JP6485917B2 - 金属薄膜を有する導電構造 - Google Patents
金属薄膜を有する導電構造 Download PDFInfo
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- JP6485917B2 JP6485917B2 JP2016077186A JP2016077186A JP6485917B2 JP 6485917 B2 JP6485917 B2 JP 6485917B2 JP 2016077186 A JP2016077186 A JP 2016077186A JP 2016077186 A JP2016077186 A JP 2016077186A JP 6485917 B2 JP6485917 B2 JP 6485917B2
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- 239000010409 thin film Substances 0.000 title claims description 99
- 229910052751 metal Inorganic materials 0.000 title claims description 77
- 239000002184 metal Substances 0.000 title claims description 77
- 239000010410 layer Substances 0.000 claims description 106
- 239000000758 substrate Substances 0.000 claims description 66
- 239000002082 metal nanoparticle Substances 0.000 claims description 60
- 239000011347 resin Substances 0.000 claims description 57
- 229920005989 resin Polymers 0.000 claims description 57
- 230000004927 fusion Effects 0.000 claims description 48
- 230000009477 glass transition Effects 0.000 claims description 32
- 239000010408 film Substances 0.000 claims description 29
- 229920001665 Poly-4-vinylphenol Polymers 0.000 claims description 18
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 8
- 230000005540 biological transmission Effects 0.000 claims description 4
- 239000012790 adhesive layer Substances 0.000 claims 2
- 238000000034 method Methods 0.000 description 54
- 239000000976 ink Substances 0.000 description 50
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- 239000011248 coating agent Substances 0.000 description 28
- 238000009832 plasma treatment Methods 0.000 description 28
- 238000000137 annealing Methods 0.000 description 26
- 238000012360 testing method Methods 0.000 description 26
- 229910052760 oxygen Inorganic materials 0.000 description 25
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 21
- 239000001301 oxygen Substances 0.000 description 21
- 238000011282 treatment Methods 0.000 description 20
- 238000004381 surface treatment Methods 0.000 description 19
- 229910052709 silver Inorganic materials 0.000 description 18
- 238000010438 heat treatment Methods 0.000 description 16
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 15
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 13
- 238000007639 printing Methods 0.000 description 13
- 239000004332 silver Substances 0.000 description 13
- 238000009826 distribution Methods 0.000 description 12
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- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
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- 238000001035 drying Methods 0.000 description 3
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- 239000007789 gas Substances 0.000 description 3
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- 238000007641 inkjet printing Methods 0.000 description 3
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- CXWXQJXEFPUFDZ-UHFFFAOYSA-N tetralin Chemical compound C1=CC=C2CCCCC2=C1 CXWXQJXEFPUFDZ-UHFFFAOYSA-N 0.000 description 3
- 229920005992 thermoplastic resin Polymers 0.000 description 3
- QPUYECUOLPXSFR-UHFFFAOYSA-N 1-methylnaphthalene Chemical compound C1=CC=C2C(C)=CC=CC2=C1 QPUYECUOLPXSFR-UHFFFAOYSA-N 0.000 description 2
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229920001780 ECTFE Polymers 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 239000006087 Silane Coupling Agent Substances 0.000 description 2
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical compound COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- NNBZCPXTIHJBJL-UHFFFAOYSA-N decalin Chemical compound C1CCCC2CCCCC21 NNBZCPXTIHJBJL-UHFFFAOYSA-N 0.000 description 2
- NZZFYRREKKOMAT-UHFFFAOYSA-N diiodomethane Chemical compound ICI NZZFYRREKKOMAT-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 229920000840 ethylene tetrafluoroethylene copolymer Polymers 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- AUHZEENZYGFFBQ-UHFFFAOYSA-N mesitylene Substances CC1=CC(C)=CC(C)=C1 AUHZEENZYGFFBQ-UHFFFAOYSA-N 0.000 description 2
- 125000001827 mesitylenyl group Chemical group [H]C1=C(C(*)=C(C([H])=C1C([H])([H])[H])C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- 238000007645 offset printing Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 229920002493 poly(chlorotrifluoroethylene) Polymers 0.000 description 2
- 239000005023 polychlorotrifluoroethylene (PCTFE) polymer Substances 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000007650 screen-printing Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- RELMFMZEBKVZJC-UHFFFAOYSA-N 1,2,3-trichlorobenzene Chemical compound ClC1=CC=CC(Cl)=C1Cl RELMFMZEBKVZJC-UHFFFAOYSA-N 0.000 description 1
- SPPWGCYEYAMHDT-UHFFFAOYSA-N 1,4-di(propan-2-yl)benzene Chemical compound CC(C)C1=CC=C(C(C)C)C=C1 SPPWGCYEYAMHDT-UHFFFAOYSA-N 0.000 description 1
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical compound ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 description 1
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 1
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004695 Polyether sulfone Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229940117389 dichlorobenzene Drugs 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000005357 flat glass 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
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920006122 polyamide resin 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
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000005361 soda-lime glass Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
- B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
- C23C24/103—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
- C23C24/106—Coating with metal alloys or metal elements only
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/12—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using thick film techniques, e.g. printing techniques to apply the conductive material or similar techniques for applying conductive paste or ink patterns
- H05K3/1208—Pretreatment of the circuit board, e.g. modifying wetting properties; Patterning by using affinity patterns
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K10/00—Organic devices specially adapted for rectifying, amplifying, oscillating or switching; Organic capacitors or resistors having potential barriers
- H10K10/40—Organic transistors
- H10K10/46—Field-effect transistors, e.g. organic thin-film transistors [OTFT]
- H10K10/462—Insulated gate field-effect transistors [IGFETs]
- H10K10/466—Lateral bottom-gate IGFETs comprising only a single gate
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K10/00—Organic devices specially adapted for rectifying, amplifying, oscillating or switching; Organic capacitors or resistors having potential barriers
- H10K10/40—Organic transistors
- H10K10/46—Field-effect transistors, e.g. organic thin-film transistors [OTFT]
- H10K10/462—Insulated gate field-effect transistors [IGFETs]
- H10K10/481—Insulated gate field-effect transistors [IGFETs] characterised by the gate conductors
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/60—Forming conductive regions or layers, e.g. electrodes
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
- H05K1/0313—Organic insulating material
- H05K1/0353—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement
- H05K1/036—Multilayers with layers of different types
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
- H05K1/0393—Flexible materials
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/09—Use of materials for the conductive, e.g. metallic pattern
- H05K1/092—Dispersed materials, e.g. conductive pastes or inks
- H05K1/097—Inks comprising nanoparticles and specially adapted for being sintered at low temperature
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/38—Improvement of the adhesion between the insulating substrate and the metal
- H05K3/381—Improvement of the adhesion between the insulating substrate and the metal by special treatment of the substrate
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Composite Materials (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing Of Printed Wiring (AREA)
- Non-Insulated Conductors (AREA)
- Manufacturing Of Electric Cables (AREA)
- Thin Film Transistor (AREA)
Description
絶縁性樹脂で形成された下地層を有する基板を準備する工程と、
前記下地層の表面に、前記絶縁性樹脂を構成する有機分子の結合を切断する物理的表面処理を施す工程と、
前記基板を200℃以下の温度で加熱処理する工程と、
前記下地層に金属ナノ粒子インクを塗布する工程と、
前記下地層のガラス転移点以上の温度で前記金属ナノ粒子インクに含まれた金属ナノ粒子を焼結させる工程と、
をこの順で含む、金属薄膜の製造方法を提供する。
絶縁性樹脂で形成された下地層を有する基板と、
前記下地層に支持された金属薄膜と、
前記下地層と前記金属薄膜との間に形成された厚さ100nm以下の融着層と、
を備え、
前記金属薄膜は、上記の方法によって形成されている、導電構造を提供する。
ポリメタクリル酸メチル(PMMA)(シグマアルドリッチジャパン社製)をメシチレンに溶解し、塗布液を得た。青板ガラス基板(ソーダライムガラス基板)の上に塗布液をスピンコート法で塗布した。得られた塗膜を150℃で1時間アニールし、厚さ100nmの下地層を基板上に形成した。プラズマクリーナー(サムコ社製 PC−300)を用い、酸素流量10sccm(standard cubic centimeter per minute)、10Pa、200W、10秒間の条件で下地層の表面に酸素プラズマ処理を施した。その後、ホットプレート上に基板を配置し、大気中、40℃(ホットプレートの表面温度)、5分間の条件で基板をアニールした。次に、下地層の上に銀ナノ粒子インク(ハリマ化成株式会社製 NPS−JL)をスピンコート法で塗布した。銀ナノ粒子インクの塗膜を150℃(ホットプレートの表面温度)、大気中、1時間の条件で焼成し、厚さ100nmのAg薄膜を形成した。これにより、サンプル1の導電構造を得た。
絶縁性樹脂として、ポリメタクリル酸メチル(PMMA)に代えて、ポリビニルフェノール(PVP)(シグマアルドリッチジャパン社製)を用いたことを除き、サンプル1と同じ方法でAg薄膜を形成した。
酸素プラズマ処理後のアニール温度を下記表1に示す各温度としたことを除き、サンプル1又は2と同じ方法でAg薄膜を形成した。
酸素プラズマ処理及びアニール処理を省略したことを除き、サンプル1又は2と同じ方法でAg薄膜を形成した。
酸素プラズマ処理後のアニール処理を省略したことを除き、サンプル1又は2と同じ方法でAg薄膜を形成した。
酸素プラズマ処理及びアニール処理を省略し、さらに、銀ナノ粒子を焼結させる工程における基板の加熱温度を120℃(下地層のガラス転移点未満)としたことを除き、サンプル1又は2と同じ方法でAg薄膜を形成した。
酸素プラズマ処理後のアニール処理を省略し、さらに、銀ナノ粒子を焼結させる工程における基板の加熱温度を120℃(下地層のガラス転移点未満)としたことを除き、サンプル1又は2と同じ方法でAg薄膜を形成した。
銀ナノ粒子を焼結させる工程における基板の加熱温度を120℃としたことを除き、サンプル12と同じ方法でAg薄膜を形成した。
作製したAg薄膜について、超薄膜スクラッチ試験機(レスカ社製 CSR−2000)を用いて、ひっかき強度を測定し、導電構造におけるAg薄膜の密着性の評価を行った。ひっかき強度の測定は、以下の条件で行い、3回の測定値の平均値を算出した。結果を表1に示す。
スタイラス:曲率半径100μm
荷重印加:0〜120mN
測定距離:1mm
スクラッチ速度:10μm/s
酸素プラズマ処理及びアニール処理を省略し、さらに、銀ナノ粒子を焼結させる工程における基板の加熱温度を180℃(下地層のガラス転移点以上の温度)としたことを除き、サンプル2と同じ方法でAg薄膜を形成した。
絶縁性樹脂として、ポリビニルフェノール(PVP)に代えて、ポリメタクリル酸メチル(PMMA)(シグマアルドリッチジャパン社製)を用いたことを除き、サンプル28と同じ方法でAg薄膜を形成した。
絶縁性樹脂として、ポリビニルフェノール(PVP)に代えて、非晶質フッ素樹脂(三井デュポンフロロケミカル社製AF1600)を用いたことを除き、サンプル28と同じ方法でAg薄膜を形成した。なお、非晶質フッ素樹脂(AF1600)のガラス転移点Tgは約160℃である。
サンプル28〜30の導電構造の断面を透過電子顕微鏡(日本電子社製 JEM−2100FE、加速電圧200kV)で観察した。TEM観察用の試料は、集束イオンビーム加工観察装置(日本電子社製 JEM−9320FIB、加速電圧5kV)を用いて作製した。結果を図4〜図7に示す。図5は、図4の部分拡大図である。
サンプル28の導電構造の深さ方向の元素分布をX線光電子分光装置(アルバックファイ社製 5600ci)で調べた。XPSの測定条件は以下の通りであった。
Arスパッタレート:約170nm/min(換算値)
分析レート:0.1min/回
X線源:Mg
検出元素:C、O、Ag、F
JIS K5600−5−7「塗膜の機械的性質−付着性(プルオフ法)」に基づいて、引き剥がし試験を行った。まず、サンプル28の導電構造を先に説明した方法で準備した。次に、図9に示すように、サンプル28の導電構造の表面にロッド12をエポキシ樹脂で接着した。基板をステージ上に固定し、ロッド12の後端部をフォースゲージ(日本電産シンポ社製 FGP−5)に固定し、Ag薄膜の厚さ方向(引き剥がす方向)に力を加えた。Ag薄膜の密着強度以上の強さで引っ張ると、Ag薄膜と下地層との界面で剥離が起こる。剥離したAg薄膜の面積とフォースゲージの値とから密着強度を算出した。サンプル29及びサンプル30の導電構造にも同じ試験を実施した。なお、導電構造の作製過程(下地層を形成した後かつプラズマ処理を行う前)で下地層の表面エネルギーも測定した。結果を表2に示す。
サンプル28の導電構造について引き剥がし試験を実施した後、ロッド12に接していた面における特定領域14を走査型電子顕微鏡(SEM−EDS、日本電子社製 JSM−7800FE、加速電圧15kV)で観察した。特定領域14は、1mm2の広さを有する正方形の領域であった。
銀ナノ粒子インクの塗膜の焼成温度を180℃に設定したことを除き、サンプル12と同じ方法でAg薄膜を形成した。
銀ナノ粒子インクの塗膜の焼成温度を180℃に設定したことを除き、サンプル9と同じ方法でAg薄膜を形成した。
絶縁性樹脂として、ポリビニルフェノール(PVP)に代えて、非晶質フッ素樹脂(三井デュポンフロロケミカル社製AF1600)を用い、酸素プラズマ処理後のアニール処理の温度を160℃に設定したことを除き、サンプル32と同じ方法でAg薄膜を形成した。
サンプル28〜30と同じ方法でサンプル31〜33の導電構造について引き剥がし試験を実施した。その後、サンプル28〜30と同じ方法で、表面SEM像、表面EDS像及びAgの濃度の分布を示すヒストグラムを得た。サンプル31についての結果を図16A〜図16Cに示す。サンプル32についての結果を図17A〜図17Cに示す。サンプル33についての結果を図18A〜図18Cに示す。
Claims (8)
- 絶縁性樹脂で形成された下地層を有する基板と、
前記下地層に支持された金属薄膜と、
前記下地層と前記金属薄膜との間に形成された厚さ100nm以下の融着層と、
を備え、
前記金属薄膜は、金属ナノ粒子の焼結層であり、
前記融着層は、前記下地層を構成する前記絶縁性樹脂と前記金属薄膜を構成する金属原子とを含む層であり、
前記金属ナノ粒子が銀ナノ粒子であり、
前記絶縁性樹脂は、ポリビニルフェノールを含む、導電構造。 - 前記導電構造の断面を透過電子顕微鏡で観察したとき、前記融着層の中の領域であって、前記絶縁性樹脂で囲まれた領域にAg(111)面に由来する格子像が観察される、請求項1に記載の導電構造。
- 前記下地層のガラス転移点が200℃以下である、請求項1又は2に記載の導電構造。
- 前記融着層は、前記金属薄膜を構成する金属と前記絶縁性樹脂とが相分離している領域と、前記金属薄膜を構成する金属と前記絶縁性樹脂とが混在している領域とが混在している構造を有する、請求項1〜3のいずれか1項に記載の導電構造。
- 前記基板は、樹脂フィルムと、前記樹脂フィルム上に形成された前記下地層と、を有する、請求項1〜4のいずれか1項に記載の導電構造。
- 前記融着層の厚さが10nm以上である、請求項1〜5のいずれか1項に記載の導電構造。
- 請求項1〜6のいずれか1項に記載の導電構造を含む薄膜トランジスタ。
- 請求項7に記載の薄膜トランジスタを含む集積回路。
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