TW202118899A - 無電鍍銅及抵消鈍化 - Google Patents
無電鍍銅及抵消鈍化 Download PDFInfo
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- TW202118899A TW202118899A TW109135203A TW109135203A TW202118899A TW 202118899 A TW202118899 A TW 202118899A TW 109135203 A TW109135203 A TW 109135203A TW 109135203 A TW109135203 A TW 109135203A TW 202118899 A TW202118899 A TW 202118899A
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- Prior art keywords
- alkyl
- copper
- substrate
- amino
- group
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- 239000010949 copper Substances 0.000 title claims abstract description 160
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 159
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 159
- 238000007747 plating Methods 0.000 title claims abstract description 47
- 238000002161 passivation Methods 0.000 title abstract description 51
- 239000000758 substrate Substances 0.000 claims abstract description 72
- 239000000203 mixture Substances 0.000 claims abstract description 47
- 238000000034 method Methods 0.000 claims abstract description 43
- 150000002460 imidazoles Chemical class 0.000 claims abstract description 13
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 77
- -1 imidazole compound Chemical class 0.000 claims description 55
- 229910052799 carbon Inorganic materials 0.000 claims description 41
- 150000001875 compounds Chemical class 0.000 claims description 37
- 239000003638 chemical reducing agent Substances 0.000 claims description 29
- 239000003054 catalyst Substances 0.000 claims description 28
- 238000009713 electroplating Methods 0.000 claims description 25
- 125000001424 substituent group Chemical group 0.000 claims description 25
- 239000001257 hydrogen Substances 0.000 claims description 24
- 229910052739 hydrogen Inorganic materials 0.000 claims description 24
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 22
- 150000001721 carbon Chemical group 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 150000001412 amines Chemical class 0.000 claims description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 11
- 125000004185 ester group Chemical group 0.000 claims description 10
- 150000002431 hydrogen Chemical class 0.000 claims description 10
- 125000004178 (C1-C4) alkyl group Chemical group 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 230000003750 conditioning effect Effects 0.000 claims description 8
- 239000012487 rinsing solution Substances 0.000 claims description 8
- 150000007513 acids Chemical class 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 125000004433 nitrogen atom Chemical group N* 0.000 claims description 7
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 7
- 125000000217 alkyl group Chemical group 0.000 claims description 5
- 125000003277 amino group Chemical group 0.000 claims description 5
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 5
- 125000006273 (C1-C3) alkyl group Chemical group 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- YWNXHTNWOQHFRL-UHFFFAOYSA-N 2-(1H-benzimidazol-2-yl)aniline Chemical compound NC1=CC=CC=C1C1=NC2=CC=CC=C2N1 YWNXHTNWOQHFRL-UHFFFAOYSA-N 0.000 claims description 3
- YDDBHCXOIBPIFS-UHFFFAOYSA-N 2-(4,5-dimethyl-1h-imidazol-2-yl)-4,5-dimethyl-1h-imidazole Chemical compound N1C(C)=C(C)N=C1C1=NC(C)=C(C)N1 YDDBHCXOIBPIFS-UHFFFAOYSA-N 0.000 claims description 3
- XWXMGTIHBYFTIE-UHFFFAOYSA-N chembl203360 Chemical compound OC1=CC=CC=C1C1=NC2=CC=CC=C2N1 XWXMGTIHBYFTIE-UHFFFAOYSA-N 0.000 claims description 3
- HAEYZZSSSUIZAN-UHFFFAOYSA-N 1h-benzimidazol-1-ium-2-ylmethylazanium;dichloride Chemical compound Cl.Cl.C1=CC=C2NC(CN)=NC2=C1 HAEYZZSSSUIZAN-UHFFFAOYSA-N 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical group 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 36
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 14
- 239000000654 additive Substances 0.000 description 13
- 229910052751 metal Inorganic materials 0.000 description 13
- 239000002184 metal Substances 0.000 description 13
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 12
- RJTANRZEWTUVMA-UHFFFAOYSA-N boron;n-methylmethanamine Chemical compound [B].CNC RJTANRZEWTUVMA-UHFFFAOYSA-N 0.000 description 11
- 150000003839 salts Chemical class 0.000 description 11
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 10
- 239000008139 complexing agent Substances 0.000 description 10
- VZOPRCCTKLAGPN-ZFJVMAEJSA-L potassium;sodium;(2r,3r)-2,3-dihydroxybutanedioate;tetrahydrate Chemical compound O.O.O.O.[Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O VZOPRCCTKLAGPN-ZFJVMAEJSA-L 0.000 description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 9
- 230000003647 oxidation Effects 0.000 description 9
- 238000007254 oxidation reaction Methods 0.000 description 9
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 8
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 8
- WQGWDDDVZFFDIG-UHFFFAOYSA-N pyrogallol Chemical compound OC1=CC=CC(O)=C1O WQGWDDDVZFFDIG-UHFFFAOYSA-N 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
- 238000005530 etching Methods 0.000 description 7
- 238000005259 measurement Methods 0.000 description 7
- 239000002243 precursor Substances 0.000 description 7
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 7
- 239000004094 surface-active agent Substances 0.000 description 7
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 239000002671 adjuvant Substances 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 229910052763 palladium Inorganic materials 0.000 description 6
- 239000003381 stabilizer Substances 0.000 description 6
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical class [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 5
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 5
- 238000004769 chrono-potentiometry Methods 0.000 description 5
- 229910001431 copper ion Inorganic materials 0.000 description 5
- 229910021645 metal ion Inorganic materials 0.000 description 5
- HELHAJAZNSDZJO-OLXYHTOASA-L sodium L-tartrate Chemical compound [Na+].[Na+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O HELHAJAZNSDZJO-OLXYHTOASA-L 0.000 description 5
- 239000001433 sodium tartrate Substances 0.000 description 5
- 229960002167 sodium tartrate Drugs 0.000 description 5
- 235000011004 sodium tartrates Nutrition 0.000 description 5
- 230000008961 swelling Effects 0.000 description 5
- 125000006526 (C1-C2) alkyl group Chemical group 0.000 description 4
- YQUVCSBJEUQKSH-UHFFFAOYSA-N 3,4-dihydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C(O)=C1 YQUVCSBJEUQKSH-UHFFFAOYSA-N 0.000 description 4
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 4
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 4
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 4
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 description 4
- RHYBFKMFHLPQPH-UHFFFAOYSA-N N-methylhydantoin Chemical compound CN1CC(=O)NC1=O RHYBFKMFHLPQPH-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- GBFLZEXEOZUWRN-VKHMYHEASA-N S-carboxymethyl-L-cysteine Chemical compound OC(=O)[C@@H](N)CSCC(O)=O GBFLZEXEOZUWRN-VKHMYHEASA-N 0.000 description 4
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 4
- 229940053195 antiepileptics hydantoin derivative Drugs 0.000 description 4
- 229960003237 betaine Drugs 0.000 description 4
- HJMZMZRCABDKKV-UHFFFAOYSA-N carbonocyanidic acid Chemical compound OC(=O)C#N HJMZMZRCABDKKV-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 229940074391 gallic acid Drugs 0.000 description 4
- 235000004515 gallic acid Nutrition 0.000 description 4
- LHGVFZTZFXWLCP-UHFFFAOYSA-N guaiacol Chemical compound COC1=CC=CC=C1O LHGVFZTZFXWLCP-UHFFFAOYSA-N 0.000 description 4
- 150000001469 hydantoins Chemical class 0.000 description 4
- 229940079877 pyrogallol Drugs 0.000 description 4
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 4
- 239000011975 tartaric acid Substances 0.000 description 4
- 235000002906 tartaric acid Nutrition 0.000 description 4
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 3
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 description 3
- 239000005751 Copper oxide Substances 0.000 description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 229910021607 Silver chloride Inorganic materials 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 239000003093 cationic surfactant Substances 0.000 description 3
- 239000002738 chelating agent Substances 0.000 description 3
- 229910000431 copper oxide Inorganic materials 0.000 description 3
- 239000003989 dielectric material Substances 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 239000008103 glucose Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 150000007522 mineralic acids Chemical class 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 239000002736 nonionic surfactant Substances 0.000 description 3
- 239000003002 pH adjusting agent Substances 0.000 description 3
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000008399 tap water Substances 0.000 description 3
- 235000020679 tap water Nutrition 0.000 description 3
- RFTORHYUCZJHDO-UHFFFAOYSA-N 1,3-dimethylimidazolidine-2,4-dione Chemical compound CN1CC(=O)N(C)C1=O RFTORHYUCZJHDO-UHFFFAOYSA-N 0.000 description 2
- VZYDKJOUEPFKMW-UHFFFAOYSA-N 2,3-dihydroxybenzenesulfonic acid Chemical compound OC1=CC=CC(S(O)(=O)=O)=C1O VZYDKJOUEPFKMW-UHFFFAOYSA-N 0.000 description 2
- QFSYADJLNBHAKO-UHFFFAOYSA-N 2,5-dihydroxy-1,4-benzoquinone Chemical compound OC1=CC(=O)C(O)=CC1=O QFSYADJLNBHAKO-UHFFFAOYSA-N 0.000 description 2
- IKQCSJBQLWJEPU-UHFFFAOYSA-N 2,5-dihydroxybenzenesulfonic acid Chemical compound OC1=CC=C(O)C(S(O)(=O)=O)=C1 IKQCSJBQLWJEPU-UHFFFAOYSA-N 0.000 description 2
- JJWCTKUQWXYIIU-UHFFFAOYSA-N 2-Benzimidazolylguanidine Chemical compound C1=CC=C2NC(N=C(N)N)=NC2=C1 JJWCTKUQWXYIIU-UHFFFAOYSA-N 0.000 description 2
- GUOVBFFLXKJFEE-UHFFFAOYSA-N 2h-benzotriazole-5-carboxylic acid Chemical compound C1=C(C(=O)O)C=CC2=NNN=C21 GUOVBFFLXKJFEE-UHFFFAOYSA-N 0.000 description 2
- BZOVBIIWPDQIHF-UHFFFAOYSA-N 3-hydroxy-2-methylbenzenesulfonic acid Chemical compound CC1=C(O)C=CC=C1S(O)(=O)=O BZOVBIIWPDQIHF-UHFFFAOYSA-N 0.000 description 2
- KDHWOCLBMVSZPG-UHFFFAOYSA-N 3-imidazol-1-ylpropan-1-amine Chemical compound NCCCN1C=CN=C1 KDHWOCLBMVSZPG-UHFFFAOYSA-N 0.000 description 2
- QPHPUQJVKQXISS-UHFFFAOYSA-N 4-oxo-4-sulfanylbutanoic acid Chemical compound OC(=O)CCC(S)=O QPHPUQJVKQXISS-UHFFFAOYSA-N 0.000 description 2
- KDCGOANMDULRCW-UHFFFAOYSA-N 7H-purine Chemical compound N1=CNC2=NC=NC2=C1 KDCGOANMDULRCW-UHFFFAOYSA-N 0.000 description 2
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- SIKJAQJRHWYJAI-UHFFFAOYSA-N Indole Chemical compound C1=CC=C2NC=CC2=C1 SIKJAQJRHWYJAI-UHFFFAOYSA-N 0.000 description 2
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- DJDFFEBSKJCGHC-UHFFFAOYSA-N Naphazoline Chemical compound Cl.C=1C=CC2=CC=CC=C2C=1CC1=NCCN1 DJDFFEBSKJCGHC-UHFFFAOYSA-N 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229930040373 Paraformaldehyde Natural products 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- JPYHHZQJCSQRJY-UHFFFAOYSA-N Phloroglucinol Natural products CCC=CCC=CCC=CCC=CCCCCC(=O)C1=C(O)C=C(O)C=C1O JPYHHZQJCSQRJY-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical group [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 2
- 239000003929 acidic solution Substances 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000005215 alkyl ethers Chemical class 0.000 description 2
- XXROGKLTLUQVRX-UHFFFAOYSA-N allyl alcohol Chemical compound OCC=C XXROGKLTLUQVRX-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 239000002280 amphoteric surfactant Substances 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical class B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 2
- 229910000085 borane Inorganic materials 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
- 239000004327 boric acid Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000001913 cellulose Chemical class 0.000 description 2
- 229920002678 cellulose Chemical class 0.000 description 2
- 235000015165 citric acid Nutrition 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 2
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 description 2
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 description 2
- 229940112669 cuprous oxide Drugs 0.000 description 2
- 238000002848 electrochemical method Methods 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 229960001867 guaiacol Drugs 0.000 description 2
- 150000004820 halides Chemical class 0.000 description 2
- WJRBRSLFGCUECM-UHFFFAOYSA-N hydantoin Chemical compound O=C1CNC(=O)N1 WJRBRSLFGCUECM-UHFFFAOYSA-N 0.000 description 2
- 229940091173 hydantoin Drugs 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 150000007529 inorganic bases Chemical class 0.000 description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
- FBSFWRHWHYMIOG-UHFFFAOYSA-N methyl 3,4,5-trihydroxybenzoate Chemical compound COC(=O)C1=CC(O)=C(O)C(O)=C1 FBSFWRHWHYMIOG-UHFFFAOYSA-N 0.000 description 2
- WXHIJDCHNDBCNY-UHFFFAOYSA-N palladium dihydride Chemical compound [PdH2] WXHIJDCHNDBCNY-UHFFFAOYSA-N 0.000 description 2
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 description 2
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- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 description 1
- FHCPAXDKURNIOZ-UHFFFAOYSA-N tetrathiafulvalene Chemical compound S1C=CSC1=C1SC=CS1 FHCPAXDKURNIOZ-UHFFFAOYSA-N 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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- C23C18/1827—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment only one step pretreatment
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
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- C23C18/1827—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment only one step pretreatment
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1837—Multistep pretreatment
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
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Abstract
在含銅的基材上無電鍍銅之前，向該基材施加含有選擇的咪唑化合物的水性組成物。該含有選擇的咪唑化合物的水性組成物抵消了該基材上的銅的鈍化以改善無電鍍銅製程。
Description
本發明關於無電鍍銅方法，以及抵消含銅基材上的銅的鈍化作用之方法。更具體地，本發明關於無電鍍銅方法，以及用含有選擇的咪唑化合物的水性組成物抵消含銅基材上的銅的鈍化作用之方法。
無電鍍銅廣泛用於金屬化工業中用於在各種類型的基材上沈積銅。例如，在印刷電路板的製造中，無電鍍銅浴用於在通孔壁和電路通道上沈積銅，作為後續電解鍍銅的基礎。無電鍍銅也用於裝飾性塑膠工業中用於在非導電表面上沈積銅，作為根據需要進一步鍍銅、鎳、金、銀和其他金屬的基礎。目前商業上使用的無電鍍銅浴含有水溶性二價銅化合物，用於二價銅離子的螯合劑或錯合劑，例如羅謝爾鹽（四水合酒石酸鉀鈉）和乙二胺四乙酸鈉鹽，還原劑，例如甲醛和甲醛先質或衍生物，以及各種添加劑，以使浴更穩定，調整鍍速和提亮銅沈積物。
在啟動時觀察到的問題，尤其是在基於酒石酸的無電鍍銅的情況下，係基材（如來自無電鍍銅的不充分引發的覆銅層壓板）的氧化或鈍化。銅鈍化的一種形式係在金屬銅的表面上形成銅氧化物如氧化亞銅（Cu2
O）和氧化銅（CuO）之微塗層。然而鈍化可能是用於防止銅腐蝕的希望之方法，在無電鍍銅中，銅表面上的氧化的存在可以抑制銅表面的希望的催化活性。此問題在基於酒石酸的無電鍍銅浴中是最常觀察到的，並可表現為在啟動時覆銅層壓板上的一系列表面著色。在銅表面上觀察到的此氧化現象還可能影響穿孔底部和內層銅表面處之銅墊，從而損害互連的可靠性。
為了解決該問題，常規方法係向含銅基材施加衝擊電壓。衝擊輥為面板表面提供還原電位，這以電解方式減少了銅表面上的表面鈍化並沈積了對無電鍍銅有活性的薄的銅種子層。然而，如果面板太小而不能跨越從陰極輥到無電浴的距離或者如果電路設計不允許所有銅表面同時連接到衝擊輥以及無電浴，則衝擊電壓可能是無效的。在此類情況下，存在並不是所有銅表面都對衝擊輥的作用產生反應的風險，正因如此，一些表面可能不能正確地引發無電鍍銅。衝擊輥被安排在無電浴之前，但不是其自身浸漬在無電溶液中（或鍍敷可能在輥上發生）。當面板跨越衝擊輥與無電浴溶液之間的距離時，衝擊電壓起作用。如果面板太小而不能跨越此距離，那麼衝擊將沒有作用。此類情況必然需要解決鈍化問題的替代方法。
因此，需要一種無電鍍銅方法以及抵消含銅基材的鈍化作用之方法。
本發明關於一種無電鍍銅方法，其包括：
a) 提供包含銅的基材；
b) 向該基材的銅施加催化劑；
c) 用包含咪唑化合物的水性組成物處理該基材的經催化的銅，其中該咪唑化合物具有下式：
(I)，
其中R1
和R2
獨立地選自氫、(C1
-C4
)烷基和酯基或R1
和R2
的碳可以一起形成取代或未取代的稠合的六員碳芳環，其中該六員碳芳環上的取代基選自由以下組成之群組：羧基、羧基(C1
-C4
)烷基、羥基、羥基(C1
-C4
)烷基、胺基和胺基(C1
-C4
)烷基，R3
係氫、羥基、羥基(C1
-C4
)烷基、胺基或胺基(C1
-C4
)烷基，並且A可以是氮原子或碳原子，其中當A係碳原子時，該碳原子可以具有選自由以下組成之群組之取代基：取代或未取代的咪唑、胍基、取代的苯基、胺基(C1
-C4
)烷基、以及萘基(C1
-C4
)烷基；
d) 向該基材的經處理的銅施加無電鍍銅浴；以及
e) 用該無電鍍銅浴在該基材的經處理的銅上無電鍍銅。
本發明還關於一種無電鍍銅方法，其包括：
a) 提供包含銅的基材；
b) 向該基材的銅施加催化劑；
c) 用包含還原劑和咪唑化合物的水性組成物處理該基材的經催化的銅，其中該咪唑化合物具有下式：(I)，
其中R1
和R2
獨立地選自氫、(C1
-C4
)烷基和酯基或R1
和R2
的碳可以一起形成取代或未取代的稠合的六員碳芳環，其中該六員碳芳環上的取代基選自由以下組成之群組：羧基、羧基(C1
-C4
)烷基、羥基、羥基(C1
-C4
)烷基、胺基和胺基(C1
-C4
)烷基，R3
係氫、羥基、羥基(C1
-C4
)烷基、胺基或胺基(C1
-C4
)烷基，並且A可以是氮原子或碳原子，其中當A係碳原子時，該碳原子可以具有選自由以下組成之群組之取代基：取代或未取代的咪唑、胍基、取代的苯基、胺基(C1
-C4
)烷基、萘基(C1
-C4
)烷基；
d) 向該基材的經處理的銅施加無電鍍銅浴；以及
e) 用該無電鍍銅浴在該基材的經處理的銅上無電鍍銅。
本發明進一步關於一種無電鍍銅方法，其包括：
a) 提供包含銅的基材；
b) 向該基材的銅施加催化劑；
c) 向該基材的經催化的銅施加還原劑；
d) 用包含咪唑化合物的水性組成物處理該基材的經催化的銅，其中該咪唑化合物具有下式：(I)，
其中R1
和R2
獨立地選自氫、(C1
-C4
)烷基和酯基或R1
和R2
的碳可以一起形成取代或未取代的稠合的六員碳芳環，其中該六員碳芳環上的取代基選自由以下組成之群組：羧基、羧基(C1
-C4
)烷基、羥基、羥基(C1
-C4
)烷基、胺基和胺基(C1
-C4
)烷基，R3
係氫、羥基、羥基(C1
-C4
)烷基、胺基或胺基(C1
-C4
)烷基，並且A可以是氮原子或碳原子，其中當A係碳原子時，該碳原子可以具有選自由以下組成之群組之取代基：取代或未取代的咪唑、胍基、取代的苯基、胺基(C1
-C4
)烷基、以及萘基(C1
-C4
)烷基；
e) 向該基材的經處理的銅施加無電鍍銅浴；以及
f) 用該無電鍍銅浴在該基材的經處理的銅上無電鍍銅。
本發明之方法抵消了基材上的銅的鈍化作用，並且能夠引發基材的銅上的無電鍍銅。本發明之方法還能夠快速引發基材的銅上的無電鍍銅。
如在整個說明書中所使用的，除非上下文另有明確說明，否則下面給出的縮寫具有以下含義：g = 克；mg = 毫克；mL = 毫升；L = 升；cm = 釐米；m = 米；mm = 毫米；μm = 微米；ppm = 百萬分率 = mg/L；sec = 秒；min. = 分鐘；°C = 攝氏度；mA = 毫安培；V = 伏特；g/L = 克/升；DI = 去離子的；Pd = 鈀；Pd(II) = +2氧化態的鈀離子；Pdº = 還原為其金屬非離子化態的鈀；Ag = 銀；Cl = 氯化物；K = 鉀；Li = 鋰；wt% = 重量百分比；Vol.% = 體積百分比；以及e.g. = 例如。
在整個說明書中，術語「鍍敷」和「沈積」可互換使用。在整個說明書中，術語「組成物」和「浴」可互換使用。術語「鈍化」意指氧化，如在銅金屬表面上的氧化亞銅和氧化銅的形成。術語「抗鈍化」意指抵消氧化作用。術語「抵消」意指針對某事物起作用以減少其力或將其中和。術語「開路電位」或「開路電壓」意指當與任何電路斷開（無外部負載連接或端子之間無外部電流流動）時設備的兩個端子之間的電位差。術語「計時電位法」意指電化學技術，其中當將恒定的還原電流施加到面板表面時工作電極的電位作為時間的函數進行監測；電流首先到達最積極的還原途徑，並且隨著每個途徑的反應物被消耗，電流被驅動到下一個最有利的反應，從而產生一系列的電位階躍。化學結構中的「--------」表示視需要的化學鍵。術語「胺基」意指具有下式的化學部分：-NR’R”，其中R’和R”可以相同或不同並且選自由氫和 (C1
-C4
)烷基組成之群組。縮寫「ca」意指大約。除非另有說明，否則所有量均為重量百分比。所有數值範圍皆為包含端值的，並且可按任何順序組合，除了此數值範圍被限制為加起來最高達100%係合乎邏輯的情況之外。
在基材上的銅金屬的無電鍍銅之前，用抗鈍化化合物的水性溶液處理基材的銅金屬以抵消基材的銅的氧化作用，以能夠引發無電鍍銅，較佳的是快速引發無電鍍銅。儘管不受理論約束，抗鈍化化合物藉由溶解抑制無電鍍銅的銅的鈍化層來抵消鈍化，或者在替代方案中，抗鈍化化合物藉由在銅表面上形成活性分子錯合物來抵消鈍化，以引發無電鍍銅。
本發明之抗鈍化化合物係咪唑化合物，其中該咪唑化合物具有下式：(I)，
其中R1
和R2
獨立地選自氫、(C1
-C4
)烷基和酯基，或R1
和R2
的碳可以一起形成取代或未取代的六員碳芳族稠環，其中該六員碳芳族稠環上的取代基選自由以下組成之群組：羧基、羧基(C1
-C4
)烷基、羥基、羥基(C1
-C4
)烷基、胺基和胺基(C1
-C4
)烷基，R3
係氫、羥基、羥基(C1
-C4
)烷基、胺基或胺基(C1
-C4
)烷基，並且A可以是氮原子或碳原子，其中當A係碳原子時，該碳原子可以具有選自由以下組成之群組之取代基：取代或未取代的咪唑、胍基、取代的苯基、胺基(C1
-C4
)烷基、以及萘基(C1
-C4
)烷基，其中該苯基上的取代基包括但不限於羥基、羥基(C1
-C4
)烷基、胺基、或胺基(C1
-C4
)烷基，並且該咪唑上的取代基包括但不限於(C1
-C4
)烷基、羥基、羥基(C1
-C4
)烷基、胺基、胺基(C1
-C4
)烷基、羧基、羧基(C1
-C4
)烷基或酯基。
較佳的是，該咪唑化合物具有下式：
(II)，
其中R1
和R2
獨立地是氫、(C1
-C3
)烷基和酯基，或R1
和R2
與所有它們的碳原子一起形成取代或未取代的六員碳芳族稠環，其中該六員碳芳族稠環上的取代基選自由以下組成之群組：羧基、羧基(C1
-C3
)烷基、羥基、羥基(C1
-C3
)烷基、胺基和胺基(C1
-C3
)烷基，R3
係氫或胺基(C1
-C2
)烷基，並且R4
選自由以下組成之群組：取代或未取代的咪唑、胍基、取代的苯基、胺基(C1
-C4
)烷基、以及萘基(C1
-C4
)烷基，其中該苯基上的取代基選自由羥基和胺基組成之群組並且該咪唑上的取代基選自由(C1
-C3
)烷基、羥基(C1
-C3
)烷基和胺基(C1
-C3
)烷基組成之群組；更較佳的是，R1
和R2
獨立地是氫、(C1
-C2
)烷基，或R1
和R2
與所有它們的碳原子一起形成未取代的六員碳芳族稠環，R3
係氫，並且R4
選自由以下組成之群組：取代的咪唑、胍基、胺基(C1
-C2
)烷基和取代的苯基，其中該咪唑上的取代基係(C1
-C2
)烷基，並且該苯基上的取代基選自由羥基和胺基組成之群組，其中該胺基係-NH2
；最較佳的是，R1
和R2
係(C1
-C2
)烷基，R3
係氫，並且R4
係取代的咪唑，其中該取代基係(C1
-C2
)烷基，或者在替代方案中，R1
和R2
與它們的碳原子一起形成未取代的六員碳芳族稠環，R3
係氫，並且R4
係胍基。
本發明之示例性的抗鈍化化合物係以下化合物：
具有下式的2,2’-雙(4,5-二甲基咪唑)：
(III)，
具有下式的2-胍基苯并咪唑：
(IV)，
具有下式的2-(胺基甲基)苯并咪唑二氫氯化物：
2HCl (V)，
具有下式的1-(3-胺基丙基)咪唑：
(VI)，
具有下式的2-(1-萘基甲基)咪唑啉鹽酸鹽：
HCl (VII)，
具有下式的2-(2-胺基苯基)-1H-苯并咪唑：
(VIII)，
具有下式的2-(2-羥基苯基)-1H-苯并咪唑：
(IX)，
具有下式的苯并三唑-5-羧酸：
(X)，以及
具有下式的二甲基-4,5-咪唑二羧酸酯：
(XI)
抗鈍化化合物可以包括在水性還原溶液中，該水性還原溶液將離子催化劑的金屬離子還原為金屬態，或者在替代方案中，抗鈍化化合物可以包括在向經催化的基材施加水性還原溶液之後所施加的水性沖洗液中。抗鈍化化合物也可以包括在水性還原溶液和水性沖洗液二者之中，該水性沖洗液係在相同的無電鍍銅方法期間向經催化的基材施加該還原溶液之後。抗鈍化化合物的混合物也可以包括在本發明之還原溶液中或水性沖洗液中。較佳的是，抗鈍化化合物以0.1 mg/L至100 mg/L、更較佳的是0.5 mg/L至50 mg/L、進一步較佳的是0.5 mg/L至10 mg/L的量被包括。
在本發明之方法中使用的水性還原溶液和水性沖洗溶液中含有的水較佳的是去離子水和蒸餾水中的至少一種，以限制附帶的雜質。
在一個實施方式中，水性還原溶液包括除了一種或多種抗鈍化化合物之外的一種或多種還原劑。還原劑包括但不限於甲醛，甲醛先質，甲醛衍生物如多聚甲醛，硼氫化物如硼氫化鈉，取代的硼氫化物，硼烷如二甲胺硼烷（DMAB），抗壞血酸、異抗壞血酸、次磷酸鹽或其鹽如次磷酸鈉，對苯二酚，鄰苯二酚，間苯二酚，醌醇，連苯三酚，偏苯三酚，間苯三酚，愈創木酚，沒食子酸，3,4-二羥基苯甲酸，苯酚磺酸，甲酚磺酸，對苯二酚磺酸（hydroquinonsulfonic acid），鄰苯二酚磺酸，或所有上述還原劑的鹽。較佳的是，還原劑選自甲醛，甲醛衍生物，甲醛先質，硼氫化物，二甲胺硼烷（DMAB），次磷酸鹽或其鹽，對苯二酚，鄰苯二酚，間苯二酚或沒食子酸。更較佳的是，還原劑選自二甲胺硼烷（DMAB），甲醛，甲醛衍生物，甲醛先質或次磷酸鈉。最較佳的是，還原劑係二甲胺硼烷（DMAB）。
還原劑以足以將催化劑的所有金屬離子還原為它們的金屬態的量包括在還原溶液中。較佳的是，還原劑以0.1 g/L至100 g/L、更較佳的是0.1 g/L至60 g/L、甚至更較佳的是0.1 g/L至10 g/L、進一步較佳的是0.1 g/L至5 g/L、最較佳的是0.1 g/L至2 g/L的量被包括。
視需要，還原溶液中可以包括一種或多種酸。此類酸包括但不限於硼酸、乙酸、檸檬酸、鹽酸、硫酸、胺基磺酸、磷酸或鏈烷磺酸。此類酸可以以0.5 g/L或更大、較佳的是0.5 g/L至20 g/L、更較佳的是1 g/L至10 g/L的量包括在水性還原溶液中。
水性還原溶液的pH範圍係從小於1至14、較佳的是1至12、更較佳的是2至10、進一步較佳的是6至8、最較佳的是7至7.5。
較佳的是，本發明之水性還原溶液由水、一種或多種抗鈍化化合物、一種或多種還原劑以及視需要一種或多種酸組成。更較佳的是，本發明之水性還原溶液由水、一種或多種抗鈍化化合物、一種或多種還原劑以及一種或多種酸組成。
在另一個實施方式中，當抗鈍化化合物包括在向經催化的基材施加還原溶液之後的水性沖洗液中時，該水性沖洗液由水和一種或多種抗鈍化化合物組成。抗鈍化化合物較佳的是以0.1 mg/L至100 mg/L、更較佳的是0.5 mg/L至50 mg/L、進一步較佳的是0.5 mg/L至10 mg/L的量包括在沖洗液中。
本發明之方法和組成物可用於在各種基材如半導體、金屬包覆和未包覆的基材如印刷電路板上無電鍍銅。此類金屬包覆和未包覆的印刷電路板可以包括熱固性樹脂，熱塑性樹脂及其組合，包括纖維如玻璃纖維，和前述的浸漬實施方式。較佳的是，基材係具有多個特徵（如通孔、穿孔或其組合）的金屬包覆的含有環氧樹脂的印刷電路或佈線板。本發明之組成物和方法可用於製造印刷電路板的水平和垂直過程二者，較佳的是，本發明之組成物和方法用於水平過程。
較佳的是，待被用本發明之組成物和方法無電鍍銅的基材係具有介電材料（如環氧樹脂或與其他常規樹脂材料組合的環氧樹脂）和多個特徵（如通孔或穿孔或通孔與穿孔的組合）的金屬包覆的基材，如印刷電路板。視需要，將板用水沖洗並清潔和脫脂，然後對通孔或穿孔壁進行去汙。準備或軟化電介質或對通孔或穿孔去汙可以藉由施加溶劑溶脹開始。
在本發明之方法中，視需要，用常規的清潔和脫脂組成物和方法對基材進行清潔或脫脂。視需要，向基材施加溶劑溶脹，對基材的通孔或穿孔進行去汙，以及各種水性沖洗液可以視需要在熟悉該項技術者熟知的常規條件和量下施加。
可以使用常規的溶劑溶脹。具體類型可以根據介電材料的類型而變化。可以進行小的實驗以確定哪種溶劑溶脹適合於特定的介電材料。溶劑溶脹包括但不限於二醇醚及其相關的醚乙酸酯。二醇醚及其相關的醚乙酸酯的常規量係熟悉該項技術者熟知的。可商購的溶劑溶脹的實例係CIRCUPOSIT™ MLB調理劑211、CIRCUPOSIT™調理劑3302A、CIRCUPOSIT™ Hole Prep 3303和CIRCUPOSIT™ Hole Prep 4120溶液（從美國德拉瓦州威明頓的杜邦™公司（DuPont™, Wilmington, DE, USA）可獲得）。
溶劑溶脹後，視需要，可以施加助劑。可以使用常規助劑。此類助劑包括硫酸、鉻酸、鹼性過錳酸鹽或電漿蝕刻。較佳的是使用鹼性過錳酸鹽作為助劑。可商購的助劑的實例係CIRCUPOSIT™助劑4130和CIRCUPOSIT™ MLB助劑3308溶液（從美國德拉瓦州威明頓的杜邦™公司可獲得）。在熟悉該項技術者熟知的常規參數和量下施加溶劑溶脹。視需要，用水沖洗基材。
如果施加助劑，則施加中和劑以中和助劑留下的任何殘留物。可以使用常規的中和劑。較佳的是，中和劑係含有一種或多種胺的水性酸性溶液或3wt%過氧化氫和3wt%硫酸的溶液。可商購的中和劑的實例係CIRCUPOSIT™ MLB中和劑216-5和CIRCUPOSIT™ MLB中和劑216-3（從杜邦™公司可獲得）。在熟悉該項技術者熟知的常規條件和量下施加助劑。視需要，用水沖洗基材。
較佳的是，在施加催化劑、含有抗鈍化化合物的水性還原溶液或由水和抗鈍化化合物組成的沖洗液以及無電鍍銅之前，向基材施加酸性或鹼性調理劑。可以使用常規的調理劑。此類調理劑可以包括熟悉該項技術者熟知的一種或多種陽離子表面活性劑、非離子表面活性劑、錯合劑和pH調節劑或緩衝劑。可商購的酸性調理劑的實例係CIRCUPOSIT™調理劑3320A和3327溶液（從杜邦™公司可獲得）。可商購的鹼性調理劑的實例包括但不限於含有一種或多種季胺和聚胺的水性鹼性表面活性劑溶液。可商購的鹼性調理劑的實例係CIRCUPOSIT™調理劑231、3325、813、860和8512溶液（從杜邦™公司可獲得）。根據熟悉該項技術者熟知的常規參數和量施加調理劑。視需要，用水沖洗基材。
視需要，可以在調節之後進行微蝕刻。可以使用常規的微蝕刻組成物。設計微蝕刻以在暴露的金屬（例如內層和表面蝕刻）上提供清潔的微粗糙的金屬表面，以增強無電鍍敷的銅和隨後的電鍍的後續黏附。微蝕刻包括但不限於50 g/L至120 g/L過硫酸鈉或氧基單過硫酸（oxymonopersulfate）鈉或鉀和硫酸（1%-2%）混合物，或通用硫酸/過氧化氫。可商購的微蝕刻組成物的實例係CIRCUPOSIT™ Microetch 3330蝕刻溶液和PREPOSIT™ 748蝕刻溶液（均從杜邦™公司可獲得）。在熟悉該項技術者熟知的常規參數下施加微蝕刻。視需要，用水沖洗基材。
視需要，然後可以將預浸料施加到微蝕刻的基材和通孔。預浸料的實例包括但不限於有機鹽，如四水合酒石酸鉀鈉或檸檬酸鈉，0.5%至3%硫酸或硝酸，或25 g/L至75 g/L氯化鈉的酸性溶液。可商購的預浸料係CIRCUPOSIT™ 6520A酸性溶液（從杜邦™公司可獲得）。在熟悉該項技術者熟知的常規參數和量下施加預浸料。
然後將催化劑施加到基材上。較佳的是，催化劑係離子催化劑。雖然設想可以使用任何包括催化金屬的適用於無電鍍金屬的常規催化劑，但較佳的是，在本發明之方法中使用鈀催化劑。可商購的鈀離子催化劑的實例係CIRCUPOSIT™ 6530催化劑。催化劑可以藉由將基材浸入催化劑溶液中，或藉由將催化劑溶液噴塗在基材上，或藉由使用常規設備將催化劑溶液霧化在基材上來施加。催化劑可以在室溫至約80°C、較佳的是約30°C至約60°C的溫度下施加。在施加催化劑之後，視需要用水沖洗基材和特徵。
在向基材施加催化劑之後，向經催化的基材施加水性還原溶液，其較佳的是包括上述一種或多種抗鈍化化合物和一種或多種常規還原劑。一種或多種抗鈍化化合物可以較佳的是以0.1 mg/L至100 mg/L、更較佳的是0.5 mg/L至50 mg/L、進一步較佳的是0.5 mg/L至10 mg/L的量包括在水性還原溶液中。已知將金屬離子還原成金屬的常規化合物可用於將催化劑的金屬離子還原成它們的金屬態。此類還原劑係以上所述之。還原劑以將基本上所有金屬離子還原為金屬（如Pd(II)至Pdº）的量被包括。較佳的是，還原劑以0.1 g/L至100 g/L、更較佳的是0.1 g/L至60 g/L、甚至更較佳的是0.1 g/L至10 g/L、進一步較佳的是0.1 g/L至5 g/L、最較佳的是0.1 g/L至2 g/L的量被包括。
視需要但較佳的是，然後用水沖洗經催化的基材。水性沖洗液可以由除了水之外的一種或多種抗鈍化化合物組成，或沖洗液可以由水組成。當一種或多種抗鈍化化合物包括在水沖洗液中時，較佳的是，該化合物以0.1 mg/L至100 mg/L、更較佳的是0.5 mg/L至50 mg/L、進一步較佳的是0.5 mg/L至10 mg/L的量被包括。
然後使用本發明之無電鍍銅組成物將基材和通孔或穿孔的壁鍍銅。本發明之無電鍍銅方法可以在室溫至約50°C的溫度下進行。較佳的是，本發明之無電鍍銅方法在室溫至約45°C的溫度下進行，更較佳的是，無電鍍銅在室溫至約40°C下進行。基材可以浸漬在本發明之無電鍍銅組成物中或無電鍍銅組成物可以噴塗在基材上。無電鍍銅方法在pH大於7的鹼性環境下進行。較佳的是，本發明之無電鍍銅方法在8至14、甚至更較佳的是10至14的pH下進行。
本發明之無電鍍銅組成物包括以下各項，較佳的是由其組成：一種或多種銅離子的來源；一種或多種穩定劑；一種或多種錯合或螫合劑；一種或多種還原劑；水；和視需要一種或多種表面活性劑，以及；視需要一種或多種pH調節劑；以及前述組分的任何對應的陽離子或陰離子；其中無電鍍銅組成物的pH大於7。
銅離子和抗衡陰離子的來源包括但不限於銅的水溶性鹵化物、硝酸鹽、乙酸鹽、硫酸鹽以及其他有機和無機鹽。此類銅鹽中的一種或多種的混合物可用於提供銅離子。實例係硫酸銅如五水合硫酸銅，氯化銅，硝酸銅，氫氧化銅和胺基磺酸銅。較佳的是，本發明之無電鍍銅組成物的一種或多種銅離子的來源範圍係0.5 g/L至30 g/L、更較佳的是1 g/L至25 g/L、甚至更較佳的是5 g/L至20 g/L、進一步較佳的是5 g/L至15 g/L、並且最較佳的是8 g/L至15 g/L。
穩定劑包括但不限於含硫的化合物，如s-羧甲基-L-半胱胺酸、硫代二乙醇酸、硫代琥珀酸、2,2'-二硫代二琥珀酸、巰基吡啶、巰基苯并噻唑、硫脲；化合物，如吡啶、嘌呤、喹啉、吲哚、吲唑、咪唑、吡𠯤或其衍生物；醇，如炔醇、烯丙醇、芳基醇或環狀苯酚；羥基取代的芳香族化合物，如甲基-3,4,5-三羥基苯甲酸酯、2,5-二羥基-1,4-苯醌或2,6-二羥基萘；羧酸，如檸檬酸、酒石酸、琥珀酸、蘋果酸、丙二酸、乳酸、乙酸或其鹽；胺；胺基酸；水溶性金屬化合物，如金屬氯化物和硫酸鹽；矽化合物，如矽烷、矽氧烷或低至中等分子量的聚矽氧烷；鍺或其氧化物或氫化物；氰化物和鐵氰化物化合物，或聚伸烷基二醇，纖維素化合物，烷基苯基乙氧基化物或聚環氧乙烷化合物；或穩定劑，如嗒𠯤、甲基哌啶、1,2-二(2-吡啶基)乙烯、1,2-二-(吡啶基)乙烯、2,2'-二吡啶基胺、2,2'-聯吡啶、2,2'-聯嘧啶、6,6'-二甲基-2,2'-聯吡啶、二-2-吡啶酮、N,N,N',N'-四乙烯二胺、萘、1.8-口奈啶、1.6-口奈啶、四硫富瓦烯、三聯吡啶、鄰苯二甲酸、間苯二甲酸或2,2'-二苯甲酸。較佳的是，穩定劑係s-羧甲基-L-半胱胺酸、硫代二乙醇酸、硫代琥珀酸、2,2’-二硫代琥珀酸、巰基吡啶、巰基苯并噻唑、2,2’-聯吡啶或其混合物，更較佳的是，穩定劑係s-羧甲基-L-半胱胺酸、2,2’-二硫代琥珀酸、巰基苯并噻唑、2,2’-聯吡啶或其混合物。此類穩定劑可以以0.5 ppm或更大、較佳的是0.5 ppm至200 ppm、進一步較佳的是1 ppm至50 ppm的量包括在無電鍍銅組成物中。
錯合或螫合劑包括但不限於四水合酒石酸鉀鈉、酒石酸鈉，水楊酸鈉，乙二胺四乙酸（EDTA）的鈉鹽，氮川乙酸或其鹼金屬鹽，葡萄糖酸，葡萄糖酸鹽，三乙醇胺，改性乙二胺四乙酸，S,S-乙二胺二琥珀酸，乙內醯脲或乙內醯脲衍生物。乙內醯脲衍生物包括但不限於1-甲基乙內醯脲、1,3-二甲基乙內醯脲或5,5-二甲基乙內醯脲。較佳的是，錯合劑選自四水合酒石酸鉀鈉，酒石酸鈉，氮川乙酸或其鹼金屬鹽如氮川乙酸的鈉鹽和鉀鹽，乙內醯脲或乙內醯脲衍生物中的一種或多種。較佳的是，EDTA及其鹽不包括在本發明之無電鍍銅組成物中。更較佳的是，錯合劑選自四水合酒石酸鉀鈉、酒石酸鈉、氮川乙酸、氮川乙酸鈉鹽或乙內醯脲衍生物。甚至更較佳的是，錯合劑選自四水合酒石酸鉀鈉、酒石酸鈉、1-甲基乙內醯脲、1,3-二甲基乙內醯脲或5,5-二甲基乙內醯脲。進一步較佳的是，錯合劑選自四水合酒石酸鉀鈉或酒石酸鈉。最較佳的是，錯合劑係四水合酒石酸鉀鈉。
錯合劑以10 g/L至150 g/L、較佳的是20 g/L至150 g/L、更較佳的是30 g/L至100 g/L的量包括在本發明之無電鍍銅組成物中。
無電鍍銅組成物中的還原劑包括但不限於甲醛，甲醛先質，甲醛衍生物如多聚甲醛，硼氫化物如硼氫化鈉，取代的硼氫化物，硼烷如二甲胺硼烷（DMAB），糖類如葡萄糖（葡糖（glucose）），葡糖，山梨糖醇，纖維素，蔗糖，甘露醇或葡糖酸內酯，次磷酸鹽或其鹽如次磷酸鈉，對苯二酚，鄰苯二酚，間苯二酚，醌醇，連苯三酚，偏苯三酚，間苯三酚，愈創木酚，沒食子酸，3,4-二羥基苯甲酸，苯酚磺酸，甲酚磺酸，對苯二酚磺酸，鄰苯二酚磺酸，鈦試劑或所有上述還原劑的鹽。較佳的是，還原劑選自甲醛，甲醛衍生物，甲醛先質，硼氫化物或次磷酸鹽或其鹽，對苯二酚，鄰苯二酚，間苯二酚或沒食子酸。更較佳的是，還原劑選自甲醛，甲醛衍生物，甲醛先質或次磷酸鈉。最較佳的是，還原劑係甲醛。
還原劑以1 g/L至10 g/L的量包括在無電鍍銅組成物中。
視需要，一種或多種pH調節劑可以包括在無電鍍銅組成物中以調節pH至鹼性pH。可以使用酸和鹼調節pH，包括有機和無機酸和鹼。較佳的是，無機酸或無機鹼或其混合物用於調節無電鍍銅組成物的pH。適用於調節無電鍍銅組成物的pH的無機酸包括例如，磷酸、硝酸、硫酸或鹽酸。適用於調節無電鍍銅組成物的pH的無機鹼包括例如，氫氧化銨、氫氧化鈉或氫氧化鉀。較佳的是，使用氫氧化鈉、氫氧化鉀或其混合物來調節無電鍍銅組成物的pH，最較佳的是，使用氫氧化鈉來調節無電鍍銅組成物的pH。
視需要，一種或多種表面活性劑可包括在本發明之無電鍍銅組成物中。此類表面活性劑包括離子表面活性劑，如陽離子和陰離子表面活性劑，非離子和兩性表面活性劑。可以使用表面活性劑的混合物。表面活性劑可以0.001 g/L至50 g/L的量，較佳的是0.01 g/L至50 g/L的量包括在組成物中。
陽離子表面活性劑包括但不限於四烷基鹵化銨、烷基三甲基鹵化銨、羥乙基烷基咪唑啉、鹵化烷基苯甲烴銨（alkylbenzalkonium halide）、烷基胺乙酸鹽、烷基胺油酸鹽和烷基胺基乙基甘胺酸。
陰離子表面活性劑包括但不限於烷基苯磺酸鹽、烷基或烷氧基萘磺酸鹽、烷基二苯基醚磺酸鹽、烷基醚磺酸鹽、烷基硫酸酯、聚氧乙烯烷基醚硫酸酯、聚氧乙烯烷基酚醚硫酸酯、高級醇磷酸單酯、聚氧化烯烷基醚磷酸（磷酸鹽）和烷基磺基琥珀酸鹽。
兩性表面活性劑包括但不限於2-烷基-N-羧甲基或乙基-N-羥乙基或甲基咪唑鎓甜菜鹼，2-烷基-N-羧甲基或乙基-N-羧甲氧基乙基咪唑鎓甜菜鹼，二甲基烷基甜菜鹼，N-烷基-β-胺基丙酸或其鹽，和脂肪酸醯胺丙基二甲基胺基乙酸甜菜鹼。
較佳的是，表面活性劑係非離子的。非離子表面活性劑包括但不限於烷基苯氧基聚乙氧基乙醇，具有20至150個重複單元的聚氧乙烯聚合物和聚氧乙烯與聚氧丙烯的無規和嵌段共聚物。
以下實例不旨在限制本發明之範圍，而是進一步說明本發明。
實例1-16（本發明）銅的抗鈍化
藉由以下揭露的製程流程藉由處理不含鑽孔特徵的200 μm厚覆銅層壓板來評估在藉由基於酒石酸的無電鍍銅浴處理覆銅層壓板（CCL）的銅表面時抗鈍化添加劑對其的作用。將具有在0.5 mg/L、2 mg/L和5 mg/L濃度下變化的抗鈍化添加劑的還原劑浴與在還原劑浴中不包括抗鈍化添加劑的對照（實例1）獲得的結果進行比較。在不存在抗鈍化添加劑的情況下在特定條件下沒有觀察到無電鍍銅引發。
1. 在約45°C下將每個CCL用20 Vol.% CIRCUPOSIT™調理劑8512鹼性調理劑溶液處理1.5 min；
2. 然後在室溫下將每個CCL用自來水沖洗30 sec；
3. 然後在約28°C下將每個CCL用CIRCUPOSIT™ 6520A預浸料溶液在pH = 2下處理30 sec；
4. 然後在約50°C下將每個CCL浸漬在20 Vol.% CIRCUPOSIT™ 6530催化劑（其為離子水性鹼性鈀催化劑濃縮物（從杜邦公司（DuPont）可獲得））中持續60 sec，其中催化劑用足夠量的碳酸鈉、氫氧化鈉或硝酸緩衝以達到9-9.5的催化劑pH；
5. 然後在室溫下將每個CCL用自來水沖洗30 sec；
6. 然後在約34°C下將每個CCL浸漬在0.6 g/L二甲胺硼烷、5 g/L硼酸、7-7.5的pH範圍以及以表1中示出的濃度的表1中示出的抗鈍化添加劑中的一種的水性溶液中持續1 min，以將鈀離子還原為鈀金屬並且同時使每個CCL的銅鈍化；
7. 然後將每個CCL用自來水沖洗30 sec；以及
8. 然後在約34°C下將每個CCL浸漬在表2的鹼性無電鍍銅浴中並鍍銅持續5 min。
[表1]
[表2]無電鍍銅浴
1
N,N,N’,N’-四(2-羥丙基)乙二胺（從西格瑪-奧德里奇公司（Sigma-Aldrich）可獲得）
| 實例 | 抗鈍化化合物 | 抗鈍化化合物結構 | 濃度（ mg/L ） |
| 1 | 無 | 無 | 0 |
| 2-4 | 2,2’-雙(4,5-二甲基咪唑) | | 0.5, 2, 5 |
| 5-7 | 2-胍基-苯并咪唑 | | 0.5, 2, 5 |
| 8-9 | 2-(胺基乙基)-苯并咪唑二氫氯化物 | | 0.5, 2 |
| 10-11 | 1-(3-胺基丙基)咪唑 | | 0.5, 2 |
| 12 | 2-(1-萘基-甲基)咪唑啉鹽酸鹽 | | 2 |
| 13 | 2-(2-胺基苯基)-1H-苯并咪唑 | | 2 |
| 14 | 2-(2-羥基苯基)-1H-苯并咪唑 | | 2 |
| 15 | 苯并三唑-5-羧酸 | | 2 |
| 16 | | 2 |
| 組分 | 量 |
| 五水合硫酸銅 | 9.6 g/L |
| 羅謝爾鹽 | 35 g/L |
| 氫氧化鈉 | 8 g/L |
| 甲醛 | 4 g/L |
| S-羧甲基半胱胺酸 | 7.5 mg/L |
| Quadrol1 | 100 mg/L |
在每個CCL上進行兩次電化學測量。在具有維持在34°C下的200 mL浴體積和再循環冷卻器的CHInstruments 760e恒電位器上進行電化學測量。當層壓板浸沒在無電鍍銅浴中時，使用具有Ag/AgCl參比電極的兩電極配置進行第一次測量，開路電位測量。在開路電位測量期間要注意不要將用於保持樣品的夾子浸沒。開路電位曲線可被分為兩組：對於實例1的對照如圖 1
所示的沒有展現出開路電位向更大的陰極電位的突然偏移（沒有無電引發）的樣品，以及如圖 2
所示的展現出開路電位向更大的陰極電位的突然偏移（無電引發）的樣品。同時圖 2
係實例6的開路電位曲線，實例2-5和實例7-16的開路電位曲線基本相同。作為對照，如圖 1
所示，在不存在抗鈍化添加劑的情況下的開路電位測量觀察到沒有無電引發。用包括抗鈍化化合物的還原溶液處理的CCL具有光滑明亮的銅沈積物。相比之下，用不含抗鈍化化合物的還原溶液處理的CCL具有粗糙且暗的銅沈積物。
在開路電位測量之後，對完全浸沒在無電鍍銅浴中的2.54 x 5.08 cm CCL區域的樣品之間的氧化物的相對量進行比較。還原氧化物的時間越長等於氧化物越多。在將CCL樣品浸沒在6M KOH/1M LiOH電解液中並使用具有Ti棒對電極和Ag/AgCl參比電極的三電極配置施加5 mA的小的陰極電流時，在視覺上評估並且藉由計時電位法測量去除的工件表面上的氧化程度。在計時電位法測量期間監測電位，並且當電位偏移至析氫電位（ca. -1.4 V）時，則認為CCL表面上的氧化物的還原係完全的。具有顯著量的待還原的氧化物的CCL在約10 sec內已經完全還原，如圖 3
關於實例6所示；然而，實例2-5和實例7-16具有基本上相同的計時電位法圖。具有較多氧化的CCL需要10倍以上的時間才能實現表面氧化的完全還原，如圖 4
關於實例1的對照所示。
實例17-34（對比）銅的鈍化
重複以上實例1-16中揭露的程序和配製物，除了包括在還原劑浴中的添加劑以及添加劑的量係表3中揭露的那些以外。
[表3]
| 實例 | 添加劑化合物 | 添加劑化合物結構 | 濃度（ mg/L ） |
| 17-18 | 1-(2-胺基苯基)-1H-吡唑 |  | 0.5, 2 |
| 19-20 | 1-(3-胺基丙基)-2-甲基-1H-咪唑 |  | 0.5, 2 |
| 21-22 | 1,2,4-三唑-3-羧酸 |  | 0.5, 2 |
| 23-24 | 1,2,4-三唑并(1,5-a)嘧啶 |  | 0.5, 2 |
| 25-26 | 1H-苯并三唑-4-磺酸 |  | 0.5, 2 |
| 27-28 | 1H-四唑-5-乙酸 |  | 0.5, 2 |
| 29-30 | 2-(甲硫基)苯并咪唑 |  | 0.5, 2 |
| 31-32 | 2-苯基咪唑 |  | 0.5, 2 |
| 33-34 | 4-(咪唑-1基)苯酚 |  | 0.5, 2 |
在具有維持在34°C下的200 mL浴體積和再循環冷卻器的CHInstruments 760e恒電位器上對每個CCL進行電化學測量。當層壓板浸沒在無電鍍銅浴中時，使用具有Ag/AgCl參比電極的兩電極配置進行開路電位測量。在開路電位測量期間要注意不要將用於保持樣品的夾子浸沒。所有樣品的開路電位曲線均未顯示出開路電位向更大的陰極電位的突然偏移（沒有無電引發）。開路電位曲線基本上與圖 1
中關於實例1的對照所示的相同。
無
[圖 1
]係示出沒有引發無電鍍銅的電位（以伏特計）相對於時間（以秒計）之開路電路圖。
[圖 2
]係示出快速引發無電鍍銅的電位（以伏特計）相對於時間（以秒計）之開路電路圖。
[圖 3
]係示出用於還原銅氧化物的短時間段的電位（以伏特計）相對於時間（以秒計）之計時電位法圖。
[圖 4
]係示出用於還原銅氧化物的長時間段的電位（以伏特計）相對於時間（以秒計）之計時電位法圖。
無
Claims (9)
- 一種無電鍍銅方法，其包括： a) 提供包含銅的基材； b) 向該基材的銅施加催化劑； c) 用包含咪唑化合物的水性組成物處理該基材的經催化的銅，其中該咪唑化合物具有下式：(I)， 其中R1 和R2 獨立地選自氫、(C1 -C4 )烷基和酯基或R1 和R2 的碳可以一起形成取代或未取代的稠合的六員碳芳環，其中該六員碳芳環上的取代基選自由以下組成之群組：羧基、羧基(C1 -C4 )烷基、羥基、羥基(C1 -C4 )烷基、胺基和胺基(C1 -C4 )烷基，R3 係氫、羥基、羥基(C1 -C4 )烷基、胺基或胺基(C1 -C4 )烷基，並且A可以是氮原子或碳原子，其中當A係碳原子時，該碳原子可以具有選自由以下組成之群組之取代基：取代或未取代的咪唑、胍基、取代的苯基、以及胺基(C1 -C4 )烷基； d) 向該基材的經處理的銅施加無電鍍銅浴；以及 e) 用該無電鍍銅浴在該基材的經處理的銅上無電鍍銅。
- 一種無電鍍銅方法，其包括： a) 提供包含銅的基材； b) 向該基材的銅施加催化劑； c) 用包含還原劑和咪唑化合物的水性組成物處理該基材的經催化的銅，其中該咪唑化合物具有下式：(I)， 其中R1 和R2 獨立地選自氫、(C1 -C4 )烷基和酯基或R1 和R2 的碳可以一起形成取代或未取代的稠合的六員碳芳環，其中該六員碳芳環上的取代基選自由以下組成之群組：羧基、羧基(C1 -C4 )烷基、羥基、羥基(C1 -C4 )烷基、胺基和胺基(C1 -C4 )烷基，R3 係氫、羥基、羥基(C1 -C4 )烷基、胺基或胺基(C1 -C4 )烷基，並且A可以是氮原子或碳原子，其中當A係碳原子時，該碳原子可以具有選自由以下組成之群組之取代基：取代或未取代的咪唑、胍基、取代的苯基、以及胺基(C1 -C4 )烷基； d) 向該基材的經處理的銅施加無電鍍銅浴；以及 e) 用該無電鍍銅浴在該基材的經處理的銅上無電鍍銅。
- 如請求項2所述之方法，其進一步包括在施加該催化劑之前，向該包含銅的基材施加調理劑。
- 如請求項2所述之方法，其進一步包括在用該包含還原劑和咪唑化合物的水性組成物處理之後，用水沖洗溶液沖洗該帶有經催化的銅的基材。
- 如請求項4所述之方法，其中該水沖洗溶液包含具有下式的咪唑化合物：(I)， 其中R1 和R2 獨立地選自氫、(C1 -C4 )烷基和酯基或R1 和R2 的碳可以一起形成取代或未取代的稠合的六員碳芳環，其中該六員碳芳環上的取代基選自由以下組成之群組：羧基、羧基(C1 -C4 )烷基、羥基、羥基(C1 -C4 )烷基、胺基和胺基(C1 -C4 )烷基，R3 係氫、羥基、羥基(C1 -C4 )烷基、胺基或胺基(C1 -C4 )烷基，並且A可以是氮原子或碳原子，其中當A係碳原子時，該碳原子可以具有選自由以下組成之群組之取代基：取代或未取代的咪唑、胍基、取代的苯基、以及胺基(C1 -C4 )烷基。
- 如請求項2所述之無電鍍銅方法，其中該咪唑化合物係以0.1 mg/L至100 mg/L的濃度。
- 如請求項2所述之無電鍍銅方法，其中該水性組成物進一步包含一種或多種酸。
- 如請求項2所述之無電鍍銅方法，其中該咪唑化合物具有下式：(II)， 其中R1 和R2 獨立地是氫、(C1 -C3 )烷基和酯基，或R1 和R2 與所有它們的碳原子一起形成取代或未取代的六員碳芳族稠環，其中該六員碳芳族稠環上的取代基選自由以下組成之群組：羧基、羧基(C1 -C3 )烷基、羥基、羥基(C1 -C3 )烷基、胺基和胺基(C1 -C3 )烷基，R3 係氫或胺基(C1 -C2 )烷基，並且R4 選自由以下組成之群組：取代或未取代的咪唑、胍基、取代的苯基、胺基(C1 -C4 )烷基、以及萘基(C1 -C4 )烷基，其中該苯基上的取代基選自由羥基和胺基組成之群組並且該咪唑上的取代基選自由(C1 -C3 )烷基、羥基(C1 -C3 )烷基和胺基(C1 -C3 )烷基組成之群組。
- 如請求項8所述之無電鍍銅方法，其中該咪唑化合物選自由以下組成之群組：2,2’-雙(4,5-二甲基咪唑)、2-胍基苯并咪唑、2-(胺基甲基)苯并咪唑二氫氯化物、2-(2-胺基苯基)-1H-苯并咪唑、2-(2-羥基苯基)-1H-苯并咪唑及其混合物。
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US16/679,373 | 2019-11-11 | ||
| US16/679,373 US20210140052A1 (en) | 2019-11-11 | 2019-11-11 | Electroless copper plating and counteracting passivation |
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| TW202118899A true TW202118899A (zh) | 2021-05-16 |
| TWI769549B TWI769549B (zh) | 2022-07-01 |
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| US (1) | US20210140052A1 (zh) |
| EP (1) | EP3819397A1 (zh) |
| JP (1) | JP7012135B2 (zh) |
| KR (1) | KR102515750B1 (zh) |
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| US4170819A (en) * | 1978-04-10 | 1979-10-16 | International Business Machines Corporation | Method of making conductive via holes in printed circuit boards |
| US4301196A (en) * | 1978-09-13 | 1981-11-17 | Kollmorgen Technologies Corp. | Electroless copper deposition process having faster plating rates |
| JPS63206476A (ja) * | 1987-02-23 | 1988-08-25 | Hitachi Chem Co Ltd | 無電解銅めつき前処理液 |
| JP3070027B2 (ja) * | 1993-04-21 | 2000-07-24 | 富士通株式会社 | 配線基板の製造方法 |
| US5518760A (en) * | 1994-10-14 | 1996-05-21 | Macdermid, Incorporated | Composition and method for selective plating |
| GB9425031D0 (en) * | 1994-12-09 | 1995-02-08 | Alpha Metals Ltd | Printed circuit board manufacture |
| JP3336535B2 (ja) * | 1995-03-22 | 2002-10-21 | マクダーミッド インコーポレーテッド | 選択的めっき用組成物及び方法 |
| JPH0978251A (ja) * | 1995-09-13 | 1997-03-25 | Hitachi Chem Co Ltd | 無電解銅めっきの前処理液 |
| JP2005002443A (ja) * | 2003-06-13 | 2005-01-06 | Ebara Corp | めっき方法及びめっき装置 |
| US7794531B2 (en) * | 2007-01-08 | 2010-09-14 | Enthone Inc. | Organic solderability preservative comprising high boiling temperature alcohol |
| CN101442885B (zh) * | 2007-11-20 | 2011-06-08 | 富葵精密组件(深圳)有限公司 | 电路板导孔的制作方法 |
| US20140199497A1 (en) * | 2013-01-14 | 2014-07-17 | Tighe A. Spurlin | Methods for reducing metal oxide surfaces to modified metal surfaces |
| GB2516607A (en) * | 2013-03-06 | 2015-02-04 | Cambridge Display Tech Ltd | Organic electronic device |
| EP2784181B1 (en) * | 2013-03-27 | 2015-12-09 | ATOTECH Deutschland GmbH | Electroless copper plating solution |
| US20150024123A1 (en) * | 2013-07-16 | 2015-01-22 | Rohm And Haas Electronic Materials Llc | Catalysts for electroless metallization containing iminodiacetic acid and derivatives |
| CN103476199B (zh) * | 2013-09-27 | 2016-02-03 | 电子科技大学 | 基于铜自催化和化学镀铜的印制电路加成制备方法 |
| US20160348245A1 (en) * | 2015-05-28 | 2016-12-01 | Macdermid, Incorporated | Method of Pretreatment for Electroless Plating |
| CN107460456B (zh) * | 2017-07-31 | 2019-08-20 | 苏州天承化工有限公司 | 一种低钯化学镀铜活化剂及制备方法 |
| US10655227B2 (en) * | 2017-10-06 | 2020-05-19 | Rohm And Haas Electronic Materials Llc | Stable electroless copper plating compositions and methods for electroless plating copper on substrates |
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- 2020-10-12 TW TW109135203A patent/TWI769549B/zh active
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- 2020-10-26 EP EP20203894.9A patent/EP3819397A1/en not_active Withdrawn
- 2020-10-28 KR KR1020200141152A patent/KR102515750B1/ko active IP Right Grant
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| US20210140052A1 (en) | 2021-05-13 |
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| KR20210056902A (ko) | 2021-05-20 |
| JP7012135B2 (ja) | 2022-01-27 |
| JP2021075785A (ja) | 2021-05-20 |
| EP3819397A1 (en) | 2021-05-12 |
| CN112779524A (zh) | 2021-05-11 |
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