CN106398398B - Metal nano conductive ink and preparation method thereof - Google Patents
Metal nano conductive ink and preparation method thereof Download PDFInfo
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- 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
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- 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
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- 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
- C09D11/30—Inkjet printing inks
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- 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
- C09D11/30—Inkjet printing inks
- C09D11/36—Inkjet printing inks based on non-aqueous solvents
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- 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
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
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Abstract
The invention discloses a metal nano conductive ink and a preparation method thereof, wherein the metal nano conductive ink comprises the following components: gold, silver and copper nano particle powder, the content is 10-60 wt%; the content of the metal organic matter which can be decomposed at low temperature is 5-20 wt%; non-volatile organic components, in an amount of 0-1 wt%; volatile organic component, the dosage is 20-80 wt%. The preparation method comprises the following steps: adding high molecular resin or its mixture into high boiling point solvent or its mixture under stirring to obtain component A; dissolving metallorganics in a low boiling point solvent, called component B; adding the nanoparticle powder to the cooled component A, and then mixing a certain volume of component B; grinding, high-speed shearing and three-roll banburying of the obtained mixture to promote dispersion to obtain a viscous component C; and adding a high-boiling-point solvent or a mixture thereof or the component A into the component C according to a certain proportion, and adjusting the viscosity of the system and the content of the metal nano particles to obtain the final metal nano conductive ink. The invention can realize low-temperature sintering, high conductivity and large-thickness printing, and is widely applied to various metal nano conductive inks and preparation methods thereof.
Description
Technical Field
The invention belongs to the field of chemical engineering, and relates to a metal nano conductive ink and a preparation method thereof, in particular to the metal nano conductive ink which can be transferred onto base materials such as PET films, coated paper and the like in ink jet, gravure and other modes, forms high conductive patterns and lines after drying and sintering, can form a printing thickness of more than 0.5um at one time, can be sintered at a low temperature of less than 150 ℃, and has the resistivity as low as 5 uomega cm.
Background
Nanomaterials are materials which have at least one dimension in the three-dimensional space in the nanoscale range (1-100nm) or which are composed of them as elementary units. When the macroscopic object is subdivided into nanometer scales, the properties of the macroscopic object in the aspects of optics, thermology, electrics, magnetics, mechanics and chemistry can be obviously changed, and the macroscopic object can be widely applied to the fields of electronics, medicine, chemical engineering, military, aerospace and the like. The metal nano material such as gold, silver, copper and the like has unique optical and electrical properties, so the metal nano material is widely applied to the fields of electronics, optics, display, sensing, energy and the like
Conventional inks are stable colloidal dispersions, typically composed of pigments, solid resins, volatile solvents, fillers and additives. Pigments provide color to conventional inks, and solid resins are film-forming materials. The traditional conductive ink is a colloid dispersion system containing micron-sized conductive particles, can form conductive patterns and lines after being dried or sintered at high temperature, and is widely applied to the fields of printed circuit boards, solar photovoltaics and the like.
If the traditional conductive ink is dried only at low temperature, the conductive particles conduct current through physical contact, so that the traditional conductive ink has high resistance, poor resistance to damp-heat aging and limited application in harsh environments such as outdoors and the like. In order to expand the application range, high-temperature sintering is generally adopted in the past to remove organic matters and melt metal particles into a whole, so that the conductivity and the stability are improved. However, the sintering temperature is generally higher than 400 ℃, which is difficult to satisfy the application of plastic-based electronic devices and products.
Recently, metal nanoparticles have been used to achieve low temperature sintering conductivity. However, the dispersion of nanoparticles is extremely difficult, and usually requires large amounts of organic materials, which are otherwise unstable in colloidal systems, undergo agglomeration, flocculation and precipitation, and ultimately affect use. However, when a large amount of organic material is used to improve the dispersion, the presence of the organic material may affect the conductivity during low-temperature sintering, and may even inhibit sintering fusion.
Disclosure of Invention
The invention aims to overcome the defects of high organic content, low effective component, high sintering temperature, thin printing thickness and the like of the metal nanoparticle ink in the prior art, particularly introduces the low-temperature decomposable metal organic as the dispersing agent of the metal nanoparticles, realizes the stable dispersion of the metal nanoparticles, and decomposes at the low temperature of less than 150 ℃ to improve the fusion of the metal nanoparticles, thereby realizing the low-temperature sintering, high conductivity and large-thickness printing.
A metal nano conductive ink comprises the following components:
1) gold, silver and copper nano particle powder with the particle size of 1-500nm, the content is 10-60 wt%;
2) metal organic matter capable of being decomposed at low temperature of less than 150 ℃ with the content of 5-20 wt%;
3) non-volatile organic components, in an amount of 0-1 wt%;
4) volatile organic component, the dosage is 20-80 wt%.
Preferably, the gold, silver and copper nano-particle powder with the particle size of 1-500nm can be prepared by chemical synthesis, physical grinding, explosion method and the like. When the metal nano particles are synthesized by a chemical method, excessive organic matters are removed by the processes of cleaning, centrifuging, precipitating and the like until the content is less than 1 wt%. When the metal nano-particles are prepared by other methods such as physical grinding, the organic content of the metal nano-particles is controlled to be less than 1 wt%.
Preferably, the metal organic matter which can be decomposed at a low temperature of less than 150 ℃ has the following structure:
M-X1-R-X2，
wherein: m is gold, silver, copper ion; r is an alkyl chain, typically R contains 1 to 4 carbon atoms to ensure low temperature volatilisation; x1 is a functional group for connecting metal ions, such as-COO-, -S-, -N-and other groups which can be matched with gold, silver and copper ions; x2 is a functional group capable of dispersing gold, silver and copper nanoparticles, such as-COOH, -SH, -NH2, glycol ether chain (the number of chain links is 1-4), propylene glycol ether chain (the number of chain links is 1-4) and polyvinylpyrrolidone chain (the number of chain links is 1-4).
Preferably, the nonvolatile organic component is a polymer resin; the polymer resin is ethyl cellulose, hydroxypropyl cellulose, acrylic resin, and polyurethane resin.
Preferably, the volatile organic component is a high boiling point solvent and a surface auxiliary agent.
Preferably, the high-boiling point solvent used is ethylene glycol propyl ether, ethylene glycol butyl ether, diethylene glycol ethyl ether, diethylene glycol propyl ether, diethylene glycol butyl ether, propylene glycol propyl ether, propylene glycol butyl ether, dipropylene glycol ethyl ether, dipropylene glycol propyl ether, dipropylene glycol butyl ether, ethylene glycol propyl ether acetate, ethylene glycol butyl ether acetate, diethylene glycol ethyl ether acetate, diethylene glycol propyl ether acetate, diethylene glycol butyl ether acetate, propylene glycol propyl ether acetate, propylene glycol butyl ether acetate, dipropylene glycol ethyl ether acetate, dipropylene glycol propyl ether acetate, dipropylene glycol butyl ether acetate, ethylene glycol, terpineol, petroleum ether.
Preferably, the surface auxiliary agent is organic amine, organic carboxylic acid, polyoxyethylene and polyoxypropylene copolymer, sorbitan fatty acid ester, sucrose fatty acid ester, polyoxyethylene fatty alcohol ether, polyoxyethylene polyester fatty alcohol ether, polyglycerol fatty acid ester, polysiloxane and polyether modified siloxane.
A preparation method of metal nano conductive ink comprises the following steps:
1. adding a certain amount of polymer resin or its mixture into the above-mentioned high-boiling-point solvent or its mixture, heating to 60-120 deg.C, dissolving for 30-120min, preparing 0-5 wt% polymer resin solution, named as component A;
2. dissolving metallorganics which can be decomposed at a low temperature of less than 150 ℃ in low boiling point solvents such as methanol, ethanol, butane, hexane, cyclohexane and the like, and obtaining a component B;
3. adding gold, silver and copper nano particle powder with the particle size within the range of 1-500nm into the cooled component A in proportion, and then mixing the component B with a certain volume;
4. grinding, high-speed shearing and three-roll banburying of the mixture obtained in the step 3) to promote dispersion to obtain a viscous component C;
5. and adding the high-boiling-point solvent or the mixture thereof or the component A into the component C according to a certain proportion, and adjusting the viscosity of the system and the content of the metal nano particles to obtain the final metal nano conductive ink.
The polymer resin is ethyl cellulose, hydroxypropyl cellulose, acrylic resin and polyurethane resin; the metal organic compound has the following structure M-X1-R-X2, wherein: m is gold, silver and copper ions, R is an alkyl chain, usually R contains 1-4 carbon atoms, X1 is a functional group for connecting metal ions, and X2 is a functional group capable of dispersing gold, silver and copper nanoparticles; the high boiling point solvent is ethylene glycol propyl ether, ethylene glycol butyl ether, diethylene glycol ethyl ether, diethylene glycol propyl ether, diethylene glycol butyl ether, propylene glycol propyl ether, propylene glycol butyl ether, dipropylene glycol ethyl ether, dipropylene glycol propyl ether, dipropylene glycol butyl ether, ethylene glycol propyl ether acetate, ethylene glycol butyl ether acetate, diethylene glycol ethyl ether acetate, diethylene glycol propyl ether acetate, diethylene glycol butyl ether acetate, propylene glycol propyl ether acetate, propylene glycol butyl ether acetate, dipropylene glycol ethyl ether acetate, dipropylene glycol propyl ether acetate, dipropylene glycol butyl ether acetate, ethylene glycol, terpineol, petroleum ether.
Due to the technical scheme, the invention has the beneficial effects that: the stable dispersion of the metal nano particles is realized, and the metal nano particles are decomposed at the low temperature of less than 150 ℃ to improve the fusion of the metal nano particles, so that the low-temperature sintering, high conductivity and large-thickness printing are realized, and the method is widely applied to various metal nano conductive inks and preparation methods thereof.
Detailed Description
The invention is further illustrated by the following specific examples:
example 1:
1) adding ethyl cellulose into dipropylene glycol butyl ether under stirring, heating to 60-80 deg.C, dissolving for 60-120min, and making into 0-50g/L polymer resin solution, named as component A;
2) dissolving a metal organic substance AgOOC-CH2OCH2CH2OCH2CH2OH which can be decomposed at low temperature into an ethanol low-boiling-point solvent to obtain a component B with the concentration of 10-40 wt%;
3) adding nano silver particle powder (with the particle size of 50-150 nm) synthesized by a polyol method into the component A, stirring to prepare dispersion liquid with the concentration of 80 wt%, and then adding the component B according to the proportion;
4) promoting dispersion of the mixture obtained in step 3) by grinding to obtain a viscous component C;
5) and adding terpineol into the component C according to a certain proportion, and adjusting the viscosity of the system and the content of the metal nano particles to obtain the silver nano conductive ink.
The silver nano conductive ink obtained in the example 1 can realize the printing with the thickness of 1-3um and the thinnest line diameter of 50um by testing with a general commercial R2R gravure device, and the low-temperature sintering resistivity of less than 150 ℃ is as low as 5u omega cm on coated paper and as low as 10u omega cm on a PET film.
Example 2:
1) adding acrylate resin into the mixed solvent of alcohol ether and alcohol ester, heating to 80-100 deg.C, dissolving for 60-120min, and making into polymer resin solution with concentration of 0-50g/L, which is called component A;
2) dissolving a metal organic substance AgOOC-CH2OCH2CH2NHCH2CH2NH2 which can be decomposed at low temperature into a methanol low-boiling-point solvent to obtain a component B with the concentration of 10-40 wt%;
3) adding nano copper particle powder (with the particle size of 200-500nm) into the component A, stirring to prepare dispersion liquid with the concentration of 80 wt%, and then adding the component B according to the proportion;
4) promoting dispersion of the mixture obtained in the step 3) by high-speed shearing to obtain a viscous component C;
5) and adding terpineol into the component C according to a certain proportion, and adjusting the viscosity of the system and the content of the metal nano particles to obtain the copper nano conductive ink.
The copper nano conductive ink obtained in the example 2 can realize the printing with the thickness of 1-3um and the thinnest line diameter of 50um by testing with a general commercial R2R gravure device, and the low-temperature sintering resistivity of less than 150 ℃ is as low as 10u omega cm on coated paper and as low as 20u omega cm on a PET film.
Example 3:
1) dissolving a metal organic substance AgSCH2CH2OCH2CH2OCH2CH2OH which can be decomposed at low temperature in an ethanol low-boiling-point solvent to obtain a component A with the concentration of 10-40 wt%;
2) adding nano silver particle powder (with the particle size of 10-50 nm) into the alcohol ether and alcohol ester mixed solvent to prepare dispersion liquid with the concentration of 80 wt%, and then adding the component A in proportion;
3) carrying out three-roll banburying on the mixture obtained in the step 2) to promote dispersion, so as to obtain a viscous component B;
4) and adding a mixed solvent such as terpineol and the like into the component B according to a certain proportion, and adjusting the viscosity of the system and the content of the metal nano particles to obtain the silver nano conductive ink.
The silver nano conductive ink obtained in the embodiment 3 can realize the printing of the thickness of 0.5-1um and the thinnest line diameter of 50um by adopting a Dimatix DMP-2831 device ink-jet printing test, and the low-temperature sintering resistivity is as low as 5 uOmega-cm on coated paper and as low as 10 uOmega-cm on a PET film at the temperature of less than 150 ℃.
Example 4:
1) dissolving a metal organic substance AgSCH2CH2NHCH2CH2N2 which can be decomposed at low temperature in an ethanol low-boiling point solvent to obtain a component A with the concentration of 10-40 wt%;
2) adding nano gold particle powder (with the particle size of 5-20 nm) into the alcohol ether and alcohol ester mixed solvent to prepare dispersion liquid with the concentration of 80 wt%, and then adding the component A in proportion;
3) grinding the mixture obtained in step 2) to promote dispersion to obtain a viscous component B;
4) and adding a mixed solvent such as terpineol and the like into the component B according to a certain proportion, and adjusting the viscosity of the system and the content of the metal nano particles to obtain the gold nano conductive ink.
The gold nano conductive ink obtained in the embodiment 4 is subjected to ink jet printing test by adopting a Dimatix DMP-2831 device, the printing with the thickness of 0.5-1um and the thinnest 50um wire diameter can be realized, the low-temperature sintering resistivity is as low as 5 uOmega-cm on coated paper at the temperature of less than 200 ℃, and the low-temperature sintering resistivity is as low as 10 uOmega-cm on a PET film.
Claims (3)
1. A metal nano conductive ink comprises the following components:
1) gold, silver and copper nano particle powder with the particle size of 1-500nm, the content is 10-60 wt%;
2) metal organic matter capable of being decomposed at low temperature of less than 150 ℃ with the content of 5-20 wt%; the metal organic matter is as follows: AgOOC-CH2OCH2CH2OCH2CH2OH、AgOOC-CH2OCH2CH2NHCH2CH2NH2、AgSCH2CH2OCH2CH2OCH2CH2OH、AgSCH2CH2NHCH2CH2N2；
3) The non-volatile organic component accounts for 0-1 wt%, and is macromolecular resin which is ethyl cellulose, hydroxypropyl cellulose, acrylic resin or polyurethane resin;
4) volatile organic component, the dosage is 20-80 wt%.
2. A preparation method of metal nano conductive ink comprises the following steps:
1) adding high molecular resin or its mixture into high boiling point solvent or its mixture under stirring, heating to 60-120 deg.C to dissolve for 30-120min, and preparing 0-5 wt% high molecular resin solution, named as component A;
2) dissolving metallorganics which can be decomposed at a low temperature of less than 150 ℃ in a low boiling point solvent of methanol, ethanol, butane, hexane and cyclohexane, and obtaining a component B;
3) adding gold, silver and copper nano-particle powder with the particle size of 1-500nm into the cooled component A, and then mixing the component B;
4) grinding, high-speed shearing and three-roll banburying of the mixture obtained in the step 3) to promote dispersion to obtain a viscous component C;
5) adding a high-boiling-point solvent or a mixture thereof or the component A into the component C according to a certain proportion, and adjusting the system viscosity and the content of metal nano particles to obtain the final metal nano conductive ink; the high polymer resin is ethyl cellulose, hydroxypropyl cellulose, acrylic resin and polyurethane resin; the metal organic matter is as follows: AgOOC-CH2OCH2CH2OCH2CH2OH、AgOOC-CH2OCH2CH2NHCH2CH2NH2、AgSCH2CH2OCH2CH2OCH2CH2OH、AgSCH2CH2NHCH2CH2N2。
3. The method for preparing metal nano conductive ink according to claim 2, wherein the method comprises the following steps: the high boiling point solvent is ethylene glycol propyl ether, ethylene glycol butyl ether, diethylene glycol ethyl ether, diethylene glycol propyl ether, diethylene glycol butyl ether, propylene glycol propyl ether, propylene glycol butyl ether, dipropylene glycol ethyl ether, dipropylene glycol propyl ether, dipropylene glycol butyl ether, ethylene glycol propyl ether acetate, ethylene glycol butyl ether acetate, diethylene glycol ethyl ether acetate, diethylene glycol propyl ether acetate, diethylene glycol butyl ether acetate, propylene glycol propyl ether acetate, propylene glycol butyl ether acetate, dipropylene glycol ethyl ether acetate, dipropylene glycol propyl ether acetate, dipropylene glycol butyl ether acetate, ethylene glycol, terpineol and petroleum ether.
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| CN110922895A (en) * | 2019-12-16 | 2020-03-27 | 广东南海启明光大科技有限公司 | Preparation process of conductive chemical coating liquid and preparation method of electric conductor |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101010388A (en) * | 2005-03-04 | 2007-08-01 | 韩商英泰股份有限公司 | Conductive inks and manufacturing method thereof |
| CN104341860A (en) * | 2013-08-01 | 2015-02-11 | 索尼公司 | Nanometer conductive ink and preparing method thereof |
| CN104419261A (en) * | 2013-09-02 | 2015-03-18 | 北京中科纳通电子技术有限公司 | Colorized conductive ink |
| CN105670384A (en) * | 2016-03-31 | 2016-06-15 | 广东南海启明光大科技有限公司 | Nano silver gravure ink and preparation method thereof |
| CN105670390A (en) * | 2008-01-30 | 2016-06-15 | 巴斯夫欧洲公司 | Conductive inks |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101010388A (en) * | 2005-03-04 | 2007-08-01 | 韩商英泰股份有限公司 | Conductive inks and manufacturing method thereof |
| CN105670390A (en) * | 2008-01-30 | 2016-06-15 | 巴斯夫欧洲公司 | Conductive inks |
| CN104341860A (en) * | 2013-08-01 | 2015-02-11 | 索尼公司 | Nanometer conductive ink and preparing method thereof |
| CN104419261A (en) * | 2013-09-02 | 2015-03-18 | 北京中科纳通电子技术有限公司 | Colorized conductive ink |
| CN105670384A (en) * | 2016-03-31 | 2016-06-15 | 广东南海启明光大科技有限公司 | Nano silver gravure ink and preparation method thereof |
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