WO2022255750A1 - 투명한 니켈 착화합물 잉크 조성물 및 이의 제조 방법 - Google Patents
투명한 니켈 착화합물 잉크 조성물 및 이의 제조 방법 Download PDFInfo
- Publication number
- WO2022255750A1 WO2022255750A1 PCT/KR2022/007650 KR2022007650W WO2022255750A1 WO 2022255750 A1 WO2022255750 A1 WO 2022255750A1 KR 2022007650 W KR2022007650 W KR 2022007650W WO 2022255750 A1 WO2022255750 A1 WO 2022255750A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- branched
- alkyl
- straight
- ink composition
- nickel complex
- Prior art date
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 465
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 228
- 239000000203 mixture Substances 0.000 title claims abstract description 123
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- 239000000654 additive Substances 0.000 claims abstract description 8
- 125000000217 alkyl group Chemical group 0.000 claims description 63
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 claims description 28
- 125000003342 alkenyl group Chemical group 0.000 claims description 22
- 125000003118 aryl group Chemical group 0.000 claims description 20
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- 125000006738 (C6-C20) heteroaryl group Chemical group 0.000 claims description 10
- WGQKYBSKWIADBV-UHFFFAOYSA-N benzylamine Chemical compound NCC1=CC=CC=C1 WGQKYBSKWIADBV-UHFFFAOYSA-N 0.000 claims description 10
- 125000000753 cycloalkyl group Chemical group 0.000 claims description 10
- 125000001072 heteroaryl group Chemical group 0.000 claims description 10
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- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 9
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 9
- BMVXCPBXGZKUPN-UHFFFAOYSA-N 1-hexanamine Chemical compound CCCCCCN BMVXCPBXGZKUPN-UHFFFAOYSA-N 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 8
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
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- 239000004793 Polystyrene Substances 0.000 claims description 6
- 125000004448 alkyl carbonyl group Chemical group 0.000 claims description 6
- IGODOXYLBBXFDW-UHFFFAOYSA-N alpha-Terpinyl acetate Chemical compound CC(=O)OC(C)(C)C1CCC(C)=CC1 IGODOXYLBBXFDW-UHFFFAOYSA-N 0.000 claims description 6
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 6
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- 239000001856 Ethyl cellulose Substances 0.000 claims description 5
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 5
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical group CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 5
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 5
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- WUOACPNHFRMFPN-SECBINFHSA-N (S)-(-)-alpha-terpineol Chemical compound CC1=CC[C@@H](C(C)(C)O)CC1 WUOACPNHFRMFPN-SECBINFHSA-N 0.000 claims description 4
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 4
- FMMGYFLWRCDVPG-UHFFFAOYSA-N 2-(diethylamino)ethanol Chemical compound C(C)N(CCO)CC.C(C)N(CCO)CC FMMGYFLWRCDVPG-UHFFFAOYSA-N 0.000 claims description 4
- QCDWFXQBSFUVSP-UHFFFAOYSA-N 2-phenoxyethanol Chemical compound OCCOC1=CC=CC=C1 QCDWFXQBSFUVSP-UHFFFAOYSA-N 0.000 claims description 4
- QCAHUFWKIQLBNB-UHFFFAOYSA-N 3-(3-methoxypropoxy)propan-1-ol Chemical compound COCCCOCCCO QCAHUFWKIQLBNB-UHFFFAOYSA-N 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims description 4
- 150000001241 acetals Chemical class 0.000 claims description 4
- -1 acryl Chemical group 0.000 claims description 4
- OVKDFILSBMEKLT-UHFFFAOYSA-N alpha-Terpineol Natural products CC(=C)C1(O)CCC(C)=CC1 OVKDFILSBMEKLT-UHFFFAOYSA-N 0.000 claims description 4
- 229940088601 alpha-terpineol Drugs 0.000 claims description 4
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 claims description 4
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- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
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- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 claims description 3
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- IBLKWZIFZMJLFL-UHFFFAOYSA-N 1-phenoxypropan-2-ol Chemical compound CC(O)COC1=CC=CC=C1 IBLKWZIFZMJLFL-UHFFFAOYSA-N 0.000 claims description 3
- HBNHCGDYYBMKJN-UHFFFAOYSA-N 2-(4-methylcyclohexyl)propan-2-yl acetate Chemical compound CC1CCC(C(C)(C)OC(C)=O)CC1 HBNHCGDYYBMKJN-UHFFFAOYSA-N 0.000 claims description 3
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- WWJLCYHYLZZXBE-UHFFFAOYSA-N 5-chloro-1,3-dihydroindol-2-one Chemical compound ClC1=CC=C2NC(=O)CC2=C1 WWJLCYHYLZZXBE-UHFFFAOYSA-N 0.000 claims description 3
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 claims description 3
- LITKNMRUUSKONC-UHFFFAOYSA-N CN(CC(C)O)C.CN(CC(C)O)C Chemical compound CN(CC(C)O)C.CN(CC(C)O)C LITKNMRUUSKONC-UHFFFAOYSA-N 0.000 claims description 3
- KGEKLUUHTZCSIP-UHFFFAOYSA-N Isobornyl acetate Natural products C1CC2(C)C(OC(=O)C)CC1C2(C)C KGEKLUUHTZCSIP-UHFFFAOYSA-N 0.000 claims description 3
- KRKIAJBQOUBNSE-GYSYKLTISA-N Isobornyl isobutyrate Chemical compound C1C[C@@]2(C)[C@H](OC(=O)C(C)C)C[C@@H]1C2(C)C KRKIAJBQOUBNSE-GYSYKLTISA-N 0.000 claims description 3
- ALQSHHUCVQOPAS-UHFFFAOYSA-N Pentane-1,5-diol Chemical compound OCCCCCO ALQSHHUCVQOPAS-UHFFFAOYSA-N 0.000 claims description 3
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- FAFMZORPAAGQFV-BREBYQMCSA-N [(1r,3r,4r)-4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl] propanoate Chemical compound C1C[C@@]2(C)[C@H](OC(=O)CC)C[C@@H]1C2(C)C FAFMZORPAAGQFV-BREBYQMCSA-N 0.000 claims description 3
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- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 4
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- 239000012046 mixed solvent Substances 0.000 description 1
- 230000001333 moisturizer Effects 0.000 description 1
- 230000003020 moisturizing effect Effects 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
- HZPNKQREYVVATQ-UHFFFAOYSA-L nickel(2+);diformate Chemical group [Ni+2].[O-]C=O.[O-]C=O HZPNKQREYVVATQ-UHFFFAOYSA-L 0.000 description 1
- JMWUYEFBFUCSAK-UHFFFAOYSA-L nickel(2+);octadecanoate Chemical compound [Ni+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O JMWUYEFBFUCSAK-UHFFFAOYSA-L 0.000 description 1
- DVTHIMLUHWEZOM-UHFFFAOYSA-L nickel(2+);octanoate Chemical compound [Ni+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O DVTHIMLUHWEZOM-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
- 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
- 150000002843 nonmetals Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
- C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
Definitions
- the present invention relates to a transparent nickel complex ink composition and a method for preparing the same, and more specifically, the nickel complex ink composition has a transparent particle-free form and has an absorbance (ABS) value of 1.0 or more in a wavelength range of 600 nm to 650 nm, wherein the The maximum diameter of nickel particles constituting the thin film formed by applying the composition to a substrate is 150 nm or less, and can be used for forming MLCC internal electrodes, electromagnetic wave shielding, solar cell electrodes, or display panel electrodes. have.
- Nickel powder is used as a material for capacitors, which are electronic components constituting electronic circuits, in particular, as a material for thick film conductors constituting internal electrodes of multilayer ceramic components such as multilayer ceramic capacitors (MLCC) and multilayer ceramic substrates.
- capacitors which are electronic components constituting electronic circuits, in particular, as a material for thick film conductors constituting internal electrodes of multilayer ceramic components such as multilayer ceramic capacitors (MLCC) and multilayer ceramic substrates.
- an internal electrode paste obtained by kneading nickel powder, a binder resin such as ethyl cellulose, and an organic solvent such as terpineol is screen-printed on a dielectric green sheet.
- the dielectric green sheets printed with the internal electrode paste are stacked and compressed so that the internal electrode paste and the dielectric green sheets are alternately overlapped, thereby obtaining a laminate.
- the obtained laminate is cut into a predetermined size, heated to remove the binder resin (hereinafter referred to as "removing binder"), and then fired at a high temperature of about 1,300 ° C. to obtain a ceramic molded body.
- removing binder the binder resin
- a multilayer ceramic capacitor can be obtained by providing an external electrode on the obtained ceramic molded body.
- the binder removal process of the laminate should be performed in an atmosphere having an extremely low oxygen concentration such as an inert atmosphere so that the non-metal is not oxidized.
- a paste composition technology minimizing the particle size is proposed, such as using an internal electrode paste containing functional particles having a particle size close to 50 nm to minimize the thickness when forming such an electrode.
- the particle content exceeds 50 parts by weight relative to 100 parts by weight of the total composition for stability of the composition, and as a result, there is a limit in that the thickness of the internal electrode cannot be reduced to 400 nm or less.
- the present inventors completed the present invention by preparing a transparent particle-free conductive nickel complex ink composition for forming MLCC internal electrodes of the multilayer ceramic capacitor.
- the transparent nickel complex ink composition is transparent and particle-free, and is competitive because it has the advantage of having a lower metal content than conventional pastes or inks, and thus has the advantage of having a low internal electrode thickness.
- Japanese Patent Application Publication No. 2008-127657 discloses a coating liquid for forming a nickel film, a method for manufacturing a nickel film, and a nickel film.
- the present invention has been made to solve the above problems, and one embodiment of the present invention provides a transparent nickel complex ink composition and a manufacturing method thereof.
- a polar portion including nickel and a compound represented by Formula 1 coordinated with the nickel; menstruum;
- a transparent nickel complex ink composition comprising; and other additives, wherein the nickel complex ink composition is transparent and particle-free, and has an absorbance (ABS) of 1.0 or more in a wavelength range of 600 nm to 650 nm. composition is provided.
- R 1 to R 3 are each independently hydrogen, linear or branched C 5 -C 20 alkyl, linear or branched C 5 -C 20 alkenyl, C 5 -C 20 cycloalkyl, C 6 -C 20 aryl unsubstituted or substituted with straight or branched C 1 -C 5 alkyl or straight or branched C 8 -C 18 alkyl, straight or branched C 1 -C 5 alkyl or straight chain or C 6 -C 20 heteroaryl or C 5 -C 20 alkylcarbonyl unsubstituted or substituted with branched C 8 -C 18 alkyl, and at least one of R 1 to R 3 is straight-chain or branched-chain C 1 - C 6 -C 20 aryl unsubstituted or substituted with C 5 alkyl or straight or branched C 8 -C 18 alkyl, straight or branched C 1 -C 5 alkyl or straight or branched C
- R 1 to R 3 are each independently hydrogen, straight-chain or branched-chain C 8 -C 18 alkyl, straight-chain or branched-chain C 8 -C 18 alkenyl, C 8 -C 18 cycloalkyl, or straight-chain or C 8 -C 18 aryl unsubstituted or substituted with branched C 1 -C 5 alkyl or straight or branched C 8 -C 18 alkyl, straight or branched C 1 -C 5 alkyl, straight chain or branched.
- It may be C 8 -C 18 heteroaryl unsubstituted or substituted with chain C 8 -C 18 alkyl, straight-chain or branched C 8 -C 18 alkyl, or straight-chain or branched C 8 -C 18 alkenyl. .
- R 1 and R 2 are hydrogen, and R 3 is straight or branched C 1 -C 5 alkyl, C 8 -C 18 aryl substituted with straight or branched C 8 -C 18 alkyl, or It may be heteroaryl, straight-chain or branched C 8 -C 18 alkyl, or straight-chain or branched C 8 -C 18 alkenyl.
- the compound represented by Formula 1 is 2-amino-1-methyl-1-propanol, n-hexylamine, hexylamine, cyclohexyl Amine (cyclohexylamine), n-octylamine, octylamine, dodecylamine, oleylamine, benzylamine, 1-dimethylamino-2-propanol (1 -dimethylamino-2-propanol), 2-(diethylamino)ethanol (2-(diethylamino)ethanol), or diphenylamine.
- the concentration of the polar part may be 8% to 72% by weight based on the total weight of the transparent nickel complex ink composition.
- the solvent is terpineol, ⁇ -terpineol, dihydro-terpineol, terpinyl acetate, dihydro terpinyl acetate, Isobornyl acetate, isobornyl propionate, isobornyl isobutyrate, ethylene glycol, propylene glycol, butylene glycol glycol), diethylene glycol, dipropylene glycol, dipropylene glycol monomethyl ether, ethylene glycol phenyl ether, propylene glycol phenyl ether phenyl ether), ethylene glycol monobutyl ether acetate, dipropylene glycol methyl ether acetate, ethanol, propanol, isopropyl alcohol, butanol, isooctyl alcohol, di A group consisting of diacetone alcohol, 1,2-pentanediol, 1,5-pentanediol, 2-methyl-2,4-pentanedio
- the other additives may include a material selected from the group consisting of a binder resin, a plasticizer, a stabilizer, a dispersing agent, a release agent, a reducing agent, a surfactant, a wetting agent, a thixotropic agent, a leveling agent, and combinations thereof.
- the binder resin is polyvinyl butyral, ethyl cellulose, polyvinyl pyrrolidone, acryl, polyvinyl acetal, polyvinyl alcohol , polyolefin, polyurethane, polystyrene, and combinations thereof.
- a maximum diameter of nickel particles in a thin film formed by applying the transparent nickel complex ink composition to a substrate may be 150 nm or less.
- the transparent nickel complex ink composition may be characterized in that it is a transparent nickel complex ink composition for forming MLCC internal electrodes, for electromagnetic wave shielding, for forming solar cell electrodes, or for forming display panel electrodes.
- Another aspect of the present invention is,
- a method for producing a transparent nickel complex ink composition comprising heating the binder resin together in the heating step, wherein the transparent nickel complex ink composition is transparent and particle-free, and has an absorbance (ABS) in a wavelength range of 600 nm to 650 nm It provides a method for producing a transparent nickel complex ink composition having a value of 1.0 or more.
- R 1 to R 3 are each independently hydrogen, straight-chain or branched-chain C 5 -C 20 alkyl, straight-chain or branched-chain C 5 -C 20 alkenyl, C 5 -C 20 cycloalkyl, or straight-chain or C 6 -C 20 aryl unsubstituted or substituted with branched C 1 -C 5 alkyl or straight or branched C 8 -C 18 alkyl, straight or branched C 1 -C 5 alkyl or straight or branched chain C 6 -C 20 heteroaryl or C 5 -C 20 alkylcarbonyl unsubstituted or substituted with C 8 -C 18 alkyl chain, and at least one of R 1 to R 3 is straight-chain or branched-chain C 1 -C C 6 -C 20 aryl unsubstituted or substituted with 5 alkyl or straight or branched C 8 -C 18 alkyl, straight or branched C 1 -C 20 al
- the nickel complex ink composition may be transparent and particle-free, and may have an absorbance (ABS) of 1.0 or more in a wavelength range of 600 nm to 650 nm.
- ABS absorbance
- the heating may be performed at less than 115°C.
- the transparent nickel complex compound ink composition is transparent and non-particle, it is possible to apply a thinner coating than a conventional paste composition, and thus, it may be possible to form a thin film.
- the maximum diameter of the nickel particles constituting the thin film formed by applying the nickel complex ink composition to the substrate is very small, less than 150 nm, and the roughness of the nickel inner electrode is small, which means that the MLCC inner electrode and the dielectric green sheet are alternately overlapped. It may be that the performance is improved by increasing the number of thin films in the MLCC of the same volume, as it leads to the advantage of high adhesion when stacked and compressed in such a way.
- FIG. 1 is a photograph showing a transparent nickel complex compound ink composition for forming an MLCC internal electrode prepared according to an embodiment and a comparative example of the present invention.
- Figure 2 is a graph showing the absorbance of the transparent nickel complex compound ink composition prepared according to one embodiment and a comparative example of the present invention.
- FIG. 3 is a photograph showing a thin film of a nickel internal electrode manufactured according to an embodiment of the present invention and a comparative example.
- FIG. 4 is a SEM photograph showing a nickel inner electrode thin film manufactured according to an embodiment and a comparative example of the present invention, respectively.
- the transparent nickel complex ink composition can be used for electrodes of various electronic devices and semiconductors containing nickel, or for electromagnetic wave shielding (EMI Shielding), for example, for forming MLCC internal electrodes, It may be a transparent nickel complex compound ink composition for electromagnetic wave shielding, solar cell electrode formation, or display panel electrode formation, preferably a nickel complex compound ink composition used for forming MLCC internal electrodes or electromagnetic wave shielding.
- EMI Shielding electromagnetic wave shielding
- Multilayer Ceramic Capacitors MLCCs
- MLCC is the English abbreviation of Multilayer Ceramic Capacitor, and it is called multilayer ceramic capacitor.
- MLCC is a capacitor with a fixed value in which a ceramic material acts as a dielectric, and is basically composed of two or more ceramic layers and a metal layer acting as an electrode.
- the composition of the ceramic material determines the MLCC's electrical behavior and hence its range of applications.
- next-generation MLCCs must have numerous stacked dielectric layers with a thickness of less than 1 ⁇ m. In particular, in the case of internal electrodes, numerous layers with a thickness of 400 nm or less are required.
- the basic principle for MLCC to store electricity is through dielectric polarization. In the absence of an external electric field, the electrical dipoles inside the dielectric are randomly distributed, showing the characteristics of an insulator. are concentrated, respectively, to be able to store electricity.
- MLCC is a key component of a passive element that has the function of temporarily charging the accumulated electricity, and has the characteristic of always discharging the current constantly by passing AC current and blocking DC current. Passive elements to be used in next-generation miniaturized and high-capacity electronic devices require MLCCs with higher capacitance.
- MLCC is formed by stacking many dielectric layers and internal electrodes in parallel and alternating.
- the inner electrode is connected to the outer end for surface mounting.
- the capacity of MLCC is expressed by the following equation,
- the thickness of the dielectric layer and the number of layers are important factors. That is, in order to increase the capacitance of the MLCC to realize high capacity, the surface area of the internal electrode should be maximized and the thickness of the dielectric thin film and the internal electrode should be minimized. However, since it is impossible to increase the area according to the demand for miniaturization of the device, it is necessary to minimize the thickness of the internal electrode and obtain high capacitance by stacking the internal electrode and the dielectric thin film in the same volume.
- the first aspect of the present application is,
- a polar portion including nickel and a compound represented by Formula 1 coordinated with the nickel; menstruum;
- a transparent nickel complex ink composition comprising; and other additives, wherein the nickel complex ink composition is transparent and particle-free, and has an absorbance (ABS) of 1.0 or more in a wavelength range of 600 nm to 650 nm. composition is provided.
- R 1 to R 3 are each independently hydrogen, linear or branched C 5 -C 20 alkyl, linear or branched C 5 -C 20 alkenyl, C 5 -C 20 cycloalkyl, C 6 -C 20 aryl unsubstituted or substituted with straight or branched C 1 -C 5 alkyl or straight or branched C 8 -C 18 alkyl, straight or branched C 1 -C 5 alkyl or straight chain or C 6 -C 20 heteroaryl or C 5 -C 20 alkylcarbonyl unsubstituted or substituted with branched C 8 -C 18 alkyl, and at least one of R 1 to R 3 is straight-chain or branched-chain C 1 - C 6 -C 20 aryl unsubstituted or substituted with C 5 alkyl or straight or branched C 8 -C 18 alkyl, straight or branched C 1 -C 5 alkyl or straight or branched C
- the transparent nickel complex compound ink composition according to the first aspect of the present disclosure and a thin film formed by applying the nickel complex compound ink composition to a substrate will be described in detail.
- the transparent nickel complex compound ink composition may be characterized in that it is transparent and particle-free. That is, in the case of the internal electrode paste, which can be referred to as a conventional nickel ink composition, functional nickel particles having a particle size close to 50 nm are included in an amount of 50 parts by weight or more relative to 100 parts by weight of the total composition for stability of the composition. Although there was a limitation that the thickness of the electrode could not be reduced to 400 nm or less, the transparent nickel complex ink composition according to the present invention is particle-free, so that the above problems do not occur, and thinning of the internal electrode can be achieved. have. Accordingly, since the internal electrodes manufactured using the transparent nickel complex ink composition can realize a larger number of internal electrode layers, miniaturization and higher capacity of the multilayer ceramic capacitor including the internal electrodes may be achieved.
- R 1 to R 3 are each independently hydrogen, linear or branched C 8 -C 18 alkyl, linear or branched C 8 -C 18 alkenyl , C 8 -C 18 cycloalkyl, straight or branched C 1 -C 5 alkyl or straight or branched C 8 -C 18 alkyl substituted or unsubstituted C 8 -C 18 aryl, straight or branched chain C 1 -C 5 alkyl, C 8 -C 18 heteroaryl unsubstituted or substituted with straight or branched C 8 -C 18 alkyl, straight or branched C 8 -C 18 alkyl or straight or branched C 8 -C 18 heteroaryl 8 -C 18 alkenyl, more preferably R 1 and R 2 are hydrogen, R 3 is straight or branched C 1 -C 5 alkyl, straight or branched C 8 -C 18 alkyl substituted C 8 -C
- the compound represented by Formula 1 is 2-amino-1-methyl-1-propanol (2-amino-1-methyl-1-propanol), normal hexylamine (n-hexylamine), Hexylamine, cyclohexylamine, n-octylamine, octylamine, dodecylamine, oleylamine, benzylamine, 1- It may be dimethylamino-2-propanol (1-dimethylamino-2-propanol), 2- (diethylamino) ethanol (2- (diethylamino) ethanol) or diphenylamine (diphenylamine). That is, a pair of unshared electrons of nitrogen included in Chemical Formula 1 may form a polar portion by forming a coordinate bond with nickel.
- the concentration of the polar part may be 8% to 72% by weight, preferably 8% to 64% by weight, more preferably 8% to 64% by weight based on the total weight of the nickel complex compound ink composition. It may be 8% to 56% by weight.
- concentration of the polar portion is less than 8% by weight relative to the total weight of the conductive nickel complex ink composition, the content of the solvent is relatively high, making it difficult to form a uniform thin film when forming a nickel internal electrode formed by applying the transparent nickel complex ink composition to a substrate. If it is more than 72% by weight, the content of the solvent is relatively small, and the polar part and the solvent may not be uniformly mixed.
- the transparent nickel complex ink composition is a solvent, terpineol (terpineol), alpha terpineol ( ⁇ -terpineol), dihydro-terpineol (dihydro-terpineol), terpineyl acetate ( terpinyl acetate), dihydro terpinyl acetate, isobornyl acetate, isobornyl propionate, isobornyl isobutyrate, ethylene glycol glycol), propylene glycol, butylene glycol, diethylene glycol, dipropylene glycol, dipropylene glycol monomethyl ether, ethylene glycol phenyl Ether (ethylene glycol phenyl ether), propylene glycol phenyl ether, ethylene glycol monobutyl ether acetate, dipropylene glycol methyl ether acetate, ethanol, propanol, isopropyl alcohol , butanol,
- the solvent is well mixed with the polar portion and has excellent wettability with respect to the surface of a substrate, particularly glass, when the transparent nickel complex compound ink composition containing the solvent is applied to a substrate, a thin thickness may be formed, and the coating Flatness can also be excellent.
- solvents with low vapor pressure such as dipropylene glycol monomethyl ether
- the number of vaporized molecules is smaller than that of general solvents, so even a small amount of heat is applied to quickly change the molecules in the liquid state to the gaseous state. can do.
- solvents with low vapor pressure such as dipropylene glycol monomethyl ether
- the coating flatness after the drying and sintering process may also be excellent because the solvent evaporates quickly while maintaining excellent wettability on the entire surface of the coating area. Therefore, when applied to the internal electrodes of a multilayer ceramic capacitor (MLCC), thinning of the internal electrodes may be achieved because wettability with dielectric green sheets serving as a base material of the internal electrodes is also excellent. Meanwhile, the amount of the solvent may be 12% to 86% by weight based on the total weight of the conductive nickel complex ink composition.
- the other additives include a material selected from the group consisting of a binder resin, a plasticizer, a stabilizer, a dispersing agent, a release agent, a reducing agent, a surfactant, a wetting agent, a thixotropic agent, a leveling agent, and combinations thereof it could be
- the binder resin is polyvinyl butyral, ethyl cellulose, polyvinyl pyrrolidone, acryl, polyvinyl acetal, polyvinyl alcohol , polyolefin, polyurethane, polystyrene, and combinations thereof.
- the binder resin is polyvinyl butyral, ethyl cellulose, polyvinyl pyrrolidone, acryl, polyvinyl acetal, polyvinyl alcohol , polyolefin, polyurethane, polystyrene, and combinations thereof.
- the humectant is 1,2-hexanediol, 1,6-hexanediol, glycerin, polyethylene glycol, polyol such as sorbitol or trehalose, amino acid, urea, lactate, or natural moisturizing agent such as PCA-Na.
- a polymer moisturizer such as factor (NMF), hyaluronate, chondroitin sulfate, or hydrolyzed collagen may be used.
- the leveling agent is an additive having a smoothing (leveling) action, and a compound containing nitrogen such as polyamine may be used.
- the transparent nickel complex compound ink composition may have an absorbance (ABS) of 1.0 or more in a wavelength range of 600 nm to 650 nm.
- ABS absorbance
- the reason why the absorbance (ABS) peak in the 600 nm to 650 nm wavelength range of the nickel complex ink composition is high is because when the unshared electron pair of nitrogen included in Chemical Formula 1 forms a coordinate bond with nickel to form a polar portion, the d of nickel It is measured that an energy level difference occurs in the orbitals, and accordingly, d orbital electrons of a low energy level of nickel absorb light of a specific wavelength in the 600 nm to 650 nm wavelength band and move to a high energy level d orbital. It may be because it becomes Meanwhile, the absorbance (ABS) value may mean a value when the concentration of the polar portion is 8% to 72% by weight based on the total weight of the conductive nickel complex ink composition.
- the second aspect of the present application is,
- the substrate may be variously applied, but may be, for example, glass, and preferably may be a dielectric green sheet serving as a substrate for internal electrodes of a multilayer ceramic capacitor (MLCC).
- MLCC multilayer ceramic capacitor
- the MLCC internal electrode transparent nickel complex ink composition is well mixed with the polar part and contains a solvent with a low vapor pressure, it has excellent wettability with the substrate and the coating area in the drying and sintering process after coating. Coating flatness after the drying and sintering process may also be excellent because the solvent evaporates quickly throughout while maintaining excellent wettability on the front surface. Therefore, when it is applied to a substrate, it may form a thin thickness, and the coating flatness may also be excellent.
- the maximum diameter of nickel particles of the thin film including the transparent nickel complex ink composition may be 150 nm or less.
- the average diameter of the nickel particles is very small, the roughness of the nickel inner electrode may be reduced. This may be due to the fact that when the MLCC internal electrodes and the dielectric green sheets are alternately stacked and compressed, the adhesion is high, increasing the number of thin films in the MLCC of the same volume and improving performance.
- preparing a nickel complex compound by mixing a nickel precursor and a compound represented by Formula 1; mixing the nickel complex compound with a solvent; and heating the nickel complex compound mixed with the solvent. It provides a method for producing a transparent nickel complex compound ink composition comprising the step of heating the binder resin together in the heating step.
- R 1 to R 3 are each independently hydrogen, linear or branched C 5 -C 20 alkyl, linear or branched C 5 -C 20 alkenyl, C 5 -C 20 cycloalkyl, C 6 -C 20 aryl unsubstituted or substituted with straight or branched C 1 -C 5 alkyl or straight or branched C 8 -C 18 alkyl, straight or branched C 1 -C 5 alkyl or straight chain or C 6 -C 20 heteroaryl or C 5 -C 20 alkylcarbonyl unsubstituted or substituted with branched C 8 -C 18 alkyl, and at least one of R 1 to R 3 is straight-chain or branched-chain C 1 - C 6 -C 20 aryl unsubstituted or substituted with C 5 alkyl or straight or branched C 8 -C 18 alkyl, straight or branched C 1 -C 5 alkyl or straight or branched C
- the method for preparing the transparent nickel complex compound ink composition includes preparing a nickel complex compound by mixing a nickel precursor and a compound represented by Formula 1 below.
- the nickel precursor is nickel formate (C 2 H 2 NiO 4 ), nickel acetate (Ni(CH 3 CO 2 ) 2 ), nickel chloride (NiCl 2 ), nickel sulfate (NiSO 4 ) , nickel acetylacetonate (Ni(C 5 H 7 O 2 ) 2 ), nickel carbonate (NiCO 3 ), nickel cyclohexanebutyrate ([C 6 H 11 (CH 2 ) 3 CO 2 ] 2 Ni), nickel nitrate ( Ni(NO 3 ) 2 ), nickel oxalate (NiC 2 O 4 ), nickel stearate (Ni(H 3 C(CH 2 ) 16 CO 2 ) 2 , nickel octanoate ([CH 3 (CH 2 ) 6 It may include a material selected from the group consisting of CO 2 ] 2 Ni) and combinations thereof, wherein the carboxyl group included in the nickel precursor is removed by evaporation to CO 2 in a subsequent
- R 1 to R 3 are each independently hydrogen, linear or branched C 8 -C 18 alkyl, linear or branched C 8 -C 18 alkenyl , C 8 -C 18 cycloalkyl, straight or branched C 1 -C 5 alkyl or straight or branched C 8 -C 18 alkyl substituted or unsubstituted C 8 -C 18 aryl, straight or branched chain C 1 -C 5 alkyl, C 8 -C 18 heteroaryl unsubstituted or substituted with straight or branched C 8 -C 18 alkyl, straight or branched C 8 -C 18 alkyl or straight or branched C 8 -C 18 heteroaryl 8 -C 18 alkenyl, more preferably R 1 and R 2 are hydrogen, R 3 is straight or branched C 1 -C 5 alkyl, straight or branched C 8 -C 18 alkyl substituted C 8 -C
- the compound represented by Formula 1 is 2-amino-1-methyl-1-propanol (2-amino-1-methyl-1-propanol), normal hexylamine (n- hexylamine, hexylamine, cyclohexylamine, n-octylamine, octylamine, dodecylamine, oleylamine, benzylamine , 1-dimethylamino-2-propanol, 2-(diethylamino)ethanol, or diphenylamine. That is, a pair of unshared electrons of nitrogen included in Chemical Formula 1 may form a polar portion by forming a coordinate bond with nickel.
- the number of moles of the compound represented by Formula 1 forming a coordination bond with the nickel precursor may be 2 to 6 times, preferably 4 times, the number of moles of the nickel precursor. That is, the nickel precursor and the compound represented by Chemical Formula 1 may form a polar portion by forming a coordination bond.
- the polar part may not be formed, and when it is greater than 6 times, due to the compound represented by Formula 1 remaining without forming a complex compound. Thereafter, during the binder removal process, many air bubbles may be generated, which may cause voids to occur in the thin film of the internal electrode, resulting in a decrease in conductivity.
- the method for preparing the transparent nickel complex compound ink composition includes mixing the nickel complex compound with a solvent.
- the amount of the mixed solvent may be 12% to 86% by weight, preferably 20% to 82% by weight, based on the total weight of the conductive nickel complex ink composition.
- the content of the solvent is less than 12% by weight, the dispersion stability of the prepared transparent nickel complex ink composition may deteriorate, and when it exceeds 86% by weight, the content of the solvent is too high compared to the nickel complex compound, so that the nickel internal electrode formed by applying to the substrate It may be difficult to form a uniform thin film.
- the specific type of the solvent has been described in the first aspect of the present application, the description thereof will be omitted in the third aspect of the present application.
- the method for preparing the transparent nickel complex compound ink composition for forming a thin film includes heating the nickel complex compound mixed with the solvent.
- the heating may be performed at less than 115° C., and through this, hydrates included in the nickel precursor may be evaporated and removed.
- the step of heating the nickel complex compound mixed with the solvent may include heating the binder resin together.
- the transparent nickel complex compound ink composition may have an absorbance (ABS) of 1.0 or more in a wavelength range of 600 nm to 650 nm.
- ABS absorbance
- the reason why the absorbance (ABS) peak in the 600 nm to 650 nm wavelength range of the nickel complex ink composition is high is because when the unshared electron pair of nitrogen included in Chemical Formula 1 forms a coordinate bond with nickel to form a polar portion, the d of nickel It is measured that an energy level difference occurs in the orbitals, and accordingly, d orbital electrons of a low energy level of nickel absorb light of a specific wavelength in the 600 nm to 650 nm wavelength band and move to a high energy level d orbital. It may be because it becomes Meanwhile, the absorbance (ABS) value may mean a value when the concentration of the polar portion is 8% to 72% by weight based on the total weight of the conductive nickel complex ink composition.
- Step 1 Preparation of a transparent nickel complex ink composition
- Nickel acetate and benzylamine were mixed at a molar ratio of 1:4 to form a nickel polar part, and 73.6 wt% of diacetone alcohol was mixed with 21.4 wt% of the polar part as a solvent, ,
- a transparent nickel complex ink composition was prepared by mixing 5 wt% of PVB as a binder in the transparent nickel complex ink and stirring at 100 ° C.
- the transparent nickel complex compound ink composition prepared in step 1 was printed on glass with a doctor blade using a 30 ⁇ m applicator and dried at 600° C. to prepare a nickel internal electrode.
- step 1 of Example 1 a nickel polar part was formed by mixing nickel acetate and cyclohexylamine in a molar ratio of 1:4, and diacetone alcohol was added to 20.6 wt% of the polar part A nickel internal electrode was prepared in the same manner as in Example 1, except that 74.4 wt% was mixed as a solvent.
- step 1 of Example 1 a nickel polar part was formed by mixing nickel acetate and n-octylamine in a molar ratio of 1:4, and diacetone alcohol (23.5 wt% of the polar part) A nickel internal electrode was prepared in the same manner as in Example 1, except that 71.5 wt% of diacetone alcohol) was mixed as a solvent.
- step 1 of Example 1 a nickel polar part was formed by mixing nickel acetate and n-octylamine in a molar ratio of 1:4, and diacetone alcohol (13.4 wt% of the polar part) A nickel internal electrode was prepared in the same manner as in Example 1, except that 81.6 wt% of diacetone alcohol) was mixed as a solvent.
- Step 1 Preparation of a transparent nickel complex ink composition
- Nickel acetate and ethylenediamine were mixed at a molar ratio of 1:2 to form a nickel polar part, and 82.0 wt% of diacetone alcohol was mixed with 13.0 wt% of the polar part as a solvent, ,
- a transparent nickel complex ink composition was prepared by mixing 5 wt% of PVB as a binder in the transparent nickel complex ink and reacting at 100 ° C.
- the transparent nickel complex compound ink composition prepared in step 1 was printed on glass with a doctor blade using a 30 ⁇ m applicator and dried at 600° C. to prepare a nickel internal electrode.
- step 1 of Comparative Example 1 nickel acetate and n-octylamine were mixed in a molar ratio of 1:4 to form a nickel polar part, and diacetone alcohol (7.2 wt% of the polar part)
- a nickel internal electrode was prepared in the same manner as in Comparative Example 1, except that 87.8 wt% of diacetone alcohol) was mixed as a solvent.
- step 1 of Comparative Example 1 nickel acetate and n-octylamine were mixed in a molar ratio of 1:4 to form a nickel polar part, and diacetone alcohol (A nickel internal electrode was prepared in the same manner as in Comparative Example 1, except that 91.3 wt% of diacetone alcohol) was mixed as a solvent.
- the transparent nickel complex ink composition prepared in step 1 of Examples 1 to 3 and the transparent nickel complex ink composition prepared in step 1 of Comparative Example 1 Photos are shown in Fig. 1a, respectively.
- FIG. 1A in the case of the transparent nickel complex compound ink composition prepared in step 1 of Examples 1 to 3 of the present invention, it was confirmed that it was transparent, and no precipitate was formed, so that it was in a particle-free state that did not contain nickel particles. .
- the transparent nickel complex ink composition prepared in step 1 of Example 3 shown in FIG. 1A, the transparent nickel complex ink composition prepared in step 1 of Example 4 shown in FIG. 1B, and the steps of Comparative Examples 2 to 3 shown in FIG. 1B As in the transparent nickel complex ink composition prepared in 1, it was confirmed that the concentration of the transparent nickel complex ink composition decreased as the content of the polar part decreased and the content of the solvent increased.
- thermoscientific's spectrophotometer BioMate 160 was used, Using this, absorbance was measured in a wavelength range of 200 nm to 900 nm, and the results are shown in FIGS. 2a to 2c and FIG. 2d, respectively.
- 2a to 2c are graphs showing the absorbance of the transparent nickel complex ink composition prepared in Step 1 of Examples 1 to 3
- FIG. 2d is a graph showing the absorbance of the transparent nickel complex ink composition prepared in Step 1 of Comparative Example 1. to be.
- the transparent nickel complex ink composition prepared in Step 1 of Examples 1 to 3 had absorbance for light in a wavelength range of about 600 nm to 750 nm. Specifically, it was confirmed that the absorbance (ABS) for light in the 650 nm wavelength band had a value of 1.5 or more.
- the transparent nickel complex ink composition prepared in Step 1 of Comparative Example 1 shown in FIG. 2D unlike the transparent nickel complex ink composition prepared in Step 1 of Examples 1 to 3 shown in FIGS. It was confirmed that absorbance for light in the wavelength range of 650 nm to 650 nm was present.
- the absorbance (ABS) for light in the 650 nm wavelength range was 2.3 or more, 1.5 or more, and 2.3 or more for the transparent nickel complex ink composition prepared in Step 1 of Examples 1 to 3, respectively, of Comparative Example 1. It was confirmed that the transparent nickel complex ink composition prepared in step 1 had a value of 1.0 or more.
- the absorbance (ABS) value for light in the 650 nm wavelength band has a value of 1.0 or more. I was able to confirm.
- thermoscientific's spectrophotometer BioMate 160 was used in order to measure the absorbance of the transparent nickel complex ink composition prepared in Step 1 of Examples 3 and 4 and the transparent nickel complex ink composition prepared in Step 1 of Comparative Examples 2 and 3. And, using this, the absorbance was measured in the 200 nm to 900 nm wavelength range, and the results are shown in FIGS. 2e, 2f, and 2g, respectively.
- Figure 2c is a graph showing the absorbance of the transparent nickel complex compound ink composition prepared in step 1 of Example 3
- Figure 2e is a graph showing the absorbance of the transparent nickel complex compound ink composition prepared in step 1 of Example 4
- 2f and 2g are graphs showing the absorbance of the transparent nickel complex ink composition prepared in Step 1 of Comparative Examples 2 and 3, respectively.
- the transparent nickel complex ink composition prepared in step 1 of Example 3 had absorbance for light in a wavelength range of about 600 nm to 750 nm. Specifically, it was confirmed that the absorbance (ABS) for light in the 650 nm wavelength range had a value of 2.3 or more.
- FIG. 2c As in the transparent nickel complex ink composition prepared in step 1 of Example 3, it was confirmed that absorbance for light in a wavelength range of 600 nm to 750 nm was present.
- the absorbance (ABS) for light in the 650 nm wavelength range was 1.4 or more for the transparent nickel complex ink composition prepared in Step 1 of Example 4, and the transparent nickel prepared in Step 1 of Comparative Examples 2 and 3. It was confirmed that the complex compound ink composition had a value of 0.7 or more and a value of 0.3 or more, respectively.
- FIG. 3A Photographs of the nickel internal electrode prepared in Step 2 of Examples 1 to 3 and the nickel internal electrode prepared in Step 2 of Comparative Example 1 are shown in FIG. 3A.
- SEM pictures were taken to observe the thin film shapes of the nickel inner electrode prepared in Step 2 of Examples 1 to 3 and the nickel inner electrode prepared in Step 2 of Comparative Example 1, and the results are shown in FIGS. 4A to 4D. shown in each.
- the average diameter is very small, whereas in 4d It was confirmed that the maximum diameter of the nickel particles constituting the thin film of the nickel inner electrode prepared in step 2 of Comparative Example 1 using ethylenediamine, a bidentate ammonium ligand, was close to 150 nm. In addition, it was confirmed that the nickel internal electrode prepared in step 2 of Example 3 had less roughness than the nickel internal electrode prepared in step 2 of Comparative Example 1.
- FIG. 3B Pictures of the nickel internal electrode prepared in step 2 of Example 4 and the nickel internal electrode prepared in step 2 of Comparative Examples 2 and 3 are shown in FIG. 3B.
- SEM photographs were taken to observe the thin film shapes of the nickel internal electrode prepared in step 2 of Example 4 and the nickel internal electrode prepared in step 2 of Comparative Examples 2 and 3, and the results are shown in FIGS. 4e to 4g. shown in each.
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Abstract
Description
Claims (13)
- 니켈 및 상기 니켈에 배위결합된 하기 화학식 1로 표시되는 화합물을 포함하는 극성부;용매; 및기타첨가제;를 포함하는 투명한 니켈 착화합물 잉크 조성물로서,상기 니켈 착화합물 잉크 조성물은 투명하고 무입자이며, 600 nm 내지 650 nm 파장대에서의 흡광도(ABS)가 1.0 이상인 값을 가지는 것인 투명한 니켈 착화합물 잉크 조성물.[화학식 1](상기 화학식 1에서,R1 내지 R3은 각각 독립적으로 수소, 직쇄 또는 분지쇄의 C5-C20 알킬, 직쇄 또는 분지쇄의 C5-C20 알케닐, C5-C20 사이클로알킬, 직쇄 또는 분지쇄의 C1-C5 알킬 또는 직쇄 또는 분지쇄의 C8-C18 알킬로 치환 또는 비치환된 C6-C20 아릴, 직쇄 또는 분지쇄의 C1-C5 알킬 또는 직쇄 또는 분지쇄의 C8-C18 알킬로 치환 또는 비치환된 C6-C20 헤테로아릴 또는 C5-C20 알킬카보닐이고,R1 내지 R3 중 적어도 하나는 직쇄 또는 분지쇄의 C1-C5 알킬 또는 직쇄 또는 분지쇄의 C8-C18 알킬로 치환 또는 비치환된 C6-C20 아릴, 직쇄 또는 분지쇄의 C1-C5 알킬 또는 직쇄 또는 분지쇄의 C8-C18 알킬로 치환 또는 비치환된 C6-C20 헤테로아릴 및 직쇄 또는 분지쇄의 C5-C20 알킬 또는 C5-C20알케닐로 이루어진 군에서 선택된 어느 하나이다.)
- 제1항에 있어서,상기 화학식 1에서, R1 내지 R3은 각각 독립적으로 수소, 직쇄 또는 분지쇄의 C8-C18 알킬, 직쇄 또는 분지쇄의 C8-C18 알케닐, C8-C18 사이클로알킬, 직쇄 또는 분지쇄의 C1-C5 알킬 또는 직쇄 또는 분지쇄의 C8-C18 알킬로 치환 또는 비치환된 C8-C18 아릴, 직쇄 또는 분지쇄의 C1-C5 알킬, 직쇄 또는 분지쇄의 C8-C18 알킬로 치환 또는 비치환된 C8-C18 헤테로아릴, 직쇄 또는 분지쇄의 C8-C18 알킬 또는 직쇄 또는 분지쇄의 C8-C18 알케닐인 것인 투명한 니켈 착화합물 잉크 조성물.
- 제1항에 있어서,상기 화학식 1에서, R1 및 R2는 수소이고, R3은 직쇄 또는 분지쇄의 C1-C5 알킬, 직쇄 또는 분지쇄의 C8-C18 알킬로 치환된 C8-C18 아릴 또는 헤테로아릴, 직쇄 또는 분지쇄의 C8-C18 알킬 또는 직쇄 또는 분지쇄의 C8-C18 알케닐인 것인 투명한 니켈 착화합물 잉크 조성물.
- 제1항에 있어서,상기 화학식 1로 표시되는 화합물은 2-아미노-1-메틸-1-프로판올(2-amino-1-methyl-1-propanol), 노르말헥실아민(n-hexylamine), 헥실아민(hexylamine), 시클로헥실아민(cyclohexylamine), 노르말옥틸아민(n-octylamine), 옥틸아민(octylamine), 도데실아민(dodecylamine), 올레일아민(oleylamine), 벤질아민(benzylamine), 1-디메틸아미노-2-프로판올(1-dimethylamino-2-propanol), 2-(디에틸아미노)에탄올(2-(diethylamino)ethanol) 또는 디페닐아민(diphenylamine)인 것인 투명한 니켈 착화합물 잉크 조성물.
- 제1항에 있어서,상기 극성부의 농도는 상기 투명한 니켈 착화합물 잉크 조성물 전체 중량 대비 8 중량% 내지 72 중량%인 것인 투명한 니켈 착화합물 잉크 조성물.
- 제1항에 있어서,상기 용매는 터피네올(terpineol), 알파터피네올(α-terpineol), 디하이드로터피네올(dihydro-terpineol), 터피닐아세테이트 (terpinyl acetate), 디하이드로터피닐아세테이트(dihydro terpinyl acetate), 이소보르닐아세테이트(isobornyl acetate), 이소보르닐프로피오네이트(isobornyl propionate), 이소보르닐이소부틸레이트(isobornyl isobutyrate), 에틸렌글리콜(ethylene glycol), 프로필렌글리콜(propylene glycol), 부틸렌글리콜(butylene glycol), 디에틸렌글리콜(diethylene glycol), 디프로필렌글리콜(dipropylene glycol), 디프로필렌글리콜모노메틸에테르(dipropylene glycol monomethyl ether), 에틸렌글리콜페닐에테르(ethylene glycol phenyl ether), 프로필렌글리콜페닐에테르(propylene glycol phenyl ether), 에틸렌글리콜모노부틸에테르아세테이트, 디프로필렌글리콜메틸에테르아세테이트, 에탄올(ethanol), 프로판올(propanol), 이소프로필알코올(isopropyl alcohol), 이소옥틸알코올(isooctyl alcohol), 부탄올(butanol), 디아세톤알코올(diacetone alcohol), 1,2-펜탄디올, 1,5-펜탄디올, 2-메틸-2,4-펜탄디올, 3-메틸-1,5-펜탄디올 및 이들의 조합들로 이루어진 군으로부터 선택되는 물질을 포함하는 것인 투명한 니켈 착화합물 잉크 조성물.
- 제1항에 있어서,상기 기타 첨가제는 바인더 수지, 가소제, 안정제, 분산제, 이형제, 환원제, 계면활성제, 습윤제, 칙소제, 레벨링제 및 이들의 조합들로 이루어진 군으로부터 선택되는 물질을 포함하는 것인 투명한 니켈 착화합물 잉크 조성물.
- 제7항에 있어서,상기 바인더 수지는 폴리비닐부티랄(polyvinyl butyral), 에틸셀룰로오스(ethyl cellulose), 폴리비닐피롤리돈(polyvinyl pyrrolidone), 아크릴(acryl), 폴리비닐아세탈(polyvinyl acetal), 폴리비닐알코올(polyvinyl alcohol), 폴리올레핀(polyolefin), 폴리우레탄(polyurethane), 폴리스티렌(polystyrene) 및 이들의 조합들로 이루어진 군으로부터 선택되는 물질을 포함하는 것인 투명한 니켈 착화합물 잉크 조성물.
- 제7항에 있어서,상기 바인더 수지는 폴리비닐부티랄(polyvinyl butyral), 에틸셀룰로오스(ethyl cellulose), 폴리비닐피롤리돈(polyvinyl pyrrolidone), 아크릴(acryl), 폴리비닐아세탈(polyvinyl acetal), 폴리비닐알코올(polyvinyl alcohol), 폴리올레핀(polyolefin), 폴리우레탄(polyurethane), 폴리스티렌(polystyrene) 및 이들의 조합들로 이루어진 군으로부터 선택되는 물질을 포함하는 것인 투명한 니켈 착화합물 잉크 조성물.
- 제1항에 있어서,상기 투명한 니켈 착화합물 잉크 조성물은 MLCC 내부전극 형성용, 전자파 차폐용, 태양전지 전극 형성용, 또는 디스플레이 패널 전극 형성용 투명한 니켈 착화합물 잉크 조성물인 것을 특징으로 하는, 투명한 니켈 착화합물 잉크 조성물.
- 니켈 전구체 및 하기 화학식 1로 표시되는 화합물을 혼합하여 니켈 착화합물을 제조하는 단계;상기 니켈 착화합물을 용매와 혼합하는 단계; 및상기 용매와 혼합된 니켈 착화합물을 가열하는 단계;상기 가열 단계에서 바인더 수지를 함께 가열하는 단계;를 포함하는 투명한 니켈 착화합물 잉크 조성물의 제조방법.[화학식 1](상기 화학식 1에서,R1 내지 R3은 각각 독립적으로 수소, 직쇄 또는 분지쇄의 C5-C20 알킬, 직쇄 또는 분지쇄의 C5-C20 알케닐, C5-C20 사이클로알킬, 직쇄 또는 분지쇄의 C1-C5 알킬 또는 직쇄 또는 분지쇄의 C8-C18 알킬로 치환 또는 비치환된 C6-C20 아릴, 직쇄 또는 분지쇄의 C1-C5 알킬 또는 직쇄 또는 분지쇄의 C8-C18 알킬로 치환 또는 비치환된 C6-C20 헤테로아릴 또는 C5-C20 알킬카보닐이고,R1 내지 R3 중 적어도 하나는 직쇄 또는 분지쇄의 C1-C5 알킬 또는 직쇄 또는 분지쇄의 C8-C18 알킬로 치환 또는 비치환된 C6-C20 아릴, 직쇄 또는 분지쇄의 C1-C5 알킬 또는 직쇄 또는 분지쇄의 C8-C18 알킬로 치환 또는 비치환된 C6-C20 헤테로아릴 및 직쇄 또는 분지쇄의 C5-C20 알킬 또는 C5-C20알케닐로 이루어진 군에서 선택된 어느 하나이다.)
- 제11항에 있어서,상기 니켈 착화합물 잉크 조성물은 투명하고 무입자이며, 600 nm 내지 650 nm 파장대에서의 흡광도(ABS)가 1.0 이상인 값을 가지는 투명한 니켈 착화합물 잉크 조성물의 제조방법.
- 제11항에 있어서,상기 가열은 115℃ 미만에서 수행되는 것인 투명한 니켈 착화합물 잉크 조성물의 제조방법.
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JP2000204495A (ja) * | 1999-01-08 | 2000-07-25 | Okuno Chem Ind Co Ltd | 電気ニッケルメッキ液 |
JP2008127657A (ja) * | 2006-11-22 | 2008-06-05 | Sumitomo Metal Mining Co Ltd | ニッケル膜形成用塗布液及びニッケル膜の製造方法並びにニッケル膜 |
JP2012131894A (ja) * | 2010-12-21 | 2012-07-12 | Tosoh Corp | 導電性インク組成物、及びそれを用いて製造された電気的導通部位 |
KR20150118424A (ko) * | 2014-04-14 | 2015-10-22 | 주식회사 두산 | 저점도 금속 잉크 조성물, 이를 이용한 적층시트, 연성 금속박 적층판 및 인쇄회로기판 |
KR20200064350A (ko) * | 2018-11-29 | 2020-06-08 | 솔브레인 주식회사 | 적층형 세라믹 커패시터의 내부전극용 도전성 잉크 조성물의 제조방법 및 이를 이용한 적층형 세라믹 커패시터의 내부전극 제조방법 |
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KR20220161883A (ko) | 2022-12-07 |
JP2024521247A (ja) | 2024-05-29 |
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