JP2014055388A - Metal coated fiber - Google Patents
Metal coated fiber Download PDFInfo
- Publication number
- JP2014055388A JP2014055388A JP2012202171A JP2012202171A JP2014055388A JP 2014055388 A JP2014055388 A JP 2014055388A JP 2012202171 A JP2012202171 A JP 2012202171A JP 2012202171 A JP2012202171 A JP 2012202171A JP 2014055388 A JP2014055388 A JP 2014055388A
- Authority
- JP
- Japan
- Prior art keywords
- metal
- fiber
- plating film
- plating
- metal plating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 151
- 239000002184 metal Substances 0.000 title claims abstract description 151
- 239000000835 fiber Substances 0.000 title claims abstract description 120
- 238000007747 plating Methods 0.000 claims abstract description 125
- 238000000034 method Methods 0.000 claims description 26
- 239000000758 substrate Substances 0.000 claims description 23
- 150000001875 compounds Chemical class 0.000 claims description 22
- 125000000623 heterocyclic group Chemical class 0.000 claims description 22
- 238000007772 electroless plating Methods 0.000 claims description 19
- 150000003839 salts Chemical class 0.000 claims description 16
- 230000003197 catalytic effect Effects 0.000 claims description 5
- 239000007800 oxidant agent Substances 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 32
- 239000002994 raw material Substances 0.000 abstract 2
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 239000002585 base Substances 0.000 description 40
- 239000007864 aqueous solution Substances 0.000 description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- 229910052802 copper Inorganic materials 0.000 description 9
- 239000010949 copper Substances 0.000 description 9
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 8
- 238000005452 bending Methods 0.000 description 7
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 229910052763 palladium Inorganic materials 0.000 description 3
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 3
- QENGPZGAWFQWCZ-UHFFFAOYSA-N 3-Methylthiophene Chemical compound CC=1C=CSC=1 QENGPZGAWFQWCZ-UHFFFAOYSA-N 0.000 description 2
- FEKWWZCCJDUWLY-UHFFFAOYSA-N 3-methyl-1h-pyrrole Chemical compound CC=1C=CNC=1 FEKWWZCCJDUWLY-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Natural products CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 229920006231 aramid fiber Polymers 0.000 description 2
- 208000028659 discharge Diseases 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 238000009832 plasma treatment Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229930192474 thiophene Natural products 0.000 description 2
- ZXSQEZNORDWBGZ-UHFFFAOYSA-N 1,3-dihydropyrrolo[2,3-b]pyridin-2-one Chemical compound C1=CN=C2NC(=O)CC2=C1 ZXSQEZNORDWBGZ-UHFFFAOYSA-N 0.000 description 1
- CTWQGTOWGFCWNW-UHFFFAOYSA-N 1,3-dimethylpyrrole Chemical compound CC=1C=CN(C)C=1 CTWQGTOWGFCWNW-UHFFFAOYSA-N 0.000 description 1
- OXHNLMTVIGZXSG-UHFFFAOYSA-N 1-Methylpyrrole Chemical compound CN1C=CC=C1 OXHNLMTVIGZXSG-UHFFFAOYSA-N 0.000 description 1
- VPUAYOJTHRDUTK-UHFFFAOYSA-N 1-ethylpyrrole Chemical compound CCN1C=CC=C1 VPUAYOJTHRDUTK-UHFFFAOYSA-N 0.000 description 1
- KTDPOCUIJQPZNJ-UHFFFAOYSA-N 1-naphthalen-1-ylpyrrole Chemical compound C1=CC=CN1C1=CC=CC2=CC=CC=C12 KTDPOCUIJQPZNJ-UHFFFAOYSA-N 0.000 description 1
- GEZGAZKEOUKLBR-UHFFFAOYSA-N 1-phenylpyrrole Chemical compound C1=CC=CN1C1=CC=CC=C1 GEZGAZKEOUKLBR-UHFFFAOYSA-N 0.000 description 1
- WAUGGYPDCQZJKK-UHFFFAOYSA-N 1h-pyrrol-3-amine Chemical compound NC=1C=CNC=1 WAUGGYPDCQZJKK-UHFFFAOYSA-N 0.000 description 1
- YMMGRPLNZPTZBS-UHFFFAOYSA-N 2,3-dihydrothieno[2,3-b][1,4]dioxine Chemical compound O1CCOC2=C1C=CS2 YMMGRPLNZPTZBS-UHFFFAOYSA-N 0.000 description 1
- GKWLILHTTGWKLQ-UHFFFAOYSA-N 2,3-dihydrothieno[3,4-b][1,4]dioxine Chemical compound O1CCOC2=CSC=C21 GKWLILHTTGWKLQ-UHFFFAOYSA-N 0.000 description 1
- DVXVUWFTCSCGMX-UHFFFAOYSA-N 2-(3-methylphenoxy)-1h-pyrrole Chemical compound CC1=CC=CC(OC=2NC=CC=2)=C1 DVXVUWFTCSCGMX-UHFFFAOYSA-N 0.000 description 1
- CUYOZAIYMLJJQY-UHFFFAOYSA-N 2-(3-methylphenyl)-1h-pyrrole Chemical compound CC1=CC=CC(C=2NC=CC=2)=C1 CUYOZAIYMLJJQY-UHFFFAOYSA-N 0.000 description 1
- FCVHZARBOWEONP-UHFFFAOYSA-N 3-butoxy-1h-pyrrole Chemical compound CCCCOC=1C=CNC=1 FCVHZARBOWEONP-UHFFFAOYSA-N 0.000 description 1
- ATWNFFKGYPYZPJ-UHFFFAOYSA-N 3-butyl-1h-pyrrole Chemical compound CCCCC=1C=CNC=1 ATWNFFKGYPYZPJ-UHFFFAOYSA-N 0.000 description 1
- KPOCSQCZXMATFR-UHFFFAOYSA-N 3-butylthiophene Chemical compound CCCCC=1C=CSC=1 KPOCSQCZXMATFR-UHFFFAOYSA-N 0.000 description 1
- JAYBIBLZTQMCAY-UHFFFAOYSA-N 3-decylthiophene Chemical compound CCCCCCCCCCC=1C=CSC=1 JAYBIBLZTQMCAY-UHFFFAOYSA-N 0.000 description 1
- RFKWIEFTBMACPZ-UHFFFAOYSA-N 3-dodecylthiophene Chemical compound CCCCCCCCCCCCC=1C=CSC=1 RFKWIEFTBMACPZ-UHFFFAOYSA-N 0.000 description 1
- KEAYXGHOGPUYPB-UHFFFAOYSA-N 3-ethoxy-1h-pyrrole Chemical compound CCOC=1C=CNC=1 KEAYXGHOGPUYPB-UHFFFAOYSA-N 0.000 description 1
- ZLQZKKYPEFVWNX-UHFFFAOYSA-N 3-ethyl-1-methylpyrrole Chemical compound CCC=1C=CN(C)C=1 ZLQZKKYPEFVWNX-UHFFFAOYSA-N 0.000 description 1
- NIBNIYBSUWLRRZ-UHFFFAOYSA-N 3-ethyl-1-phenylpyrrole Chemical compound C1=C(CC)C=CN1C1=CC=CC=C1 NIBNIYBSUWLRRZ-UHFFFAOYSA-N 0.000 description 1
- RLLBWIDEGAIFPI-UHFFFAOYSA-N 3-ethyl-1h-pyrrole Chemical compound CCC=1C=CNC=1 RLLBWIDEGAIFPI-UHFFFAOYSA-N 0.000 description 1
- IUUMHORDQCAXQU-UHFFFAOYSA-N 3-heptylthiophene Chemical compound CCCCCCCC=1C=CSC=1 IUUMHORDQCAXQU-UHFFFAOYSA-N 0.000 description 1
- JEDHEMYZURJGRQ-UHFFFAOYSA-N 3-hexylthiophene Chemical compound CCCCCCC=1C=CSC=1 JEDHEMYZURJGRQ-UHFFFAOYSA-N 0.000 description 1
- OTODBDQJLMYYKQ-UHFFFAOYSA-N 3-methoxy-1h-pyrrole Chemical compound COC=1C=CNC=1 OTODBDQJLMYYKQ-UHFFFAOYSA-N 0.000 description 1
- RFSKGCVUDQRZSD-UHFFFAOYSA-N 3-methoxythiophene Chemical compound COC=1C=CSC=1 RFSKGCVUDQRZSD-UHFFFAOYSA-N 0.000 description 1
- UAHOVFOZEICOPL-UHFFFAOYSA-N 3-methyl-1-phenylpyrrole Chemical compound C1=C(C)C=CN1C1=CC=CC=C1 UAHOVFOZEICOPL-UHFFFAOYSA-N 0.000 description 1
- MVZGPBJYYQDJGD-UHFFFAOYSA-N 3-naphthalen-1-yl-1h-pyrrole Chemical compound N1C=CC(C=2C3=CC=CC=C3C=CC=2)=C1 MVZGPBJYYQDJGD-UHFFFAOYSA-N 0.000 description 1
- HKGNMDIQKJTZLY-UHFFFAOYSA-N 3-naphthalen-1-yloxythiophene Chemical compound C=1C=CC2=CC=CC=C2C=1OC=1C=CSC=1 HKGNMDIQKJTZLY-UHFFFAOYSA-N 0.000 description 1
- UUHSVAMCIZLNDQ-UHFFFAOYSA-N 3-nonylthiophene Chemical compound CCCCCCCCCC=1C=CSC=1 UUHSVAMCIZLNDQ-UHFFFAOYSA-N 0.000 description 1
- WQYWXQCOYRZFAV-UHFFFAOYSA-N 3-octylthiophene Chemical compound CCCCCCCCC=1C=CSC=1 WQYWXQCOYRZFAV-UHFFFAOYSA-N 0.000 description 1
- PIQKSZYJGUXAQF-UHFFFAOYSA-N 3-pentylthiophene Chemical compound CCCCCC=1C=CSC=1 PIQKSZYJGUXAQF-UHFFFAOYSA-N 0.000 description 1
- BNQPUGPPVNNKBK-UHFFFAOYSA-N 3-phenoxy-1h-pyrrole Chemical compound C=1C=CC=CC=1OC=1C=CNC=1 BNQPUGPPVNNKBK-UHFFFAOYSA-N 0.000 description 1
- LJDRAKFYYGCAQC-UHFFFAOYSA-N 3-phenyl-1h-pyrrole Chemical compound N1C=CC(C=2C=CC=CC=2)=C1 LJDRAKFYYGCAQC-UHFFFAOYSA-N 0.000 description 1
- ISILMSBNKVBVAW-UHFFFAOYSA-N 3-propoxy-1h-pyrrole Chemical compound CCCOC=1C=CNC=1 ISILMSBNKVBVAW-UHFFFAOYSA-N 0.000 description 1
- STIIRMZYURVVGK-UHFFFAOYSA-N 3-undecylthiophene Chemical compound CCCCCCCCCCCC=1C=CSC=1 STIIRMZYURVVGK-UHFFFAOYSA-N 0.000 description 1
- RBWNDBNSJFCLBZ-UHFFFAOYSA-N 7-methyl-5,6,7,8-tetrahydro-3h-[1]benzothiolo[2,3-d]pyrimidine-4-thione Chemical compound N1=CNC(=S)C2=C1SC1=C2CCC(C)C1 RBWNDBNSJFCLBZ-UHFFFAOYSA-N 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229920000271 Kevlar® Polymers 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000009954 braiding Methods 0.000 description 1
- ODWXUNBKCRECNW-UHFFFAOYSA-M bromocopper(1+) Chemical compound Br[Cu+] ODWXUNBKCRECNW-UHFFFAOYSA-M 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- 229940116318 copper carbonate Drugs 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 1
- YRNNKGFMTBWUGL-UHFFFAOYSA-L copper(ii) perchlorate Chemical compound [Cu+2].[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O YRNNKGFMTBWUGL-UHFFFAOYSA-L 0.000 description 1
- GEZOTWYUIKXWOA-UHFFFAOYSA-L copper;carbonate Chemical compound [Cu+2].[O-]C([O-])=O GEZOTWYUIKXWOA-UHFFFAOYSA-L 0.000 description 1
- IJCCOEGCVILSMZ-UHFFFAOYSA-L copper;dichlorate Chemical compound [Cu+2].[O-]Cl(=O)=O.[O-]Cl(=O)=O IJCCOEGCVILSMZ-UHFFFAOYSA-L 0.000 description 1
- QYCVHILLJSYYBD-UHFFFAOYSA-L copper;oxalate Chemical compound [Cu+2].[O-]C(=O)C([O-])=O QYCVHILLJSYYBD-UHFFFAOYSA-L 0.000 description 1
- 238000003851 corona treatment Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- ZUVOYUDQAUHLLG-OLXYHTOASA-L disilver;(2r,3r)-2,3-dihydroxybutanedioate Chemical compound [Ag+].[Ag+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O ZUVOYUDQAUHLLG-OLXYHTOASA-L 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 239000004761 kevlar Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- AERISNWCJCOZBP-UHFFFAOYSA-N n,n-diethyl-1h-pyrrol-3-amine Chemical compound CCN(CC)C=1C=CNC=1 AERISNWCJCOZBP-UHFFFAOYSA-N 0.000 description 1
- QCCWVNLOJADEAV-UHFFFAOYSA-N n,n-dimethyl-1h-pyrrol-3-amine Chemical compound CN(C)C=1C=CNC=1 QCCWVNLOJADEAV-UHFFFAOYSA-N 0.000 description 1
- DKJLVDCRIQEANB-UHFFFAOYSA-N n,n-diphenyl-1h-pyrrol-3-amine Chemical compound N1C=CC(N(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 DKJLVDCRIQEANB-UHFFFAOYSA-N 0.000 description 1
- SSDXUPFKOUSWHH-UHFFFAOYSA-N n-(3-phenylnaphthalen-1-yl)-1h-pyrrol-2-amine Chemical compound C=1C(C=2C=CC=CC=2)=CC2=CC=CC=C2C=1NC1=CC=CN1 SSDXUPFKOUSWHH-UHFFFAOYSA-N 0.000 description 1
- VRLPFKWKOHFJAB-UHFFFAOYSA-N n-phenyl-1h-pyrrol-2-amine Chemical compound C=1C=CC=CC=1NC1=CC=CN1 VRLPFKWKOHFJAB-UHFFFAOYSA-N 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229940078494 nickel acetate Drugs 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- UQPSGBZICXWIAG-UHFFFAOYSA-L nickel(2+);dibromide;trihydrate Chemical compound O.O.O.Br[Ni]Br UQPSGBZICXWIAG-UHFFFAOYSA-L 0.000 description 1
- DOLZKNFSRCEOFV-UHFFFAOYSA-L nickel(2+);oxalate Chemical compound [Ni+2].[O-]C(=O)C([O-])=O DOLZKNFSRCEOFV-UHFFFAOYSA-L 0.000 description 1
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000002940 palladium Chemical class 0.000 description 1
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 description 1
- INIOZDBICVTGEO-UHFFFAOYSA-L palladium(ii) bromide Chemical compound Br[Pd]Br INIOZDBICVTGEO-UHFFFAOYSA-L 0.000 description 1
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- -1 polyparaphenylene benzobisoxazole Polymers 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 description 1
- 229940071536 silver acetate Drugs 0.000 description 1
- 229910001958 silver carbonate Inorganic materials 0.000 description 1
- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 description 1
- 229940096017 silver fluoride Drugs 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- REYHXKZHIMGNSE-UHFFFAOYSA-M silver monofluoride Chemical compound [F-].[Ag+] REYHXKZHIMGNSE-UHFFFAOYSA-M 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- KKKDGYXNGYJJRX-UHFFFAOYSA-M silver nitrite Chemical compound [Ag+].[O-]N=O KKKDGYXNGYJJRX-UHFFFAOYSA-M 0.000 description 1
- XNGYKPINNDWGGF-UHFFFAOYSA-L silver oxalate Chemical compound [Ag+].[Ag+].[O-]C(=O)C([O-])=O XNGYKPINNDWGGF-UHFFFAOYSA-L 0.000 description 1
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 description 1
- 229910000367 silver sulfate Inorganic materials 0.000 description 1
- FLESIOBKYPIHQI-UHFFFAOYSA-M silver;2,2-dimethylpropanoate Chemical compound [Ag+].CC(C)(C)C([O-])=O FLESIOBKYPIHQI-UHFFFAOYSA-M 0.000 description 1
- CYLMOXYXYHNGHZ-UHFFFAOYSA-M silver;propanoate Chemical compound [Ag+].CCC([O-])=O CYLMOXYXYHNGHZ-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Images
Abstract
Description
本発明は、電線の中心線や信号線、シールド線などの用途に使用できる金属被覆繊維に関する。 The present invention relates to a metal-coated fiber that can be used for applications such as a center line, a signal line, and a shield line of an electric wire.
従来の電線やシールド線には銅線が用いられ、自動車、電子機器、オーディオ機器等に使用されている。しかし、頻繁に屈曲やねじれが加わる用途では金属疲労により、銅線が断線しやすい問題があった。更に、取り付け加工時の引張りにより、銅線が断線しやすい問題もあった。 Copper wires are used for conventional electric wires and shield wires, and are used in automobiles, electronic devices, audio devices and the like. However, in applications where bending and twisting are frequently applied, there is a problem that the copper wire is likely to break due to metal fatigue. Further, there is a problem that the copper wire is easily broken due to the tension during the mounting process.
これら問題を解決するために、例えば特許文献１記載の装置で、マルチフィラメントのような繊維束の表面に金属めっき膜を設けたものが提案されている。 In order to solve these problems, for example, an apparatus described in Patent Document 1 in which a metal plating film is provided on the surface of a fiber bundle such as a multifilament has been proposed.
しかしながら、特許文献１の装置で、マルチフィラメントのような繊維束の表面に金属めっき膜を設けたものは、図２に示すように金属めっき膜を設ける前の繊維束の形状に比べて扁平になり易く、即ち、後述の扁平率が３を超えた金属被覆繊維となり易く、結果、柔軟性が悪く、屈曲時に金属めっき膜が割れ、しかも密着性や引張強度が低下する問題があった。更に、扁平率が３を超えた金属被覆繊維は、後加工において、ねじれや糸切れが発生しやすく、生産性が低下する問題があった。 However, the apparatus of Patent Document 1 in which a metal plating film is provided on the surface of a fiber bundle such as a multifilament is flatter than the shape of the fiber bundle before the metal plating film is provided as shown in FIG. In other words, there is a problem that a metal-coated fiber having a flatness ratio exceeding 3 described later tends to be obtained, and as a result, the flexibility is poor, the metal plating film is cracked when bent, and adhesion and tensile strength are lowered. Furthermore, the metal-coated fiber having a flatness ratio exceeding 3 is liable to be twisted or broken during post-processing, resulting in a problem of reduced productivity.
そこで、本発明は、有機繊維基材としてマルチフィラメントのような繊維束の表面に、金属めっき膜を設けても、屈曲時に金属めっき膜が割れることなく、かつ密着性や引張強度が低下し難い金属被覆繊維を提供することを目的とする。 Therefore, in the present invention, even when a metal plating film is provided on the surface of a fiber bundle such as a multifilament as an organic fiber base material, the metal plating film is not cracked at the time of bending, and adhesion and tensile strength are not easily lowered. An object is to provide a metal-coated fiber.
本発明の金属被覆繊維は、有機繊維基材に金属めっき膜を設けた金属被覆繊維であって、有機繊維基材は、マルチフィラメントからなり、金属めっき膜のめっき率が５０％以上であり、得られた金属被覆繊維における断面繊維の扁平率が１〜３であることを特徴とする。 The metal-coated fiber of the present invention is a metal-coated fiber in which a metal plating film is provided on an organic fiber substrate, the organic fiber substrate is made of a multifilament, and the plating rate of the metal plating film is 50% or more, The flatness of the cross-section fiber in the obtained metal-coated fiber is 1 to 3.
本発明の金属被覆繊維は、有機繊維基材としてマルチフィラメントのような繊維束の表面に、金属めっき膜を設けても、屈曲時に金属めっき膜が割れることなく、かつ密着性や引張強度が低下し難いものである。 The metal-coated fiber according to the present invention has a metal plating film that is not cracked when bent even when a metal plating film is provided on the surface of a fiber bundle such as a multifilament as an organic fiber base material, and adhesion and tensile strength are reduced. It is difficult to do.
本発明について詳細に説明する。
本発明は、有機繊維基材に金属めっき膜を設けた金属被覆繊維であって、有機繊維基材は、マルチフィラメントからなり、金属めっき膜のめっき率が５０％以上であり、得られた金属被覆繊維における断面繊維の扁平率が１〜３であることを特徴とする。なお、本発明の金属被覆繊維は、マルチフィラメントにおけるモノフィラメント(単糸)１本１本に金属めっき膜が形成されているものである。
The present invention will be described in detail.
The present invention is a metal-coated fiber in which a metal plating film is provided on an organic fiber substrate, the organic fiber substrate is made of a multifilament, and the plating rate of the metal plating film is 50% or more, and the obtained metal The flatness of the cross-sectional fiber in the coated fiber is 1 to 3. The metal-coated fibers of the present invention are those in which a metal plating film is formed on each monofilament (single yarn) in a multifilament.
(１)有機繊維基材
本発明に使用する前記有機繊維基材としては、マルチフィラメントであれば特に限定されない。また、ここでいう「マルチフィラメント」とは、モノフィラメント(単糸)の断面形状が真円又は真円に近い形状であり、かつ、そのモノフィラメント(単糸)を数本から数千本合わせて１本の糸としたものである。なお、モノフィラメント(単糸)の断面形状が真円又は真円に近い形状でないものを、数本から数千本合わせて１本の糸としたマルチフィラメントは、後述する扁平率が３を超える傾向にあるため好ましくない。
(1) Organic fiber substrate The organic fiber substrate used in the present invention is not particularly limited as long as it is a multifilament. The “multifilament” here is a monofilament (single yarn) whose cross-sectional shape is a perfect circle or a shape close to a perfect circle, and the monofilament (single yarn) is a combination of several to several thousand. It is a string of books. In addition, multifilaments in which the cross-sectional shape of a monofilament (single yarn) is not a perfect circle or a shape close to a perfect circle, and a single filament combined with several to several thousand tend to have a flatness ratio described later of more than 3. Therefore, it is not preferable.
また、前記マルチフィラメントは、撚糸加工を行ってもよい。撚糸加工を行う際には、下記式１の撚糸係数ｋ＝４２００以下がよく、好ましくは５００〜４２００のものが好ましい。（式１）ｋ＝Ｔ×√Ｄ (Ｔ＝撚糸回数(Ｔ／ｍ)、Ｄ＝総繊度(ｄｔｅｘ))
このように「撚糸係数ｋ」とは、Ｔ＝撚糸回数に、√Ｄ＝総繊度を掛け算した値である。
Further, the multifilament may be subjected to twisting processing. When performing the twisting process, the twisting coefficient k of the following formula 1 is preferably 4200 or less, and preferably 500 to 4200. (Expression 1) k = T × √D (T = number of twisted yarns (T / m), D = total fineness (dtex))
Thus, “twisted yarn coefficient k” is a value obtained by multiplying T = twisted yarn count by √D = total fineness.
また、ここでいう「Ｄ＝総繊度(ｄｔｅｘ)」とは、糸の太さを表すものである。糸の断面は真円ではなく様々な形が考えられることから、長さと重さの比でその太さを表現する。フィラメント糸の場合は『デシテックス（ｄｔｅｘ）』が用いられる。なお、デシテックスは１０,０００ｍあたりのグラム数である。 Further, “D = total fineness (dtex)” here represents the thickness of the yarn. Since the cross-section of the thread is not a perfect circle, but can have various shapes, the thickness is expressed by the ratio of length to weight. In the case of a filament yarn, “decitex (dtex)” is used. Decitex is the number of grams per 10,000 m.
また、ここでいう「Ｔ＝撚糸回数(Ｔ／ｍ)」とは、１ｍあたりの撚り回数である。 Further, “T = twisted yarn number (T / m)” here is the number of twists per 1 m.
本発明の有機繊維基材の材料としては、特に限定されないが、アラミド繊維、芳香族ポリエステル繊維、ポリパラフェニレンベンゾビスオキサゾール繊維などの高強度特性を有するものが望ましい。 The material of the organic fiber base material of the present invention is not particularly limited, but materials having high strength properties such as aramid fiber, aromatic polyester fiber, polyparaphenylene benzobisoxazole fiber are desirable.
また、本発明の有機繊維基材の表面上に、複素環を有する高分子化合物層と酸化剤として機能し且つ無電解めっきの触媒能力を有する金属塩とから構成されるめっき下地層を設け、該めっき下地層上に無電解めっき法により金属めっき膜を設けてもよい。 Moreover, on the surface of the organic fiber base material of the present invention, a plating base layer composed of a polymer compound layer having a heterocyclic ring and a metal salt that functions as an oxidizing agent and has a catalytic ability for electroless plating is provided. A metal plating film may be provided on the plating base layer by an electroless plating method.
また、前記めっき下地層を形成する前に有機繊維基材の表面を親水化処理してもよい。該基材表面に親水化処理を施すことで、複素環を有する化合物層が該基材表面から発生した官能基と水素結合し、密着性を高めることができる。また、めっき下地層（＝複素環を有する化合物と金属塩とを含有する層）を形成しやすくなり、無電解めっき法による金属めっき膜の析出性と密着性が良好になる。
該基材表面を親水化処理する方法としては、任意の適切な方法が採用され得る。前記親水化処理は、例えば、乾式処理でもよく、湿式処理でもよい。乾式処理としては、例えば、コロナ放電処理、プラズマ処理(窒素やアルゴンガスを用いたプラズマ処理は除く)及びグロー放電処理などの放電処理；オゾン処理；ＵＶオゾン処理；紫外線処理及び電子線処理などの電離活性線処理などが挙げられる。湿式処理としては、例えば、水、アセトンなどの溶媒を用いた超音波処理；アルカリ処理；アンカーコート処理などが挙げられる。これらの処理は、単独で行ってもよいし、２つ以上を組み合せて行ってもよい。
Moreover, you may hydrophilize the surface of an organic fiber base material before forming the said plating base layer. By subjecting the surface of the base material to a hydrophilic treatment, the compound layer having a heterocyclic ring can be hydrogen-bonded with a functional group generated from the surface of the base material, thereby improving adhesion. Moreover, it becomes easy to form a plating underlayer (= a layer containing a compound having a heterocyclic ring and a metal salt), and the deposition and adhesion of the metal plating film by the electroless plating method are improved.
Any appropriate method can be adopted as a method for hydrophilizing the substrate surface. The hydrophilic treatment may be, for example, a dry treatment or a wet treatment. Examples of the dry treatment include discharge treatment such as corona discharge treatment, plasma treatment (excluding plasma treatment using nitrogen or argon gas) and glow discharge treatment; ozone treatment; UV ozone treatment; ultraviolet ray treatment and electron beam treatment. Examples include ionizing active ray treatment. Examples of the wet treatment include ultrasonic treatment using a solvent such as water and acetone; alkali treatment; anchor coat treatment. These processes may be performed independently or in combination of two or more.
前記複素環を有する化合物としては、例えば、ピロール、Ｎ−メチルピロール、Ｎ−エチルピロール、Ｎ−フェニルピロール、Ｎ−ナフチルピロール、Ｎ−メチル−３−メチルピロール、Ｎ−メチル−３−エチルピロール、Ｎ−フェニル−３−メチルピロール、Ｎ−フェニル−３−エチルピロール、３−メチルピロール、３−エチルピロール、３−ｎ−ブチルピロール、３−メトキシピロール、３−エトキシピロール、３−ｎ−プロポキシピロール、３−ｎ−ブトキシピロール、３−フェニルピロール、３−トルイルピロール、３−ナフチルピロール、３−フェノキシピロール、３−メチルフェノキシピロール、３−アミノピロール、３−ジメチルアミノピロール、３−ジエチルアミノピロール、３−ジフェニルアミノピロール、３−メチルフェニルアミノピロール及び３−フェニルナフチルアミノピロール等のピロール誘導体；チオフェン、３−メチルチオフェン、３−ｎ−ブチルチオフェン、３−ｎ−ペンチルチオフェン、３−ｎ−ヘキシルチオフェン、３−ｎ−ヘプチルチオフェン、３−ｎ−オクチルチオフェン、３−ｎ−ノニルチオフェン、３−ｎ−デシルチオフェン、３−ｎ−ウンデシルチオフェン、３−ｎ−ドデシルチオフェン、３−メトキシチオフェン、３−ナフトキシチオフェン及び３，４−エチレンジオキシチオフェン等のチオフェン誘導体等が挙げられ、好ましくはピロール、チオフェン及び３，４−エチレンジオキシチオフェン等が挙げられ、より好ましくはピロールが挙げられる。 Examples of the compound having a heterocyclic ring include pyrrole, N-methylpyrrole, N-ethylpyrrole, N-phenylpyrrole, N-naphthylpyrrole, N-methyl-3-methylpyrrole, and N-methyl-3-ethylpyrrole. N-phenyl-3-methylpyrrole, N-phenyl-3-ethylpyrrole, 3-methylpyrrole, 3-ethylpyrrole, 3-n-butylpyrrole, 3-methoxypyrrole, 3-ethoxypyrrole, 3-n- Propoxypyrrole, 3-n-butoxypyrrole, 3-phenylpyrrole, 3-toluylpyrrole, 3-naphthylpyrrole, 3-phenoxypyrrole, 3-methylphenoxypyrrole, 3-aminopyrrole, 3-dimethylaminopyrrole, 3-diethylamino Pyrrole, 3-diphenylaminopyrrole, 3-methyl Pyrrole derivatives such as phenylaminopyrrole and 3-phenylnaphthylaminopyrrole; thiophene, 3-methylthiophene, 3-n-butylthiophene, 3-n-pentylthiophene, 3-n-hexylthiophene, 3-n-heptylthiophene, 3-n-octylthiophene, 3-n-nonylthiophene, 3-n-decylthiophene, 3-n-undecylthiophene, 3-n-dodecylthiophene, 3-methoxythiophene, 3-naphthoxythiophene and 3,4 -Thiophene derivatives, such as ethylenedioxythiophene, etc. are mentioned, Preferably pyrrole, thiophene, 3, 4- ethylenedioxythiophene, etc. are mentioned, More preferably, pyrrole is mentioned.
また、前記複素環を有する化合物を高分子化する際の処理温度は、本発明に使用される。複素環を有する化合物の種類によって適宜選択されるが、好ましくは１０℃〜１３０℃である。 Moreover, the processing temperature at the time of polymerizing the compound which has the said heterocyclic ring is used for this invention. Although it is appropriately selected depending on the type of compound having a heterocyclic ring, it is preferably 10 ° C to 130 ° C.
また、前記酸化剤として機能し且つ無電解めっきの触媒能力を有する金属塩としては、例えば、硝酸銀、酢酸銀、硫酸銀、過塩素酸銀等、フッ化銀、亜硝酸銀、塩化銀、臭化銀、プロピオン酸銀、酒石酸銀、メチルエチル酢酸銀、トリメチル酢酸銀、炭酸銀、シュウ酸銀、雷酸銀の銀塩；硝酸銅、硫酸銅、塩化銅、塩素酸銅、過塩素酸銅、臭化銅、酢酸銅、炭酸銅、シュウ酸銅等の銅塩；硝酸ニッケル、硫酸ニッケル、塩化ニッケル、臭化ニッケル、酢酸ニッケル、炭酸ニッケル、シュウ酸ニッケル等のニッケル塩；硫酸パラジウム、硝酸パラジウム、酢酸パラジウム、塩化パラジウム、臭化パラジウム、ヨウ化パラジウム等のパラジウム塩などが挙げられる。この中でも、ハロゲン化物が好ましく、特に塩化パラジウムが好ましい。 Examples of the metal salt that functions as the oxidizing agent and has the electroless plating catalytic ability include, for example, silver nitrate, silver acetate, silver sulfate, silver perchlorate, silver fluoride, silver nitrite, silver chloride, bromide. Silver, silver propionate, silver tartrate, silver methyl ethyl acetate, silver trimethyl acetate, silver carbonate, silver oxalate, silver thrombate; copper nitrate, copper sulfate, copper chloride, copper chlorate, copper perchlorate, Copper salts such as copper bromide, copper acetate, copper carbonate, copper oxalate; nickel salts such as nickel nitrate, nickel sulfate, nickel chloride, nickel bromide, nickel acetate, nickel carbonate, nickel oxalate; palladium sulfate, palladium nitrate And palladium salts such as palladium acetate, palladium chloride, palladium bromide and palladium iodide. Among these, halides are preferable, and palladium chloride is particularly preferable.
前記めっき下地層（複素環を有する高分子化合物層及び該層に吸着された無電解めっきの触媒能力を有する金属塩から構成される）の形成方法としては、以下の（ａ）乃至（ｃ）のいずれかを採用することができる。
（ａ）前記有機繊維基材を、（ｉ）複素環を有する化合物と（ｉｉ）酸化剤として機能し且つ無電解めっきの触媒能力を有する金属塩とを含む水溶液に浸漬し、そして引き上げる工程を含む方法
（ｂ）前記有機繊維基材を、前記複素環を有する化合物を含む水溶液に浸漬し、そして引き上げた材料を、前記金属塩を含む水溶液に浸漬する工程を含む方法
（ｃ）前記有機繊維基材を、前記金属塩を含む水溶液に浸漬し、そして引き上げた材料を、前記複素環を有する化合物を含む蒸気に接触する工程を含む方法 前記各方法は、当業者に既知である手段を利用して行うことができる。
The following (a) to (c) are used as a method for forming the plating base layer (consisting of a polymer compound layer having a heterocyclic ring and a metal salt having electroless plating catalytic ability adsorbed on the layer). Either of these can be employed.
(A) a step of immersing the organic fiber base material in an aqueous solution containing (i) a compound having a heterocyclic ring and (ii) a metal salt that functions as an oxidizing agent and has a catalytic ability for electroless plating, and then pulling up (B) a method comprising: immersing the organic fiber substrate in an aqueous solution containing the compound having a heterocyclic ring; and immersing the pulled material in an aqueous solution containing the metal salt (c) the organic fiber A method comprising the steps of immersing a substrate in an aqueous solution containing the metal salt and contacting the pulled material with a vapor containing the compound having a heterocyclic ring. Each method utilizes means known to those skilled in the art. Can be done.
前記（ａ）の方法において、前記複素環を有する化合物及び金属塩を含む水溶液を調製する場合、複素環を有する化合物と金属塩（＝複素環を有する化合物／金属塩）の濃度比は０．１〜８０であり、好ましくは０．１〜４０である。濃度比が０．１未満であると複素環を有する化合物の酸化状態及び重合化が不十分となり、また金属塩についても還元状態が不十分となるため、無電解めっきの触媒として作用することが困難となる。一方、濃度比が８０より大きいと、金属塩が材料上に均一に付着することができないため、その後のめっき処理よりにおいて、金属めっき膜も均一に形成しない虞があるからである。
また、材料を、前記複素環を有する化合物及び金属塩を含む水溶液に浸漬させる工程の処理温度は、１０℃〜１３０℃であり、処理時間は、０．１分〜１２０分、好ましくは２０分〜６０分である。
In the method (a), when an aqueous solution containing the compound having a heterocyclic ring and a metal salt is prepared, the concentration ratio of the compound having a heterocyclic ring and the metal salt (= compound having a heterocyclic ring / metal salt) is 0. It is 1-80, Preferably it is 0.1-40. When the concentration ratio is less than 0.1, the oxidation state and polymerization of the compound having a heterocyclic ring are insufficient, and the reduction state of the metal salt is also insufficient, so that it can act as a catalyst for electroless plating. It becomes difficult. On the other hand, if the concentration ratio is greater than 80, the metal salt cannot be uniformly deposited on the material, so that the metal plating film may not be formed uniformly in the subsequent plating process.
The treatment temperature in the step of immersing the material in the aqueous solution containing the compound having a heterocyclic ring and the metal salt is 10 ° C. to 130 ° C., and the treatment time is 0.1 minute to 120 minutes, preferably 20 minutes. ~ 60 minutes.
前記（ｂ）の方法において、前記複素環を有する化合物を含む水溶液の濃度は、５×１０-4〜０．９Ｍであり、好ましくは０．０１〜０．５Ｍである。
また、材料を、前記複素環を有する化合物を含む水溶液に浸漬させる工程の処理温度は、１０℃〜１３０℃であり、処理時間は、０．１分〜５０分、好ましくは１分〜４０分である。
In the method (b), the concentration of the aqueous solution containing the compound having a heterocyclic ring is 5 × 10 −4 to 0.9M, preferably 0.01 to 0.5M.
Further, the treatment temperature of the step of immersing the material in the aqueous solution containing the compound having a heterocyclic ring is 10 ° C. to 130 ° C., and the treatment time is 0.1 minute to 50 minutes, preferably 1 minute to 40 minutes. It is.
前記（ｂ）及び（ｃ）の方法において、好ましい、前記金属塩を含む水溶液としては、０．０２％塩化パラジウム−０．０１％塩酸水溶液（ｐＨ３）である。
また、材料を、前記金属塩を含む水溶液に浸漬させる工程における処理温度は、１０℃〜１３０℃であり、処理時間は、０．１分〜５０分、好ましくは１分〜４０分である。
In the methods (b) and (c), a preferable aqueous solution containing the metal salt is 0.02% palladium chloride-0.01% hydrochloric acid aqueous solution (pH 3).
The treatment temperature in the step of immersing the material in the aqueous solution containing the metal salt is 10 ° C. to 130 ° C., and the treatment time is 0.1 minute to 50 minutes, preferably 1 minute to 40 minutes.
前記（ｃ）の方法において、複素環を有する化合物を含む蒸気としては、上記の複素環を有する化合物を含む水溶液を気化させた蒸気でもよいが、好ましくは複素環を有する化合物そのものを気化させた蒸気である。
また、複素環を有する化合物を含む蒸気に接触させる工程における処理温度は、１０℃〜１３０℃であり、処理時間は、０．１分〜４０分、好ましくは１分〜３０分であり、処理圧力は、常圧若しくは減圧状態であってもよい。
In the method (c), the vapor containing the compound having a heterocyclic ring may be a vapor obtained by vaporizing an aqueous solution containing the compound having a heterocyclic ring, but preferably the compound itself having a heterocyclic ring is vaporized. Steam.
The treatment temperature in the step of contacting with the vapor containing the compound having a heterocyclic ring is 10 ° C. to 130 ° C., the treatment time is 0.1 minutes to 40 minutes, preferably 1 minute to 30 minutes, The pressure may be normal pressure or reduced pressure.
(２) 金属めっき膜
本発明の金属めっき膜は、めっき率が５０％以上となるように設ければよい。
また、ここでいう「めっき率」とは、本発明の金属被覆繊維における金属めっき膜の重量を、金属めっき前の有機繊維基材の重量で割った値である。つまり、めっき率(％)＝金属被覆繊維における金属めっき膜の重量／金属めっき前の有機繊維基材の重量×１００で算出した値である。なお、金属被覆繊維における金属めっき膜の重量は、金属被覆繊維の重量を金属めっき前の有機繊維基材の重量で差し引いて求めることができる。つまり、（金属被覆繊維における金属めっき膜の重量）＝（金属被覆繊維の重量）−（金属めっき前の有機繊維基材の重量）で求めることができる。
このめっき率が５０％未満であると、マルチフィラメントからなる有機繊維基材のモノフィラメント(単糸)１本１本に均一に金属めっき膜が形成されない、即ち、マルチフィラメントにおいて金属めっき膜が析出しない部分が出来、結果、密着性を低下させると共に、抵抗値が高くなるため、例えば電線の中心線や信号線、シールド材として機能しない場合がある。
(2) Metal plating film The metal plating film of this invention should just be provided so that a plating rate may be 50% or more.
Further, the “plating rate” referred to here is a value obtained by dividing the weight of the metal plating film in the metal-coated fiber of the present invention by the weight of the organic fiber substrate before metal plating. That is, the plating rate (%) = the value calculated by the weight of the metal plating film in the metal-coated fiber / the weight of the organic fiber base material before metal plating × 100. In addition, the weight of the metal plating film in the metal-coated fiber can be obtained by subtracting the weight of the metal-coated fiber by the weight of the organic fiber substrate before metal plating. That is, (weight of metal plating film in metal-coated fiber) = (weight of metal-coated fiber) − (weight of organic fiber substrate before metal plating) can be obtained.
When this plating rate is less than 50%, a metal plating film is not uniformly formed on each monofilament (single yarn) of an organic fiber substrate made of multifilaments, that is, no metal plating film is deposited on the multifilaments. A portion is formed, and as a result, the adhesiveness is lowered and the resistance value is increased. For example, the wire may not function as a center line, a signal line, or a shield material.
本発明の金属めっき膜は、有機繊維基材に金属めっき膜を形成する方法であれば、どのような方法でもよく、例えば無電解めっきや電気めっき等の湿式めっき法、蒸着等の乾式めっき法を適宜採用すればよい。 The metal plating film of the present invention may be any method as long as it is a method for forming a metal plating film on an organic fiber substrate, for example, a wet plating method such as electroless plating or electroplating, or a dry plating method such as vapor deposition. May be adopted as appropriate.
本発明の金属めっき膜は、例えば、前記めっき下地層上に無電解めっき法を用いて金属めっき膜を形成することもできる。その場合、上記（ａ）乃至（ｃ）の方法で、有機繊維基材の表面にめっき下地層を設け、続いてめっき液に浸され、これにより無電解めっき法による金属めっき膜が形成される。
めっき液としては、通常、無電解めっきに使用されるめっき液であれば、特に限定されない。すなわち、無電解めっきに使用できる金属としては、例えば、銅、金、銀、ニッケル、及びクロム等、全て適用することができるが、銅が好ましい。無電解めっき浴の具体例としては、具体的には、ＡＴＳアドカッパーＩＷ浴（奥野製薬工業(株)製）等が挙げられる。
無電解めっきの処理温度は、２０℃〜５０℃、好ましくは３０℃〜４０℃であり、処理時間は１０分〜４０分、好ましくは１５分〜３０分である。
The metal plating film of this invention can also form a metal plating film on the said plating base layer using an electroless-plating method, for example. In that case, a plating base layer is provided on the surface of the organic fiber substrate by the above methods (a) to (c), and subsequently immersed in a plating solution, thereby forming a metal plating film by an electroless plating method. .
The plating solution is not particularly limited as long as it is a plating solution usually used for electroless plating. That is, as a metal that can be used for electroless plating, for example, copper, gold, silver, nickel, chromium, and the like can be applied, but copper is preferable. Specific examples of the electroless plating bath include ATS add-copper IW bath (Okuno Pharmaceutical Co., Ltd.) and the like.
The treatment temperature for electroless plating is 20 ° C. to 50 ° C., preferably 30 ° C. to 40 ° C., and the treatment time is 10 minutes to 40 minutes, preferably 15 minutes to 30 minutes.
また、無電解めっき法により形成された金属めっき膜の厚みは、０．３〜３μｍとすることが好ましい。この金属めっき膜の厚みが３μｍを超えると、柔軟性が低下する場合があり、厚みが０．３μｍ未満であると、例えば電線の中心線や信号線、シールド材として機能しない場合がある。 Moreover, it is preferable that the thickness of the metal plating film formed by the electroless plating method is 0.3 to 3 μm. When the thickness of the metal plating film exceeds 3 μm, the flexibility may be lowered, and when the thickness is less than 0.3 μm, for example, the metal plating film may not function as a center line, a signal line, or a shielding material of the electric wire.
また、無電解めっき法により形成された金属めっき膜上に、溶融錫めっきや電気めっき
を行ってもよい。特に、耐熱性の高い有機繊維基材を使用した場合、溶融錫めっきが有効
である。
Alternatively, hot tin plating or electroplating may be performed on a metal plating film formed by an electroless plating method. In particular, when an organic fiber base material having high heat resistance is used, hot-dip tin plating is effective.
(３)金属被覆繊維
本発明の金属被覆繊維は、マルチフィラメントからなる有機繊維基材に金属めっき膜を設けたものであり、金属めっき膜のめっき率が５０％であると共に、金属被覆繊維における断面繊維の扁平率が１〜３であればよい。
また、ここでいう「扁平率」とは、金属被覆繊維における繊維断面を観察し、長辺ａと短辺ｂの長さを測定し、扁平率＝ａ／ｂで算出した値である。
そして、金属めっき膜を形成する際、マルチフィラメントからなる有機繊維基材に張力を掛けない状態、例えば有機繊維基材をかせ状態で金属めっき膜を形成すると、得られた金属被覆繊維における断面繊維の扁平率を１〜３にすることができ、図１に示すようにマルチフィラメントにおけるモノフィラメント(単糸)１本１本に金属めっき膜が形成され、柔軟性に優れるため、屈曲時に金属めっき膜が割れず、更には密着性や引張強度の低下が少ない。
それに対し、金属めっき膜を形成する際、マルチフィラメントからなる有機繊維基材に張力を掛けた状態、例えば有機繊維基材を穴の開いた筒に張力でソフトワインディングしてチーズ状の巻糸体で金属めっき膜を形成すると、得られた金属被覆繊維における断面繊維の扁平率が３を超え、図２に示すような扁平状の金属被覆繊維となり、マルチフィラメントにおけるモノフィラメント(単糸)１本１本に金属めっき膜が形成されない上、マルチフィラメントの周囲を覆うように金属めっき膜が形成されてしまうため、柔軟性が悪く、屈曲時に金属めっき膜が割れ、更には密着性と引張強度が低下してしまう。
(3) Metal-coated fiber The metal-coated fiber of the present invention is obtained by providing a metal plating film on an organic fiber substrate made of multifilament, and the plating rate of the metal plating film is 50%. The flatness of the cross-sectional fiber should just be 1-3.
Further, the “flatness” herein is a value calculated by observing the fiber cross section of the metal-coated fiber, measuring the lengths of the long side a and the short side b, and the flatness = a / b.
And, when forming the metal plating film, when the metal plating film is formed in a state in which the organic fiber base made of multifilament is not tensioned, for example, in a state in which the organic fiber base is laid, the cross-sectional fiber in the obtained metal-coated fiber As shown in FIG. 1, a metal plating film is formed on each monofilament (single yarn) in a multifilament, and is excellent in flexibility. Does not break, and there is little decrease in adhesion and tensile strength.
On the other hand, when forming a metal plating film, a tension is applied to the organic fiber substrate made of multifilament, for example, the organic fiber substrate is soft-winded with a tension in a tube with a hole, and a cheese-like wound body When the metal plating film is formed, the flatness of the cross-section fiber in the obtained metal-coated fiber exceeds 3, and a flat metal-coated fiber as shown in FIG. 2 is obtained. One monofilament (single yarn) in a multifilament 1 Since the metal plating film is not formed on the book and the metal plating film is formed so as to cover the periphery of the multifilament, the flexibility is poor, the metal plating film is cracked when bent, and the adhesion and the tensile strength are lowered. Resulting in.
次に、本発明を実施例により更に詳細に説明するが、本発明は実施例に限定されるものでない。 EXAMPLES Next, although an Example demonstrates this invention still in detail, this invention is not limited to an Example.
[実施例１]
＜めっき下地層＞
ピロールモノマー６．５ｍＭ、塩化パラジウム水溶液０．２５ｍＭ、及び塩酸１０ｍＭをイオン交換水に加えて、混合液を得た。そして、この混合液中に、マルチフィラメント（東レ・デュポン(株)製のＫｅｖｌａｒ、アラミド繊維、総繊度＝１１０ｄｔｅｘ、撚糸回数＝１００Ｔ／ｍ）からなる有機繊維基材を８０℃で３０分間浸漬し、その後、イオン交換水で洗浄し、乾燥させてめっき下地層を形成したマルチフィラメントからなる有機繊維基材を得た。
＜無電解めっき＞
次に、前記めっき下地層を形成したマルチフィラメントからなる有機繊維基材をかせ状態にし、めっき液 (メルテックス(株)製のメルプレートＣＵ５１００Ｐ)に５０℃で１０分間浸漬し、前記めっき下地層上に銅膜からなる金属めっき膜を形成した金属被覆繊維を得た。
なお、得られた金属被覆繊維は、マルチフィラメントにおけるモノフィラメント(単糸)１本１本に金属めっき膜が形成されていた。
[Example 1]
<Plating underlayer>
A pyrrole monomer 6.5 mM, palladium chloride aqueous solution 0.25 mM, and hydrochloric acid 10 mM were added to ion-exchange water, and the liquid mixture was obtained. Then, an organic fiber substrate made of multifilament (Kevlar, aramid fiber, total fineness = 110 dtex, number of twists = 100 T / m, manufactured by Toray DuPont Co., Ltd.) is immersed in this mixed solution at 80 ° C. for 30 minutes. Then, the organic fiber base material which consists of the multifilament which wash | cleaned with ion-exchange water and was made to dry and formed the plating foundation layer was obtained.
<Electroless plating>
Next, the organic fiber base material composed of multifilaments on which the plating base layer is formed is skeined and immersed in a plating solution (Melplate CU5100P manufactured by Meltex Co., Ltd.) for 10 minutes at 50 ° C. A metal-coated fiber on which a metal plating film made of a copper film was formed was obtained.
In addition, as for the obtained metal covering fiber, the metal plating film was formed in each monofilament (single yarn) in a multifilament.
［実施例２］
実施例１と同様の操作を行い、めっき下地層を形成したマルチフィラメントからなる有機繊維基材を得た。
次に、前記めっき下地層を形成したマルチフィラメントからなる有機繊維基材をかせ状態にし、めっき液 (メルテックス(株)製のメルプレートＣＵ５１００Ｐ)に５０℃で５分間浸漬し、前記めっき下地層上に銅膜からなる金属めっき膜を形成した金属被覆繊維を得た。
なお、得られた金属被覆繊維は、マルチフィラメントにおけるモノフィラメント(単糸)１本１本に金属めっき膜が形成されていた。
[Example 2]
The same operation as in Example 1 was performed to obtain an organic fiber base material composed of multifilaments on which a plating base layer was formed.
Next, the organic fiber base material composed of multifilaments on which the plating base layer is formed is skeined and immersed in a plating solution (Melplate CU5100P manufactured by Meltex Co., Ltd.) for 5 minutes at 50 ° C. A metal-coated fiber on which a metal plating film made of a copper film was formed was obtained.
In addition, as for the obtained metal covering fiber, the metal plating film was formed in each monofilament (single yarn) in a multifilament.
［比較例１］
実施例１と同様の操作を行い、めっき下地層を形成したマルチフィラメントからなる有機繊維基材を得た。
次に、前記めっき下地層を形成したマルチフィラメントからなる有機繊維基材を、穴の開いた筒に張力３０ｇでソフトワインディングしてチーズ状の巻糸体にした。
次に、前記チーズ状の巻糸体をめっき液 (メルテックス(株)製のメルプレートＣＵ５１００Ｐ)に浸漬させ、流量２０Ｌ／ｍｉｎで内側から外側へめっき液を循環させ、５０℃で３０分間処理を行った。その後、イオン交換水で水洗いし、脱水と乾燥を行って前記めっき下地層上に銅膜からなる金属めっき膜を形成した金属被覆繊維を得た。
なお、得られた金属被覆繊維は、マルチフィラメントにおけるモノフィラメント(単糸)１本１本に金属めっき膜が形成されない上、マルチフィラメントの周囲を覆うように金属めっき膜が形成されていた。
[Comparative Example 1]
The same operation as in Example 1 was performed to obtain an organic fiber base material composed of multifilaments on which a plating base layer was formed.
Next, the organic fiber base material composed of multifilaments on which the plating base layer was formed was soft-wound into a tube with a hole at a tension of 30 g to obtain a cheese-like wound body.
Next, the cheese-like wound body is immersed in a plating solution (Melplate CU5100P manufactured by Meltex Co., Ltd.), the plating solution is circulated from the inside to the outside at a flow rate of 20 L / min, and treated at 50 ° C. for 30 minutes. Went. Thereafter, it was washed with ion-exchanged water, dehydrated and dried to obtain a metal-coated fiber in which a metal plating film made of a copper film was formed on the plating base layer.
In the obtained metal-coated fiber, a metal plating film was not formed on each monofilament (single yarn) in a multifilament, and a metal plating film was formed so as to cover the periphery of the multifilament.
［比較例２］
実施例１と同様の操作を行い、めっき下地層を形成したマルチフィラメントからなる有機繊維基材を得た。
次に、前記めっき下地層を形成したマルチフィラメントからなる有機繊維基材を、穴の開いた筒に張力３０ｇでソフトワインディングしてチーズ状の巻糸体にした。
次に、前記チーズ状の巻糸体をめっき液 (メルテックス(株)製のメルプレートＣＵ５１００Ｐ)に浸漬させ、流量２０Ｌ／ｍｉｎで内側から外側へめっき液を循環させ、５０℃で６０分間処理を行った。その後、イオン交換水で水洗いし、脱水と乾燥を行って前記めっき下地層上に銅膜からなる金属めっき膜を形成した金属被覆繊維を得た。
なお、得られた金属被覆繊維は、マルチフィラメントにおけるモノフィラメント(単糸)１本１本に金属めっき膜が形成されない上、マルチフィラメントの周囲を覆うように金属めっき膜が形成されていた。
[Comparative Example 2]
The same operation as in Example 1 was performed to obtain an organic fiber base material composed of multifilaments on which a plating base layer was formed.
Next, the organic fiber base material composed of multifilaments on which the plating base layer was formed was soft-wound into a tube with a hole at a tension of 30 g to obtain a cheese-like wound body.
Next, the cheese-like wound body is immersed in a plating solution (Melplate CU5100P manufactured by Meltex Co., Ltd.), and the plating solution is circulated from the inside to the outside at a flow rate of 20 L / min, and treated at 50 ° C. for 60 minutes. Went. Thereafter, it was washed with ion-exchanged water, dehydrated and dried to obtain a metal-coated fiber in which a metal plating film made of a copper film was formed on the plating base layer.
In the obtained metal-coated fiber, a metal plating film was not formed on each monofilament (single yarn) in a multifilament, and a metal plating film was formed so as to cover the periphery of the multifilament.
［比較例３］
実施例１と同様の操作を行い、めっき下地層を形成したマルチフィラメントからなる有機繊維基材を得た。
次に、前記めっき下地層を形成したマルチフィラメントからなる有機繊維基材をかせ状態にし、めっき液 (メルテックス(株)製のメルプレートＣＵ５１００Ｐ)に５０℃で３分間浸漬し、前記めっき下地層上に銅膜からなる金属めっき膜を形成した金属被覆繊維を得た。
なお、得られた金属被覆繊維は、マルチフィラメントにおけるモノフィラメント(単糸)１本１本に均一に金属めっき膜が形成されていなかった、即ち金属めっき膜が析出していない部分があった。
[Comparative Example 3]
The same operation as in Example 1 was performed to obtain an organic fiber base material composed of multifilaments on which a plating base layer was formed.
Next, the organic fiber base material composed of multifilaments on which the plating base layer is formed is skeined and immersed in a plating solution (Melplate CU5100P manufactured by Meltex Co., Ltd.) for 3 minutes at 50 ° C. A metal-coated fiber on which a metal plating film made of a copper film was formed was obtained.
In addition, the obtained metal-coated fiber had a portion in which the metal plating film was not uniformly formed on each monofilament (single yarn) in the multifilament, that is, the metal plating film was not deposited.
試験例１
上記で製造した実施例１〜２、並びに比較例１〜３の金属被覆繊維において、各種の評価試験を行いその結果を表１に纏めた。
尚、評価試験項目及びその評価方法・評価基準は以下の通りである。
Test example 1
Various evaluation tests were performed on the metal-coated fibers of Examples 1 and 2 and Comparative Examples 1 to 3 manufactured above, and the results are summarized in Table 1.
The evaluation test items, evaluation methods and evaluation criteria are as follows.
(扁平率)
金属被覆繊維における繊維断面を観察し、長辺ａと短辺ｂの長さを測定し、扁平率＝ａ／ｂを算出した。
(Flat rate)
The cross section of the metal-coated fiber was observed, the lengths of the long side a and the short side b were measured, and the flatness ratio = a / b was calculated.
(めっき率)
金属被覆繊維における金属めっき膜の重量を、金属めっき前の有機繊維基材の重量で割った値である。つまり、めっき率(％)＝金属被覆繊維における金属めっき膜の重量／金属めっき前の有機繊維基材の重量×１００で算出した。
(Plating rate)
It is a value obtained by dividing the weight of the metal plating film in the metal-coated fiber by the weight of the organic fiber substrate before metal plating. That is, the plating rate (%) was calculated by the weight of metal plating film in metal-coated fiber / weight of organic fiber base material before metal plating × 100.
(抵抗値)
デジタルテスター(ＣＵＳＴＯＭ(株)製のＣＤＭ−２０００Ｄ)を用いて、金属被覆繊維の１ｍあたりの抵抗を２端子間で測定した。
(Resistance value)
Using a digital tester (CDM-2000D manufactured by CUSTOM Corp.), the resistance per 1 m of the metal-coated fiber was measured between two terminals.
(密着性)
編組機(共立(株)製)を用いて、２０ｍの編組線加工を行った際に、金属被覆繊維同士の擦れ合いによる金属めっき膜の剥離状態を評価した。
○：金属めっき膜の剥離なし
×：金属めっき膜の剥離あり
(Adhesion)
Using a braiding machine (manufactured by Kyoritsu Co., Ltd.), when a 20 m braided wire was processed, the peeled state of the metal plating film due to the rubbing of the metal-coated fibers was evaluated.
○: No metal plating film peeling ×: Metal plating film peeling
(屈曲試験)
ＭＩＴ耐折度試験機(テスター産業(株))にて、荷重２．９Ｎ、屈曲角度２７０°、屈曲半径０．３８ｍｍ、屈曲速度１７５回／ｍｉｎの条件下で金属被覆繊維を１００回屈曲させ、屈曲後の表面状態を観察し、金属めっき膜の割れを評価した。
○：金属めっき膜の割れなし
×：金属めっき膜の割れあり
(Bending test)
Using a MIT folding resistance tester (Tester Sangyo Co., Ltd.), the metal-coated fiber was bent 100 times under the conditions of a load of 2.9 N, a bending angle of 270 °, a bending radius of 0.38 mm, and a bending speed of 175 times / min. The surface state after bending was observed and the crack of the metal plating film was evaluated.
○: Metal plating film is not cracked ×: Metal plating film is cracked
(引張強度保持率)
１）金属被覆繊維について、ＪＩＳ Ｌ１０１３化学繊維フィラメント系試験方法に準じて引張試験を実施した。
続いて、２）耐圧力容器に金属被覆繊維とイオン交換水を投入し、１５０℃で３時間浸漬させた金属被覆繊維について、ＪＩＳ Ｌ１０１３化学繊維フィラメント系試験方法に準じて引張試験を実施した。
そして、１）金属被覆繊維の引張強度を１００％として、２）金属被覆繊維の引張強度を相対的に評価した。
(Tensile strength retention)
1) The metal-coated fiber was subjected to a tensile test according to the JIS L1013 chemical fiber filament test method.
Subsequently, 2) A metal-coated fiber and ion-exchanged water were put into a pressure-resistant container, and a tensile test was performed on the metal-coated fiber immersed at 150 ° C. for 3 hours according to the JIS L1013 chemical fiber filament system test method.
Then, 1) the tensile strength of the metal-coated fiber was 100%, and 2) the tensile strength of the metal-coated fiber was relatively evaluated.
Claims (2)
有機繊維基材は、マルチフィラメントからなり、
金属めっき膜のめっき率が５０％以上であり、
得られた金属被覆繊維における断面繊維の扁平率が１〜３であることを特徴とする金属繊維。 A metal-coated fiber provided with a metal plating film on an organic fiber substrate,
The organic fiber substrate consists of multifilaments,
The plating rate of the metal plating film is 50% or more,
A metal fiber, wherein the cross-sectional fiber has a flatness ratio of 1 to 3 in the obtained metal-coated fiber.
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