CN115261834A - 用于减少铜和铜合金电路的光学反射率的方法和触摸屏装置 - Google Patents
用于减少铜和铜合金电路的光学反射率的方法和触摸屏装置 Download PDFInfo
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- CN115261834A CN115261834A CN202210839862.8A CN202210839862A CN115261834A CN 115261834 A CN115261834 A CN 115261834A CN 202210839862 A CN202210839862 A CN 202210839862A CN 115261834 A CN115261834 A CN 115261834A
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- Prior art keywords
- copper
- palladium
- alloy
- plating
- copper alloy
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 192
- 239000010949 copper Substances 0.000 title claims abstract description 188
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 187
- 229910000881 Cu alloy Inorganic materials 0.000 title claims abstract description 145
- 238000000034 method Methods 0.000 title claims abstract description 71
- 238000001579 optical reflectometry Methods 0.000 title claims abstract description 26
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 160
- 238000007747 plating Methods 0.000 claims abstract description 129
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 84
- 238000007654 immersion Methods 0.000 claims abstract description 50
- 229910001252 Pd alloy Inorganic materials 0.000 claims abstract description 42
- 239000000758 substrate Substances 0.000 claims description 49
- -1 palladium ions Chemical class 0.000 claims description 43
- 229910052751 metal Inorganic materials 0.000 claims description 37
- 239000002184 metal Substances 0.000 claims description 37
- 239000002253 acid Substances 0.000 claims description 33
- 238000000151 deposition Methods 0.000 claims description 28
- 238000009713 electroplating Methods 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 19
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 15
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 13
- 229910001431 copper ion Inorganic materials 0.000 claims description 13
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 12
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 12
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 12
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 12
- 239000003638 chemical reducing agent Substances 0.000 claims description 11
- 239000008139 complexing agent Substances 0.000 claims description 10
- 230000003287 optical effect Effects 0.000 claims description 9
- 239000000654 additive Substances 0.000 claims description 8
- 230000000996 additive effect Effects 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- 229920003023 plastic Polymers 0.000 claims description 5
- 239000004033 plastic Substances 0.000 claims description 5
- 239000003381 stabilizer Substances 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- 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 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 239000004020 conductor Substances 0.000 claims description 3
- 229910052744 lithium Inorganic materials 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 5
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 239000000203 mixture Substances 0.000 description 18
- 230000003197 catalytic effect Effects 0.000 description 17
- 239000000976 ink Substances 0.000 description 17
- 229910001092 metal group alloy Inorganic materials 0.000 description 15
- 150000002739 metals Chemical class 0.000 description 15
- 238000005229 chemical vapour deposition Methods 0.000 description 14
- 230000008021 deposition Effects 0.000 description 14
- 238000005240 physical vapour deposition Methods 0.000 description 14
- 238000011282 treatment Methods 0.000 description 14
- 229910052757 nitrogen Inorganic materials 0.000 description 12
- 239000000243 solution Substances 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 229910045601 alloy Inorganic materials 0.000 description 9
- 239000000956 alloy Substances 0.000 description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 150000002431 hydrogen Chemical class 0.000 description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 8
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 7
- 238000001723 curing Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 6
- HHLFWLYXYJOTON-UHFFFAOYSA-N glyoxylic acid Chemical compound OC(=O)C=O HHLFWLYXYJOTON-UHFFFAOYSA-N 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 5
- 229910052750 molybdenum Inorganic materials 0.000 description 5
- 239000011733 molybdenum Substances 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 229920000139 polyethylene terephthalate Polymers 0.000 description 5
- 239000005020 polyethylene terephthalate Substances 0.000 description 5
- 229910052709 silver Inorganic materials 0.000 description 5
- 239000004332 silver Substances 0.000 description 5
- 229910052719 titanium Inorganic materials 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000005751 Copper oxide Substances 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 4
- 150000007513 acids Chemical class 0.000 description 4
- 230000004913 activation Effects 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000011889 copper foil Substances 0.000 description 4
- 229910000431 copper oxide Inorganic materials 0.000 description 4
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 150000002940 palladium Chemical class 0.000 description 4
- 229910052697 platinum Inorganic materials 0.000 description 4
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 4
- 238000007740 vapor deposition Methods 0.000 description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical class OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 3
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 3
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical class CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 238000007772 electroless plating Methods 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 230000000977 initiatory effect Effects 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 229910052758 niobium Inorganic materials 0.000 description 3
- 239000010955 niobium Substances 0.000 description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 3
- UEZVMMHDMIWARA-UHFFFAOYSA-M phosphonate Chemical compound [O-]P(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-M 0.000 description 3
- 229910052703 rhodium Inorganic materials 0.000 description 3
- 239000010948 rhodium Substances 0.000 description 3
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 3
- 229910052707 ruthenium Inorganic materials 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 229910052715 tantalum Inorganic materials 0.000 description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910052726 zirconium Inorganic materials 0.000 description 3
- ISQSUCKLLKRTBZ-UHFFFAOYSA-N (phosphonomethylamino)methylphosphonic acid Chemical compound OP(O)(=O)CNCP(O)(O)=O ISQSUCKLLKRTBZ-UHFFFAOYSA-N 0.000 description 2
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 description 2
- URDCARMUOSMFFI-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(2-hydroxyethyl)amino]acetic acid Chemical class OCCN(CC(O)=O)CCN(CC(O)=O)CC(O)=O URDCARMUOSMFFI-UHFFFAOYSA-N 0.000 description 2
- 229920002284 Cellulose triacetate Polymers 0.000 description 2
- 239000005749 Copper compound Substances 0.000 description 2
- 229920000089 Cyclic olefin copolymer Polymers 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical class OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 2
- DBVJJBKOTRCVKF-UHFFFAOYSA-N Etidronic acid Chemical compound OP(=O)(O)C(O)(C)P(O)(O)=O DBVJJBKOTRCVKF-UHFFFAOYSA-N 0.000 description 2
- 229910001111 Fine metal Inorganic materials 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
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- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 2
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- 238000005260 corrosion Methods 0.000 description 2
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- 150000002500 ions Chemical class 0.000 description 2
- 229910052741 iridium Inorganic materials 0.000 description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- YACKEPLHDIMKIO-UHFFFAOYSA-N methylphosphonic acid Chemical compound CP(O)(O)=O YACKEPLHDIMKIO-UHFFFAOYSA-N 0.000 description 2
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- 150000002894 organic compounds Chemical class 0.000 description 2
- 229910052762 osmium Inorganic materials 0.000 description 2
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- XFNJVJPLKCPIBV-UHFFFAOYSA-N trimethylenediamine Chemical compound NCCCN XFNJVJPLKCPIBV-UHFFFAOYSA-N 0.000 description 2
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 1
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- QQIRJGBXQREIFL-UHFFFAOYSA-N butanedioic acid;ethane-1,2-diamine Chemical compound NCCN.OC(=O)CCC(O)=O QQIRJGBXQREIFL-UHFFFAOYSA-N 0.000 description 1
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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
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- 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
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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- H05K1/0274—Optical details, e.g. printed circuits comprising integral optical means
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- H—ELECTRICITY
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
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- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/18—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material
- H05K3/181—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material by electroless plating
Abstract
本发明是关于用于一种用于减少铜和铜合金电路的光学反射率的方法和触摸屏装置,其中钯或钯合金的薄层通过浸镀式电镀沉积到所述铜或铜合金上。借此获得浅灰色或浅灰黑色或黑色的钝色层,且减少所述铜或铜合金电路的光学反射率。根据本发明的方法特别适合于制造图像显示装置、触摸屏装置及相关电子组件。
Description
本申请为申请日2015年8月7日,申请号201580043321.2,名称为“用于减少铜和铜合金电路的光学反射率的方法和触摸屏装置”的发明专利申请的分案申请。
技术领域
本发明涉及一种用于减少电子组件(诸如图像显示装置和触摸屏装置)制造中铜和铜合金电路的光学反射率的方法。
背景技术
电子组件(诸如图像显示装置和触摸屏装置)的电路可通过不同方法制造。所述电路最常包括铜或铜合金,归因于所述材料的高电导率。
所述电路可(例如)通过物理气相沉积法(PVD)(诸如溅镀)或化学气相沉积方法(CVD)(其中铜或铜合金沉积到介电衬底上)制造。任选地,首先将粘着层(例如,钛、钼的层,或包括钛层和钼层的多层堆栈)沉积到衬底上,接着沉积为电路的主要贡献者的铜或铜合金。
在另一种用于将电路沉积到电子组件(诸如,图像显示装置和触摸屏装置)制造中的介电衬底上的方法中,通过铜或铜合金的无电电镀,将电路沉积到用贵金属活化的衬底上。所述在用贵金属活化的衬底上的无电(自催化)电镀法揭示于EP 2 524 976 A1中。
电子组件(诸如,图像显示装置和触摸屏装置)的电路还可通过添加剂方法制造,其中将催化墨沉积到介电衬底材料(诸如,聚对苯二甲酸伸乙酯(PET)箔)上,且其后将其固化。固化催化墨接着用作电镀基体,其用于上面铜和铜合金的无电(自催化)电镀。所述额外铜或铜合金层为必需的,以便获得用于电路图案(其通常不仅仅通过固化催化墨获得)的所需电导率。用于将金属和金属合金(诸如,铜和铜合金)无电电镀至固化催化墨上的方法(例如)揭示于EP 13188464.5中。
在另一种制造方法中,电路通过将铜或铜合金电镀至附着至介电衬底的导电图案或层上来沉积。
独立于用于将铜或铜合金沉积到衬底上的方法的所述铜或铜电路的一个缺点为有光泽的表面的强光学反射率(其导致所述电路的光学可见度,不管极窄电路线宽为(例如)50μm、20μm、10μm和10μm以下)和用于图像显示装置和触摸屏装置的专有电路图案几何形状(诸如矩形或六边形网格)。
用于减少电子组件(诸如,图像显示装置和触摸屏装置)制造中铜和铜合金表面的光学反射率的不同方法于此项技术中已知。
用于电子组件(诸如,触摸屏装置)制造中的铜电路的变黑程序揭示于US 2013/0162547 A1中,其中将铜表面化学氧化成棕色Cu2O和黑色CuO。借此,铜电路表面的光学反射减少。
用于电子组件(诸如,触摸屏装置)制造中的铜电路的另一个化学氧化程序揭示于US 2014/0057045 A1中。用化学物质(诸如,硒化合物、硫酸盐化合物或三唑化合物)处理铜表面,以便获得变暗铜表面,且借此减少铜电路的光学反射率。
用于减少由银制成的电路的光学反射率的方法揭示于US 7,985,527 B2中。首先通过化学氧化处理将银变黑,接着通过将所述银氧化物与包括钯离子或金属钯的溶液接触来稳定形成的黑色银氧化物。
背景技术中所揭示的所述化学氧化处理的缺点为所述脆性的表面氧化层的弱机械稳定性,且对底层的铜表面或银表面具有低粘着度。相应地,所述变黑电路缺乏可靠性。
所述化学氧化处理的另一个缺点为电路管线的铜于氧化铜形成期间消耗。相应地,部分初始铜电路转化成非导电铜氧化物,且所述铜电路的特定的电阻率在铜氧化物形成之后增加。
EP 0 926 263 A2涉和用于将树脂层粘结至粗糙化铜箔以便形成多层印刷电路板的方法。方法涉及微蚀刻所述铜箔,且其后将铜箔与助粘组合物接触,所述助粘组合物包括还原剂和选自由以下各者组成的群组的金属:金、银、钯、钌、铑、锌、镍、钴、铁和上述金属的合金。在一个实施例中,浸镀式钯溶液与微蚀刻溶液一起用作助粘层。方法并不涉及电路的形成。处理的目的为提供粗糙化铜箔,其后层压至树脂层。根据EP 0 926 263 A2的方法导致形成多层电路板。其并不揭示适用于图像显示装置和触摸屏的铜电路的制造。US 2008/0224314 A1揭示铜互连表面上的顶盖层的形成。顶盖层(参看第[0003]段)可为Ni、Ni(P)、Ni(Co)、或Co(P)。第[0003]段,顶盖层用以于嵌花铜特征上形成扩散障壁和防腐蚀层。推荐将“活化层”(诸如,钯)沉积到用以促进另一种金属之后续沉积的铜互连的表面上。US2008/0224314 A1并不揭示铜或铜合金电路的形成,其上面已沉积钯或钯合金作为最外层。
本发明的目标
本发明的目标为提供一种用于减少具有足够机械稳定性和低电阻率电路的电子装置(诸如,图像显示装置和触摸屏装置)制造中的铜和铜合金表面的光学反射率的方法。
发明内容
此目标通过一种用于减少铜和铜合金电路的光学反射率的方法来解决,其以此顺序包括以下步骤
(i)提供介电衬底,
(ii)将铜或铜合金沉积到所述介电衬底上,前提是当铜或铜合金通过无电(自催化)电镀或电镀来沉积时所述介电衬底包括电镀基体,及
(iii)通过浸镀式电镀,将钯或钯合金层沉积到所述铜或铜合金上,且借此减少所述铜或铜合金的光学反射率
且其中结构化步骤(ii)中沉积的铜或铜合金以在步骤(iii)之前或在步骤(iii)之后形成电路。
在本发明的意义内,沉积和沉积铜或铜合金包含物理气相沉积法(PVD)(诸如,溅镀)或化学气相沉积法(CVD)、无电(自催化)或电镀,借此将铜或铜合金沉积到介电衬底上。
所得铜或铜合金电路(具有沉积于所述表面上的薄、浸镀式电镀的钯或钯合金层)具有所需与未处理铜或铜合金电路相比减少的光学反射率,及与通过背景技术中已知氧化处理所获得的变黑铜或铜合金表面相比改良的机械稳定性。此外,所述铜或铜合金电路的耐腐蚀性增加。
此外,浸镀式电镀的钯或钯合金层为极薄的,其意思是仅小部分所述铜或铜合金电路在浸镀式电镀期间经消耗。从而,所述铜或铜合金电路的电阻率也按需要为低的。用于减少铜和铜合金表面的光学反射率的方法特别地适于电子组件(诸如,图像显示装置和触摸屏装置)制造。
本发明进一步提供一种包括铜或铜合金电路及通过浸镀式电镀沉积到所述铜或铜合金电路上的钯或钯合金层的触摸屏装置。
附图说明
图1展示用根据本发明的方法处理铜电路的图像(实例4)。FIB/SEM分析于FEINova NanoLab 600Dual Beam FIB上进行。用于FIB切口的关注区域为涂布有碳的溅镀以实现与底层钯的良好对比。将第二层铂施加于碳层之上,其需要进行FIB测量。
图2展示用根据本发明的方法处理铜电路的图像(实例3)。FIB/SEM分析进行于FEINova NanoLab 600Dual Beam FIB上。用于FIB切口的关注区域为涂布有碳的溅镀以实现与底层钯良好对比。将第二层铂施加于碳层之上,其需要进行FIB测量。
具体实施方式
用于电子组件(诸如,图像显示装置和触摸屏装置)的适合介电衬底材料包括塑料材料和玻璃材料。
适合的塑料材料的实例包括聚对苯二甲酸伸乙酯(PET)、聚丙烯酸酯、聚氨甲酸酯(PU)、环氧树脂、聚酰亚氨、聚烯烃、聚碳酸酯(PC)、聚甲基丙烯酸甲酯(PMMA)、聚萘二甲酸伸乙酯(PEN)、聚醚砜(PES)、环烯聚合物(COC)、三乙酰纤维素(TAC)、聚乙烯醇(PVA)和聚苯乙烯(PS)。
适合的玻璃材料的实例包括二氧化硅玻璃(非晶硅二氧化物材料)、钠钙玻璃、漂浮玻璃、氟化物玻璃、铝硅酸盐玻璃、磷酸盐玻璃、硼酸盐玻璃、硼硅酸盐玻璃、硫族化物玻璃、蓝宝石玻璃和玻璃陶瓷材料。
介电衬底材料可呈硬质薄片或可弯曲箔的形式提供。
优选地,介电衬底材料选自在塑料材料和玻璃材料中的光学透明材料。由铜或铜合金制成的电路可通过不同方法沉积到介电衬底上。所述电路可直接沉积成所需图案,或所述图案在铜或铜合金沉积之后通过选择性去除部分铜或铜合金层形成。
根据本发明方法,通过浸镀式电镀将钯或钯合金层沉积到所述铜或铜合金上可在电路已经形成所需图案之后或之前进行。
根据本本发明的第一实施例,步骤为
(iii)通过浸镀式电镀,将钯或钯合金层沉积到铜或铜合金上于步骤(ii)中所沉积的铜或铜合金(其经结构化以仅在步骤(iii)之后形成电路)上执行。
根据本发明的第二和优选实施例,步骤为
(iii)通过浸镀式电镀,将钯或钯合金层沉积到铜或铜合金上于步骤(ii)中所沉积的铜或铜合金(其经结构化以在步骤(iii)之前形成电路)上执行。
铜和铜合金电路可通过选自包括以下各者的群的方法沉积到介电质上:物理气相沉积(PVD)、化学气相沉积(CVD)、无电(自催化)电镀和电镀,其限制条件为当铜或铜合金通过无电(自催化)电镀或电镀来沉积时所述介电衬底包括电镀基体。
在本发明的第一实施例中,由铜或铜合金制成的所述电路通过气相沉积法(诸如,PVD、CVD)和相关方法(诸如,等离子加强CVD)直接沉积到介电衬底上。用于铜或铜合金的沉积的所述方法为此项技术中已知。
在第二实施例中,由铜或铜合金制成的电路通过气相沉积法(诸如,PVD和CVD)及相关技术沉积到附着至介电衬底的粘着层上。
用于此第二实施例的适合粘着层材料为(例如)钼、钛、锆、铝、铬、钨、铌、钽、上述的合金和多层堆栈。所述粘着层还可通过气相沉积法(诸如,PVD和CVD)及相关方法来沉积。
在本发明的第三实施例中,由铜或铜合金制成的电路通过无电(自催化)电镀沉积到介电衬底上。需要介电衬底之上的电镀基体。否则,不可能将铜或铜合金自催化电镀至介电衬底上。
无电(自催化)电镀电解质应理解为包括化学还原剂的电镀电解质,且用于自催化电镀。
在本发明的第四实施例中,通过电镀,将由铜或铜合金制成的电路沉积到介电衬底(其于本文中也是指“电镀基体”)的导电部分上。所述导电部分可为(例如)通过气相沉积法(诸如,PVD、CVD)及相关技术沉积到介电衬底上的金属或金属合金层。
用于上面电镀铜和铜合金的另一种类型的适合电镀基体为导电聚合物,诸如聚噻吩、聚呲咯和聚苯氨和上述衍生物,其例如通过浸渍涂布或旋转涂布、压花等,可沉积到介电衬底上。
常规铜或铜合金电镀浴可用于在介电衬底之上形成电路。适合的铜或铜合金电镀浴组合物为此项技术中已知,且(例如)揭示于“现代电镀(Modern Electroplating)”,第4版,M.Schlesinger和M.Paunovic编,John Wiley&Sons,Inc.,2000,第61至103页中。特别适合的电镀浴组合物包括铜离子、酸、有机添加剂和卤化物离子的来源。
术语“电镀基体”本文定义为优选地于介电衬底之上的表面或部分表面,其包括催化活性金属,且借此引发上面铜或铜合金的无电(自催化)电镀,和/或提供用于上面的铜和铜合金的连续电镀的导电材料。
包括于引发铜或铜合金的无电(自催化)电镀的电镀基体中的适合金属和金属合金进一步于本文中称作“催化活性金属”。
用于引发上面铜或铜合金的无电(自催化)电镀的所述电镀基体的适合催化活性金属和金属合金为(例如)铜、银、金、钌、铑、钯、锇、铱和铂、混合物及其合金。催化活性金属或金属合金可(例如)呈离子的形式、作为胶体、作为嵌入粘合剂中的金属粒子和作为包括(例如)通过PVD、CVD及相关技术沉积的所述金属的层来提供。
相应地,电镀基体包括引发上面铜或铜合金的无电(自催化)电镀的催化活性金属或引发上面铜或铜合金的电镀的导电材料。
根据本发明的电镀基体于此项技术中还称为“晶种层”。电镀基体或晶种层与上面沉积的电路的区别在于比用作电路的铜或铜合金层薄得多的所述电镀基体厚度。相应地,电镀基体不适合于输送用于给定电子组件的所需电流。电镀基体的厚度仅为一定纳米,例如1至50nm,然而电路的厚度优选地为至少500nm或甚至1μm或1μm以上,以便于给定电子组件,诸如触摸屏装置中承载所需电流量。
所述电镀基体可直接或(例如)在具有粘着层的所述介电衬底的表面改质之后沉积到介电衬底上。用于呈离子和胶体形式的所述催化活性金属的适合粘着层为(例如)含氮物质和羟基羧酸。
金属,诸如钼、钛、锆、铝、铬、钨、铌、钽及其合金提供塑料材料和玻璃材料上电路的极良好的粘着性,但不引发铜或铜合金的无电(自催化)电镀。相应地,对于所述“非催化”金属和金属合金,在上面无电(自催化)电镀铜或铜合金之前需要用催化活性金属活化。
用于将铜或铜合金无电(自催化)电镀至粘着层(选自钼、钛、锆、铝、铬、钨、铌、钽和其合金)上的方法揭示于EP 2 524 976A1中。
用于包括呈离子或胶状形式的催化活性金属的铜和铜合金的无电(自催化)电镀的适合电镀基体(例如)揭示于ASM手册(ASM Handbook),第5卷,表面工程(SurfaceEngineering),1194,第317至318页中。
用于铜或铜合金的无电(自催化)电镀和铜和铜合金的电镀的另一种类型适合电镀基体为金属和金属合金,其通过PVD或CVD方法呈薄层或图案的形式沉积到介电衬底上。如果沉积为电镀基体的所述金属或金属合金层对于铜或铜合金的无电(自催化)电镀为催化活性的,那么不需要用于无电(自催化)电镀的进一步活化。
用于铜和铜合金的无电(自催化)电镀的另一种类型的适合电镀基体为催化墨,其包括粘合剂材料和在沉积催化墨至介电衬底上之后可转化成精细金属或金属合金粒子的催化活性金属或其混合物或其前驱体的精细粒子。
精细金属或金属合金粒子(或其前驱体在活化之后)充当用于铜和铜合金的无电(自催化)电镀的电镀基体。
催化墨中的“催化活性金属”由对于待通过无电(自催化)电镀沉积的金属或金属合金为催化活性的金属和/或金属合金的精细粒子组成。所述催化活性金属或金属合金为此项技术中已知。适合的催化活性金属为(例如)铜、银、金、钌、铑、钯、锇、铱和铂、其混合物和合金。
包括催化活性金属粒子的适合催化墨揭示于(例如)US 8,202,567 B2和WO 2014/009927 A2中。
催化墨中的粘合剂优选地选自无机粘合剂、高分子粘合剂和混合无机高分子粘合剂。
催化墨可通过方法(诸如,网版印刷、压花、喷墨印刷、弹性凸版印刷、凹版印刷、平版印刷、压印及其类似方法)沉积到介电衬底上。
催化墨在沉积到介电衬底上之后的固化意思是干燥、凝固及将催化墨固定至介电衬底的方法。适合的固化方法为(例如)通过红外线加热器加热、用紫外线加热器固化、用激光固化、用对流加热器固化等。
然后,将铜或铜合金层通过无电(自催化)电镀沉积到所述固化催化墨上。用于将金属和金属合金(诸如,铜和铜合金)无电(自催化)电镀至固化催化墨上的适合方法揭示于EP 13188464.5中。
用于本发明所有实施例的铜和铜合金沉积的适合无电(自催化)电镀电解质包括铜离子来源和任选的第二金属离子、至少一种络合剂、至少一种稳定剂添加剂和还原剂来源。
铜离子的浓度优选范围介于1至5g/l。
至少一种络合剂的浓度优选范围介于5至50g/l。
还原剂的浓度优选范围介于2至20g/l。
铜离子来源优选地选自水溶性铜盐及其它水溶性铜化合物。
铜离子来源更优选地选自包括以下各者的群组:硫酸铜、氯化铜、硝酸铜、乙酸铜、甲烷磺酸铜、氢氧化铜;上述的水合物和混合物。
至少一种络合剂优选地选自由羧酸、聚羧酸、羟基羧酸、氨基羧酸、烷醇氨和上述酸的盐组成的群组。
至少一种络合剂更优选地选自包括以下各者的群组:聚氨基单丁二酸、聚氨基二丁二酸、酒石酸盐、N,N,N',N'-四-(2-羟丙基)-乙二胺、N'-(2-羟乙基)-乙二胺-N,N,N'-三乙酸、乙二胺-四乙酸、其盐和混合物。
优选聚氨基单丁二酸包含乙二胺单丁二酸、二亚乙基三胺单丁二酸、三伸乙基四氨单丁二酸、1,6-己二氨单丁二酸、四伸乙基五氨单丁二酸、2-羟基伸丙基-1,3-二氨单丁二酸、1,2-丙二氨单丁二酸、1,3-丙二氨单丁二酸、顺环己二氨单丁二酸、反环己二氨单丁二酸和伸乙基双(氧基伸乙基氮基)单丁二酸。
优选聚氨基二丁二酸包含乙二胺-N,N'-二丁二酸、二伸乙基三氨-N,N"-二丁二酸、三伸乙基四氨-N,N"'-二丁二酸、1,6-己二氨N,N'-二丁二酸、四伸乙基五氨-N,N""-二丁二酸、2-羟基伸丙基-1,3-二氨-N,N'-二丁二酸、1,2丙二氨-N,N'-二丁二酸、1,3-丙二氨-N,N"-二丁二酸、顺环己二氨-N,N'-二丁二酸、反环己二氨-N,N'-二丁二酸和伸乙基双(氧基伸乙基氮基)-N,N'-二丁二酸。
用于无电铜电镀电解质的适合稳定剂添加剂为(例如)化合物,诸如巯基苯并噻唑、硫脲及其衍生物、各种其它硫化合物、氰化物和/或亚铁氰化物和/或钴氰化盐、聚乙二醇衍生物、杂环氮化合物,诸如2,2'-二吡啶基、甲基丁炔醇和丙腈。此外,分子氧还可通过使稳定空气流穿过铜电解质用作稳定剂添加剂(ASM手册,第5卷:表面工程,第311至312页)。
所述电镀浴组合物优选地为碱,且视情况可包括碱物质,诸如氢氧化钠和/或氢氧化钾,以便获得所需pH值。用于根据本发明的方法的步骤(ii)的无电(自催化)电镀浴的pH值更优选地范围介于11至14、最优选地12.5至13.5。
还原剂优选地选自包括以下各者的群组:甲醛、次磷酸盐离子、乙醛酸、二甲氨硼烷、硼氢化物及其混合物。
用于第二金属离子(除铜离子以外)的任选的来源为(例如)金属(诸如,镍)的水溶性盐和水溶性化合物。
用于铜和铜合金的无电电镀的优选电镀浴包括用于铜离子的来源和用于第二金属离子的任选的来源、以下各者的来源:作为还原剂的甲醛或乙醛酸和作为络合剂的至少一种聚氨基二丁二酸、或至少一种聚氨基单丁二酸、或至少一种聚氨基二丁二酸和至少一种聚氨基单丁二酸或酒石酸盐的混合物、N,N,N',N'-肆-(2-羟丙基)-乙二胺和N'-(2-羟乙基)-乙二胺-N,N,N'-三乙酸的混合物或N,N,N',N'-肆-(2-羟丙基)-乙二胺和乙二胺四乙酸及其盐的混合物。所述络合剂尤其优选地与作为还原剂的乙醛酸组合。
用于铜和铜合金的无电(自催化)电镀的电镀浴在步骤(ii)期间优选地保持在20至60℃、更优选地25至55℃且最优选地25至45℃范围内的温度。
介电衬底优选地与无电(自催化)电镀浴在步骤(ii)期间接触历时0.5至20分钟、更优选地1至15分钟且最优选地2至10分钟。如果需要特别薄或厚的铜或铜合金层,那么电镀时间还可在所述范围之外。
借此,所获得的铜或铜合金电路具有铜色的光泽表面和高光学反射率。
结构化步骤(ii)中沉积的铜或铜合金以在步骤(iii)之前或在步骤(iii)之后,即在通过浸镀式电镀将钯或钯合金层沉积到所述铜或铜合金上之前或之后形成电路,且借此减少铜或铜合金的光学反射率。自沉积铜或铜合金形成电路的方法为此项技术中已知。
步骤(ii)中形成电路的铜或铜合金的无电(自催化)电镀可于水平、卷盘至卷盘、垂直和垂直输送化电镀设备中进行。所述设备为此项技术中已知。
步骤(ii)中形成电路的铜或铜合金的电镀可于水平、卷盘至卷盘、垂直和垂直输送化电镀设备中进行。所述设备为此项技术中已知。
根据本发明的方法的步骤(ii)中铜或铜合金的气相沉积可于PVD和CVD方法的标准设备中进行。所述设备和适合的PVD及CVD方法为此项技术中已知。
在本发明的一个实施例中,在步骤(ii)和(iii)之间,步骤(ii)中获得的铜或铜合金电路接着与包括至少一种膦酸盐化合物的调节剂溶液接触。任选的调节剂溶液优选地为水溶液。术语“膦酸盐化合物”本文中定义为含有-C-PO(OH)2和/或-C-PO(OR2)基团的有机化合物,其中R选自包括以下各者的群组:经取代和不经取代的烷基、芳基和烷芳基。
当步骤(iii)中施加的浸镀式电镀浴包括膦酸盐化合物时,此实施例尤佳。
更优选地,至少一种膦酸盐化合物选自根据式(1)的化合物
其中
R1选自由以下各者组成的群组:
R2选自由以下各者组成的群组:
R3选自由以下各者组成的群组:
R4选自由以下各者组成的群组:
n为整数且范围介于1至6;m为整数且范围介于1至6;o为整数且范围介于1至6;p为整数且范围介于1至6且
X选自由以下各者组成的群组:氢和适合的反离子。适合的反离子为(例如)锂、钠、钾和铵。
更优选地,R1和R3为
且
优选地,n、m、o和p分别选自1和2。更优选地,n、m为1;且o和p为2。
任选的调节剂溶液中的至少一种膦酸盐化合物最优选地选自包括以下各者的群组:1-羟基乙烷-1,1,-二膦酸、羟乙基氨基二(亚甲基膦酸)、羧甲基氨基二(亚甲基膦酸)、氨基参(亚甲基膦酸)、氮基参(亚甲基膦酸)、乙二胺四(亚甲基膦酸)、己二氨四(亚甲基膦酸)、N-(膦酰甲基)酰亚氨二乙酸、二伸乙基三氨-N,N,N',N”,N”-五-(甲基膦酸)、2-丁烷膦酸盐1,2,4-三甲酸、乙烷-1,2-双(亚氨基双-(甲基膦酸))和2-膦酸丁烷-1,2,4-三甲酸。
任选的调节剂溶液中的至少一种膦酸盐化合物的浓度优选范围介于0.3至20mmol/l、更优选地0.3至20mmol/l和甚至更优选地0.3至8mmol/l。
介电衬底视情况可在步骤(ii)与步骤(iii)之间与酸性水溶液接触。所述酸性水溶液优选地具有在0.5至2范围内的pH值,且包括硫酸。铜表面的所述处理用于清洁而不用于蚀刻目的。因此,通常在根据本发明的步骤(ii)与步骤(iii)之间的清洁步骤中不采用所谓的微蚀刻溶液(其含有氧化剂以自表面蚀刻掉铜)。
当在步骤(ii)与步骤(iii)之间使用所述水性酸性溶液时,根据本发明的方法的步骤(ii)中沉积的铜或铜合金的表面经清洁,且更优选地适于钯或钯合金沉积其上(步骤(iii))。
接着,将钯或钯合金层沉积到通过浸镀式电镀在根据本发明的方法的步骤(ii)中获得的铜或铜合金的表面上。
将包括铜或铜合金的介电衬底与浸镀式电镀浴接触。借此,将钯或钯合金的薄层沉积到所述铜或铜合金的表面上。
在根据本发明的浸镀式反应中,通过沉积的铜或铜合金的铜还原钯离子以于铜或铜合金表面上形成还原的金属钯薄膜。相应地,氧化来自铜或铜合金表面的金属铜以形成溶解于浸镀式电镀溶液中的铜离子。此类型反应为选择性的,即钯或钯合金沉积仅于铜或铜合金上进行。
步骤(iii)中浸镀式钯或钯合金沉积到铜或铜合金上可根据2个实施例:
1.结构化步骤(ii)中沉积的铜或铜合金以在于步骤(iii)中沉积钯或钯合金之前形成电路。在此实施例中,钯或钯合金仅选择性地沉积于铜或铜合金电路上。
2.结构化步骤(ii)中沉积的铜或铜合金以在于步骤(iii)中沉积钯或钯合金之后形成电路。在此实施例中,钯或钯合金沉积于铜或铜合金整个表面上。之后仅结构化铜以形成相对应的电路。在此实施例中,通过与铜或铜合金一起的结构化工艺,钯还自表面去除。
通过根据本发明的方法的步骤(iii)的处理,铜或铜合金的颜色自有光泽的铜色变化至钝钝灰色或钝浅灰黑色或钝黑色,其取决于沉积到铜或铜合金电路上的钯或钯合金的厚度,浸镀式电镀浴组合物和电镀参数,诸如在电镀期间的电镀浴温度。借此,所述铜或铜合金的光学反射率减少。
所得钯或钯合金沉积物的颜色可通过色度计测量,且颜色通过L*a*b*色空间系统(由Commission Internationale de I'Eclairage于1976引入)加以描述。值L*指示亮度且a*和b*指示颜色方向。正值a*指示红色,同时负值a*意思是绿色。正值b*指示黄色,且负值b*意思是蓝色。当a*和b*的绝对值增加时,那么颜色的饱和度也增加。值L*范围介于0至100,其中0指示黑色,且100意思是白色。因此,对于本发明的钯或钯合金沉积物,需要低L*值。
绝对值取决于特定技术涂覆变化。通常,经处理的铜或铜合金表面的光学反射率根据涂覆类型和周围衬底表面的反射率加以调整。
在用钯浸镀式溶液处理之前,铜表面的L*值一般在50或较高范围内。处理之后,L*值明显地减少至在10至40或优选地20至35之间的范围。因此,在钯或钯合金沉积之后,铜或铜合金的颜色为钝灰色或钝浅灰黑色或钝黑色。
本发明的暗色钯沉积物的b*值在-15.0至+15.0范围内。因此,本发明的暗色钯沉积物的暗色色调在介于淡黄色或淡褐色至蓝色或浅灰色范围内。
本发明的暗色钯沉积物的a*值在-10.0至+10.0范围内。因此,本发明的暗色钯沉积物的暗色色调几乎不受a*值影响,且暗色钯沉积物的颜色内a*的小偏差不为人眼可见。用本发明方法生成的钯沉积物的L*、a*和b*值于表1中展示。
钯或钯合金层的厚度优选范围介于1至300nm、更优选地10至200nm、甚至更优选地25至100nm且最优选地30至60nm。借此,实现光学反射率的所需减少,且同时与铜或铜合金的表面上形成氧化铜的变黑方法相比,较少铜经氧化(且作为铜或铜合金电路的导电部分损耗)。
用于沉积钯或钯合金层至所述铜或铜合金上的适合浸镀式电镀浴组合物包括至少一种溶剂和钯离子来源。
在浸镀式电镀期间,在铜合金的情形下的铜及其它金属经氧化,且在钯合金的情形下钯及其它金属经还原至金属状态,借此沉积到铜或铜合金的外表面上。此电镀机制将所述浸镀式电镀与例如无电(自催化)电镀(其利用电镀浴中的化学还原剂)和电镀(其利用施加至衬底的导电部分和至少一个阳极的外部电流)区别开来。
用于根据本发明的方法的步骤(iii)的浸镀式电镀浴优选地为酸性电镀浴,更优选地所述电镀浴具有在0.5至4范围内、且最优选地在1至2范围内的pH值。
浸镀式电镀浴中钯离子来源选自水溶性钯盐和水溶性钯络合物。适合的水溶性钯盐为例如,硫酸钯、乙酸钯、硝酸钯、氯化钯和过氯酸钯。适合的水溶性钯络合物为例如,钯(II)离子与烷基氨(诸如,乙二胺)和反离子(诸如,硫酸根、硝酸根等)的络合物。
浸镀式电镀浴中的钯离子的浓度优选范围介于0.01至1g/l、更优选地0.05至0.3g/l。
浸镀式电镀浴的溶剂优选地为水。
根据本发明的方法的步骤(iii)中采用的浸镀式电镀浴优选地进一步包括酸。适合的酸为例如,硫酸、磺酸、羧酸和其混合物。
如果浸镀式电镀浴的pH值太低,那么其可通过添加碱性物质(诸如,氢氧化钠或氢氧化钾水溶液)来增加以便获得所需pH值。
浸镀式电镀浴优选地进一步包括至少一种膦酸盐化合物(其于本文中定义为含有-C-PO(OH)2和/或-C-PO(OR)2基团的有机化合物,其中R选自包括以下各者的群组:经取代和不经取代的烷基、芳基和烷芳基)。
更优选地,至少一种膦酸盐化合物选自根据式(1)的化合物
其中
R1选自由以下各者组成的群组:
R2选自由以下各者组成的群组:
R3选自由以下各者组成的群组:
R4选自由以下各者组成的群组:
n为整数且范围介于1至6;m为整数且范围介于1至6;o为整数且范围介于1至6;p为整数且范围介于1至6且
X选自由以下各者组成的群组:氢和适合的反离子。适合的反离子为(例如)锂、钠、钾和铵。
更优选地,R1和R3为
及
优选地,n、m、o和p分别选自1和2。更优选地,n、m为1;且o和p为2。
浸镀式电镀浴中任选的至少一种膦酸盐化合物最优选地选自包括以下各者的群组:1-羟基乙烷-1,1,-二膦酸、羟乙基氨基二(亚甲基膦酸)、羧甲基氨基二(亚甲基膦酸)、氨基参(亚甲基膦酸)、氮基参(亚甲基膦酸)、乙二胺四(亚甲基膦酸)、己二氨四(亚甲基膦酸)、N-(膦酰甲基)酰亚氨二乙酸、二伸乙基三氨-N,N,N',N”,N”-五-(甲基膦酸)、2-丁烷膦酸盐1,2,4-三甲酸、乙烷-1,2-双(亚氨基双-(甲基膦酸))和2-膦酸丁烷-1,2,4-三甲酸。
浸镀式电镀浴中任选的至少一种膦酸盐化合物的浓度优选范围介于0.3至20mmol/l、更优选地1.5至8mmol/l。
当自包括上述膦酸盐化合物中的至少一者的浸镀式电镀浴沉积钯或钯合金层时,铜或铜合金电路的光学反射率甚至更加减少(实例4)。出人意料地,进一步研究展示钯铜合金获自包括至少一种膦酸盐化合物的浸镀式电镀浴。所述钯铜合金层的颜色比获自浸镀式电镀浴(其不含所述膦酸盐化合物)的钯层的钝灰色或钝浅灰黑色甚至更暗。相应地,当使用包括至少一种膦酸盐化合物的浸镀式电镀浴时,铜或铜合金表面的光学反射率甚至进一步减少。
在不受理论束缚的情况下,申请者相信膦酸盐化合物的添加影响钯或钯合金至铜或铜合金上的浸镀式沉积机制。在化石而非化合物存在下的沉积更加受控,且常常出现于底层金属层中的空隙可明显地减少。在本发明情形中,当使用膦酸盐添加剂时,钯和铜反应之间的交换的确于铜或铜合金中导致较少空隙。此于实例中建立。
此外,在膦酸盐化合物存在下,更加受控的机制允许优选地控制用于减少铜或铜合金的光学反射率的钯或钯合金层的颜色。
浸镀式电镀浴中进一步任选的组分为例如,表面活性剂、用于卤化物离子的来源(诸如,NaCl)、缓冲剂和用于钯离子的络合剂。
用于浸镀式电镀浴中作为任选的成分的钯离子的适合络合剂选自包括以下各者的群组:一级氨、二级氨和三级氨。适合的氨为例如乙二胺、1,3-二氨基-丙烷、1,2-双(3-氨基-丙基-氨基)乙烷、2-二乙基-氨基-乙基-氨、二伸乙基三氨、二伸乙基-三氨-五-乙酸、硝基乙酸、N-(2-羟基-乙基)-乙二胺、乙二胺-N,N-二乙酸、2-(二甲基-氨基)-乙基-氨、1,2-二氨基-丙基-氨、1,3-二氨基-丙基-氨、3-(甲基-氨基)-丙基-氨、3-(二甲基-氨基)-丙基-氨、3-(二乙基-氨基)-丙基-氨、双-(3-氨基-丙基)-氨、1,2-双-(3-氨基-丙基)-烷基-氨、二伸乙基三氨、三伸乙基四氨、四伸乙基五氨、五伸乙基六氨及其混合物。
如果钯合金于根据本发明的方法的步骤(iii)中沉积,那么浸镀式电镀浴进一步包括用于除钯以外金属的金属离子的来源。步骤(iii)中待与钯一起沉积的适合金属为例如铜。存在于浸镀式电镀浴中的铜离子可衍生自与铜或铜合金电路的浸镀式电镀反应,且经还原且与钯一起再沉积到铜或铜合金电路上以形成钯铜合金。
铜离子还可呈水溶性铜盐(诸如,硫酸铜)和/或水溶性铜化合物的形式添加至用于根据本发明的方法的步骤(iii)中的浸镀式电镀浴,以便获得钯铜合金层。铜离子的浓度优选范围介于50至100mg/l。
钯铜合金优选为本发明的步骤(iii)中沉积的钯合金,因为所述合金具有特别地暗色和暗淡之外观。相应地,铜或铜合金电路的光学反射率比纯钯沉积到铜或铜合金电路上的情形下甚至更加减少。
术语“合金”本文定义为包括独立钯和合金元素域的金属间化合物、金属间相和金属沉积物。
在根据本发明的方法的步骤(iii)期间,浸镀式电镀浴优选地保持在20至60℃之间、更优选地在20至40℃之间的范围内的温度。
在步骤(iii)期间,包括铜或铜合金的衬底优选地与浸镀式电镀浴接触20至180s、更优选地30或45至120s。
包括铜或铜合金的衬底可与本发明的步骤(iii)中施加的浸镀式电镀浴(例如,在水平、卷盘至卷盘、垂直和垂直输送化电镀设备中)接触。所述设备为此项技术中已知。
优选地,无其它金属或金属合金层沉积到根据本发明的方法的步骤(iii)中获得的钯或钯合金层上。在此实施例中,钯或钯合金层于铜或铜合金电路上形成最外层金属层。
实例
现将参考以下非限制性实例说明本发明。
一般工序:
具有30×40mm2的尺寸且包括固化催化墨的图案作为电镀基体的PET条在所有实例中使用。经图案化催化墨的线宽在4和12μm之间。
自包括铜离子来源、作为还原剂的甲醛和作为络合剂的酒石酸盐的无电(自催化)电镀浴,将铜沉积到固化催化墨上。在电镀期间,电镀浴温度保持在35℃,且电镀时间为6min。
L*、a*和b*值通过光学显微镜图像的统计评估测量。所有值基于每个图像的4个测量值(每个测量值大于3000像素)。
实例1(比较)
无钯或钯合金层沉积到通过无电(自催化)电镀沉积的铜电路上。
相应地,铜电路具有光泽的、铜色表面,其具有非所需的高光学反射率(参看颜色值的表1)。
实例2(比较)
将通过无电(自催化)电镀沉积的铜电路根据US 2013/0162547 A1进行“变黑”处理。通过将铜电路与包括氢氧化钠和亚氯酸钠的水溶液接触,在所述铜电路表面上形成黑色氧化铜。
铜表面的光学反射率减少,但黑色氧化铜涂层可用白色毛巾擦拭掉。相应地,铜电路之上变黑层的粘着度不足。
实例3
通过浸镀式电镀,将钯层自由水、硫酸钯和硫酸组成的电镀浴沉积到铜层上。
通过所述处理,获得足够粘着、钝灰色沉积物,且铜表面的光学反射率减少。
根据着色方案,不同处理时间(30s、60s和90s)的值于表1中展示。可以看出,着色在不同处理时间保持近似恒定。
图2展示根据本发明的方法处理的铜电路的FIB(聚焦离子束)图像。铜层上形成具有约100nm的厚度不均匀钯层。一些空隙通过铜电路中浸镀式交换反应形成。空隙的量应尽可能低,但对于本发明的技术应用仍可接受。
实例4
通过浸镀式电镀,将均匀钯层自由水、硫酸钯、硫酸和膦酸盐化合物(氨基-参-(亚甲基膦酸))组成的电镀浴沉积到铜层上。
获得足够粘着、钝浅灰黑色沉积物,且通过所述处理减少铜表面的光学反射率,甚至大于在膦酸盐化合物(实例3)不存在的情况下。
根据着色方案,不同处理时间(30s、60s和90s)的值于表1中展示。可以看出,在不同处理时间,着色改变,且可取决于所需涂覆加以控制。此较好控制归因于浸镀式钯溶液中膦酸盐添加剂。
图1展示根据本发明的方法处理的铜电路的FIB(聚焦离子束)图像。铜层上形成具有约100nm厚度的钯层。当使用根据相比于实例3(图2)之前实例4(含有膦酸盐添加剂)的浸镀式组合物时,空隙的量甚至更少。
表1
Claims (11)
1.一种用于减少铜和铜合金电路的光学反射率的方法,其通过上面沉积钯或钯合金的金属层来实现,其以此顺序包括以下步骤
(i)提供介电衬底,
(ii)将铜或铜合金沉积到所述介电衬底上,前提是当铜或铜合金通过无电(自催化)电镀或电镀来沉积时所述介电衬底包括电镀基体,及
(iii)通过浸镀式电镀,将钯或钯合金层沉积到所述铜或铜合金上,且借此减少所述铜或铜合金的光学反射率,
其中自包括钯离子来源、酸和至少一种膦酸盐化合物的水性电镀浴,在步骤(iii)中沉积所述钯或钯合金,
其中通过所述浸镀式电镀,所述钯离子通过经沉积的所述铜或铜合金的金属铜还原,
且其中结构化步骤(ii)中沉积的铜或铜合金以在步骤(iii)之前或在步骤(iii)之后形成电路,
其中所述至少一种膦酸盐化合物的浓度范围介于0.15mmol/l至20mmol/l,用于步骤(iii)中的所述电镀浴的pH值范围介于0.5至4.0,所述水性电镀浴不包含钯离子的还原剂,且所述钯或钯合金层的厚度范围介于1至300nm,
其中所述至少一种膦酸盐化合物选自包括根据式(1)的化合物的群组
其中
R1选自由以下各者组成的群组:
R2选自由以下各者组成的群组:
R3选自由以下各者组成的群组:
R4选自由以下各者组成的群组:
n为整数且范围介于1至6;m为整数且范围介于1至6;o为整数且范围介于1至6;p为整数且范围介于1至6且
X选自由以下各者组成的群组:氢、锂、钠、钾和铵。
2.根据权利要求1所述的方法,其中结构化步骤(ii)中沉积的所述铜或铜合金以于步骤(iii)之前形成电路。
3.根据权利要求1所述的方法,其中结构化步骤(ii)中沉积的所述铜或铜合金以于步骤(iii)之后形成电路。
4.根据上述权利要求中任一权利要求所述的方法,其中步骤(iii)中形成的所述钯或钯合金层为最外层金属层。
5.根据权利要求1至3中任一权利要求所述的方法,其中所述介电衬底选自由玻璃材料和塑料材料组成的群。
6.根据权利要求1至3中任一权利要求所述的方法,其中自包括铜离子来源、还原剂、至少一种络合剂和至少一种稳定剂添加剂的电镀浴,通过无电(自催化)电镀沉积所述铜或铜合金。
7.根据权利要求1至3中任一权利要求所述的方法,其中所述电镀基体包括引发上面铜或铜合金的无电(自催化)电镀的催化活性金属或引发上面铜或铜合金的电镀的导电材料。
8.根据权利要求1至3中任一权利要求所述的方法,其中步骤(iii)中沉积的钯合金为钯铜合金。
9.一种通过根据上述权利要求中任一权利要求所述的方法获得的浸镀式钯或钯合金层的用途,其用于减少铜或铜合金电路的光学反射率。
10.根据权利要求9所述的用途,其中所述光学反射率相比铜或铜合金电路的初始光学反射率减少30%至80%。
11.一种包括铜或铜合金电路和钯或钯合金层的触摸屏装置,所述钯或钯合金层通过浸镀式电镀沉积到所述铜或铜合金电路上。
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