CN101805538B - Lower-temperature sintered conductive ink - Google Patents
Lower-temperature sintered conductive ink Download PDFInfo
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- CN101805538B CN101805538B CN201010145957.7A CN201010145957A CN101805538B CN 101805538 B CN101805538 B CN 101805538B CN 201010145957 A CN201010145957 A CN 201010145957A CN 101805538 B CN101805538 B CN 101805538B
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Abstract
The invention discloses a low-temperature quickly sintered conductive ink for use in ink jet printing, which comprises 1 to 70 weight percent of nano metal particles, 0.1 to 10 weight percent of dispersant, 25 to 98 weight percent of solvent and 0.01 to 36 weight percent of additive, wherein the additive is one or a mixture of two or more of a surfactant, a reducer, a defoamer, an adhesive, a preservative and a humectants. Compared with the prior art, the low-temperature sintered conductive ink can reduce sintering temperature and keep the high conductivity of a wire. For example, at a sintering temperature of 150 DEG C, the conductive ink can make the resistance of a silver wire reach 10 to 7ohm.m. Therefore, the conductive ink can enlarge the range of substrates to which the conductive ink is applied in ink jet printing and reduce energy consumption, and has a great significance for the cost control and environmental protection of manufacturers.
Description
Technical field
The present invention relates to the conductive ink for spray ink Printing, particularly low temperature sintering conductive ink.
Background technology
Inkjet technology be a kind of contactless, without pressure, without the printing technique of forme, widespread use is at present in daily life.Inkjet technology can be applied in flexible solid substrate, for example in various films and rough base, produce electrical element etc., so for the RFID tag (RFID) that is at present high-speed development period, printed circuit board (PCB) (PCB), flexible display, the industries such as flexible solar photovoltaic cell, inkjet technology receives much concern.
With regard to board production, traditional method has the methods such as etching and silk screen printing.Etching method is a kind of comparatively traditional manufacture circuit card or the method with the electronic circuit of certain flexibility, the operation that its etching subtracts needs a large amount of water for cleaning and solvent, seriously polluted, and material use efficiency is very low, has caused waste of raw materials and cost to rise; In addition, etching method complex procedures, energy consumption is many.Compared with etching method, the advantage of silk screen print method is that its input to production unit is lower, and material use efficiency is also relatively high, but silk screen print method still needs pallet in advance, and cannot avoid the waste of slurry; In addition, silk screen print method still belongs to contact processing, and printing quality is relevant with several factors, and quality product is more difficult control often.Ink-jet printing process belongs to contactless working method, is conductive particle to be scattered in to solvent form electrically conductive ink, utilizes computer control, by printing type, electrically conductive ink is accurately deposited to the needed position of substrate.From technique, ink-jet printing process is particluarly suitable for manufacturing in flexible substrates electron device; From material, it can accomplish the almost utilization ratio of zero waste of raw metal; From the angle of environmental protection, it has avoided the desired a large amount of operations of etch process, thereby reduces discharge, reduces energy consumption.So ink-jet printing process is to realize the Perfected process that flexible substrates electronic circuit is manufactured.
The key of ink-jet printing process is the preparation of various functional inks, and wherein conductive dispersions is ink-jet printing ink, i.e. the preparation of conductive ink, especially basis wherein.The essence of conductive ink is the dispersion system of conductive particle, and common conductive particle has conductive polymer material, graphite-like, pottery and metal etc.Wherein, conductive polymer material, graphite-like, the general conductivity of ceramic conductive particle are poor, are not suitable for use in conducting wire.Metallic conduction particle has gold and silver, copper etc. to be commonly used for the metal of conductor, metal and their alloys such as iron, nickel, aluminium, zinc, lead.At present, more to the research of simple substance silver particle ink, stronger because simple substance silver has unreactiveness, be difficult for oxidized feature, when considering conductivity, production and transport cost, use cost, the cost performance of silver-colored ink is higher.In addition, the research of elemental copper particle ink is also had to relevant report, still, the chemical property of copper is comparatively active, is difficult for preparation and uses, also higher to the requirement of equipment, thereby has increased the complexity of application cost and whole system.
The performance index of conductive ink are mainly: 1) electric conductivity: the ink that contains conductive particle generally will be through the process of solvent evaporates and sintering after depositing to substrate with inkjet printing methods, form continuous electrical conductor, owing to having inevitable impurity and space, and larger resistance between particle, its electric conductivity is not as good as pure metal conductor; 2) printability: the droplet volume ejecting during spray ink Printing generally below tens of skins rise, so require conductive ink to there is good mobility and continuity, with the effect that guarantees to print; The characterization parameter of printability generally has stability, viscosity, surface tension, rate of drying, granular size and solids content etc.; 3) sintering characteristic: conductive ink needs through heat treated after printing to remove or to reduce the content of solvent and other non-conductive additives, sinters low-melting-point nano metallic particles into continuous solid body simultaneously; Sintering temperature, heat-up time and whether to need special gas environment etc. be the index of weighing sintering characteristic.
In general, improve the electric conductivity that sintering temperature can improve remaining solid metal after sintering to a certain extent, because temperature is higher, the speed of the decomposition such as most of additive and solvent and volatilization is faster, and the resistance producing due to defect between metal nanoparticle is also less.But at high temperature all easily there is qualitative change in most of flexible base materials, the variation that too high sintering temperature may make base material produce shape, color, snappiness etc., thus production and use are impacted.Therefore; conductive ink at a lower temperature sintering also can obtain good electroconductibility; can greatly improve conductive ink in all kinds of suprabasil universalities, reduce energy consumption simultaneously, for cost control and the protection of bad border of manufacturing enterprise, have very important meaning.
Chinese invention patent application prospectus CN101010388A discloses a kind of conductive ink, and its main component is metal complex, and sintering temperature needs 200 ℃, still higher; In addition, the character of complex compound has limited the speed that resolves into metal simple-substance, needs the calcination time of growing.Chinese invention patent application prospectus CN101448904A discloses a kind of inkjet ink composition that contains high molecular weight linear, the satellite droplet forming in the time of can reducing spray ink Printing, but this patent does not relate to sintering process and the sintering temperature of electrically conductive ink.Chinese invention patent application prospectus CN1671805A discloses a kind of electrical-conductive nanometer metal ink preparation method who needs sintering temperature and low, but, electrical-conductive nanometer metal ink prepared by the method is applicable to coating process complete processing, is not the conductive ink in inkjet technology.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of low temperature sintering conductive ink for the deficiencies in the prior art.
The present invention solves the problems of the technologies described above adopted technical scheme: low temperature sintering conductive ink, by weight percentage, comprises following component:
Nano-metal particle 1%～70%;
Dispersion agent 0.1%～10%;
Solvent 25%～98%;
Additive 0.01%～36%;
Wherein, additive is the one or more kinds of combinations in tensio-active agent, reductive agent, defoamer, tackiness agent, sanitas, wetting Agent for Printing Inks.
For optimizing technique scheme, the measure of taking also comprises:
Above-mentioned additive comprises following component:
Tensio-active agent 0.1～10%;
Reductive agent 0.01%～10%;
Defoamer 0.01%～1%;
Tackiness agent 0.01%～5%;
Sanitas 0.01%～5%;
Wetting Agent for Printing Inks 0.01%～5%;
Above-mentioned nano-metal particle is a kind of or two or more compositions in gold and silver, copper, iron, nickel, aluminium, zinc, lead; The size of above-mentioned nano-metal particle is 1nm～200nm;
Above-mentioned dispersion agent is the composition of micromolecular compound, macromolecular compound or described micromolecular compound and described macromolecular compound; Described micromolecular compound and described macromolecular compound are containing a kind of element in aerobic, nitrogen phosphate and sulfur element or two or more elements;
Above-mentioned micromolecular compound is alkyl sulfhydryl, alkyl acid, alkylamine, alkylphosphonic acid carboxylic acid or the micromolecular compound containing ring texture; Above-mentioned macromolecular compound is polyvinyl alcohol, polyoxyethylene glycol, polyvinylpyrrolidone, polymethyl acrylic acid, polymeric amide, polyaniline, polyethers, urethane, gelatin or Sudan Gum-arabic;
Compared with prior art, low temperature sintering conductive ink of the present invention can keep the conductivity that wire is good when reducing sintering temperature, for example, under the sintering temperature of 150 ℃, can make the resistivity of silver-colored wire reach 10
-7Ω m, thereby can improve the substrate scope of conductive ink application in inkjet technology, reduce energy consumption simultaneously, for cost control and the environment protection of manufacturing enterprise, there is very important meaning.Can greatly improve conductive ink exists
Accompanying drawing explanation
Fig. 1 is the SEM picture that the present invention can low-temperature sintering conductive ink conductive particle before sintering;
Fig. 2 be the present invention can low-temperature sintering conductive ink at the SEM picture of 150 ℃ of sintering conductive particle after 30 minutes.
Embodiment
Below in conjunction with accompanying drawing, embodiment is described in further detail the present invention.
Fig. 1 and Fig. 2 are that the present invention can the effect schematic diagram of low-temperature sintering conductive ink before and after sintering.
By weight percentage, low temperature sintering conductive ink of the present invention comprises following component: 1%～70% nano-metal particle, 0.1%～10% dispersion agent, 25%～98% solvent additive and 0.01%～36% additive; Wherein, additive is the one or more kinds of combinations in tensio-active agent, reductive agent, defoamer, tackiness agent, sanitas, wetting Agent for Printing Inks.
A kind of optimum combination mode of additive is: comprise 0.1～10% tensio-active agent, 0.01%～10% reductive agent, 0.01%～1% defoamer, 0.01%～5% tackiness agent, 0.01%～5% sanitas and 0.01%～5% wetting Agent for Printing Inks.
Nano-metal particle is that gold and silver, copper etc. are commonly used for metal and their alloys such as the metal of conductor and iron, nickel, aluminium, zinc, lead.Nano-metal particle can be sheet, and needle-like is spherical, approximate spherical, flakey, dendroid or other arbitrary shapes and their combination.Nano-metal particle can be monocrystalline, polycrystalline or amorphous.Nano-metal particle is of a size of between 1nm～200nm, is preferably 10nm～100nm.The method of preparing nano-metal particle is not specifically limited, and can be vapor phase process, liquid phase method, and mechanical process and other methods for the preparation of nanometer powder or colloidal sol are prepared nano-metal particle.Nano-metal particle can or cause particle surface or inner impure with other form doped with non-metals elements by surface oxidation, sulfuration.Impure can being removed by subsequent technique that these are caused by non-metallic element, also can retain, but does not substantially affect the electric conductivity of the conductor of final formation.
The effect of dispersion agent be make nano-metal particle can be in solvent stable dispersion.Dispersion agent is micromolecular compound, macromolecular compound or their combination containing one or more elements in the elements such as aerobic, nitrogen phosphate and sulfur.Micromolecular compound dispersion agent can be selected but be not limited to alkyl sulfhydryl, alkyl acid, alkylamine, alkylphosphonic acid carboxylic acid, for example, containing the micromolecular compound of ring texture and their ionic compound, an alkali metal salt and halogenide.Macromolecular compound dispersion agent is the macromolecular compound containing with element groups such as oxygen, sulphur, phosphorus, nitrogen, can select but be not limited to polyvinyl alcohol, polyoxyethylene glycol, polyvinylpyrrolidone, polymethyl acrylic acid, polymeric amide, polyaniline, polyethers, urethane, gelatin, Sudan Gum-arabic etc.The molecular weight of macromolecule dispersing agent is 3000 to 1,000 ten thousand, preferably 3000 to 1,000,000.Dispersion agent can add in metal nanoparticle preparation process, also can in the building-up process of conductive ink, add.
In order to make conductive ink Fast Sintering at low temperatures, the consumption of dispersion agent can not be too high, otherwise its degradation speed will be affected.The usage quantity of dispersion agent determines the dispersion efficiency of metal nanoparticle by this dispersion agent, and for different metal nanoparticles, the dispersion agent using is also different.In dispersion agent used in the present invention, contain the group with metal nanoparticle with the atom of strong complex ability, therefore the usage quantity of dispersion agent can reduce.For example, silver nano-grain is used the macromolecule dispersing agent of nitrogen-containing group, and gold nano grain is used the macromolecule dispersing agent of sulfur-containing group.
Solvent can be water and organic solvent.Organic solvent can be selected but be not limited to ethanol, 1-propyl alcohol, n-butyl alcohol, 1-amylalcohol, 1-hexanol, hexalin, 1-heptanol, R-GLYCIDOL, benzylalcohol, methyl-cyclohexanol, 2-methyl-1-butene alcohol, 3-methyl-2-butanols, 4-methyl-2-amylalcohol, Virahol, 2-ethyl butanol, 2-Ethylhexyl Alcohol, sec-n-octyl alcohol, terpinol, dihydro-terpineol, 2-methyl cellosolve, cellosolvo, 2-n-butoxy ethanol, 2-phenoxyethyl alcohol, Trivalin SF, ethyl carbitol, normal-butyl Trivalin SF, diacetone alcohol, heptane, octane, nonane, decane, undecane, dodecane, tridecane, the tetradecane, pentadecane, n-Hexadecane, pyrroles, N-Methyl pyrrolidone, chloroform, benzene, toluene, one or more among dimethylbenzene etc. are through the mixed solvent of proportioning.
Tensio-active agent, can be identical with dispersion agent for reducing the surface tension of ink, can be also other tensio-active agent.Tensio-active agent can be non-ionic type, cationic, anionic and amphoteric ion type.Tensio-active agent can be selected but be not limited to stearic acid, oleic acid, lauric acid, Sodium dodecylbenzene sulfonate, trolamine, sodium laurylsulfate, sodium laurylsulfonate, quaternary ammonium compound, hydroxypropylcellulose, sodiun alginate, pectic acid sodium, Walocel MT 20.000PV, carboxymethyl starch, methacrylic acid graft starch, the poly-acid of shell, vinylpyridine copolymer, polysiloxane, polyvinyl ether, polyvinyl alcohol, polyacrylamide, polymine, maleic acid and polyoxyethylene, polymine, polyoxypropylene, the segmented copolymer of polyoxy butylene or polystyrene etc.
Reductive agent is not oxidized for the protection of the nano-metal particle of conductive ink in production, transportation and use procedure, to guarantee the electric conductivity of the finished product.Reductive agent can be selected but be not limited to sodium borohydride, sodium hypophosphite, xitix, S-WAT, hydrazine hydrate, formic acid, oxalic acid, methyl sodium hydrosulfite, formaldehyde, zinc powder or iron powder etc.
Defoamer is for eliminating the bubble that conductive ink in use produces, can select but be not limited to polysiloxane, polyethers, silicone emulsion, higher alcohols, tributyl phosphate, the fatty acid ester compounded thing of higher alcohols, polyoxypropylene, organic silicon modified by polyether and commercialization defoamer, as BYK series etc.
Tackiness agent is for improving the sticking power between wire and the substrate forming after conductive ink sintering.Tackiness agent can be selected but be not limited to resol, epoxy resin, Vinyl Acetate Copolymer, polyvinyl acetate, polyacrylic ester, chloroprene rubber, styrene-butadiene rubber(SBR), silicon rubber, starch, shellac etc.
Sanitas is for keeping conductive ink performance stable after long-time preservation.Sanitas can be selected but be not limited to Sodium Benzoate, potassium sorbate, dehydroacetic acid (DHA), Sodium dehydroacetate, parabens, sodium Diacetate, calcium propionate, Sodium.alpha.-hydroxypropionate, tennecetin, hydrogen peroxide etc.
Wetting Agent for Printing Inks is for controlling conductive ink rate of drying in use, to guarantee the better mobility of conductive ink and continuity.Wetting Agent for Printing Inks can be selected but be not limited to propylene glycol, glycerine, sorbyl alcohol, glycerol, polyoxyethylene glycol, hexylene glycol, Xylitol, polypropylene glycol etc.
Be below the synthetic specific embodiment of low temperature sintering conductive ink of the present invention, the present invention is suitable for but is not limited to these embodiment.In each embodiment, umber and percentage ratio are by weight.
Embodiment 1:
By the ball shape silver powder of 10 parts, particle diameter is 50～80 nanometers, be dispersed in the Virahol of 70 parts, and the polyoxyethylene glycol that the molecular weight that then adds 10 parts is 10000, by gained solution, with ultrasonic dispersion after 30 minutes, centrifugal 10 minutes of 3000rpm, then filters; After filtration, in solution, add the glycerol of 5 parts as wetting Agent for Printing Inks, the polysiloxane of 1 part is as defoamer, and the epoxy resin of 2 parts is as tackiness agent, and the potassium sorbate of 2 parts is as sanitas, under 200rpm, stir 30 minutes, obtain low temperature sintering conductive ink.
The above-mentioned conductive ink that takes a morsel is dried after 1 hour and is used field emission scanning electron microscope (SEM) to observe at 100 ℃, as shown in Figure 1, can see that the metallic particles in this conductive ink is discrete shape distribution.
The above-mentioned conductive ink preparing for example, is printed as to pre-fabricated patterns by ink-jet printer (Epson ME1 ink-jet printer) on paper, and sintering obtained sintered product after 30 minutes at 150 ℃, use SEM to observe this sintered product, as shown in Figure 2, can find out that the silver-colored particle in this conductive ink has sintered conductive silver wire into.The resistivity of using four probe method to record this silver wire is 10
-7Ω m.
Embodiment 2:
20 parts of Silver Nitrates are dissolved in 50 parts of water, add the polyoxyethylene glycol that 10 parts of molecular weight are 100000,500rpm stirs heating in water bath to 50 ℃ after 60 minutes to be continued to stir and drip 10 part of 50% sodium borohydride as reductive agent, drip rear lasting stirring 30 minutes, then 3000rpm filters after centrifugal 30 minutes; After filtration, gained solution is carried out to electrodialysis 20 minutes, add again the glycerol of 5 parts as wetting Agent for Printing Inks, the polysiloxane of 1 part is as defoamer, the stearic acid of 1 part is as tensio-active agent, the epoxy resin of 2 parts is as tackiness agent, the potassium sorbate of 1 part is as sanitas, and then 200rpm stirs 30 minutes, obtains low temperature sintering conductive ink.
By above-mentioned, can by self-control ink-jet apparatus, on paper, be printed as pre-fabricated patterns by low-temperature sintering conductive ink, and sintering obtained sintered product after 30 minutes at 150 ℃, use SEM to observe this sintered product, as shown in Figure 2, can find out that the silver-colored particle in this conductive ink has sintered conductive silver wire into.The resistivity of using four probe method to record this silver wire is 10
-7Ω m.
Embodiment 3:
25 parts of Silver Nitrates are dissolved in 50 parts of water, add the polymethyl acrylic acid that 10 parts of molecular weight are 200000,500rpm stirs after 60 minutes and adds 2 parts of polysiloxane as defoamer, 1000rpm stirs, add again 10 part of 50% hydrazine hydrate as reductive agent, continue to stir 10 minutes, then 3000rpm filters after centrifugal 30 minutes; After filtration, in gained solution, add 3 parts of glycerol as wetting Agent for Printing Inks, 1 part of potassium sorbate is as sanitas, and 200rpm stirred after 30 minutes, obtained low temperature sintering conductive ink.
Above-mentioned low temperature sintering conductive ink is printed as to pre-fabricated patterns on paper by home-built equipment, and sintering obtained sintered product after 30 minutes at 130 ℃, use SEM to observe this sintered product, result is similar to Figure 2, can find out that the silver-colored particle in this conductive ink has sintered conductive silver wire into, obtain conductive silver wire, the resistivity of using four probe method to record this silver wire is 10
-6Ω m.
Embodiment 4:
30 parts of Silver Nitrates are dissolved in 50 parts of water, add the polymethyl acrylic acid that 10 parts of molecular weight are 200000,500rpm stirs after 60 minutes and adds 1 part of polysiloxane as defoamer, 1000rpm stirs, add again 7 part of 50% hydrazine hydrate as reductive agent, continue to stir 10 minutes, then 3000rpm filters for centrifugal 30 minutes; After filtration, in gained solution, add 1 part of glycerol as wetting Agent for Printing Inks, 1 part of potassium sorbate is as sanitas, and 200rpm stirred after 30 minutes, obtained low temperature sintering conductive ink.
Above-mentioned ink is printed as to pre-fabricated patterns by ink-jet printer Epson ME1 on paper, and sintering obtained sintered product after 30 minutes at 140 ℃, use SEM to observe this sintered product, result is similar to Figure 2, can find out that the silver-colored particle in this conductive ink has sintered conductive silver wire into, obtain conductive silver wire, the resistivity of using four probe method to record this silver wire is 5 × 10
-7Ω m.
Embodiment 5:
Other condition is with embodiment 1, and difference is that the ball shape silver powder in embodiment 1 is got to 50 parts, is dispersed in the Virahol of 30 parts, the polyoxyethylene glycol that the molecular weight that adds 10 parts is 10000, by gained solution, with ultrasonic dispersion after 60 minutes, centrifugal 10 minutes of 3000rpm, then filters; After filtration, in solution, add the glycerol of 5 parts as wetting Agent for Printing Inks, the polysiloxane of 1 part is as defoamer, and the epoxy resin of 2 parts is as tackiness agent, and the potassium sorbate of 2 parts is as sanitas, under 200rpm, stir 30 minutes, obtain low temperature sintering conductive ink.
The above-mentioned conductive ink that takes a morsel is dried after 1 hour and is used SEM to observe at 100 ℃, as shown in Figure 1, can see that the metallic particles in this conductive ink is discrete shape distribution.
The above-mentioned conductive ink preparing for example, is printed as to pre-fabricated patterns by ink-jet printer (Epson ME1 ink-jet printer) on paper, and sintering obtained sintered product after 30 minutes at 150 ℃, use SEM to observe this sintered product, similar to Figure 2, the silver-colored particle in conductive ink has sintered conductive silver wire into.The resistivity of using four probe method to record this silver wire is 10
-7Ω m.
Most preferred embodiment of the present invention is illustrated, and the various variations of being made by those of ordinary skills or remodeling can not depart from the scope of the present invention.
Claims (2)
1. low temperature sintering conductive ink, in parts by weight, is comprised of following component:
2. low temperature sintering conductive ink, in parts by weight, is comprised of following component:
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