CN101560349A - Jet conductive ink - Google Patents
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- CN101560349A CN101560349A CN 200910082080 CN200910082080A CN101560349A CN 101560349 A CN101560349 A CN 101560349A CN 200910082080 CN200910082080 CN 200910082080 CN 200910082080 A CN200910082080 A CN 200910082080A CN 101560349 A CN101560349 A CN 101560349A
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Abstract
The invention relates to jet conductive ink, which is film printing electronic paste and is suitable for ink jet printing, and belongs to the field of printed electronics. The jet conductive ink comprises the following components in portion by weight: 1 to 29 portions of conductive particles, 60 to 85 portions of solvent, 1 to 5 portions of humectant, 1 to 5 portions of pH regulator, 1 to 5 portions of surfactant, and 1 to 3 portions of bonding material. The cost of a method for the jet conductive ink is low, and the conductive silver in the conductive paste is reduced to less than 29 portions by weight; the method has a mild post treatment process, and the post treatment temperature of a printed product is reduced to about 100 DEG C by using nano silver to replace micro silver; and through an ink jet printing mode as required, the thickness of an obtained conductive film is about 1 micron, and the resistance reaches about 1 ohm.
Description
Technical field
The present invention relates to a kind of jet conductive ink.Jet conductive ink of the present invention contains granular conducting material, and performances such as its viscosity, pH value, surface tension all are applicable to spray ink Printing.This conductive ink belongs to the film printing electric slurry, is applied to print electronic applications.
Background technology
Follow the progress of digitizing printing technology, the ink jet printing in the non-impact printing has obtained to develop rapidly, and its Application Areas day by day enlarges.Simultaneously, the development of printing electronic material and technology provides chance also for the combination of printed-wiring board (PWB) (PCB) preparation, flexible show electrode and electromagnetic shielding material and printing technology.In order to reduce the cost of conducting wire and even less radio-frequency (RFID) antenna transmitting antenna, the precious metal consumption that solves the traditional technology existence to a certain extent is big, problems such as treating processes contaminate environment.Need that conductivity is good, the printing rete is thin, industrialization film printing ink easily.
Jet conductive ink belongs to the film printing electronic material, at aspects such as traditional circuit printing, the printing of flexible display circuit and solar-energy photo-voltaic cells, potential use is widely arranged all.At present, actual application prospect and the closest with people's relation of living is arranged most, will be low-costly and in high volume, the making of many kinds RFID antenna.RFID label by printed electronics is made can apply to from food to the medicine, from electrical equipment to the automobile etc. on the various intelligent packagings.
Generally speaking, the solid content of conducting metal is more than 60% in the thick film conductor paste, and granularity by silk screen printing, through Temperature Treatment more than 400 ℃, obtains satisfactory conductive layer afterwards afterwards about 10 microns.Existing problems are, and are big as the noble metal dosage of electro-conductive material on the one hand, the cost height; On the other hand, printing postheat treatment temperature height, the printing element range of choice is narrow.
In order to reduce cost, reduce post-processing temperature, enlarge the printing material range of choice, so that can select to be beneficial to the stock of natural degradation, use non-toxic organic solvent class material as far as possible,, need the exploitation bullion content low based on water, be convenient to printing, be convenient to than the ink jet printing conductive ink that obtains electroconductibility after handling under the lesser temps.
Common ink for ink-jet print, pigment or dyestuff solid content about 5%, easy stable existence.Metallic particles is being applicable under the low viscosity condition of spray ink Printing the stable suspersion difficulty than great.Particularly in order to satisfy the electroconductibility needs, the ratio of metallic particles in ink will acquire a certain degree, and the stable suspersion of this moment is just more difficult.As printed-wiring board (PWB) or RFID transmitting antenna, also must satisfy certain lines accuracy requirement.Simultaneously, ink also must be able to be stablized smoothly the minute aperture by ink gun, and these all need the granularity of solids component in the ink to want little of to a certain degree.
Water base ink for ink-jet print is made of component shown in the following form
Table 1 water-based ink component
Constitute each component ratio of ink, need to make the ink of formation have certain printability through optimizing.
Application number is 200710079807.9 patent of invention, relate to a kind of conductive ink composition that is used for spray ink Printing, more particularly, relate to the conductive ink composition that is used for spray ink Printing, it comprises: the metal nanoparticle of 30～85 weight parts, the solvent of 10～60 weight parts, the wetting agent of 10～30 weight parts, this wetting agent is by making based on the compound of glycol or polyvalent alcohol, and the ether compound additive based on glycol that is used to regulate viscosity of 0.1～10 weight part.This invention shortcoming is that the solid content of metal nanoparticle is still higher, and concrete printing effect data are not provided.
Therefore, the solid content of developing a kind of metal nanoparticle is lower, is fit to the high precision spray ink Printing, and the jet conductive ink of good conductivity becomes the difficult problem that solution is badly in need of in the present technique field.
Summary of the invention
One of purpose of the present invention is a kind of electro-conductive material ink for ink-jet print with certain metal solid content of exploitation, this ink is applicable to the high precision spray ink Printing that the printing electronics needs, through after the constituent optimization, the printability of this ink, satisfy ink-jet printer and normally print requirement, this ink is by spray ink Printing, and the thermal treatment through about 100 ℃ can access reasonable electroconductibility.
The objective of the invention is to reach by the following technical programs:
A kind of jet conductive ink, its composition comprises:
The conductive particle of 1～29 weight part;
The solvent of 60～85 weight parts;
The wetting Agent for Printing Inks of 1～5 weight part;
The pH regulator agent of 1～5 weight part;
The tensio-active agent of 1～5 weight part;
The connection material of 1～3 weight part.
A kind of optimized technical scheme is characterized in that: described jet conductive ink also comprises the sanitas of 0.2～2 weight part, and sanitas is common ink for ink-jet print compounds such as phenylcarbinol class commonly used.
A kind of optimized technical scheme is characterized in that: described conductive particle is metal simple-substance or alloy, as is selected from a kind of in gold (Au), silver (Ag), copper (Cu), iron (Fe), tin (Sn), aluminium (Al) etc. or its alloy.The particle size distribution of conductive particle is 10～400nm, and 20～200nm is advisable, and it is better to be controlled at 50～100nm.The electroconductibility of metal simple-substance, particularly argent is better.
A kind of optimized technical scheme is characterized in that: described conductive particle uses inorganic salt compound, for example Sodium hexametaphosphate 99; Also can be various polymkeric substance, polyvinylpyrrolidone (PVP) for example, polyamine compound, polyoxyethylene glycol, natural high moleculer eompound gelatin, Sudan Gum-arabic; The compositing conducting macromolecular compound, for example Polythiophene compound etc. coats as dispersion agent, can use separately, also can compositely use, as the dispersion stabilizer of conductive particle in polar solvent.
A kind of optimized technical scheme is characterized in that: described conductive particle is the silver nano-grain that is coated by polyvinylpyrrolidone, and granularity is 50～150nm.
A kind of optimized technical scheme is characterized in that: described solvent is a polar solvent, as small molecular alcohol compounds such as water, ethanol, Virahol, butanols, and ethylene glycol monobutyl ether, ether compounds such as ethylene glycol monoemethyl ether use separately or composite use;
A kind of optimized technical scheme is characterized in that: described wetting Agent for Printing Inks comprises a kind of independent use or the multiple composite use in the polyol compounds such as triglycol, ethylene glycol, propylene glycol, glycerol.
A kind of optimized technical scheme is characterized in that: described pH regulator agent is a sodium phosphate.
A kind of optimized technical scheme is characterized in that: described tensio-active agent is polyethenoxy ether class nonionogenic tenside, for example ET-135.
A kind of optimized technical scheme is characterized in that: described connection material is polymkeric substance such as PVB, PVA.
The invention provides a kind of spray ink Printing conductive ink, by certain way, generate the also nano-scale metal particles of stable existence in polar solvent, this particle has and corresponding to printability of ink-jet printer requirement and physical and chemical performance in stable suspension.
When select using some special metal particle for example silvery being made ink,, can not add or few adding preservative agent because nanometer silver has certain kill bacteria effect.
Beneficial effect
1, the present invention has gentle aftertreatment technology, replaces micron silver with nanometer silver, and the printed matter post-processing temperature is reduced to about 100 ℃;
2, cost of the present invention is low, and the conductive silver particle weight part in the electrocondution slurry is reduced to below 29, is lower than expensive that common electrocondution slurry 50～70% solid contents cause;
3, the present invention prepares the nanometer silver slurry by chemical process, adds dispersion agent, stablizer of suitable molecular weight and quantity etc., and the weight part that makes the conductive particle thing is 1～29; Through after the constituent optimization, the printability of this ink satisfies ink-jet printer and normally prints requirement, is applicable to the high precision spray ink Printing that the printing electronics needs; By the drop on demand ink jet mode of printing, obtain conducting film thickness about 1 micron, resistance reaches about 1 ohm.
The present invention will be further described below in conjunction with the drawings and specific embodiments, but and do not mean that limiting the scope of the invention.
Description of drawings
Fig. 1-a and Fig. 1-b are respectively nanometer silver UV, visible light absorption curve and distribution of particle sizes test result.
Fig. 2 is for printing the circuit specimen page.
Fig. 3 is that different experiments example nano silver conductive ink is printed the specimen page scanning electron microscope image.
Fig. 4 is a sem photograph before and after the sodium rice silver conductive ink spray ink Printing conductive layer low-temperature heat treatment.
Embodiment
Generally speaking, the physical and chemical performance of ink-jet printing ink must satisfy following condition, can adapt to ink-jet printer and normally print requirement:
The typical performance index of table 2 ink jet ink for printing
The present invention prepares the hydrazine hydrate solution and the silver nitrate solution of 0.1～6.25mol/L different concns; Under the protection of PVP, the reductive agent hydrazine hydrate under suitable stirring velocity, is added dropwise in the silver nitrate aqueous solution, change reactant ratio, can make solid content is that 1～30 weight part, granularity are the nanometer silver emulsion of the different silver contents of 10～400nm.
The nanometer silver emulsion that experiment makes adds 1～5 wetting Agent for Printing Inks, 1～5 pH regulator agent, and 1～5 tensio-active agent, 1～3 connection material stirred about 30 minutes, mixed; Making parameters reach the requirement that machine is printed, is the micro-filtrate membrane filtration of 0.2～1.2 μ m by the aperture, guarantees that silver-colored particle can pass through ink gun smoothly, obtain can computer experiment jet conductive ink.
Embodiment 1 preparation nanometer silver emulsion jet conductive ink
Concrete enforcement of the present invention, by reference " preparation of nano-silver conductive film and spectroscopy analysis thereof " (Mo Lixin, Li Luhai, Li Yaling etc., spectroscopy and spectroscopic analysis 2007.12, P2502) method prepares the silver-colored particle suspension liquid of granularity in 20～400nm scope, selects polyvinylpyrrolidone (PVP) as dispersion stabilizer.
Get silver nitrate solution and hydrazine hydrate solution that equal-volume concentration is all 0.25mol/L, get PVP/ Silver Nitrate (mass ratio)=1.75, making ink jet ink nano silver solid content is 1.2%, is of a size of 50～100nm;
In the nano-silver conductive grain emulsion that obtains, add wetting Agent for Printing Inks, pH regulator agent, tensio-active agent, connection material according to weight part, stirred 30 minutes, mix; Is the micro-filtrate membrane filtration of 0.2～1.2 μ m with the mixed solution of gained by the aperture, obtains jet conductive ink, and its composition sees Table 3.
Using EPSON ME1+ type printer, is print media with U.S. good (BeiJing, China Linkage good skill video new material technology company limited product) the clearance type ink-jet printing paper of planting, and prints the specimen page experiment.Duplicate printing three times obtain specimen page.The specimen page of duplicate printing three times at 120 ℃ of sintering 10min, is obtained the specimen page after the thermal treatment, use the digital multimeter test resistance.
Embodiment 2 preparation nanometer silver emulsion jet conductive inks
Get silver nitrate solution and hydrazine hydrate solution that equal-volume concentration is all 0.75mol/L, get PVP/ Silver Nitrate (mass ratio)=2, making ink jet ink nano silver solid content is 3.6%.Be of a size of 70～120nm.Preparation process is with embodiment 1, and the composition that obtains jet conductive ink sees Table 3.
Embodiment 3 preparation nanometer silver emulsion jet conductive inks
Get silver nitrate solution and hydrazine hydrate solution that equal-volume concentration is all 2.25mol/L, get PVP/ Silver Nitrate (mass ratio)=4, making ink jet ink nano silver solid content is 10.9%.Be of a size of 100～150nm; Preparation process is with embodiment 1, and the composition that obtains jet conductive ink sees Table 3.
Embodiment 4 preparation nanometer silver emulsion jet conductive inks
Get silver nitrate solution and hydrazine hydrate solution that equal-volume concentration is all 6.25mol/L, get PVP/ Silver Nitrate (mass ratio)=4, making ink jet ink nano silver solid content is 29%.Be of a size of 100～150nm; Preparation process is with embodiment 1, and the composition that obtains jet conductive ink sees Table 3.
The composition (weight part) of the resultant jet conductive ink of table 3 embodiment 1-4
Described jet conductive ink can also add the sanitas of 0.2～2 weight part, and sanitas is a common ink for ink-jet print phenylcarbinol compounds commonly used.
Can be with reference to method for preparing metal simple-substance or alloy nano particle emulsion as gold (Au), silver (Ag), copper (Cu), iron (Fe), tin (Sn), aluminium (Al) etc. or its alloy, add wetting Agent for Printing Inks, pH regulator agent, tensio-active agent, connection material according to weight part, after stirring, filtering, obtain jet conductive ink.
Test result:
By the uv-vis spectra test, confirm that synthetic silver particle is a nanoscale particle, Fig. 1-a and Fig. 1-b are respectively nanometer silver UV, visible light absorption curve and distribution of particle sizes test result.
Through the ink that preparation obtains, printing effect is good, and Fig. 2 is for printing the circuit specimen page.
By scanning electron microscope, studied the structure that different printing times obtain printing conductive layer, referring to Fig. 3, for different embodiment nano silver conductive inks are printed specimen page scanning electron microscope image (500 *), left side figure is that embodiment 1 prints, and middle figure is that embodiment 2 prints, and right figure is that embodiment 3 prints.
Through the conductive layer after the low-temperature heat processing, conductive effect is good, and the Electronic Speculum effect before and after handling is obviously different, and after Overheating Treatment, metallic particles connects; Well, referring to Fig. 4, for sodium rice silver conductive ink spray ink Printing conductive layer low-temperature heat treatment is handled front and back sem photograph (500 *), before left side figure is sintering, after right figure is sintering.
The ink for ink-jet print that the different embodiment of table 4 obtain is printed circuit conductive effect contrast table
| Sequence number | Nanometer silver (weight part) | Line resistance after printing (Ω/cm) | Line resistance after 120 ℃ of processing (Ω/cm) |
| Embodiment 1 | 1.2 | 1000 | 26 |
| Embodiment 2 | 3.6 | 856 | 15 |
| Embodiment 3 | 10.9 | 40 | 1.4 |
| Embodiment 4 | 29 | 35 | 0.5 |
Claims (9)
1, a kind of jet conductive ink, its composition comprises (weight part):
1～29 conductive particle;
60～85 solvent;
1～5 wetting Agent for Printing Inks;
1～5 pH regulator agent;
1～5 tensio-active agent;
1～3 connection material.
2, jet conductive ink according to claim 1 is characterized in that: described jet conductive ink also comprises the sanitas of 0.2～2 weight part, and sanitas is a common ink for ink-jet print phenylcarbinol compounds commonly used.
3, jet conductive ink according to claim 1, it is characterized in that: described conductive particle is for being selected from a kind of in gold (Au), silver (Ag), copper (Cu), iron (Fe), tin (Sn), aluminium (Al) or its alloy, and the granularity of conductive particle is 10～400nm.
4, jet conductive ink according to claim 1 is characterized in that: one or more in described conductive particle use Sodium hexametaphosphate 99, polyvinylpyrrolidone, polyamine compound, polyoxyethylene glycol, gelatin, Sudan Gum-arabic, the Polythiophene compound coat as dispersion agent.
5, jet conductive ink according to claim 1 is characterized in that: described conductive particle is the silver nano-grain that is coated by polyvinylpyrrolidone, and granularity is 50～150nm.
6, jet conductive ink according to claim 1 is characterized in that: described solvent is to be selected from water, ethanol, Virahol, butanols, ethylene glycol monobutyl ether, the ethylene glycol monoemethyl ether one or more.
7, jet conductive ink according to claim 1 is characterized in that: described wetting Agent for Printing Inks is to be selected from triglycol, ethylene glycol, propylene glycol, the glycerol one or more.
8, jet conductive ink according to claim 1 is characterized in that: described pH regulator agent is a sodium phosphate; Described tensio-active agent is the polyethenoxy ether class nonionogenic tenside; Described connection material is PVB.
9, jet conductive ink according to claim 8 is characterized in that: described polyethenoxy ether class nonionogenic tenside is ET-135.
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