CN117940605A - Method for producing composite material to be plated and method for producing anisotropic conductive sheet - Google Patents
Method for producing composite material to be plated and method for producing anisotropic conductive sheet Download PDFInfo
- Publication number
- CN117940605A CN117940605A CN202280061623.2A CN202280061623A CN117940605A CN 117940605 A CN117940605 A CN 117940605A CN 202280061623 A CN202280061623 A CN 202280061623A CN 117940605 A CN117940605 A CN 117940605A
- Authority
- CN
- China
- Prior art keywords
- composite material
- plated
- heat
- silicone resin
- resin portion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000002131 composite material Substances 0.000 title claims abstract description 123
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 41
- 238000007747 plating Methods 0.000 claims abstract description 78
- 239000000243 solution Substances 0.000 claims abstract description 76
- 229920002050 silicone resin Polymers 0.000 claims abstract description 73
- 229920006015 heat resistant resin Polymers 0.000 claims abstract description 70
- 239000003513 alkali Substances 0.000 claims abstract description 56
- 238000007772 electroless plating Methods 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 43
- 239000003054 catalyst Substances 0.000 claims abstract description 34
- 239000007788 liquid Substances 0.000 claims abstract description 33
- 239000011951 cationic catalyst Substances 0.000 claims abstract description 14
- 230000001678 irradiating effect Effects 0.000 claims abstract description 8
- 239000012670 alkaline solution Substances 0.000 claims abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 230000000149 penetrating effect Effects 0.000 claims description 6
- 229920005989 resin Polymers 0.000 abstract description 25
- 239000011347 resin Substances 0.000 abstract description 25
- 239000010410 layer Substances 0.000 description 102
- 229910052751 metal Inorganic materials 0.000 description 17
- 239000002184 metal Substances 0.000 description 17
- 238000009832 plasma treatment Methods 0.000 description 17
- 125000000896 monocarboxylic acid group Chemical group 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 13
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 13
- 239000003638 chemical reducing agent Substances 0.000 description 12
- 239000002253 acid Substances 0.000 description 11
- 238000007689 inspection Methods 0.000 description 11
- -1 siloxane structure Chemical group 0.000 description 11
- 239000000758 substrate Substances 0.000 description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 238000006386 neutralization reaction Methods 0.000 description 7
- 229910052763 palladium Inorganic materials 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 7
- 238000009210 therapy by ultrasound Methods 0.000 description 7
- 238000003851 corona treatment Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 229910021645 metal ion Inorganic materials 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 4
- 229910008051 Si-OH Inorganic materials 0.000 description 4
- 229910006358 Si—OH Inorganic materials 0.000 description 4
- 238000000137 annealing Methods 0.000 description 4
- 208000028659 discharge Diseases 0.000 description 4
- 230000009477 glass transition Effects 0.000 description 4
- 230000000873 masking effect Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- 229920002379 silicone rubber Polymers 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000004696 Poly ether ether ketone Substances 0.000 description 3
- 239000004642 Polyimide Substances 0.000 description 3
- 238000007259 addition reaction Methods 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 239000007809 chemical reaction catalyst Substances 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 3
- 238000010030 laminating Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 3
- 229920002530 polyetherether ketone Polymers 0.000 description 3
- 229920001721 polyimide Polymers 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 239000003381 stabilizer Substances 0.000 description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Chemical compound CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 2
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- 229910052786 argon 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
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 150000001735 carboxylic acids Chemical class 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- HHLFWLYXYJOTON-UHFFFAOYSA-N glyoxylic acid Chemical compound OC(=O)C=O HHLFWLYXYJOTON-UHFFFAOYSA-N 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 150000001451 organic peroxides Chemical class 0.000 description 2
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 description 2
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 2
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 description 2
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000004080 punching Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- URAYPUMNDPQOKB-UHFFFAOYSA-N triacetin Chemical compound CC(=O)OCC(OC(C)=O)COC(C)=O URAYPUMNDPQOKB-UHFFFAOYSA-N 0.000 description 2
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 1
- JTXMVXSTHSMVQF-UHFFFAOYSA-N 2-acetyloxyethyl acetate Chemical compound CC(=O)OCCOC(C)=O JTXMVXSTHSMVQF-UHFFFAOYSA-N 0.000 description 1
- AHXGXXJEEHFHDK-UHFFFAOYSA-N 6-[(6-hydroxynaphthalen-2-yl)disulfanyl]naphthalen-2-ol Chemical compound C1=C(O)C=CC2=CC(SSC3=CC4=CC=C(C=C4C=C3)O)=CC=C21 AHXGXXJEEHFHDK-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004475 Arginine Substances 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 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 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 1
- 235000003973 Hibiscus mutabilis Nutrition 0.000 description 1
- 244000048199 Hibiscus mutabilis Species 0.000 description 1
- AHLPHDHHMVZTML-BYPYZUCNSA-N L-Ornithine Chemical compound NCCC[C@H](N)C(O)=O AHLPHDHHMVZTML-BYPYZUCNSA-N 0.000 description 1
- ODKSFYDXXFIFQN-BYPYZUCNSA-P L-argininium(2+) Chemical compound NC(=[NH2+])NCCC[C@H]([NH3+])C(O)=O ODKSFYDXXFIFQN-BYPYZUCNSA-P 0.000 description 1
- KDXKERNSBIXSRK-YFKPBYRVSA-N L-lysine Chemical compound NCCCC[C@H](N)C(O)=O KDXKERNSBIXSRK-YFKPBYRVSA-N 0.000 description 1
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 description 1
- 239000004472 Lysine Substances 0.000 description 1
- WRQNANDWMGAFTP-UHFFFAOYSA-N Methylacetoacetic acid Chemical compound COC(=O)CC(C)=O WRQNANDWMGAFTP-UHFFFAOYSA-N 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- AHLPHDHHMVZTML-UHFFFAOYSA-N Orn-delta-NH2 Natural products NCCCC(N)C(O)=O AHLPHDHHMVZTML-UHFFFAOYSA-N 0.000 description 1
- UTJLXEIPEHZYQJ-UHFFFAOYSA-N Ornithine Natural products OC(=O)C(C)CCCN UTJLXEIPEHZYQJ-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004695 Polyether sulfone Substances 0.000 description 1
- 239000004697 Polyetherimide Substances 0.000 description 1
- 239000004734 Polyphenylene sulfide Substances 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- RBYGDVHOECIAFC-UHFFFAOYSA-L acetonitrile;palladium(2+);dichloride Chemical compound [Cl-].[Cl-].[Pd+2].CC#N.CC#N RBYGDVHOECIAFC-UHFFFAOYSA-L 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 229940045985 antineoplastic platinum compound Drugs 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- ODKSFYDXXFIFQN-UHFFFAOYSA-N arginine Natural products OC(=O)C(N)CCCNC(N)=N ODKSFYDXXFIFQN-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- WXNOJTUTEXAZLD-UHFFFAOYSA-L benzonitrile;dichloropalladium Chemical compound Cl[Pd]Cl.N#CC1=CC=CC=C1.N#CC1=CC=CC=C1 WXNOJTUTEXAZLD-UHFFFAOYSA-L 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- RJTANRZEWTUVMA-UHFFFAOYSA-N boron;n-methylmethanamine Chemical compound [B].CNC RJTANRZEWTUVMA-UHFFFAOYSA-N 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 1
- VBDQNUWZQXYUDP-UHFFFAOYSA-L dichloropalladium;ethane-1,2-diamine Chemical compound [Cl-].[Cl-].[Pd+2].NCCN.NCCN VBDQNUWZQXYUDP-UHFFFAOYSA-L 0.000 description 1
- UBPGILLNMDGSDS-UHFFFAOYSA-N diethylene glycol diacetate Chemical compound CC(=O)OCCOCCOC(C)=O UBPGILLNMDGSDS-UHFFFAOYSA-N 0.000 description 1
- UYAAVKFHBMJOJZ-UHFFFAOYSA-N diimidazo[1,3-b:1',3'-e]pyrazine-5,10-dione Chemical compound O=C1C2=CN=CN2C(=O)C2=CN=CN12 UYAAVKFHBMJOJZ-UHFFFAOYSA-N 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000001087 glyceryl triacetate Substances 0.000 description 1
- 235000013773 glyceryl triacetate Nutrition 0.000 description 1
- 125000002795 guanidino group Chemical group C(N)(=N)N* 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 229940098779 methanesulfonic acid Drugs 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 229960003104 ornithine Drugs 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000006174 pH buffer Substances 0.000 description 1
- 150000002940 palladium Chemical class 0.000 description 1
- LWHYKTAISUZRAD-UHFFFAOYSA-L palladium(2+);carbonate Chemical compound [Pd+2].[O-]C([O-])=O LWHYKTAISUZRAD-UHFFFAOYSA-L 0.000 description 1
- INIOZDBICVTGEO-UHFFFAOYSA-L palladium(ii) bromide Chemical compound Br[Pd]Br INIOZDBICVTGEO-UHFFFAOYSA-L 0.000 description 1
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 150000003058 platinum compounds Chemical class 0.000 description 1
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920001230 polyarylate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920001601 polyetherimide Polymers 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229940116423 propylene glycol diacetate Drugs 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 235000011006 sodium potassium tartrate Nutrition 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 229960002622 triacetin Drugs 0.000 description 1
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
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- 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
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/2006—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30
- C23C18/2046—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30 by chemical pretreatment
- C23C18/2073—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
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1635—Composition of the substrate
- C23C18/1639—Substrates other than metallic, e.g. inorganic or organic or non-conductive
- C23C18/1641—Organic substrates, e.g. resin, plastic
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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
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
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- 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
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/2006—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30
- C23C18/2026—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30 by radiant energy
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- 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
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/2006—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30
- C23C18/2026—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30 by radiant energy
- C23C18/204—Radiation, e.g. UV, laser
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- 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
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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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Abstract
The present invention addresses the problem of providing a method for producing a composite material to be plated, which can form a plated layer with good adhesion to each of a plurality of resin portions containing different resins. The method for manufacturing a composite material to be plated for solving the above problems comprises the following steps: a step of preparing a composite material having a heat-resistant resin portion containing a heat-resistant resin and a silicone resin portion containing a silicone resin; a step of treating the plated area of the composite material with an alkali solution; a step of irradiating the plating area treated with the alkaline solution with plasma; a step of bringing a liquid containing a cationic catalyst into contact with the plating target region irradiated with the plasma; and a step of performing electroless plating treatment on the plated region that has been brought into contact with the liquid containing the catalyst, wherein the plated region includes at least a part of the heat-resistant resin portion and at least a part of the silicone resin portion.
Description
Technical Field
The present invention relates to a method for producing a composite material to be plated and a method for producing an anisotropic conductive sheet.
Background
Conventionally, a plating layer has been formed on an insulating substrate made of a resin or the like for the purpose of imparting electromagnetic wave or electric conductivity, imparting electric heat, or improving the design of a product. As a method for forming a plating layer on the surface of an insulating substrate, a sputtering plating method or the like is known. In this method, a metal layer is formed on the surface of an insulating base material by a sputtering method, and then electroplating is performed. Therefore, an expensive sputtering apparatus is required, and there is a problem in terms of productivity and the like.
On the other hand, as a method for forming a plating layer, an electroless plating method is also known. According to the electroless plating method, a metal plating layer can be efficiently formed on the surface of an insulating substrate. However, depending on the type of insulating substrate, adhesion to the plating layer may be low. Therefore, patent document 1 proposes to improve adhesion of a plating layer by treating the surface of an insulating substrate with an alkaline solution before forming the plating layer. Patent document 2 proposes to further treat the substrate with an aqueous alkali solution and then with an aqueous amino acid solution or the like, thereby improving the adhesion of the plating layer.
Prior art literature
Patent literature
Patent document 1: japanese patent application laid-open No. 2021-5624
Patent document 2: japanese patent laid-open No. 2007-563443
Disclosure of Invention
Problems to be solved by the invention
According to the method of patent document 1 or patent document 2, adhesion between an insulating substrate containing a single resin and a plating layer can be improved. However, the adhesion between each resin and the plating layer is different for a composite material comprising different resins and a plurality of resin layers laminated, a composite material comprising different resins and a plurality of members combined, or the like. Therefore, there are the following problems: the plating layer is not adhered to a part of the area (resin); or even if a plating layer can be formed, peeling or the like occurs when stress is applied to the composite material. In addition, particularly when the composite material contains a silicone resin, it is difficult to improve adhesion between the region containing the silicone resin and the plating layer.
The purpose of the present invention is to provide a method for producing a composite material to be plated and a method for producing an anisotropic conductive sheet, wherein a plating layer can be formed with good adhesion to each of a plurality of resin portions containing different resins.
Means for solving the problems
The invention provides a method for manufacturing a plated composite material, which comprises the following steps: a step of preparing a composite material having a heat-resistant resin portion containing a heat-resistant resin and a silicone resin portion containing a silicone resin; a step of treating the plated area of the composite material with an alkali solution; a step of irradiating the plating area treated with the alkaline solution with plasma; a step of bringing a liquid containing a cationic catalyst into contact with the plating target region irradiated with the plasma; and a step of performing electroless plating treatment on the plated region that has been brought into contact with the liquid containing the catalyst, wherein the plated region includes at least a part of the heat-resistant resin portion and at least a part of the silicone resin portion.
The invention also provides a manufacturing method of the anisotropic conductive sheet, which comprises the following steps: a step of preparing an insulating sheet having a through hole penetrating a first surface located on one side in the thickness direction and a second surface located on the other side, the first surface being formed by stacking a heat-resistant resin layer containing a heat-resistant resin and a silicone resin layer containing a silicone resin in the thickness direction; a step of treating the outer wall of the through hole of the insulating sheet with an alkali solution; a step of irradiating the outer wall treated with the alkali solution with plasma; a step of bringing a liquid containing a cationic catalyst into contact with the outer wall irradiated with the plasma; and a step of performing electroless plating treatment on the outer wall that has been brought into contact with the liquid containing the catalyst.
Effects of the invention
According to the method for producing a composite material to be plated of the present invention, a plating layer can be formed with good adhesion to each of a plurality of resin portions containing different resins.
Drawings
Fig. 1A is a photograph of the surface of an untreated silicone resin portion taken with a scanning electron microscope;
Fig. 1B is a photograph of the surface of the silicone resin portion after the alkali solution treatment with a scanning electron microscope;
Fig. 1C is a photograph of the surface of the silicone resin portion after the plasma irradiation step by scanning electron microscopy.
Fig. 2A is a plan view showing an example of the structure of an anisotropic conductive sheet manufactured by the method for manufacturing an anisotropic conductive sheet of the present invention;
fig. 2B is an enlarged partial cross-sectional view of line 1B-1B of fig. 2A.
FIG. 3 is a graph showing the amounts of COOH groups on the surface of a heat-resistant resin portion before contact with a catalyst-containing liquid in examples and comparative examples.
FIG. 4 is a graph showing the amount of Si-OH bonds on the surface of the silicone resin portion.
Detailed Description
The method for producing a composite material to be plated and the method for producing an anisotropic conductive sheet according to the present invention will be described below with reference to specific embodiments. However, the method for producing the composite material to be plated according to the present invention is not limited to this method.
1. Method for producing plated composite material
The method for manufacturing the plated composite material of the present invention comprises the following steps: a step of preparing a composite material having a heat-resistant resin portion containing a heat-resistant resin and a silicone resin portion containing a silicone resin (hereinafter also referred to as a "composite material preparation step"); a step of treating the plated area of the composite material with an alkali solution (hereinafter also referred to as "alkali solution treatment step"); a step of irradiating a plating target area treated with an alkali solution with plasma (hereinafter also referred to as "plasma irradiation step"); a step of bringing a liquid containing a cationic catalyst into contact with a region to be plated to which plasma is irradiated (hereinafter also referred to as a "catalyst contact step"); and a step of performing electroless plating treatment on the plating target area that has been brought into contact with the catalyst-containing liquid (hereinafter also referred to as "electroless plating treatment step"). Other steps may be included within a range that does not impair the effects and objects of the present invention.
As described above, when a plating layer is formed on a composite material surface having a plurality of resin portions containing different resins, adhesion force between each resin portion and the plating layer is different. Therefore, there is a problem that the plating layer does not adhere to a part of the resin portion, or is easily peeled from a portion having weak adhesion to the plating layer. In contrast, in the method for producing a composite material to be plated according to the present invention, the alkali solution treatment step and the plasma irradiation step are sequentially performed on the area to be plated of the composite material, and then the catalyst contact step and the electroless plating treatment step are performed. By sequentially performing the alkali solution treatment step and the plasma irradiation step, the adhesion between the regions containing the respective resins (the heat-resistant resin portion and the silicone resin portion in the present invention) and the plating layer is significantly improved, and a composite material to be plated having high adhesion of the plating layer can be obtained in either region.
The reason for this is considered as follows. Fig. 1A shows a photograph of the surface of an untreated silicone resin portion (hereinafter also referred to as "SEM photograph") taken with a scanning electron microscope, fig. 1B shows an SEM photograph of an alkali solution-treated silicone resin portion, and fig. 1C shows an SEM photograph of a silicone resin portion after a plasma irradiation process. As shown in fig. 1A, a large amount of aggregates exist on the surface of the untreated silicone resin portion. If such aggregates are present, the plating layer is less likely to adhere to the surface of the silicone resin portion when the plating layer is formed, and the plating layer is likely to be peeled off.
On the other hand, when the silicone resin portion is treated with an alkali solution, the aggregates are removed and the surface is smoothed as shown in fig. 1B. Then, when the silicone resin portion is subjected to plasma treatment, si—oh groups are introduced into the surface thereof. Therefore, it is considered that the coating layer is physically and chemically easily adhered to the silicone resin portion, and the adhesion to the coating layer is improved. On the other hand, in the same manner as in the heat-resistant resin portion, the foreign matter is removed by the alkali solution treatment step or COOH groups are introduced into the surface thereof by the plasma irradiation step. Therefore, it is considered that the adhesion between the heat-resistant resin portion and the plating layer is also improved.
In addition, according to intensive studies by the present inventors, it was confirmed that: the amount of Si-OH groups on the surface of the silicone resin portion and the amount of COOH groups on the surface of the heat-resistant resin portion are large, and thus the plating layer cannot be sufficiently adhered. As will be shown in detail in examples to be described later, for example, if only the plasma irradiation step is performed without performing the alkali solution treatment step, the amounts of si—oh groups and COOH groups in the respective regions increase. However, if a plating layer is formed in these regions, peeling occurs. That is, as described above, it is considered that the introduction of si—oh groups and COOH groups after the surface of each region has been sufficiently smoothed or normalized by the alkali solution treatment step is very important for the adhesion of the plating layer. Hereinafter, each step of the method for producing a composite material to be plated according to the present invention will be described.
(1) Composite material preparation step
In the composite material preparation step, a composite material having a heat-resistant resin portion and a silicone resin portion is prepared. The shape of the composite material is not particularly limited, and may be, for example, a flat plate shape or a three-dimensional shape. May be appropriately selected according to the use of the composite material to be plated.
The shape of each of the heat-resistant resin portion and the silicone resin portion is not particularly limited, as long as the heat-resistant resin portion and the silicone resin portion are disposed on the surface of the composite material so that a part of the heat-resistant resin portion and a part of the silicone resin portion are exposed, respectively. The composite material may have a structure in which a heat-resistant resin portion and a silicone resin portion are laminated as in an insulating sheet of an anisotropic conductive sheet described later. The composite material may be a structure in which a member made of a heat-resistant resin portion and a member made of a silicone resin portion are connected or bonded. The composite material may include a region other than the heat-resistant resin portion or the silicone resin portion, that is, a region made of a heat-resistant resin or a resin other than the silicone resin, a region made of a metal or a ceramic, or the like, as long as the object and effect of the present invention are not impaired.
The heat-resistant resin contained in the heat-resistant resin portion is preferably a resin having high heat resistance, that is, a resin having high glass transition temperature. The glass transition temperature of the heat-resistant resin may be appropriately selected depending on the use of the composite material to be plated. When the composite material to be plated is an anisotropic conductive sheet to be described later, the glass transition temperature of the heat-resistant resin is preferably 150 ℃ or higher, more preferably 150 to 500 ℃. Glass transition temperature of heat-resistant resin according to JIS K7095: 2012, measurement is performed.
The heat-resistant resin is preferably a resin which is hardly corroded by a chemical agent used in an alkali solution treatment step or an electroless plating treatment step, which will be described later. Examples of such heat-resistant resins include: engineering plastics such as polyamide, polycarbonate, polyarylate, polysulfone, polyethersulfone, polyphenylene sulfide, polyetheretherketone, polyimide, and polyetherimide, acrylic resin, polyurethane resin, epoxy resin, and olefin resin. The heat-resistant resin portion may contain only one of these heat-resistant resins, or may contain two or more kinds. The heat-resistant resin portion may further contain other components such as a filler, if necessary.
On the other hand, the silicone resin contained in the silicone resin portion may be any resin having a siloxane structure, and examples thereof include: polydimethylsiloxanes, polyphenylmethylsiloxanes, polyalkylalkenylsiloxanes, polyalkylhydrosiloxanes, and the like. The silicone resin may be an addition-crosslinked product of a silicone elastomer composition containing an organopolysiloxane having a silicon hydrogen group (SiH group), an organopolysiloxane having a vinyl group, and an addition reaction catalyst, or an addition-crosslinked product of a silicone rubber composition containing an organopolysiloxane having a vinyl group and an addition reaction catalyst. Further, the silicone elastomer composition may be a crosslinked product of a silicone elastomer composition containing an organopolysiloxane having SiCH 3 groups and an organic peroxide curing agent.
Examples of the above-mentioned addition reaction catalyst include metals, metal compounds, metal complexes, and the like having catalytic activity for hydrosilylation reaction, and specifically include platinum, platinum compounds, complexes thereof, and the like. In addition, examples of the organic peroxide curing agent include benzoyl peroxide, bis-2, 4-dichloroperoxide, dicumyl peroxide, di-t-butyl peroxide and the like. The silicone resin portion may further contain components other than silicone resins such as a thickener, a silane coupling agent, and a filler, as required, in addition to the silicone resin.
(2) Alkali solution treatment process
In the alkali solution treatment step, the plated area of the composite material is treated with an alkali solution. In the present specification, the plated region of the composite material means a region where a plating layer is formed by an electroless plating treatment process described later. For example, the entire surface of the composite material may be used as the plated region, or only a part of the surface may be used as the plated region. In addition, only one portion of the composite material may be used as a plated region, or a plurality of regions may be used as plated regions. Further, it is sufficient that at least a part of the heat-resistant resin portion and at least a part of the silicone resin portion are contained in any part of the plated region. For example, the plated region may be a combination of a region composed only of the heat-resistant resin portion and a region composed only of the silicone resin portion. But more preferably one plated area includes both the heat-resistant resin portion and the silicone resin portion. In the conventional method, when a plating layer is formed on a region including both the heat-resistant resin portion and the silicone resin portion, peeling of the plating layer is particularly likely to occur. In contrast, according to the method of the present invention, a plating layer having excellent adhesion can be formed even in such a region.
The method of treating the above-mentioned plated area with the alkali solution is not particularly limited. It is also possible to contact only the plating target area with the alkali solution, but from the viewpoint of production efficiency, it is preferable to impregnate the composite material with the alkali solution and contact the entire composite material with the alkali solution.
The type of the alkali solution is not limited as long as the surface state of the plating area can be adjusted or foreign matter adhering to the surface of the plating area can be removed. Examples of the alkali solution include aqueous sodium hydroxide solution, aqueous potassium hydroxide solution, aqueous lithium hydroxide solution, and the like. Among them, sodium hydroxide aqueous solution is preferable.
The pH of the alkaline solution is more preferably 12 or more. In the case of using sodium hydroxide or potassium hydroxide as the alkali solution, the concentration thereof is preferably about 1 to 100g/L, more preferably 5 to 50g/L. If the concentration of the alkali solution is within this range, the plated area can be treated to a desired surface state without deteriorating the composite material.
The temperature of the alkaline solution when contacted with the composite is preferably 20 to 90 ℃, more preferably 40 to 70 ℃. If the temperature of the alkali solution is within this range, the surface of the plated area can be treated efficiently.
Further, the time for contacting the composite material with the alkali solution is preferably about 10 minutes to 50 minutes, and more preferably about 15 minutes to 40 minutes. If the range is within this range, the plated region can be sufficiently treated. On the other hand, it is difficult to deteriorate the composite material, and the plated composite material can be efficiently produced.
In addition, when the plating area of the composite material is brought into contact with the alkali solution, the ultrasonic treatment may be performed simultaneously. If the ultrasonic treatment is performed simultaneously, foreign matter and the like adhering to the surface of the plating region can be removed efficiently. In addition, when the plated area is a through hole, a recess, or the like provided in the composite material, the alkali solution can be introduced into the plated area. The conditions of the ultrasonic treatment are not particularly limited, and may be, for example, 20 to 60 kHz.
After the alkali solution is treated, the alkali solution attached to the composite material may be neutralized with an acid solution. The neutralization method is not particularly limited, and examples thereof include a method of applying an acid solution to a desired region and a method of immersing the entire composite material in the acid solution. Specific examples of the acid solution used for neutralization include inorganic acids such as sulfuric acid, hydrochloric acid, nitric acid, etc., organic acids such as acetic acid, methanesulfonic acid, sulfamic acid, etc. Among them, sulfuric acid or hydrochloric acid is preferable from the viewpoints of operability, availability, cost, and the like. The pH and type of the acid solution may be appropriately selected depending on the pH and type of the alkali solution.
The temperature of the acid solution when in contact with the composite material is preferably 10 to 70 ℃, more preferably 20 to 60 ℃. If the temperature of the acid solution is within this range, the surface of the plated area can be treated efficiently.
Further, the time for contacting the composite material with the acid solution is preferably about 10 seconds to 10 minutes, more preferably about 30 seconds to 5 minutes. If the range is within this range, the plated region can be sufficiently treated. On the other hand, it is difficult to deteriorate the composite material, and the plated composite material can be efficiently produced.
In addition, when the composite material is brought into contact with an acid solution, ultrasonic treatment may be performed. If the ultrasonic treatment is performed simultaneously, a sufficient amount of the acid solution can be introduced into the region to be plated even when the region to be plated is a through hole, a recess, or the like provided in the composite material. The conditions of the ultrasonic treatment are not particularly limited, and may be the same as in the case of treatment with an alkali solution.
(3) Plasma irradiation step
In the plasma irradiation step, plasma is irradiated to the plating target area after the alkali solution treatment step. The plasma irradiation may be performed from only one direction or from a plurality of directions for the composite material. For example, the sheet-like composite material may be plasma-irradiated from both the front surface and the back surface. The plasma irradiation may be performed only on the plating region, or may be performed on the entire composite material.
The method of irradiating the plasma is not particularly limited, and a known plasma irradiation method, such as atmospheric pressure plasma irradiation and vacuum plasma irradiation (low temperature plasma irradiation), can be employed.
In the atmospheric pressure plasma irradiation, discharge treatment is performed in a gas atmosphere in which one or two or more kinds of carboxylic acids such as air, water vapor, argon, nitrogen, helium, carbon dioxide, carbon monoxide, alcohols such as isopropyl alcohol, and acrylic acid are mixed.
In vacuum plasma irradiation (low-temperature plasma irradiation), for example, the composite material is placed in an internal electrode type discharge treatment apparatus having counter electrodes composed of drum electrodes and a plurality of rod electrodes. Then, the pressure in the apparatus is preferably about 1 to 20Pa, more preferably 10Pa or less, and a high voltage of direct current or alternating current is applied between the electrodes under the treatment gas atmosphere to discharge the gas. As a result, a plasma of the process gas is generated, and the composite material is processed by the plasma.
As the process gas, for example, one or two or more kinds of carboxylic acids such as argon, nitrogen, helium, carbon dioxide, carbon monoxide, air, water vapor, alcohols such as isopropyl alcohol, and acrylic acid may be mixed and used.
Among the above-mentioned plasma irradiation, vacuum plasma irradiation is preferable, and oxygen plasma irradiation using an oxygen-containing gas as a process gas is particularly preferable. When oxygen plasma is irradiated, COOH groups can be efficiently introduced into the surface of the region containing the heat-resistant resin layer, and further si—oh groups can be efficiently introduced into the surface of the silicone resin portion.
The oxygen supply amount is preferably 5 to 40 ml/min, more preferably 10 to 30 ml/min.
The high-frequency power at the time of plasma irradiation is not particularly limited, and for example, when the treatment time is about 1 minute, the high-frequency power is preferably 75 to 150W, more preferably 90 to 125W. If the output power at the time of plasma irradiation is 75W or more, plasma can be sufficiently generated, and processing can be efficiently performed. On the other hand, if the output power is 150W or less, the composite material can be processed without being degraded.
The plasma irradiation time is preferably 0.1 to 5 minutes, more preferably 0.5 to 2 minutes. When plasma irradiation is performed for 0.5 minutes or longer, COOH groups can be introduced into the surface of the region containing the heat-resistant resin layer, or si—oh groups can be introduced into the surface of the silicone resin portion. On the other hand, if the time is 2 minutes or less, the composite material can be treated without being damaged.
(4) Catalyst contact step
The catalyst contacting step is a step of contacting the plating target area after the plasma irradiation step with a liquid containing a cationic catalyst.
As a method of bringing the liquid containing the cationic catalyst into contact with the plating target area, for example, a method of immersing in a solution containing the cationic catalyst may be employed, but the method is not limited thereto. In the case where only a part of the area of the composite material is used as the plating area, masking treatment may be performed by applying a resist or the like to prevent the catalyst from adhering to the portion other than the plating area.
The liquid containing the cationic catalyst may be any liquid that contains a metal ion (cation) as a catalyst in an electroless plating treatment step described later. Examples of the metal to be the catalyst include Ag, cu, al, ni, co, fe, pd and the like. Among them, ag or Pd is preferable, and Pd is particularly preferable from the viewpoint of catalytic ability.
The metal is contained in the liquid containing the catalyst in the form of a metal salt or a complex. The counter ion of the metal in the metal salt and the kind of the ligand in the complex may be appropriately selected according to the kind of the metal.
Examples of palladium salts include palladium acetate, palladium chloride, palladium nitrate, palladium bromide, palladium carbonate, palladium sulfate, bis (benzonitrile) dichloropalladium (II), bis (acetonitrile) dichloropalladium (II), bis (ethylenediamine) palladium (II) chloride, and the like. Among them, palladium chloride, palladium nitrate, palladium acetate, and palladium sulfate are preferable from the viewpoints of ease of handling and solubility.
Examples of the complexing agent constituting the palladium complex include basic amino acids having a cationic group (for example, amino group and guanidino group) such as lysine, arginine, ornithine, etc., tetrakis (triphenylphosphine) and tribenzylacetone.
The catalyst-containing liquid generally contains a solvent for dispersing or dissolving the metal salt or complex. The type of solvent is not particularly limited as long as it does not attack the composite material. Examples thereof include: water, methyl acetoacetate, ethyl acetoacetate, ethylene glycol diacetate, cyclohexanone, acetylacetone, acetophenone, 2- (1-cyclohexenyl), propylene glycol diacetate, glyceryl triacetate, diethylene glycol diacetate, 1, 4-dioxane, N-methylpyrrolidone, dimethyl carbonate, dimethyl cellosolve, and the like.
The catalyst solution may contain a pH buffer such as boric acid or sodium borate within a range that does not impair the effect of the present invention.
The temperature of the catalyst-containing liquid when the composite material is brought into contact with the cationic catalyst-containing liquid is preferably 20 to 60 ℃, more preferably 30 to 50 ℃. When the temperature of the catalyst-containing liquid is 20 ℃ or higher, the metal ions can be efficiently reacted with COOH groups and si—oh groups in the plating region. On the other hand, if the temperature is 60 ℃ or lower, the composite material is hardly affected.
The contact time of the composite material with the catalyst-containing liquid is preferably 0.5 to 10 minutes, more preferably 1 to 5 minutes. When the contact time of the liquid containing the cationic catalyst is 0.5 minutes or longer, the metal ions can be efficiently reacted with COOH groups and si—oh groups in the plating region. On the other hand, if it is 10 minutes or less, it is difficult to affect the composite material.
The metal ions may be reduced after being introduced into the surface of the composite material. The reduction may be performed in the electroless plating treatment step described later, or may be performed by treating with a reducing agent (catalyst activation liquid) before the electroless plating treatment step is performed. For example, the composite material may be immersed in a solution containing a reducing agent.
Examples of the reducing agent include boron-based reducing agents such as sodium borohydride, dimethylamine borane, boric acid, formaldehyde, hypophosphorous acid, and the like.
The temperature of the reducing agent when treated with the reducing agent, and the contact time of the composite material with the reducing agent may be appropriately selected according to the kind of the reducing agent.
(5) Electroless plating treatment process
In the electroless plating treatment step, electroless plating treatment is performed on the plated area to which the metal as a catalyst is attached. In the electroless plating treatment step, an electroless plating bath containing metal ions to be deposited as a plating product is brought into contact with the plating target area, and the metal is deposited on the surface of the plating target area by chemical reaction. The method of contacting the electroless plating bath with the plated region is not particularly limited, and only the plated region may be contacted with the electroless plating bath, or the entire composite material may be immersed in the electroless plating bath. In the case where only a part of the area of the composite material is used as the plating target area, masking treatment may be performed by applying a resist or the like to prevent the electroless plating bath from adhering to the portion other than the plating target area.
Electroless plating baths typically contain salts, reducing agents, solvents, stabilizers, and the like, which are the starting materials for the desired plating layer. Examples of the metal constituting the plating layer include copper, tin, lead, nickel, gold, palladium, rhodium, and the like, and one or a combination of two or more of these metals may be used. Among them, copper or gold is preferable from the viewpoint of conductivity, for example, in the production of a conductive layer or the like of an anisotropic conductive sheet to be described later.
The reducing agent, solvent, and stabilizer may be appropriately selected according to the kind of the metal. For example, in the case of forming a plating layer composed of copper, the electroless plating bath may contain: for example, organic compounds such as CuSO 4, a reducing agent such as HCOH, glyoxylic acid or a salt thereof, a chelating agent such as EDTA, rochelle salt, a stabilizer such as trialkanolamine, water, a solvent such as ketones (acetone, etc.), alcohols (methanol, ethanol, isopropanol, etc.), 2' -bipyridyldisulfide, 6' -dithiobisnicotinic acid, 2' -dithiobisbenzoic acid, bis (6-hydroxy-2-naphthyl) disulfide, etc.
The temperature of the electroless plating bath when the composite material is brought into contact with the electroless plating bath is preferably 25 to 70 ℃, more preferably 30 to 50 ℃. When the temperature of the electroless plating bath is 25 ℃ or higher, the plating layer can be efficiently formed. On the other hand, if the temperature is 70 ℃ or lower, the composite material is hardly affected.
The contact time of the composite material with the electroless plating bath is preferably 3 to 45 minutes, more preferably 10 to 30 minutes. When the contact time of the electroless plating bath is 3 minutes or longer, the plating layer can be efficiently formed. On the other hand, if the time is 45 minutes or less, the composite material is hardly affected. Thus, a composite material to be plated having a desired plating layer formed in the area to be plated can be obtained. After the contact with the electroless plating bath, annealing treatment or the like may be performed as needed. The annealing treatment is preferably performed at a temperature of about 100 to 150℃and the treatment time is preferably 5 to 30 minutes.
2. Method for manufacturing anisotropic conductive sheet
According to the above-described method for producing a composite material to be plated, an anisotropic conductive sheet can be produced. The anisotropic conductive sheet in the present specification refers to a sheet having conductivity in the thickness direction and insulation in the surface direction. The anisotropic conductive sheet can be used as a probe (contact) in electrical inspection. The anisotropic conductive sheet produced by the method of the present invention has: an insulating sheet having a heat-resistant resin layer containing a heat-resistant resin and a silicone resin layer containing a silicone resin laminated in a thickness direction and having a through hole penetrating a first surface located on one side in the thickness direction and a second surface located on the other side; and a conductive layer (plating layer) formed in the through hole.
The anisotropic conductive sheet is disposed between the substrate of the electrical inspection device and the inspection object so as to reliably make electrical contact between the electrode of the substrate of the electrical inspection device and the terminal of the inspection object. In addition, in the electrical inspection, a press-in load is applied to reliably electrically connect the substrate of the electrical inspection apparatus and the inspection object. Therefore, the anisotropic conductive sheet is required to be easily elastically deformed in the thickness direction. Therefore, an insulating sheet is being studied as a sheet formed by laminating a heat-resistant resin layer having a relatively high elastic modulus, a silicone resin layer having a low elastic modulus, and the like. However, in the conventional technique, it is difficult to form a plating layer having high adhesion to both the heat-resistant resin layer and the silicone resin layer. Therefore, when the conductive layer is formed by electroplating, the conductive layer is easily peeled off when a press-in load is applied.
In contrast, if the anisotropic conductive sheet is manufactured by the above-described method for manufacturing a composite material to be plated, a plating layer (conductive layer) having good adhesion to both the heat-resistant resin layer and the silicone resin layer can be formed, and a highly reliable anisotropic conductive sheet can be obtained. The structure of the anisotropic conductive sheet will be described first, and then the manufacturing method will be described.
(1) Structure of anisotropic conductive sheet
Fig. 2A and 2B show an example of the structure of an anisotropic conductive sheet manufactured by the method for manufacturing an anisotropic conductive sheet of the present invention. The structure of the anisotropic conductive sheet is not limited to this structure. Fig. 2A is a plan view of the anisotropic conductive sheet 10, and fig. 2B is an enlarged partial sectional view of the anisotropic conductive sheet 10 of fig. 2A taken along line 1B-1B.
As shown in fig. 2A and 2B, the anisotropic conductive sheet 10 includes: an insulating sheet 11 having a plurality of through holes 12; and a plurality of conductive layers 13 (for example, two conductive layers 13 surrounded by a broken line in fig. 2B) arranged in correspondence with the plurality of through holes 12, respectively.
The insulating sheet 11 is a sheet formed by laminating a silicone resin layer 11A and two heat-resistant resin layers 11B and 11C. The silicone resin contained in the silicone resin layer 11A is the same as the silicone resin contained in the silicone resin portion of the composite material to be plated. The heat-resistant resin contained in the heat-resistant resin layers 11B and 11C is the same as the heat-resistant resin contained in the heat-resistant resin portion of the composite material to be plated. The two heat-resistant resin layers 11B and 11C may be layers containing the same resin or layers containing different resins. The insulating sheet 11 may include an adhesive layer (not shown) between the silicone resin layer 11A and the heat-resistant resin layers 11B and 11C, if necessary.
On the other hand, the shape of the through-hole 12 is not particularly limited, and may be, for example, columnar. The through hole 12 may be cylindrical, prismatic, or other shapes. The cross section orthogonal to the axial direction of the through hole 12 is, for example, circular, elliptical, quadrangular, or other polygonal shape.
The through hole 12 may be a hole formed by any method, and may be a hole formed by machining (e.g., punching or punching) or a hole formed by laser machining.
The thickness of the insulating sheet 11 is not limited as long as it can insulate the substrate of the electrical inspection apparatus from the inspection object, and is preferably 40 to 500 μm, more preferably 100 to 300 μm.
On the other hand, the conductive layer 13 is a layer formed on the outer wall 12c of the through hole 12 by electroless plating. The conductive layer 13 of the unit surrounded by a broken line functions as one conductive path (refer to fig. 2B). The volume resistivity of the material constituting the conductive layer 13 is not particularly limited as long as it is sufficient to be conductive, and is preferably 1.0X10X10X -4 Ω·cm or less, more preferably 1.0X110X -6~1.0×10-9 Ω·cm. The volume resistivity of the material constituting the conductive layer 13 can be measured by the method described in ASTM D991.
The thickness of the conductive layer 13 is not particularly limited as long as it is in a range where sufficient conduction can be obtained. In general, the thickness of the conductive layer 13 is preferably 0.1 to 5. Mu.m. If the thickness of the conductive layer 13 is equal to or greater than a certain value, sufficient conduction is easily obtained, and if it is equal to or less than a certain value, it is difficult to block the through hole 12 or damage the terminal of the inspection object by contact with the conductive layer 13. The thickness of the conductive layer 13 is a thickness in a direction perpendicular to the thickness direction of the insulating sheet 11.
In fig. 2B, the conductive layer 13 is formed only on the outer wall 12c of the through hole 12, but the conductive layer 13 may be formed on the first surface and the second surface of the insulating sheet 11.
(2) Method for manufacturing anisotropic conductive sheet
The anisotropic conductive sheet can be manufactured by a method comprising the steps of: a step of preparing an insulating sheet having a heat-resistant resin layer containing a heat-resistant resin and a silicone resin layer containing a silicone resin laminated in the thickness direction and having a through hole penetrating a first surface located on one side in the thickness direction and a second surface located on the other side (hereinafter also referred to as an "insulating sheet preparation step"); a step of treating the outer wall of the through hole of the insulating sheet with an alkali solution (hereinafter also referred to as "alkali solution treatment step"); a step of irradiating the outer wall treated with the alkali solution with plasma (hereinafter also referred to as "plasma irradiation step"); a step of bringing a liquid containing a cationic catalyst into contact with the outer wall subjected to the plasma treatment (hereinafter also referred to as a "catalyst contact step"); and a step of subjecting the outer wall that has been brought into contact with the catalyst-containing liquid to electroless plating treatment (hereinafter also referred to as "electroless plating treatment step"). Other steps may be included within a range that does not impair the effects and objects of the present invention.
In the insulating sheet preparation step, an insulating sheet is prepared, which is formed by laminating the heat-resistant resin layer containing a heat-resistant resin and the silicone resin layer containing a silicone resin in the thickness direction, and has a through hole penetrating through a first surface located on one side in the thickness direction and a second surface located on the other side. In the insulating sheet preparation step, for example, a heat-resistant resin layer and a silicone resin layer may be laminated, or a through hole may be formed.
In the alkali solution treatment step, the outer wall of the through hole of the insulating sheet is treated with an alkali solution. The alkali solution treatment step may be the same as the alkali solution treatment step in the method for producing a composite material to be plated.
In the plasma irradiation step, the outer wall of the through hole of the insulating sheet is subjected to plasma treatment. The plasma irradiation step may be similar to the plasma irradiation step in the method for producing a composite material to be plated, and COOH groups and si—oh groups can be introduced into the outer wall of the through hole by, for example, performing oxygen plasma treatment or the like from both surfaces of the insulating sheet.
In the catalyst contact step, a liquid containing a cationic catalyst is brought into contact with the outer wall of the through-hole subjected to the plasma treatment. The catalyst contact step may be the same as the catalyst contact step in the method for producing a composite material to be plated, but may be performed by masking, for example, by applying a resist or the like, to prevent the catalyst from adhering to a region other than the outer wall of the through hole.
In the electroless plating treatment step, the outer wall that has been in contact with the catalyst-containing liquid is subjected to electroless plating treatment. The electroless plating process may be the same as the electroless plating process of the method for producing a composite material to be plated, but may be performed by masking, for example, by applying a resist or the like, to prevent the formation of a plating layer in a region other than the outer wall of the through hole. Further, after forming the plating layer also in the region other than the outer wall of the through hole (for example, the first surface and the second surface of the insulating sheet), the plating layer in the unnecessary region may be removed.
In the method for producing the anisotropic conductive sheet, annealing treatment or the like may be performed as needed in the same manner as the method for producing the composite material to be plated.
Examples
The present invention will be described below with reference to examples. The scope of the invention is not to be interpreted in a limiting manner by the examples.
Example 1
(1) Preparation of composite materials
2 Sheets of a heat-resistant resin film (EXPEEK manufactured by Kurabo Co., ltd.) containing Polyetheretherketone (PEEK) and having a thickness of 9 μm were prepared. Next, a silicone resin film (manufactured by Hibiscus-sinensis rubber industry Co., ltd.) containing Polydimethylsiloxane (PDMS) and having a thickness of 300 μm was prepared. Then, heat-resistant resin films are disposed on both surfaces of the silicone resin film, respectively, and these films are bonded. Next, the through-holes are formed so as to be connected from one heat-resistant resin film surface (first surface) to the other heat-resistant resin film surface (second surface) of the laminate. The through hole is manufactured by laser. The through-hole had a cylindrical shape with a diameter of 70. Mu.m.
(2) Treatment with alkaline solution and neutralization treatment
The above composite material was immersed in a 50℃sodium hydroxide solution (concentration 20g/L, pH 13.4) for 30 minutes. In addition, ultrasonic (frequency 40 kHz) treatment was also performed simultaneously with the dipping. Then, the composite material was taken out and immersed in sulfuric acid (concentrated sulfuric acid: 100ml/L solution) for 1 minute. At this time, ultrasonic treatment (frequency 40 kHz) was also performed.
(3) Vacuum plasma treatment
Then, vacuum plasma treatment was performed for 1 minute from each of the first surface side and the second surface side of the composite material. The plasma treatment conditions were as follows.
(Plasma treatment conditions)
Plasma irradiation device: PDC210 manufactured by Dai and science Co
Output power: 100W
Atmospheric pressure: 5Pa
Oxygen supply amount: 20 ml/min
Oscillation frequency: 13.56MHz
High frequency power: 125W
The treatment time is as follows: for 1 minute
(4) Treatment with catalyst-containing liquids
The above-mentioned composite material after the plasma treatment was immersed in a palladium ion complex solution (TOP SAPINA CATALYST, 100ppm of palladium concentration, manufactured by Aomu pharmaceutical industry Co.) heated to 40℃for 2 minutes, and palladium ions were attached to the surface of the composite material. Then, the palladium ion was reduced by immersing in a reducing agent (TOP SAPINA Accelerator manufactured by Aofield pharmaceutical industry Co., ltd.) for 1.5 minutes.
(5) Electroless plating treatment
The above composite material was immersed in a solution containing 50mL ATS Adocopper IW-A, 80mL ATS Adocopper IW-M, 15mL ATS Adocopper C, 3mL ATS Adocopper R-N (all manufactured by Aohan pharmaceutical industry Co., ltd.) at 35℃for 15 minutes.
(6) Annealing treatment
The composite material after the electroless plating treatment was annealed at 110℃for 20 minutes to obtain a plated composite material (anisotropic conductive sheet).
Example 2
A composite material to be plated was obtained in the same manner as in example 1, except that the plasma output during plasma treatment was changed to 150W.
Example 3
A plated composite material was obtained in the same manner as in example 1, except that the type of the heat-resistant resin film was changed to Polyimide (PI) having a thickness of 7.5 μm (Kapton 30EN, manufactured by eastern-dupont).
Comparative example 1
A composite material to be plated was obtained in the same manner as in example 1, except that the treatment with an alkali solution, the neutralization treatment, and the vacuum plasma treatment were not performed.
Comparative example 2
A composite material to be plated was obtained in the same manner as in example 1, except that the neutralization treatment and the vacuum plasma treatment were not performed.
Comparative example 3
A composite material to be plated was obtained in the same manner as in example 1, except that the vacuum plasma treatment was not performed.
Comparative example 4
A composite material to be plated was obtained in the same manner as in example 1, except that the corona treatment was performed under the following conditions instead of the plasma treatment.
(Corona treatment conditions)
Corona treatment device: TEC-4AX manufactured by CHUN Motor Co., ltd
Output power: 90 W.0.4 m/min
Discharge gap: 1mm of
Atmosphere: atmospheric pressure
Operating temperature: 25 DEG C
Comparative example 5
A composite material to be plated was obtained in the same manner as in example 1, except that the treatment with an alkali solution and the neutralization treatment were not performed.
Comparative example 6
A composite material to be plated was obtained in the same manner as in example 1, except that after preparing the composite material, vacuum plasma treatment was performed, and then treatment with an alkali solution and neutralization treatment were performed.
(Evaluation)
The coated composite materials produced in the examples and comparative examples were subjected to a cross cut tape peel test of the coating layer according to a cross cut test (JIS Z1522). The results were evaluated according to the following criteria.
And (2) the following steps: no peeling
Delta: peeling of 5% or less
X: peeling exceeding 5%
TABLE 1
*1 Corona treatment *2 corona treatment is performed prior to alkali solution treatment
As shown in table 1, by subjecting the composite material to treatment with an alkali solution, plasma irradiation, treatment with a liquid containing a catalyst, and electroless plating treatment, a plating layer having good adhesion to both the heat-resistant resin layer and the silicone resin layer can be formed (examples 1 to 3). On the other hand, it was confirmed that in any of the cases where plasma irradiation was not performed (comparative examples 1 to 4), where treatment with an alkali solution was not performed (comparative examples 1 and 5), where the order of plasma irradiation and treatment with an alkali solution was reversed (comparative example 6), there were cases where deposition was not performed during plating, peeling occurred during plating, and a plating layer with sufficient adhesion could not be obtained.
In addition, the amounts of COOH groups on the surface of the heat-resistant resin portion before the catalyst-containing liquid was contacted in each of examples and comparative examples are shown in fig. 3, and the amounts of si—oh groups on the surface of the silicone resin portion before the catalyst-containing liquid was contacted are shown in fig. 4. The amount of COOH groups and the amount of Si-OH groups were measured by X-ray photoelectron spectroscopy, and as binding energy, COOH was measured from the peak value of C1s around 289eV, and Si-OH was measured from the peak value of Si2p around 104eV by calculating the atomic percentage. As shown in fig. 3 and 4, the amount of COOH groups and the amount of si—oh groups were increased by sequentially performing the treatment with the alkali solution and the plasma irradiation (example 1). Further, based on the results obtained when only plasma irradiation was performed (comparative example 5), it was found that the adhesion of the plating layer was not improved although the amount of COOH groups and the amount of si—oh groups were simply increased. That is, it is considered that, regarding the adhesion of the electroless plating layer, not only the treatment by plasma treatment but also the alkali solution treatment is important.
The present application claims priority based on japanese patent application No. 2021-161758 filed at 2021, 9 and 30. The entire contents described in the specification and drawings of this application are incorporated into the specification of the present application.
Industrial applicability
According to the method for producing a composite material to be plated of the present invention, a composite material to be plated having high adhesion between the composite material and the plating layer can be produced. Therefore, it is very useful in manufacturing anisotropic conductive sheets and various products.
Symbol description
10: Anisotropic conductive sheet
11: Insulating sheet
11A: silicone resin layer
11B, 11C: heat resistant resin layer
12: Through hole
12C: outer wall
13: And a conductive layer.
Claims (5)
1. A method for manufacturing a plated composite material includes the following steps:
a step of preparing a composite material having a heat-resistant resin portion containing a heat-resistant resin and a silicone resin portion containing a silicone resin;
a step of treating the plated area of the composite material with an alkali solution;
a step of irradiating the plating area treated with the alkaline solution with plasma;
A step of bringing a liquid containing a cationic catalyst into contact with the plating target region irradiated with the plasma; and
A step of performing electroless plating treatment on the plating target area contacted with the liquid containing the catalyst,
Wherein the plated region includes at least a part of the heat-resistant resin portion and at least a part of the silicone resin portion.
2. The method of producing a plated composite material according to claim 1, wherein the plasma is oxygen plasma.
3. The method for producing a plated composite material according to claim 1 or 2, wherein the high-frequency power of the plasma is 75W to 150W.
4. The method for producing a composite material to be plated according to claim 1 to 3, wherein,
In the composite material, the heat-resistant resin portion and the silicone resin portion are laminated in a thickness direction,
The composite material further has a through hole penetrating through the first surface on one side in the thickness direction and the second surface on the other side,
The plated area is an outer wall of the through hole.
5. A method for manufacturing an anisotropic conductive sheet includes the steps of:
A step of preparing an insulating sheet having a through hole penetrating a first surface located on one side in the thickness direction and a second surface located on the other side, the first surface being formed by stacking a heat-resistant resin layer containing a heat-resistant resin and a silicone resin layer containing a silicone resin in the thickness direction;
a step of treating the outer wall of the through hole of the insulating sheet with an alkali solution;
a step of irradiating the outer wall treated with the alkali solution with plasma;
A step of bringing a liquid containing a cationic catalyst into contact with the outer wall irradiated with the plasma; and
And a step of performing electroless plating treatment on the outer wall that has been brought into contact with the liquid containing the catalyst.
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PCT/JP2022/026177 WO2023053647A1 (en) | 2021-09-30 | 2022-06-30 | Method for manufacturing composite material to be plated and method for manufacturing anisotropic electroconductive sheet |
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JPH05110247A (en) * | 1991-10-18 | 1993-04-30 | Shin Etsu Chem Co Ltd | Manufacture of board for flexible printed wiring |
US7033648B1 (en) * | 1995-02-06 | 2006-04-25 | International Business Machines Corporations | Means of seeding and metallizing polyimide |
JP4708920B2 (en) | 2005-08-26 | 2011-06-22 | 荏原ユージライト株式会社 | Method for forming metal plating film on polyimide resin |
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WO2014017291A1 (en) * | 2012-07-26 | 2014-01-30 | 学校法人 関東学院 | Method for imparting electrical conductivity to silicone resin, and silicone resin provided with metallic coating film |
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WO2018084804A1 (en) * | 2016-11-03 | 2018-05-11 | Agency For Science, Technology And Research | Electroless nickel plating of silicone rubber |
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