KR20190026475A - Manufacturing method of nickel-plated CuS-PAN fibers for EMI-shielding - Google Patents
Manufacturing method of nickel-plated CuS-PAN fibers for EMI-shielding Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 64
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 8
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 36
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000007772 electroless plating Methods 0.000 claims abstract description 6
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 39
- 239000000243 solution Substances 0.000 claims description 34
- 239000007864 aqueous solution Substances 0.000 claims description 18
- 101150003085 Pdcl gene Proteins 0.000 claims description 13
- 238000004891 communication Methods 0.000 abstract description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 abstract 1
- 238000007747 plating Methods 0.000 description 19
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 18
- 230000004913 activation Effects 0.000 description 15
- 229910052718 tin Inorganic materials 0.000 description 12
- 229910052759 nickel Inorganic materials 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 238000004381 surface treatment Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
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- OHVLMTFVQDZYHP-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CN1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O OHVLMTFVQDZYHP-UHFFFAOYSA-N 0.000 description 1
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
- APLNAFMUEHKRLM-UHFFFAOYSA-N 2-[5-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-1,3,4-oxadiazol-2-yl]-1-(3,4,6,7-tetrahydroimidazo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1=NN=C(O1)CC(=O)N1CC2=C(CC1)N=CN2 APLNAFMUEHKRLM-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- WTFUTSCZYYCBAY-SXBRIOAWSA-N 6-[(E)-C-[[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]methyl]-N-hydroxycarbonimidoyl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C/C(=N/O)/C1=CC2=C(NC(O2)=O)C=C1 WTFUTSCZYYCBAY-SXBRIOAWSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
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- 239000002781 deodorant agent Substances 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000007257 malfunction Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 229920005594 polymer fiber Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
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- D—TEXTILES; PAPER
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic Table; Titanates; Zirconates; Stannates; Plumbates
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/49—Oxides or hydroxides of elements of Groups 8, 9,10 or 18 of the Periodic Table; Ferrates; Cobaltates; Nickelates; Ruthenates; Osmates; Rhodates; Iridates; Palladates; Platinates
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- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
- H05K9/009—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive fibres, e.g. metal fibres, carbon fibres, metallised textile fibres, electro-conductive mesh, woven, non-woven mat, fleece, cross-linked
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Abstract
Description
본 발명은 전자파 차폐용 니켈이 도금된 CuS-PAN 섬유의 제조방법에 관한 것으로서, 더욱 상세하게는 PAN(Poly acrylonitrile)계 섬유를 주석용액에 담지, 상기 주석용액에 담지한 섬유를 팔라듐 용액에 담지, 상기 팔라듐 용액에 담지한 섬유를 무전해 도금하여 제조하는 것이다.More particularly, the present invention relates to a method of producing a CuS-PAN fiber coated with nickel for electro-magnetic shielding, and more particularly, to a method for producing a CuS-PAN fiber by electrodepositing PAN (Poly acrylonitrile) , And the fibers supported on the palladium solution are electroless-plated.
최근 비대칭 디지털 가입자선(ADSL)이 폭발적으로 보급되고 있고, 차세대 휴대폰이나 도로 교통 시스템(ITS)이 개시되는 등 전자파 차폐 대책을 필요로 하는 분야는 더욱 다양해지고 있다. 또한 소형화, 경량화 등의 추세를 보이고 있는 PC나 휴대폰, 디지털 기기의 급속한 보급은 직장이나 가정에까지도 전자파의 홍수를 초래하고 있어, 일렉트로닉스 산업의 발전과 함께 전자파 장해의 위협이 더욱 높아지고 있다.Recently, asymmetric digital subscriber line (ADSL) is spreading explosively, and next-generation mobile phones and road traffic system (ITS) are being launched, and fields requiring electromagnetic shielding measures are becoming more diverse. In addition, the rapid spread of PCs, mobile phones and digital devices, which are showing trends such as miniaturization and light weight, is causing a flood of electromagnetic waves even at work or at home, and the threat of electromagnetic interference is further increased with the development of the electronics industry.
이러한 전자파 장해는 컴퓨터의 오동작에서부터 공장의 전소 사고에 이르기까지 다양하게 나타나고 있으며, 나아가 전자파가 인체에 부정적인 영향을 미치는 연구 결과가 속속 발표되면서 건강에 대한 우려와 관심도 높아지고 있는 가운데, 선진국을 중심으로 전자파 장해에 대한 규제 강화와 대책 마련에 부심하고 있는 실정이다. 따라서 다양한 전자전기 제품에 대한 전자파차폐 기술은 일렉트로닉스 산업의 핵심 기술 분야로 떠오르고 있다.These electromagnetic disturbances are manifested in various ways from malfunctions of computers to accident of factories in factories. Furthermore, as research results that electromagnetic waves have a negative effect on the human body have been announced successively, concern and concern about health have been increasing. It is a fact that the government is trying to strengthen regulations on obstacles and to prepare countermeasures. Therefore, electromagnetic shielding technology for various electronic appliances is emerging as a core technology field of the electronics industry.
한 예로써, 고분자 섬유의 경우 방오성, 항균성, 소취성, 방취성, 자외선 차단성, 방전성, 전자파차폐성 등 여러 특수기능을 부여한 고부가 기능성 섬유에 대한 연구개발이 활발하게 수행되고 있다. 합성섬유에는 PAN계 탄소섬유가 있는데, 탄소섬유는 흑연의 결정을 섬유의 축방향으로 배열시킨 것으로 항공 우주 분야에서 사용되고 있고, 신소재로서 많은 분야에서 다양하게 이용되고 있다.As an example, in the case of polymer fibers, research and development on high value-added functional fibers imparting various special functions such as antifouling property, antimicrobial property, deodorant property, antistatic property, ultraviolet barrier property, discharge property and electromagnetic wave shielding property are actively carried out. There are PAN-based carbon fibers in synthetic fibers. Carbon fibers are arranged in the axial direction of graphite crystals. They are used in the aerospace field and are widely used in many fields as new materials.
다만 합성섬유는 전기부도체이기 때문에 발생한 정전기를 방전하지 못할 뿐만 아니라 전자파 차폐효율이 낮다는 단점을 가지고 있어, 정전기 및 전자파에 의한 여러 심각한 장해를 방지할 수 없기 때문에 정전기 발생 및 전자파투과를 억제할 수 있는 기술 개발이 시급한 실정이다.However, since synthetic fibers are not electrically conductive, they can not discharge generated static electricity and have a disadvantage of low electromagnetic wave shielding efficiency. Therefore, it is impossible to prevent various serious disturbances caused by static electricity and electromagnetic waves, Technology development is urgent.
본 발명은, 전자파 차폐용 니켈이 도금된 CuS-PAN 섬유의 제조방법에 관한 것으로서 CuS-PAN 섬유에 주석 및 팔라듐의 농도와 시간에 따라 표면처리를 진행하고, 일정 농도비의 니켈 도금액에 일정 온도를 유지하며 무전해 도금을 하여 최종적으로 기존 PAN섬유 대비 전기 전도도 및 전자파 차폐효율이 증대된 니켈도금 CuS-PAN 섬유를 제조하는 방법을 제공함에 있다.The present invention relates to a method for producing CuS-PAN fibers coated with nickel for electromagnetic wave shielding, wherein CuS-PAN fibers are subjected to surface treatment according to the concentration and time of tin and palladium, and a predetermined temperature is applied to a nickel plating solution The present invention also provides a method of manufacturing a nickel-plated CuS-PAN fiber in which electromechanical plating is carried out while maintaining the electrical conductivity and electromagnetic shielding efficiency of the PAN fiber.
상기 목적을 달성하기 위하여, 본 발명은 (a) PAN(Poly acrylonitrile)계 섬유를 주석용액에 담지하는 단계, (b) 상기 주석용액에 담지한 섬유를 팔라듐 용액에 담지하는 단계 및 (c) 상기 팔라듐 용액에 담지한 섬유를 무전해 도금하는 단계를 포함하는 것을 특징으로 하는 전자파 차폐용 섬유 제조방법을 제공한다.(B) supporting the fiber supported on the tin solution on a palladium solution; and (c) drying the fiber supported on the tin solution. And a step of electroless plating the fibers carried on the palladium solution.
본 발명의 일실시예에 따르면 상기 (a)단계에서 상기 주석용액은 0.2 내지 10 M 농도의 SnCl2 수용액인 것을 특징으로 한다.According to an embodiment of the present invention, in the step (a), the tin solution may contain SnCl 2 Aqueous solution.
상기 (a)단계에서, 상기 PAN계 섬유를 주석용액에 1분 내지 120분 동안 담지하는 것을 특징으로 할 수 있다.In the step (a), the PAN-based fibers may be supported on the tin solution for 1 minute to 120 minutes.
본 발명의 다른 일실시예에 따르면 상기 (b)단계에서, 상기 팔라듐 용액은 0.1 내지 10 M 농도의 PdCl2 수용액인 것을 특징으로 한다.According to another embodiment of the present invention, in the step (b), the palladium solution is an aqueous PdCl 2 solution of 0.1 to 10 M concentration.
또는 상기 (b)단계에서, 상기 주석용액에 담지한 섬유를 팔라듐 용액에 1분 내지 120분 동안 담지하는 것을 특징으로 할 수 있다.Alternatively, in the step (b), the fiber supported on the tin solution may be supported on the palladium solution for 1 minute to 120 minutes.
상기와 같은 본 발명에 따르면, 우수한 전기전도도 및 전자파 차폐특성을 가진 니켈이 도금된 CuS-PAN 섬유를 제조하여 전기·전자 제품, 항공, 선박 등의 통신기기에서 유입되는 전자파를 차폐함으로써 내장재 등의 용도로 응용될 수 있다.As described above, according to the present invention, nickel-plated CuS-PAN fibers having excellent electrical conductivity and electromagnetic shielding properties are manufactured to shield electromagnetic waves flowing from communication devices such as electric and electronic products, aviation, It can be applied to applications.
도 1은 본 발명의 제조방법으로 얻어진 전자파 차폐용 니켈이 도금된 CuS-PAN 섬유의 SEM 사진이다.
도 2는 각각 다르게 처리된 PAN섬유들의 전자파 차폐효율을 보여준다.BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is an SEM photograph of nickel-plated CuS-PAN fibers obtained by the manufacturing method of the present invention.
Figure 2 shows the EMI shielding efficiencies of the differently treated PAN fibers.
이하, 본 발명을 상세히 설명한다.Hereinafter, the present invention will be described in detail.
본 발명에서 전자파 차폐용 (a) PAN(Poly acrylonitrile)계 섬유를 주석용액에 담지하는 단계; (b) 상기 주석용액에 담지한 섬유를 팔라듐 용액에 담지하는 단계; 및 (c) 상기 팔라듐 용액에 담지한 섬유를 무전해 도금하는 단계;를 포함하는 전자파 차폐용 섬유 제조방법을 제공한다.(A) supporting poly (acrylonitrile) -based fibers for electromagnetic wave shielding in a tin solution; (b) supporting the fiber supported on the tin solution in a palladium solution; And (c) electroless plating the fiber supported on the palladium solution.
상기 (a)단계에서 PAN계 섬유는 CuS-PAN계 섬유일 수 있고 상기 주석용액은 0.2 내지 10 M 농도, 바람직하게는 2 내지 8M농도, 더욱 바람직하게는 2 내지 4 M농도의 SnCl2 수용액인 것을 특징으로 한다. 이 때 상기 PAN계 섬유를 주석용액에 1분 내지 120분 동안 바람직하게는 20 내지 90분, 더욱 바람직하게는 20 내지 60분 동안 담지한다. 이는 상온에서 교반 없이 진행되는데, 섬유 표면에 Sn 핵을 형성하는 표면처리를 위함이다.In the step (a), the PAN-based fiber may be CuS-PAN-based fiber, and the tin solution may contain SnCl 2 at a concentration of 0.2 to 10 M, preferably 2 to 8 M, more preferably 2 to 4 M Aqueous solution. At this time, the PAN-based fibers are supported on the tin solution for 1 to 120 minutes, preferably 20 to 90 minutes, more preferably 20 to 60 minutes. This is carried out at room temperature without stirring, for surface treatment to form Sn nuclei on the fiber surface.
상기 (b)단계에서, 팔라듐 용액은 0.1 내지 10 M 농도 바람직하게는 2 내지 8 M 농도, 더욱 바람직하게는 2 내지 4M농도의 PdCl2 수용액이고 상기 주석용액에 담지한 섬유를 팔라듐 용액에 1분 내지 120분 동안 바람직하게는 20 내지 90분동안 더욱 바람직하게는 10 내지 30분 동안 담지한다. 이는 섬유의 표면활성화를 위해서 진행되며 이로 인해 섬유 표면에 Sn과 Pd 핵이 동시 형성하게 한다.In step (b), the palladium solution is a PdCl 2 aqueous solution having a concentration of 0.1 to 10 M, preferably 2 to 8 M, more preferably 2 to 4 M, and the fiber supported on the tin solution is added to the palladium solution for 1 minute To 120 minutes, preferably 20 to 90 minutes, more preferably 10 to 30 minutes. This is done to activate the surface of the fiber, which causes the Sn and Pd nuclei to co-form on the fiber surface.
또한, 상기 (c) 단계에서, 상기 팔라듐 용액에 담지한 섬유를 무전해 도금시키는데 무전해 니켈도금을 위해 니켈염인 NiSO46H2O를 150 내지 400g/L, NiCl26H2O를 10 내지 50g/L의 농도로 각각 사용한다. 또한, 착화제로써 Na3C6H5O71.5H2O를 3 내지 50g/L, 환원제로써 NaH2PO22H2O를 30 내지 150g/L, 안정제로 NH4Cl를 30 내지 200g/L, PbNO3를 10 내지 150g/L의 농도로 사용한다. 이렇게 제조된 용액에 상기 표면 처리된 CuS-PAN 섬유를 담지하고, 20 내지 150oC에서 10초 내지 30분간 담지한 후, 0회내지 4회 세척하여 무전해 도금시킨다.In addition, in the step (c), the electroless plating of the fibers supported on the palladium solution may be performed by electroless nickel plating, NiSO 4 6H 2 O, which is a nickel salt, 150-400 g / L, NiCl 2 6H 2 O, And 50 g / L, respectively. Also, Na 3 C 6 H 5 O 7 1.5H 2 O 3 to 50 g / L as a complexing agent, 30 to 150 g / L of NaH 2 PO 2 2H 2 O as a reducing agent, NH 3 Cl 30 to 200 g / L and PbNO 3 at a concentration of 10 to 150 g / L. The surface-treated CuS-PAN fibers are supported on the thus-prepared solution, supported at 20 to 150 ° C for 10 seconds to 30 minutes, washed with 0 to 4 times to perform electroless plating.
이와 같은 단계를 통해 도 1의 니켈 도금된 CuS-PAN섬유를 제조할 수 있다. 도 2에서는 각각 PAN섬유, CuS-PAN섬유, 니켈 도금된 CuS-PAN섬유의 전자파 차폐 효율을 비교하는 그래프를 보여준다. 그래프에서 보다시피 니켈 도금된 섬유는 그렇지 않은 섬유의 약 두 배 이상의 차폐효율을 나타내는 바 효과가 뛰어나다.The nickel-plated CuS-PAN fibers of FIG. 1 can be prepared through these steps. FIG. 2 shows graphs comparing electromagnetic wave shielding efficiencies of PAN fibers, CuS-PAN fibers, and nickel-plated CuS-PAN fibers, respectively. As can be seen in the graph, the nickel plated fibers exhibit shielding efficiencies of about twice as much as those of the non-nickel plated fibers.
이하, 실시예를 통하여 본 발명을 더욱 상세히 설명하고자 한다. 이들 실시예는 오로지 본 발명을 예시하기 위한 것으로서, 본 발명의 범위가 이들 실시예에 의해 제한되는 것으로 해석되지는 않는 것은 당업계에서 통상의 지식을 가진 자에게 있어서 자명할 것이다.Hereinafter, the present invention will be described in more detail with reference to Examples. It is to be understood by those skilled in the art that these examples are for illustrative purposes only and that the scope of the present invention is not construed as being limited by these examples.
측정예Measurement example 1. 전자파 차폐효율 측정 1. Measurement of electromagnetic wave shielding efficiency
EMI-shielding tester (Agilent, USA)를 통해 ASTM D4935-89 규격으로 본 발명에서 제조한 전자파 차폐용 니켈이 도금된 CuS-PAN 섬유의 전자파 차폐효율을 측정하였다.EMI shielding tester (Agilent, USA) was used to measure the electromagnetic wave shielding efficiency of the nickel-plated CuS-PAN fiber manufactured by the present invention according to ASTM D4935-89.
실시예 1. Example 1 .
CuS-PAN 섬유를 0.2M 농도의 SnCl2 수용액에 상온에서 교반없이 1분 동안 담지하여 섬유표면에 Sn 핵을 생성한다. 또한, 제조된 섬유는 0.1M 농도의 PdCl2 수용액에 상온에서 교반없이 1분 동안 담지하여 표면에 Sn/Pd 핵이 동시 형성되게 한다.The CuS-PAN fibers are supported on an aqueous solution of SnCl 2 at a concentration of 0.2M for 1 minute at room temperature without stirring to form Sn nuclei on the fiber surface. In addition, the prepared fibers were impregnated with a 0.1 M PdCl 2 aqueous solution for 1 minute at room temperature without stirring, so that Sn / Pd nuclei were simultaneously formed on the surface.
그 후, 상기 표면처리 된 CuS-PAN 섬유의 무전해 니켈도금을 위해 NiSO46H2O 280g/L, NiCl26H2O 40g/L, Na3C6H5O71.5H2O 15g/L, NaH2PO22H2O 100g/L, NH4Cl 100g/L 및 PbNO3 30g/L의 조성을 가지는 니켈 무전해 도금용액에 상기 처리된 섬유를 넣고, pH 6을 유지한 상태에서 20oC의 온도에서 1분간 담지 하여 전자파 차폐용 니켈 도금된 CuS-PAN 섬유를 제조한다.Then, for the electroless nickel plating of the surface-treated CuS-PAN fibers, 280 g / L of NiSO 4 6H 2 O, 40 g / L of NiCl 2 6H 2 O, 15 g / L of Na 3 C 6 H 5 O 7 1.5H 2 O, L, NaH 2 PO 2 2H 2 o 100g / L, NH 4 Cl 100g / L and PbNO 3 30g / L composition having nickel electroless put the treated fiber to the plating solution, while maintaining the pH 6 20 o C for 1 minute to prepare nickel-plated CuS-PAN fibers for electromagnetic wave shielding.
실시예Example 2. 2.
상기 실시예 1과 동일하게 과정을 실시하되, SnCl2 수용액 농도를 1M로 하고, 활성화시간을 5분으로 한다. 또한, PdCl2 활성화시간을 5분으로 하고, pH 7을 유지한 상태에서 도금 온도를 40oC로 하고, 도금 시간을 3분으로 하여 전자파 차폐용 니켈 도금된 CuS-PAN 섬유를 제조한다.The same procedure as in Example 1 was carried out except that the concentration of the SnCl 2 aqueous solution was 1 M and the activation time was 5 minutes. Further, nickel-plated CuS-PAN fibers for electromagnetic wave shielding were prepared by setting the plating temperature to 40 ° C and the plating time to 3 minutes while maintaining the PdCl 2 activation time to 5 minutes and maintaining the pH of 7.
실시예Example 3. 3.
상기 실시예 2와 동일하게 과정을 실시하되, SnCl2 수용액 농도를 2M로 하고, 활성화시간을 20분으로 한다. 또한, PdCl2 수용액 농도를 2M로 하고, 시간은 20분으로 하여 표면 활성화를 진행한다. pH 8을 유지한 상태에서 도금 온도를 60oC로 하고, 도금 시간을 5분으로 하며 최종적으로 1회 세척하여 전자파 차폐용 니켈 도금된 CuS-PAN 섬유를 제조한다.The same procedure as in Example 2 was carried out except that the SnCl 2 aqueous solution concentration was 2 M and the activation time was 20 minutes. Further, surface activation is carried out by setting the PdCl 2 aqueous solution concentration to 2 M and the time to 20 minutes. The nickel-plated CuS-PAN fiber for electromagnetic wave shielding is prepared by maintaining the plating temperature at 60 ° C. while maintaining the pH of 8, and the plating time at 5 minutes.
실시예Example 4. 4.
상기 실시예 3과 동일하게 과정을 실시하되, SnCl2 표면처리 시간을 30분으로 하고, PdCl2 활성화 시간은 30분으로 한다. 또한, pH 8.5을 유지한 상태에서 도금 온도를 90oC로 하고, 도금 시간을 10분으로 하며 최종적으로 1회 세척하여 전자파 차폐용 니켈 도금된 CuS-PAN 섬유를 제조한다.The same procedure as in Example 3 was carried out except that the SnCl 2 surface treatment time was 30 minutes and the PdCl 2 activation time was 30 minutes. The nickel-plated CuS-PAN fiber for electromagnetic wave shielding is prepared by maintaining the plating temperature at 90 ° C while maintaining the pH of 8.5 and the plating time at 10 minutes.
실시예Example 5. 5.
상기 실시예 4와 동일하게 과정을 실시하되, SnCl2 수용액 농도를 4M로 하고, PdCl2 수용액 농도는 4M로 하고, 시간은 60분으로 하여 표면 활성화를 진행한다. 또한, 세척횟수를 2회로 하여 전자파 차폐용 니켈 도금된 CuS-PAN 섬유를 제조한다.The same procedure as in Example 4 was carried out except that the surface activation was carried out at a SnCl 2 aqueous solution concentration of 4M, a PdCl 2 aqueous solution concentration of 4M and a time of 60 minutes. In addition, the number of times of cleaning is two times to prepare nickel-plated CuS-PAN fibers for electromagnetic wave shielding.
실시예Example 6. 6.
상기 실시예 5와 동일하게 과정을 실시하되, SnCl2 수용액 농도를 6M로 하고, 활성화시간을 60분으로 한다. 또한, PdCl2 수용액 농도를 6M로 하여 표면 활성화를 진행한다. pH 9을 유지한 상태에서 도금 온도를 120oC로 하고, 도금 시간을 20분으로 하여 전자파 차폐용 니켈 도금된 CuS-PAN 섬유를 제조한다.The same procedure as in Example 5 was carried out except that the concentration of SnCl 2 aqueous solution was 6M and the activation time was 60 minutes. Further, the surface activation is carried out by setting the PdCl 2 aqueous solution concentration to 6M. The nickel-plated CuS-PAN fibers for electromagnetic wave shielding were prepared at a plating temperature of 120 ° C and a plating time of 20 minutes while maintaining the pH of 9.
실시예Example 7. 7.
상기 실시예 6과 동일하게 과정을 실시하되, SnCl2 수용액 농도를 8M로 하고, 활성화시간을 90분으로 한다. 또한, PdCl2 수용액 농도를 6M로 하고, 시간은 90분으로 하여 표면 활성화를 진행한다. pH 8을 유지한 상태에서 도금 시간을 30분으로 하며 최종적으로 3회 세척하여 전자파 차폐용 니켈 도금된 CuS-PAN 섬유를 제조한다.The procedure is the same as in Example 6 except that the SnCl 2 aqueous solution concentration is 8 M and the activation time is 90 minutes. Further, the surface activation is carried out by setting the PdCl 2 aqueous solution concentration to 6 M and the time to 90 minutes. The plating time was 30 minutes while maintaining the pH of 8, and finally, the resultant was washed three times to prepare nickel-plated CuS-PAN fibers for electromagnetic shielding.
실시예Example 8. 8.
상기 실시예 7과 동일하게 과정을 실시하되, SnCl2 수용액 농도를 10M로 하고, 활성화시간을 120분으로 한다. 또한, PdCl2 수용액 농도를 10M로 하고, 시간은 120분으로 하여 표면 활성화를 진행한다. pH 10을 유지한 상태에서 도금 온도를 150oC로 하고, 최종적으로 4회 세척하여 전자파 차폐용 니켈 도금된 CuS-PAN 섬유를 제조한다.The same procedure as in Example 7 was carried out except that the concentration of SnCl 2 aqueous solution was 10 M and the activation time was 120 minutes. Further, the surface activation is carried out by setting the PdCl 2 aqueous solution concentration to 10 M and the time to 120 minutes. The nickel-plated CuS-PAN fiber for electromagnetic wave shielding is prepared by maintaining the plating temperature at 150 ° C while maintaining the pH of 10, and finally washing it four times.
비교예Comparative Example 1. One.
상기 실시예 4와 동일하게 과정을 실시하되, 표면처리를 하지 않고 니켈 도금된 CuS-PAN 섬유를 제조하였다.The procedure of Example 4 was followed except that nickel-plated CuS-PAN fibers were prepared without surface treatment.
비교예Comparative Example 2. 2.
상기 실시예 4와 동일하게 과정을 실시하되, 무전해 니켈도금을 하지 않고 니켈 도금된 CuS-PAN 섬유를 제조하였다.The procedure of Example 4 was followed except that nickel-plated CuS-PAN fibers were prepared without electroless nickel plating.
아래 표 1은 각 실시예들과 비교예를 정리하였고, 표 2에서는 본 발명의 제조방법에 의해 제조된 CuS-PAN 섬유의 전자파 차폐효율을 정리하였다.Table 1 below summarizes the respective examples and comparative examples. Table 2 summarizes the electromagnetic wave shielding efficiency of the CuS-PAN fibers produced by the manufacturing method of the present invention.
활성화 농도(M)SnCl 2
Activation concentration (M)
활성화 시간(min)SnCl 2
Activation time (min)
농도(M)PdCl 2
Concentration (M)
활성화
시간(min)PdCl 2
Activation
Time (min)
pHPlating solution
pH
이상, 본 발명의 내용의 특정한 부분을 상세히 기술하였는바, 당업계의 통상의 지식을 가진 자에게 있어서, 이러한 구체적인 기술은 단지 바람직한 실시양태일 뿐이며, 이에 의해 본 발명의 범위가 제한되는 것이 아닌 점은 명백할 것이다. 따라서, 본 발명의 실질적인 범위는 첨부된 청구항들과 그것들의 등가물에 의해 의하여 정의된다고 할 것이다. Having described specific portions of the present invention in detail, those skilled in the art will appreciate that these specific descriptions are only for the preferred embodiment and that the scope of the present invention is not limited thereby. It will be obvious. Accordingly, the actual scope of the present invention will be defined by the appended claims and their equivalents.
Claims (5)
(b) 상기 주석용액에 담지한 섬유를 팔라듐 용액에 담지하는 단계; 및
(c) 상기 팔라듐 용액에 담지한 섬유를 무전해 도금하는 단계;를 포함하는 것을 특징으로 하는 전자파 차폐용 섬유 제조방법.
(a) supporting PAN (poly acrylonitrile) -based fibers in a tin solution;
(b) supporting the fiber supported on the tin solution in a palladium solution; And
(c) electroless plating the fibers carried on the palladium solution.
상기 (a)단계에서 상기 주석용액은 0.2 내지 10 M 농도의 SnCl2 수용액인 것을 특징으로 하는 전자파 차폐용 섬유 제조방법.
The method according to claim 1,
In the step (a), the tin solution may contain SnCl 2 Wherein the fiber is an aqueous solution.
상기 (a)단계에서, 상기 PAN계 섬유를 주석용액에 1분 내지 120분 동안 담지하는 것을 특징으로 하는 전자파 차폐용 섬유 제조방법.
The method according to claim 1,
The method for producing electromagnetic interference (EMI) shielding fibers according to claim 1, wherein in the step (a), the PAN-based fibers are supported on the tin solution for 1 minute to 120 minutes.
상기 (b)단계에서, 상기 팔라듐 용액은 0.1 내지 10 M 농도의 PdCl2 수용액인 것을 특징으로 하는 전자파 차폐용 섬유 제조방법.
The method according to claim 1,
Wherein the palladium solution is an aqueous solution of PdCl 2 at a concentration of 0.1 to 10 M in the step (b).
상기 (b)단계에서, 상기 주석용액에 담지한 섬유를 팔라듐 용액에 1분 내지 120분 동안 담지하는 것을 특징으로 하는 전자파 차폐용 섬유 제조방법.The method according to claim 1,
Wherein the step (b) comprises supporting the fibers supported on the tin solution in a palladium solution for 1 minute to 120 minutes.
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| KR101725116B1 (en) * | 2016-01-08 | 2017-04-26 | 우석대학교 산학협력단 | Manufacturing Method for Ni Micro Tube by Electroless Plating Method and Epoxy-Carbon-Ni Micro Tube Composite for Fuel Cells Using Thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20210057473A (en) * | 2019-11-12 | 2021-05-21 | 전주대학교 산학협력단 | Manufacturing method of metal-plated carbon mats for EMI-shielding |
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