CN105504998A - Low-temperature-sintered organic metal conductive ink and preparing method thereof - Google Patents
Low-temperature-sintered organic metal conductive ink and preparing method thereof Download PDFInfo
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- CN105504998A CN105504998A CN201511000727.0A CN201511000727A CN105504998A CN 105504998 A CN105504998 A CN 105504998A CN 201511000727 A CN201511000727 A CN 201511000727A CN 105504998 A CN105504998 A CN 105504998A
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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
Abstract
The invention relates to the technical field of conductive inks, in particular to a low-temperature-sintered organic metal conductive ink and a preparing method thereof. The low-temperature-sintered organic metal conductive ink is characterized by comprising, by weight, 10%-25% of silver salt, 30%-60% of solvent, 20%-40% of complexing agent, 0.1%-5.0% of viscosity modifier and 0.1%-3.0% of surface active agent. Compared with the prior art, the good-stability low-temperature-sintered organic metal conductive ink and the preparing method thereof are provided, and the conductive ink can have the good electrical conductivity at the low sintering temperature, can be printed on multiple base materials, and can be used for flexible electronic printing.
Description
Technical field
The present invention relates to conductive ink technology field, specifically one can low-temperature sintering organo-metallic conductive ink and preparation method thereof.
Background technology
Along with the demand to electronics high precision high integration, inkjet technology is shown up prominently in printed electronics field gradually.Because spray ink Printing can realize drop on demand ink jet, and fast, convenient, relative to traditional masterplate formula printing, the waste of raw material can be reduced, therefore attracted the research of each side related personnel.In ink-jet printed electronics, what be mainly concerned with is printer, ink and base material.Good adaptability must be had between three just to obtain device of good performance.For realizing high precision, the aperture of the shower nozzle of ink-jet printer is little as much as possible, in this respect, market has had the print cartridge of 1pl, by regulating print parameters, can obtain good ink droplet.Base material aspect, can carry out modification by certain processing mode to substrate surface, can have good film forming properties to make ink on base material.Therefore, most critical is exactly the ink that can be used for spray ink Printing.This ink must should adapt to printer, obtains good ink droplet, can possess good electroconductibility again, and in use performance deterioration can not occur, and impact uses.The conductive ink meeting these performances can be applied to the aspects such as RF identification (RFID), Organic Light Emitting Diode (OLED), printed circuit board (PCB) (PCB), flexible sensor.
Electro-conductive material in conventional conductive ink can be divided into two classes, and a class is nonmetal, and a class is metal.In radio frequency ink, mainly carbonaceous material, but its electroconductibility is lower than metal, and therefore the application of metal system conductive ink is more wide.In metallic substance, good conductivity first to count gold, silver and bronze.But the price of gold is the most expensive comparatively speaking, what therefore apply is not very extensive.The price of silver is taken second place, and copper is the most cheap.But copper exists a maximum problem to be oxidized exactly.Particularly size is more little is more easily oxidized.Therefore, in conductive ink, account for and leading will count silver-colored conductive ink.
Silver conductive ink can be divided into two classes, granule type and agranular type.For granule type silver conductive ink, mainly prepare the Argent grain that particle diameter is very little, and want can be good scatter, do not reunite, in order to avoid blocking printer head, then by these Granular composite in a solvent, adjusting viscosity and surface tension, can obtain granule type conductive ink.For granule type conductive ink, the preparation process more complicated of particle, needs by high speed centrifugation usually to obtain particle.In addition, in storage process, once particle generating portion is reunited, so just there will be the phenomenon of blocking shower nozzle.For these features, agranular type ink can avoid these potential problems.Therefore, agranular type conductive ink has potential using value.
In order to realize flexible printing, need ink can realize sintering at a lower temperature.Conventional plastic basis material comprises PET and PI, and wherein the temperature that can bear of PI is higher, but price is more expensive.PET low price, but can bear do high-temperature about about 150 DEG C.Therefore, to for flexible ink jet printing, ink just can must realize fully sintered below 150 DEG C, has the electroconductibility that can meet application.
Summary of the invention
The present invention is for overcoming the deficiencies in the prior art, there is provided one to have good stability, low temperature sintering organo-metallic conductive ink and preparation method thereof, this conductive ink can obtain good electroconductibility at a relatively low sintering temperature, and can be printed on multiple base material, can be used for the printing of flexible electronic.
For achieving the above object, design one can low-temperature sintering organo-metallic conductive ink, it is characterized in that: comprise silver salt, solvent, complexing agent, viscosity modifier and tensio-active agent, wherein the weight percent content of silver salt is 10-25%, the weight percent content of solvent is 30-60%, the weight percent content of complexing agent is 20 ~ 40%, and the weight percent content of viscosity modifier is 0.1%-5.0%, and the weight percent of tensio-active agent is 0.1% ~ 3.0%.
Described silver salt is one or more mixing in silver carbonate, Silver Nitrate, silver citrate, Silver monoacetate, neodecanoic acid silver, beta-keto acid silver-colored, 2-[2-(2-methoxyethoxy) oxyethyl group] Silver monoacetate, lauric acid silver, silver oxalate.
Described solvent is one or more mixing in methyl alcohol, ethanol, ethylene glycol, glycol ether, glycerol, Virahol, 1,2-PD, ethylene glycol monomethyl ether, ethylene glycol monobutyl ether, Macrogol 200, poly(oxyethylene glycol) 400, toluene.
Described complexing agent is ammoniacal liquor, quadrol, Isopropylamine, ammonium oxalate, hexahydroaniline, methane amide, diethylamine, triethylamine, n-Butyl Amine 99, n-octyl amine, 2-amino-2-methyl-1-propanol, thanomin, diethanolamine, trolamine, 2-(ethylamino) ethanol, 2-(dimethylamino) ethanol, 2-(diethylin) ethanol, 1-amino-2-propyl alcohol (α-amino isopropyl alcohol), ethyldiethanolamine, one or more mixing in butyl diethanolamine.
Described viscosity modifier is one or more mixing in Macrogol 200, polyoxyethylene glycol-300, PEG-4000, ethylene glycol, glycerol, glycol ether, 1,2-PD, Terpineol 350; Or be conducting polymer Polythiophene or polyacetylene; Described Polythiophene is one or more mixing in poly-3 methyl thiophene, poly-3-ethylthiophene, poly-3-propyl group thiophene, poly-3-butyl thiophene, poly-3-amylic thiophene, poly-3-hexyl thiophene, poly-3-heptyl thiophene, poly-3-octyl thiophene, poly-3-nonyl thiophene, poly-3.4-ethene dioxythiophene, polyphenylene thiophene; Described polyacetylene is for poly-(2,5-diheptyl) is to phenylenevinylene.
Described tensio-active agent is one or more mixing in polyoxyethylene glycol, polyvinylpyrrolidone, polyvinyl alcohol, sodium polystyrene sulfonate, Sodium dodecylbenzene sulfonate, polyacrylamide, cetyl trimethylammonium bromide, xitix.
Can the preparation method of low-temperature sintering organo-metallic conductive ink, concrete preparation flow is as follows:
(1) using alcohols as solvent, appropriate amine is added as complexing agent, at room temperature stir about 30min;
(2) appropriate silver salt is added and be stirred to precipitation in the solution obtained by step (1) and dissolve completely;
(3) by the solution 0.22um pin membrane filtration obtained by step (2), orange solution is obtained; (4) tensio-active agent, viscosity modifier are added in the solution obtained by step (3), stir, namely obtaining can low-temperature sintering organo-metallic conductive ink.
Described can low-temperature sintering organo-metallic conductive ink be orange-yellow settled solution.
Described can the silver content of low-temperature sintering organo-metallic conductive ink between 5% ~ 20%.
Described the sintering temperature of low-temperature sintering organo-metallic conductive ink can be low to moderate 90 DEG C, preferred sintering temperature is 100 DEG C ~ 140 DEG C.
Described can be printed on different base materials by common ink-jet printer by low-temperature sintering organo-metallic conductive ink, after subzero treatment can low-temperature sintering organo-metallic conductive ink can to obtain electroconductibility good, the conductive pattern that adhesive ability is strong, described base material can be glass, plastics, silicon chip, paper etc.
In order to applicable spray ink Printing, can the viscosity of low-temperature sintering organo-metallic conductive ink be 2cP ~ 20cP, preferably 5cP ~ 12cP.
The present invention compared with the existing technology, there is provided one to have good stability, low temperature sintering organo-metallic conductive ink and preparation method thereof, this conductive ink can obtain good electroconductibility at a relatively low sintering temperature, and can be printed on multiple base material, can be used for the printing of flexible electronic.
The preparation method of this conductive ink is simple, by being added by silver salt in the solution for preparing, being stirred to after dissolving completely and filtering, can obtaining, in order to be adapted to different printers, needing to carry out certain adjustment to viscosity and surface tension.
Of the present invention can low-temperature sintering organo-metallic conductive ink be settled solution, and viscosity is at 2 ~ 20cP, and silver content is 5% ~ 20%, and smell is comparatively gentle, can not produce too major injury to human body and environment, be applicable to normal domestic use printer, the circuit of preparation has good electroconductibility.
Accompanying drawing explanation
Fig. 1 is the thermal analysis curve of the conductive ink in the embodiment of the present invention 1.
Fig. 2 is the scanning electron microscope (SEM) photograph of the conductive ink in the embodiment of the present invention 1 at 90 DEG C of sintering.
Fig. 3 is the square resistance of the silverskin of conductive ink after differing temps and different time process in the embodiment of the present invention 1.
Fig. 4 is the XRD figure spectrum of the silver conductive film obtained in the embodiment of the present invention 2.
Embodiment
Embodiment 1
By even for the methanol mixed of the 2-amino-2-methyl-1-propanol of 15ml and 22.5ml, after stirring 30min, add 4g silver carbonate, continue to stir, until dissolve completely, then through 0.22um pin membrane filtration, obtain orange-yellow conductive ink.
As shown in Figure 1, as can be seen from the figure silver content is about 13% to the thermal analysis curve of gained ink.Gained ink droplet is on slide glass, and after 90 DEG C of sintering 20min, its surface topography as shown in Figure 2.Square resistance is 0.019 Ω/.The viscosity being recorded this ink by BrookfieldLV-II type rotational viscosimeter is 5.2cP.
Added by prepared ink in Epson R230 ink-cases of printers, heat-treat under differing temps different time after printing twice, the relation of its square resistance and temperature and time as shown in Figure 3.
Embodiment 2
By even for the methanol mixed of the 2-amino-2-methyl-1-propanol of 15ml and 15ml, after stirring 30min, add 4g silver carbonate, continue to stir, until dissolve completely, then through 0.22um pin membrane filtration, obtain orange-yellow conductive ink.
A small amount of tensio-active agent and viscosity modifier is added in above-mentioned ink.The viscosity being recorded this ink by BrookfieldLV-II type rotational viscosimeter is 8.3cP.Through 140 DEG C of thermal treatment 10min, square resistance is 0.035 Ω/.XRD sign is carried out to the silverskin obtained, as shown in Figure 4.
Embodiment 3
By even for the methanol mixed of the 1-amino-2-propyl alcohol of 12ml and 24ml, after stirring 30min, add 4g silver carbonate, continue to stir, until dissolve completely, then through 0.22um pin membrane filtration, obtain orange-yellow conductive ink.
A small amount of tensio-active agent and viscosity modifier is added in above-mentioned ink.The viscosity being recorded this ink by BrookfieldLV-II type rotational viscosimeter is 4cP.Through 140 DEG C of thermal treatment 10min, square resistance is 0.045 Ω/.
Claims (10)
1. one kind can low-temperature sintering organo-metallic conductive ink, it is characterized in that: comprise silver salt, solvent, complexing agent, viscosity modifier and tensio-active agent, wherein the weight percent content of silver salt is 10-25%, the weight percent content of solvent is 30-60%, the weight percent content of complexing agent is 20 ~ 40%, the weight percent content of viscosity modifier is 0.1%-5.0%, and the weight percent of tensio-active agent is 0.1% ~ 3.0%.
2. one according to claim 1 can low-temperature sintering organo-metallic conductive ink, it is characterized in that: described silver salt is that silver carbonate, Silver Nitrate, silver citrate, Silver monoacetate, neodecanoic acid silver, beta-keto acid are silver-colored, one or more mixing in 2-[2-(2-methoxyethoxy) oxyethyl group] Silver monoacetate, lauric acid silver, silver oxalate.
3. one according to claim 1 can low-temperature sintering organo-metallic conductive ink, it is characterized in that: described solvent is one or more mixing in methyl alcohol, ethanol, ethylene glycol, glycol ether, glycerol, Virahol, 1,2-PD, ethylene glycol monomethyl ether, ethylene glycol monobutyl ether, Macrogol 200, poly(oxyethylene glycol) 400, toluene.
4. one according to claim 1 can low-temperature sintering organo-metallic conductive ink, it is characterized in that: described complexing agent is ammoniacal liquor, quadrol, Isopropylamine, ammonium oxalate, hexahydroaniline, methane amide, diethylamine, triethylamine, n-Butyl Amine 99, n-octyl amine, 2-amino-2-methyl-1-propanol, thanomin, diethanolamine, trolamine, 2-(ethylamino) ethanol, 2-(dimethylamino) ethanol, 2-(diethylin) ethanol, 1-amino-2-propyl alcohol (α-amino isopropyl alcohol), ethyldiethanolamine, one or more mixing in butyl diethanolamine.
5. one according to claim 1 can low-temperature sintering organo-metallic conductive ink, it is characterized in that: described viscosity modifier is one or more mixing in Macrogol 200, Liquid Macrogol, poly(oxyethylene glycol) 400, ethylene glycol, glycerol, glycol ether, 1,2-PD, Terpineol 350; Or be conducting polymer Polythiophene or polyacetylene; Described Polythiophene is one or more mixing in poly-3 methyl thiophene, poly-3-ethylthiophene, poly-3-propyl group thiophene, poly-3-butyl thiophene, poly-3-amylic thiophene, poly-3-hexyl thiophene, poly-3-heptyl thiophene, poly-3-octyl thiophene, poly-3-nonyl thiophene, poly-3.4-ethene dioxythiophene, polyphenylene thiophene; Described polyacetylene is for poly-(2,5-diheptyl) is to phenylenevinylene.
6. one according to claim 1 can low-temperature sintering organo-metallic conductive ink, it is characterized in that: described tensio-active agent is one or more mixing in polyoxyethylene glycol, polyvinylpyrrolidone, polyvinyl alcohol, sodium polystyrene sulfonate, Sodium dodecylbenzene sulfonate, polyacrylamide, cetyl trimethylammonium bromide, xitix.
7. can the preparation method of low-temperature sintering organo-metallic conductive ink, it is characterized in that: concrete preparation flow is as follows:
(1) using alcohols as solvent, appropriate amine is added as complexing agent, at room temperature stir about 30min;
(2) appropriate silver salt is added and be stirred to precipitation in the solution obtained by step (1) and dissolve completely;
(3) by the solution 0.22um pin membrane filtration obtained by step (2), orange solution is obtained; (4) tensio-active agent, viscosity modifier are added in the solution obtained by step (3), stir, namely obtaining can low-temperature sintering organo-metallic conductive ink.
8. according to claim 7 a kind of can the preparation method of low-temperature sintering organo-metallic conductive ink, it is characterized in that: described can low-temperature sintering organo-metallic conductive ink be orange-yellow settled solution.
9. according to claim 7 a kind of can the preparation method of low-temperature sintering organo-metallic conductive ink, it is characterized in that: described can the silver content of low-temperature sintering organo-metallic conductive ink between 5% ~ 20%.
10. according to claim 7 a kind of can the preparation method of low-temperature sintering organo-metallic conductive ink, it is characterized in that: described the sintering temperature of low-temperature sintering organo-metallic conductive ink can be low to moderate 90 DEG C, preferred sintering temperature is 100 DEG C ~ 140 DEG C.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108963102A (en) * | 2017-12-29 | 2018-12-07 | 广东聚华印刷显示技术有限公司 | The preparation method of OLED device |
| CN110258137A (en) * | 2019-07-24 | 2019-09-20 | 浙江海印数码科技有限公司 | A kind of high-adaptability digit printing ink and preparation method thereof |
| CN110382637A (en) * | 2017-02-08 | 2019-10-25 | 加拿大国家研究委员会 | Printable molecular ink |
| CN111647315A (en) * | 2020-05-29 | 2020-09-11 | 东南大学 | Silver-based conductive ink and preparation method and application thereof |
| CN113223748A (en) * | 2021-05-12 | 2021-08-06 | 东南大学 | Low-temperature sintered conductive silver paste, and preparation method and application thereof |
| CN113234359A (en) * | 2021-05-26 | 2021-08-10 | 南京邮电大学 | Electronic transmission material ink for ink-jet printing and preparation method and application thereof |
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| CN102321402A (en) * | 2011-08-16 | 2012-01-18 | 天津大学 | Agranular transparent conductive ink and its preparation method |
| CN104845449A (en) * | 2015-05-08 | 2015-08-19 | 天津科技大学 | Preparation and application of RFID antenna-based inkjet conductive ink |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110382637A (en) * | 2017-02-08 | 2019-10-25 | 加拿大国家研究委员会 | Printable molecular ink |
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| CN108963102A (en) * | 2017-12-29 | 2018-12-07 | 广东聚华印刷显示技术有限公司 | The preparation method of OLED device |
| CN110258137A (en) * | 2019-07-24 | 2019-09-20 | 浙江海印数码科技有限公司 | A kind of high-adaptability digit printing ink and preparation method thereof |
| CN111647315A (en) * | 2020-05-29 | 2020-09-11 | 东南大学 | Silver-based conductive ink and preparation method and application thereof |
| CN111647315B (en) * | 2020-05-29 | 2022-06-07 | 东南大学 | Silver-based conductive ink and preparation method and application thereof |
| CN113223748A (en) * | 2021-05-12 | 2021-08-06 | 东南大学 | Low-temperature sintered conductive silver paste, and preparation method and application thereof |
| CN113234359A (en) * | 2021-05-26 | 2021-08-10 | 南京邮电大学 | Electronic transmission material ink for ink-jet printing and preparation method and application thereof |
| CN113234359B (en) * | 2021-05-26 | 2022-09-16 | 南京邮电大学 | Electronic transmission material ink for ink-jet printing and preparation method and application thereof |
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