with 65 DEG C of hot water,
It dries spare；When rolled copper foil has just rolled, surface is more smooth, it is therefore desirable to which the greasy dirt and oxide layer for removing its surface make
Its surface recovery activity, for guarantee rolled copper foil surface clean it is clean, rolled copper foil is immersed in three times in cleaning solution into
Row cleaning, impregnates 1.5min every time, is both needed to be cleaned with 65 DEG C of hot water three times after impregnating every time；
For the greasy dirt and oxide layer for effectively removing rolled copper foil surface, cleaning solution is optimized in the present embodiment, this is clear
Washing lotion is by following weight percent at being grouped as:
18% glyceride, 12.5% fatty alcohol polyoxyethylene ether, 10% sulfuric acid, 2% ethyl alcohol, 2% potassium pyrophosphate and
55.5% pure water；
Anionic surfactant, nonionic surfactant and sulfuric acid etc. are carried out reasonable compatibility by the cleaning solution, are made
Its greasy dirt and oxide layer that can remove rolled copper foil surface simultaneously, cleaning efficiency are high；
S2, it is roughened for the first time: coarsening solution is added into electroplating rectifier, is 18A/dm in current density2, temperature be 35 DEG C
Under the conditions of to rolled copper foil be electroplated 15S；
Roughening is to improve surface area of the rolled copper foil in conjunction with substrate, in turn to generate copper tumor on rolled copper foil surface
Reinforce the binding force between rolled copper foil and substrate, for the effect for improving roughening, coarsening solution is optimized in the present embodiment, should
Coarsening solution includes 20g/L copper sulphate, 70g/L sulfuric acid, 4g/L iron sulfite and 2g/L nickel sulfate, when configuration, by copper sulphate, sulphur
Acid, iron sulfite and nickel sulfate sequentially add in pure water according to said ratio, and stir and evenly mix；
S3, solidify for the first time: solidify liquid being added into electroplating rectifier, be 18A/dm in current density2, temperature be 50 DEG C
Under the conditions of to rolled copper foil be electroplated 12S；
Solidification plays reinforcement effect to roughening structure, firm foundation is provided for subsequent processing, to improve cured effect
Solidify liquid is optimized in fruit, the present embodiment, which includes 65g/L copper sulphate, 95g/L sulfuric acid and 2.5g/L lecithin
When configuration, copper sulphate, sulfuric acid and lecithin are sequentially added in pure water according to said ratio, and is stirred and evenly mixed for rouge；
S4, secondary roughening: coarsening solution described in first time roughening step is added into electroplating rectifier, in current density
For 10A/dm2, temperature be 25 DEG C under the conditions of to rolled copper foil be electroplated 8.5S, it is secondary be roughened improve rolled copper foil roughening effect
Fruit substantially increases its binding force between substrate；
S5, secondary curing: solidify liquid described in first time curing schedule is added into electroplating rectifier, in current density
For 13.5A/dm2, temperature be 38 DEG C under the conditions of to rolled copper foil be electroplated 7.5S, secondary curing be for secondary roughening structure into
Row consolidation process；
S6, nickel plating lanthanum alloy: nickel lanthanum alloy plating solution being added into electroplating rectifier, is 15A/dm in current density2, temperature
40S, nickel and lanthanum are electroplated to rolled copper foil under the conditions of being 58 DEG C and form nickel by the surface that induced codeposition acts on rolled copper foil
Lanthanum alloy refractory layer improves the heat resistance and high temperature peel strength of copper foil；
For the heat resistance for improving copper foil, resistance to hot-dip coating is optimized in the present embodiment, the nickel lanthanum alloy plating solution packet
40g/L nickel sulfamic acid, 25g/L lanthanum chloride, 4g/L urea and 2.5g/L sodium pyrophosphate are included, when configuration, by nickel sulfamic acid, chlorine
Change lanthanum, urea and sodium pyrophosphate sequentially add in pure water according to said ratio, and stir and evenly mix, then with citric acid by plating solution
PH is adjusted to 4.5；
S7, plating tungsten kirsite: tungsten zinc alloy bath being added into electroplating rectifier, is 8A/dm in current density2, temperature
20S, using sodium tungstate as main salt, salt supplemented by zinc nitrate, in the surface shape of rolled copper foil are electroplated to rolled copper foil under the conditions of being 45 DEG C
At the second refractory layer, i.e. plating tungsten refractory layer, the heat resistance and high temperature peel strength of copper foil are further increased；
For the heat resistance for improving copper foil, the second resistance to hot-dip coating is optimized in the present embodiment, the tungsten kirsite plating
Liquid includes 25g/L sodium tungstate, 12.5g/L zinc nitrate, 1.5g/L lauryl sodium sulfate and 2.5g/L sodium citrate, when configuration,
Sodium tungstate, zinc nitrate, lauryl sodium sulfate and sodium citrate are sequentially added in pure water according to said ratio, and stirred mixed
It is even, PH is then adjusted to 4 with boric acid solution；
S8, passivation: for the heat resistant coating for removing rolled copper foil excess surface, avoiding its influence to subsequent processing process,
Rolled copper foil after plating tungsten kirsite is immersed in 50 DEG C of warm water before passivation and cleans three times by the present embodiment, then will passivation
Liquid is heated to 45 DEG C, and finally rolled copper foil is immersed in passivating solution and is passivated 30s；
Passivation is to form one layer of fine and close oxidation-resistant film on the surface of rolled copper foil, connects rolled copper foil directly with air
Touching, improves its corrosion resistance, and for the inoxidizability for improving rolled copper foil, passivating solution is optimized in the present embodiment, this is blunt
Changing liquid includes 8g/L titanium trichloride, 10g/L phytic acid, 12mL/L hydrogen peroxide, 14g/L calgon, when configuration, by tri-chlorination
Titanium, phytic acid, hydrogen peroxide and calgon sequentially add in pure water according to said ratio, and stir and evenly mix, and then use nitric acid
The PH of passivating solution is adjusted to 2；
S9, drying: the rolled copper foil after passivation is placed in 55 DEG C of baking ovens and dries 9h；
S10, silane coupling agent processing: first with the silane coupling agent alcoholic solution of dehydrated alcohol configuration 4%, the silane coupling agent
Using silane coupling agent kh550, then the rolling aluminum foil after drying is impregnated in silane coupling agent alcoholic solution, is taken out after 12s,
Solidify 2h under the conditions of finally placing it in 75 DEG C, the facing operation of rolled copper foil can be completed, silane coupling agent handles work
Sequence can be further improved the corrosion resistance of rolled copper foil.
Comparative example:
Comparative example is common rolled copper foil process of surface treatment, specific as follows:
(1), oil removing: rolled copper foil is immersed in 3min in 15% sodium hydroxide solution, is then cleaned three times with clear water；
(2), pickling: rolled copper foil is immersed in 3min in 10% sulfuric acid solution, is then cleaned three times with clear water；
(3), it is roughened: coarsening solution is added into electroplating bath, is 40A/dm in current density2, temperature be 30 DEG C under the conditions of it is right
5S is electroplated in rolled copper foil；
The coarsening solution includes 30g/L copper sulphate, 90g/L sulfuric acid, 4g/L gelatin and 1g/L GaAs；
(4), solidify: coarsening solution being added into electroplating bath, be 30A/dm in current density2, temperature be 50 DEG C under the conditions of it is right
8S is electroplated in rolled copper foil；
The solidify liquid includes 60g/L copper sulphate and 105g/L sulfuric acid；
(5), zinc-nickel alloy: admiro plating solution being added into electroplating bath, is 20A/dm in current density2, temperature be
45S is electroplated to rolled copper foil under the conditions of 50 DEG C；
The admiro plating solution includes zinc sulfate 60g/L, nickel sulfate 40g/L, sodium acetate 40g/L and sodium sulphate 40g/L, is used
The PH of plating solution is adjusted to 4 by dilute sulfuric acid；
(6), it is passivated: passivating solution being first heated to 65 DEG C, the rolled copper foil after zinc-nickel alloy is then immersed in passivation
3min is passivated in liquid；
The passivating solution includes 50g/L chromium chloride, 125g/L sodium nitrate and 50g/L sodium fluoride, with nitric acid by the PH tune of plating solution
It saves to 2；
(7), silane coupling agent is handled: the rolling aluminum foil after passivation is impregnated in 10% silane coupling agent alcoholic solution, it should
Silane coupling agent mainly uses silane coupling agent KH560, takes out after 1min, is finally air-dried with 150 DEG C of hot wind.
Performance test:
(1) peel strength measures:
Experimental design:
Using embodiment 1-7 and comparative example as experimental group, the rolled copper foil being prepared in embodiment and comparative example is led to
It crosses laminating machine and copper-clad plate is made in resin substrate pressing, then by rolling copper in tensile testing machine testing example and comparative example
Peel strength (N/mm) between foil and resin substrate, record minimum load (Lm, N) value and tested batten width (Ws,
Mm), each experimental group measures 3 repetitions, and average minimum load (Lm, N) value and average tested sample width (Ws, mm) is taken to make
For final result.
The calculation formula of peel strength (N/mm) is as follows:
Peel strength (N/mm)=minimum load (Lm)/tested batten width (Ws)
Experimental result:
It can be seen that embodiment 1-7 from the peel strength test result of the rolled copper foil in embodiment 1-7 and comparative example
In the peel strength (N/mm) of rolled copper foil be 2.09-2.23, and the peel strength (N/ of the rolled copper foil in comparative example
Mm) it is 1.57, illustrates that there is better peel strength, the combination between substrate using the obtained rolled copper foil of the present invention
Property is more preferable.
The peel strength of embodiment 1-7 and the rolled copper foil in comparative example measures table
| Group | Peel strength (N/mm) |
| Embodiment 1 | 2.15 |
| Embodiment 2 | 2.23 |
| Embodiment 3 | 2.09 |
| Embodiment 4 | 2.17 |
| Embodiment 5 | 2.22 |
| Embodiment 6 | 2.19 |
| Embodiment 7 | 2.17 |
| Comparative example | 1.57 |
(2) corrosion resistance test (salt spray test):
Experimental design:
Respectively using the rolled copper foil being prepared in embodiment 1-7 and comparative example as experimental group, with cycle corrosion test case
Corrosion resistance test is carried out to the rolled copper foil of each experimental group, it is 33-37 DEG C in temperature that each experimental group, which tests three repetitions, pH
Value uses 5% sodium chloride solution to carry out nanospray experiment under the conditions of being 6.5~7.2, observe 1 time, examine every 3h when experiment carries out
Sample is looked into either with or without there is corrosion phenomenon, such as observes corrosion phenomenon, stops experiment immediately, and record the time corroded.
Experimental result:
It is found by corrosion resistance test experiments, when experiment proceeds to 119h, the rolled copper foil in comparative example goes out
Show slight corrosion phenomenon, occurs small and irregular white rust spot on copper foil, and the rolled copper foil in embodiment 1-7 does not have then
Occur corrosion phenomenon, it is seen then that there is better corrosion resistance using the obtained rolled copper foil of the present invention.
(3) heat resistance is tested:
Experimental design:
Respectively using the rolled copper foil being prepared in embodiment 1-7 and comparative example as experimental group, by the copper foil of each experimental group
It is respectively placed in 288 DEG C, 300 DEG C and 350 DEG C of tin soldering liquid and impregnates 1min, it is existing either with or without discovery blistering that sample is observed after taking-up
As each experimental group tests three repetitions.
Experimental result:
It is found by heat resistance test experiments, the rolled copper foil being prepared in embodiment 1-7 and comparative example is at 288 DEG C
With in 300 DEG C of tin soldering liquid impregnate 1min after there is no bubble phenomenons；But after impregnating 1min in 350 DEG C of tin soldering liquid,
Apparent foaming phenomena has occurred in rolled copper foil in comparative example, and blistering does not occur yet for the rolled copper foil in embodiment 1-7 now
As, it is seen then that there is better heat resistance using the obtained rolled copper foil of the present invention, much higher than the standard (288 DEG C) in market.
(4) surface roughness measurement:
Experimental design:
The surface roughness (Ra) of rolled copper foil is that absolute distance counts between the upper summit on sample to be tested surface and the lowest point
Average value is the important parameter for reflecting sample surface profiles feature, and surface roughness is lower, is more conducive to make low-dielectric loss
Circuit.This experiment using the rolled copper foil being prepared in embodiment 1-7 and comparative example as experimental group, uses surface roughness respectively
Measuring instrument carries out surface roughness measurement to the rolled copper foil sample of each experimental group, randomly chooses 5 on the surface of copper foil sample
Point measures, and records the upper summit of each point and the height value of the lowest point respectively, and the average value for calculating 5 measurements can obtain
The surface roughness (R) of copper foil.
Experimental result:
It can be seen that implementation from surface roughness (Ra) measurement result of the rolled copper foil in embodiment 1-7 and comparative example
The surface roughness (Ra) of rolled copper foil in example 1-7 is 0.96-1.11, and the surface roughness of the rolled copper foil in comparative example
(Ra) it is 1.57, illustrates that there is lower surface roughness using the obtained rolled copper foil of the present invention, be more able to satisfy high-end height
The request signal transmission of frequency printed circuit.
The surface roughness (Ra) of embodiment 1-7 and the rolled copper foil in comparative example measures table
| Group | Surface roughness (Ra) |
| Embodiment 1 | 1.11 |
| Embodiment 2 | 0.96 |
| Embodiment 3 | 1.07 |
| Embodiment 4 | 1.04 |
| Embodiment 5 | 1.03 |
| Embodiment 6 | 1.09 |
| Embodiment 7 | 1.07 |
| Comparative example | 1.57 |
Above the embodiments of the present invention are described in detail, but the present invention is not limited to described embodiments.It is right
For those skilled in the art, in the case where not departing from the principle of the invention and spirit, these embodiments are carried out more
Kind change, modification, replacement and modification, still fall in protection scope of the present invention.
Claims (10)
1. a kind of process of surface treatment of rolled copper foil, it is characterised in that: the following steps are included:
S1, cleaning: rolled copper foil being immersed in cleaning solution and is cleaned, and is cleaned three times after taking-up with 50~80 DEG C of hot water,
It dries spare；
The cleaning solution is by following weight percent at being grouped as:
15-20% anionic surfactant, 10-15% nonionic surfactant, 8-12% sulfuric acid, 1-3% solubilizer, 1-
3% builder and 47-65% pure water；
S2, it is roughened for the first time: coarsening solution is added into electroplating rectifier, is 15~20A/dm in current density2, temperature 30-40
12-18S is electroplated to rolled copper foil under the conditions of DEG C；
The coarsening solution includes 15-25g/L copper sulphate, 60~80g/L sulfuric acid, 3-5g/L iron sulfite and 1-3g/L nickel sulfate；
S3, solidify for the first time: solidify liquid being added into electroplating rectifier, be 15~20A/dm in current density2, temperature 45-55
8-15S is electroplated to rolled copper foil under the conditions of DEG C；
The solidify liquid includes 60-70g/L copper sulphate, 90~100g/L sulfuric acid and 2-3g/L lecithin；
S4, secondary roughening: coarsening solution described in first time roughening step being added into electroplating rectifier, is 8 in current density
~12A/dm2, temperature be 20-30 DEG C under the conditions of to rolled copper foil be electroplated 7-10S；
S5, secondary curing: solidify liquid described in first time curing schedule being added into electroplating rectifier, is 12 in current density
~15A/dm2, temperature be 35-40 DEG C under the conditions of to rolled copper foil be electroplated 5-10S；
S6, nickel plating lanthanum alloy: nickel lanthanum alloy plating solution being added into electroplating rectifier, is 10~20A/dm in current density2, temperature
30-50S is electroplated to rolled copper foil under the conditions of being 50-65 DEG C；
The nickel lanthanum alloy plating solution includes 35-45g/L nickel sulfamic acid, 20-30g/L lanthanum chloride, 3-5g/L urea and 2-3g/L
The PH of plating solution is adjusted to 3-6 with citric acid by stabilizer；
S7, plating tungsten kirsite: tungsten zinc alloy bath being added into electroplating rectifier, is 5~10A/dm in current density2, temperature be
15-25S is electroplated to rolled copper foil under the conditions of 40-50 DEG C；
The tungsten zinc alloy bath include 20-30g/L sodium tungstate, 10-15g/L zinc nitrate, 1-2g/L lauryl sodium sulfate and
PH is adjusted to 3-5 with boric acid solution by 2-3g/L stabilizer；
S8, passivation: passivating solution is first heated to 40-50 DEG C, then rolled copper foil is immersed in passivating solution and is passivated 25-35s；
The passivating solution includes 6-10g/L titanium trichloride, 8-12g/L phytic acid, 8-15mL/L hydrogen peroxide, the inclined phosphorus of 10-18g/L six
The PH of passivating solution is adjusted to 1-3 with nitric acid by sour sodium；
S9, drying: the rolled copper foil after passivation is placed in 50-60 DEG C of baking oven and dries 8-10h；
S10, silane coupling agent processing:, then will be after drying first with the silane coupling agent alcoholic solution of dehydrated alcohol configuration 3-5%
Rolling aluminum foil is impregnated in silane coupling agent alcoholic solution, is taken out after 10-15s, solidifies 1- under the conditions of finally placing it in 70-80 DEG C
The facing operation of rolled copper foil can be completed in 3h.
2. a kind of process of surface treatment of rolled copper foil according to claim 1, it is characterised in that: in the S1 step
In, rolled copper foil is immersed in cleaning solution in three times and is cleaned, impregnates 1-2min every time, be both needed to after impregnating every time with 50~
80 DEG C of hot water cleans three times.
3. a kind of process of surface treatment of rolled copper foil according to claim 1, it is characterised in that: the anionic surface
Activating agent is any one in neopelex, odium stearate, laruyl alcohol, vinethene and glyceride.
4. a kind of process of surface treatment of rolled copper foil according to claim 1, it is characterised in that: the non-ionic surface
Activating agent is fatty alcohol polyoxyethylene ether, cocoanut fatty acid diethanolamide, alkyl phenol polyoxyethylene ether and fatty acid polyoxy
Any one in vinyl acetate.
5. a kind of process of surface treatment of rolled copper foil according to claim 1, it is characterised in that: the solubilizer is second
Any one in alcohol, isopropanol and butanol.
6. a kind of process of surface treatment of rolled copper foil according to claim 1, it is characterised in that: the builder is coke
Sodium phosphate, potassium pyrophosphate, sodium nitrite, sodium benzoate, any one in sodium sulphate.
7. a kind of process of surface treatment of rolled copper foil according to claim 1, it is characterised in that: in the S6 step
Stabilizer is sodium pyrophosphate.
8. a kind of process of surface treatment of rolled copper foil according to claim 1, it is characterised in that: in the S7 step
Stabilizer is sodium citrate.
9. a kind of process of surface treatment of rolled copper foil according to claim 1, it is characterised in that: in the S9 step
Before passivation, the rolled copper foil after plating tungsten kirsite is immersed in 45-55 DEG C of warm water and is cleaned three times.
10. a kind of process of surface treatment of rolled copper foil according to claim 1, it is characterised in that: described silane coupled
Agent is silane coupling agent kh550.
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| CN113337862A (en) * | 2021-04-12 | 2021-09-03 | 浙江花园新能源有限公司 | Surface treatment process of 0.1 mm ultra-width rolled copper foil |
| CN113430596A (en) * | 2021-07-23 | 2021-09-24 | 赛莱克斯微系统科技（北京）有限公司 | Through-silicon-via copper electroplating solution and electroplating method thereof |
| CN114059132A (en) * | 2021-10-13 | 2022-02-18 | 江苏穗实科技有限公司 | High-performance heat radiation heat dissipation copper foil material |
| CN116075068A (en) * | 2022-12-27 | 2023-05-05 | 南通赛可特电子有限公司 | Cleaning and antioxidation process for preventing copper surface from oxidization based on copper foil of printed circuit board |
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