CN102220045A - Low-temperature-sintered solvent-based nano-silver electroconductive ink and preparation process thereof - Google Patents
Low-temperature-sintered solvent-based nano-silver electroconductive ink and preparation process thereof Download PDFInfo
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Abstract
The present invention discloses electroconductive ink used for printing electronics and a preparation process thereof. The preparation process comprises the specific steps: sufficiently dissolving a silver salt, a complexing agent, a stabilizer and a protective agent in a solvent, gradually heating to 20-70 DEG C, adding a reducing agent to the reaction system after the temperature is stable, persistently stirring to react for 10-30 minutes and gradually cooling; precipitating by adjusting the pH value and/or adding a polar solvent after cooling; stirring, centrifuging or vacuum-filtering, and washing in sequence with ethanol or deionized water and acetone for multiple times so as to obtain stable nano-silver power or slurry; and stirring and ultrasonically dispersing nano-silver and additives in a solvent with a dielectric constant of 2-40, and then sealing and preserving. The preparation process provided by the invention is simple in operation, has the advantages of high feasibility, mild reaction conditions, short reaction time and high efficiency; and moreover, the nano-silver electroconductive ink has small nano-silver particle size and high stability and is suitable for mass production, thus meeting environmentally-friendly and energy-saving modern production requirements.
Description
Affiliated technical field
The invention discloses a kind of printed electronics with electrically conductive ink and preparation method thereof, it is simple to relate in particular to a kind of operating procedure, good stability, nano-silver conductive printing ink that sintering temperature is low and preparation method thereof.
Background technology
Along with printing technology more and more with other industry technology infiltration takes place to intersect, a series of new interleaving techniquess have been produced." printed electronics technology " (Printable Electronics Technology) is exactly that printing technology and electronic technology organically merge, and is the another important breakthrough of present technical development.It is at various matrixes by printing technology, particularly make various electronic circuits or device on the flexible substrate, make it have new technique such as functions such as electric transmission, signal emission, electromagnetic shielding, opto-electronic conversion, and additive process, the various electron devices of high speed printing fabrication techniques and circuit have been taked, compare photoengraving subtractive process technology commonly used before this, to having produced great influence with the industrial structure on the economic face of electronics firm, electrically conductive ink then prints the core integral part of electronic material just.
Silver powder becomes the focus of electrically conductive ink research because of having factors such as good chemical stability, high specific conductivity and moderate cost.Publication number by Samsung Electro-Mechanics Co., Ltd's application is to disclose a kind of conductive ink composition that is used for spray ink Printing in the CN101089058 patent, it comprises: the metal nanoparticle of 30-85 weight part, the solvent of 10-60 weight fraction, the wetting agent of 10-30 weight fraction, this wetting agent is made up of the compound that gives glycol or many alcohol, and the etherate additive based on glycol that is used to regulate viscosity of 0.1-10 weight part.This invention is when using inkjet-printing device to form lead-in wire, and the viscosity that can regulate printing ink keeps high density.But it is numerous to invent prescription, and the non-conductive composition of multidigit, will influence the electroconductibility of the finished product when solidifying to form lead-in wire, and the consistency of metal-powder and matrix also is that this invents insoluble problem in addition.The disclosed patent of Chinese patent CN1671805A is low conductive nano ink of sintering temperature and preparation method thereof, and this method discloses the novel method of making the cost effect of the electrically conductive ink that comprises nano metal powder.This invention prescription is complicated, is difficult to solve the uniform problem of specific conductivity equally.Disclosed a kind of conductive ink composition is a kind of thermoset electrically conductive ink among the Chinese patent CN1354208, is used for through hole connection or similar electrical equipment or electronic applications, so that stable electrical connection to be provided.This invention is carrier with Resins, epoxy, is that conductive component forms with silver, copper etc.This method has solved the unique advantage of solvent evaporates, but specific conductivity low be its critical defect.
Summary of the invention
The present invention is directed to the problem that exists in the background technology, it is simple to have proposed a kind of technology, rapidly and efficiently, stable conductivity, implementation and operation is strong, and the novel conductive printing ink of energy-conserving and environment-protective and preparation method thereof.This invents described a kind of low sintering solvent-borne type nano-silver conductive printing ink and preparation method thereof; concrete steps comprise: 1) with silver salt and complexing agent; stablizer; protective material fully is dissolved in the solvent; be warming up to 20-70 ℃ gradually; behind the temperature-stable reductive agent is added in the reaction system, continue afterwards after stirring reaction 10-30 minute, gradually cooling.The cooling back is by regulating pH value or adding polar solvent, and perhaps two kinds of methods adopt simultaneously and make its precipitation.Stir the centrifugal or suction filtration in back, then successively for several times, can obtain stabilized nano silver powder or soup compound with ethanol or deionized water, acetone repetitive scrubbing; 2) with nanometer silver, additive is by stirring ultra-sonic dispersion in specific inductivity is 2～40 solvent, and sealing is preserved and got final product.
Silver salt described in the step 1) can be one or several in the silver-colored title complex such as Silver monoacetate, Silver Nitrate, silver nitrite, silver carbonate, Sulfuric acid disilver salt, Trisilver phosphate or chitosan silver;
The complexing agent that is adopted in the step 1) can be that ammoniacal liquor, fatty amine, alcamines, amides, alicyclic ring amine, aromatic amine, naphthalene are one or several in other amines such as amine and polymine, azanol, and its addition is 1 for the mol ratio of itself and silver salt: 10-10: 1;
Stablizer described in the step 1) can be a valeric acid, carbon atom numbers such as oleic acid be 5-11 lipid acid, the acid of unsaturated fatty acids class, contain one or several of fragrant lopps acid, the acid of alicyclic ring class, its addition is 0.1-10 for the mol ratio of itself and silver salt: 1;
Solvent described in the step 1) can be deionized water, ethanol, also can be one or more mixture in many alcoholic solvents such as ethylene glycol, Virahol, glycerol or glycol ether that blending ratio is any;
Reductive agent described in the step 1) is one or several in sodium borohydride, hydrazine hydrate, inferior sodium phosphate, the vitamins C, and its addition is that the mol ratio of reductive agent and silver salt is 1-8: 1; : the regulation range of pH value is 1-8 in the step 1);
The polar solvent that is added in the step 1) can be that specific inductivity such as tetrahydrofuran (THF), ethanol, butanols, acetone are solvent of 15-40 and composition thereof, and its addition is 1 for the volume ratio of itself and reaction solvent: 10-5: 10;
The solvent of the nonpolar or low-pole step 2) can be benzene,toluene,xylene, sherwood oil, and the carbon atom number is wherein one or several such as the alkane of 3-15 or isoparaffin, and its specific inductivity is 2～14;
The particle diameter of described nanometer silver is 3-15nm, and the content in electrically conductive ink is 5-70wt%;
Step 2) additive described in can be hexadecyldimethyl benzyl ammonium ammonium chloride (1631), octadecyl trimethyl ammonium chloride (1831), cation guar gum (C-14S), the positively charged ion panthenol, positively charged ion silicone oil, dimethyl dodecyl amine oxide cats products such as (OB-2), also can be anion surfactants such as polyoxyethylenated alcohol sodium sulfate and sodium lauryl sulphate, it also can be Varion CDG-K, amphotericses such as carboxylic acid type tetrahydroglyoxaline, can also be alkylol amide (FFA), fatty alcohol-polyoxyethylene ether (AE), alkylphenol polyoxyethylene nonionogenic tensides such as (APE or OP), its addition is the 0.1-2wt% of total weight;
Described a kind of low sintering solvent-borne type nano-silver conductive printing ink and preparation method thereof is characterized in that: described nanometer silver is 50-150 ℃ in the sintering temperature of electrically conductive ink, and specific conductivity is greater than 1mS/cm.
Beneficial effect of the present invention:
1, nano metal content height of the present invention, specific conductivity height, application prospect is wide;
2, product technology of the present invention is simple, efficient is high, workable, be fit to scale operation;
3, little, the narrowly distributing of the electrically conductive ink nanometer silver particle diameter of the present invention preparation, content height, stability are high, and be good with solvent compatibility;
4, sintering temperature of the present invention is low, and bazardous waste produces few, and energy consumption is few, meets the requirement of modernization " energy-conserving and environment-protective, green production ".
Description of drawings
The present invention is further described below in conjunction with drawings and Examples.
Fig. 1 is the transmission electron microscope photo in the electrically conductive ink.
Fig. 2 is nanometer silver transmission electron microscope photo TGA figure in the electrically conductive ink.
Fig. 3 is the XRD figure spectrum of electrically conductive ink.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Example 1: with 1 part of Silver Nitrate and 0.5 part of ammoniacal liquor, 2 parts of valeric acids fully are dissolved in the mixed solvent (volume ratio of second alcohol and water is 2: 1) of etoh solvent and water, be warming up to 30 ℃ gradually, after the stirring and dissolving 1.1 parts of reductive agent hydrazine hydrates are added in the reaction system, continue stirring reaction afterwards about 20 minutes, cooling gradually.The cooling back is about 6.0 by regulating pH value, centrifugal after stirring, then use ethanol and deionized water and acetone repetitive scrubbing three times successively, 30 ℃ of vacuum-dryings, then 5g nanometer silver and 0.5g dimethyl dodecyl amine oxide are got final product by stirring ultra-sonic dispersion in 10g ethanol, seal to preserve.Sampling is printed back 70 ℃ of sintering by shower nozzle, and recording its resistivity is 1.2mS/cm.
Example 2: with 1 part of Silver Nitrate and 0.5 part of trolamine, 2 parts of positive enanthic acid fully are dissolved in the mixed solvent (volume ratio of second alcohol and water is 1: 5) of etoh solvent and water, be warming up to 30 ℃ gradually, after the stirring and dissolving 1 part of borane reducing agent potassium hydride KH is added in the reaction system, continue stirring reaction afterwards about 20 minutes, cooling gradually.The cooling back is about 6.0 by regulating pH value, centrifugal after stirring, then use ethanol and deionized water and acetone repetitive scrubbing three times successively, suction filtration then, with 30 ℃ of vacuum-dryings of nano-silver powder, 7g nanometer silver and 1g octadecyl trimethyl ammonium chloride (1831) are got final product by stirring ultra-sonic dispersion in the 10g tetrahydrofuran (THF), seal to preserve.Sampling is printed back 120 ℃ of sintering by shower nozzle, and recording its resistivity is 1.5mS/cm.
Example 3: with 1 part of Silver Nitrate and 0.5 part of trolamine, 2 parts of 3-hexenoic acids fully are dissolved in the mixed solvent (volume ratio of second alcohol and water is 3: 5) of etoh solvent and water, be warming up to 30 ℃ gradually, after the stirring and dissolving 1 part of borane reducing agent potassium hydride KH is added in the reaction system, continue stirring reaction afterwards about 20 minutes, cooling gradually.The cooling back is about 6.0 by regulating pH value, centrifugal after stirring, then use ethanol and deionized water and acetone repetitive scrubbing three times successively, suction filtration then, with 30 ℃ of vacuum-dryings of nano-silver powder, 7g nanometer silver and 1g octadecyl trimethyl ammonium chloride (1831) are got final product by stirring ultra-sonic dispersion in 10 Virahols, seal to preserve.Sampling is printed back 80 ℃ of sintering by shower nozzle, and recording its resistivity is 1.43mS/cm.
Example 4: with 2 parts of Silver Nitrates and 1 part of lauryl amine, 2 parts of n-capric acid fully are dissolved in the mixed solvent (volume ratio of ethylene glycol and water is 2: 5) of solvent ethylene glycol and water, be warming up to 70 ℃ gradually, after the stirring and dissolving 2 parts in reductive agent xitix is added in the reaction system, continue stirring reaction afterwards about 30 minutes, cooling gradually.The cooling back is about 4.0 by regulating pH value, centrifugal after stirring, then use ethanol and deionized water and acetone repetitive scrubbing three times successively, suction filtration then, with 30 ℃ of vacuum-dryings of nano-silver powder, 3g nanometer silver and 0.2g cation guar gum are got final product by stirring ultra-sonic dispersion in the 10g normal heptane, seal to preserve.Sampling is printed back 140 ℃ of sintering by shower nozzle, and recording its resistivity is 1.15mS/cm.
Example 5: with 1 part of Sulfuric acid disilver salt and 0.5 part of positive pelargonamide, 2 parts of pelargonic acids fully are dissolved in the mixed solvent (volume ratio of glycerol and water is 4: 7) of solvent glycerol and water, be warming up to 70 ℃ gradually, after the stirring and dissolving 3 parts of reductive agent glucose are added in the reaction system, continue stirring reaction afterwards about 20 minutes, cooling gradually.The cooling back is about 6.0 by regulating pH value, centrifugal after stirring, then use ethanol and deionized water and acetone repetitive scrubbing three times successively, suction filtration then, with 30 ℃ of vacuum-dryings of nano-silver powder, 6g nanometer silver and 1g fatty alcohol-polyoxyethylene ether are got final product by stirring ultra-sonic dispersion in methyl ethyl ketone, seal to preserve.Sampling is printed back 140 ℃ of sintering by shower nozzle, and recording its resistivity is 1.31mS/cm.。
Example 6: with 1 part of silver citrate and 0.5 part of naphthylamines, 2 parts of 3-methyl-naphthoic acids fully are dissolved in the mixed solvent (volume ratio of glycol ether and water is 1: 5) of solvent glycol ether and water, be warming up to 50 ℃ gradually, after the stirring and dissolving 1 part of reductive agent inferior sodium phosphate is added in the reaction system, continue stirring reaction afterwards about 30 minutes, cooling gradually.The cooling back is about 2.0 by regulating pH value, centrifugal after stirring, then use ethanol and deionized water and acetone repetitive scrubbing three times successively, suction filtration then, with 30 ℃ of vacuum-dryings of nano-silver powder, 5g nanometer silver and 0.6g alkylphenol polyoxyethylene are got final product by stirring ultra-sonic dispersion in 10g acetone, seal to preserve.Sampling is printed back 80 ℃ of sintering by shower nozzle, and recording its resistivity is 1.26mS/cm.
Claims (12)
1. low sintering solvent-borne type nano-silver conductive printing ink and preparation method thereof.Concrete steps of the present invention comprise: 1) silver salt and complexing agent, stablizer, protective material fully are dissolved in the solvent, are warming up to 20-70 ℃ gradually, behind the temperature-stable reductive agent is added in the reaction system, continue afterwards after stirring reaction 10-30 minute, gradually cooling.The cooling back is by regulating pH value or adding polar solvent, and perhaps two kinds of methods adopt simultaneously and make its precipitation.Stir the centrifugal or suction filtration in back, then successively for several times, can obtain stabilized nano silver powder or soup compound with ethanol or deionized water, acetone repetitive scrubbing; 2) with nanometer silver, additive is by stirring ultra-sonic dispersion in specific inductivity is 2～40 solvent, and sealing is preserved and got final product.
2. according to claim item 1 described a kind of low sintering solvent-borne type nano-silver conductive printing ink and preparation method thereof, it is characterized in that: silver salt described in the step 1) can be one or several in the silver-colored title complex such as Silver monoacetate, Silver Nitrate, silver nitrite, silver carbonate, Sulfuric acid disilver salt, Trisilver phosphate or chitosan silver.
3. according to claim item 1 described a kind of low sintering solvent-borne type nano-silver conductive printing ink and preparation method thereof, it is characterized in that: the complexing agent that is adopted in the step 1) can be that ammoniacal liquor, fatty amine, alcamines, amides, alicyclic ring amine, aromatic amine, naphthalene are one or several in other amines such as amine and polymine, azanol, and its addition is 1 for the mol ratio of itself and silver salt: 10-10: 1.
4. according to claim item 1 described a kind of low sintering solvent-borne type nano-silver conductive printing ink and preparation method thereof, it is characterized in that: stablizer described in the step 1) can be carbon atom numbers such as valeric acid, oleic acid be 5-11 lipid acid, the acid of unsaturated fatty acids class, contain one or several of fragrant lopps acid, the acid of alicyclic ring class, its addition is 0.1-10 for the mol ratio of itself and silver salt: 1.
5. according to claim item 1 described a kind of low sintering solvent-borne type nano-silver conductive printing ink and preparation method thereof, it is characterized in that: solvent described in the step 1) can be deionized water, ethanol, also can be one or more the mixture in many alcoholic solvents such as ethylene glycol, Virahol, glycerol or glycol ether, blending ratio be any.
6. according to claim item 1 described a kind of low sintering solvent-borne type nano-silver conductive printing ink and preparation method thereof, it is characterized in that: reductive agent described in the step 1) is one or several in sodium borohydride, hydrazine hydrate, inferior sodium phosphate, the vitamins C, and its addition is that the mol ratio of reductive agent and silver salt is 1-8: 1.
7. according to claim item 1 described a kind of low sintering solvent-borne type nano-silver conductive printing ink and preparation method thereof, it is characterized in that: the regulation range of pH value is 1-8 in the step 1).
8. according to claim item 1 described a kind of low sintering solvent-borne type nano-silver conductive printing ink and preparation method thereof, it is characterized in that: the polar solvent that is added in the step 1) can be that specific inductivity such as tetrahydrofuran (THF), ethanol, butanols, acetone are solvent of 15-40 and composition thereof, and its addition is 1 for the volume ratio of itself and reaction solvent: 10-5: 10.
9. according to claim item 1 described a kind of low sintering solvent-borne type nano-silver conductive printing ink and preparation method thereof, it is characterized in that: step 2) described in solvent nonpolar or low-pole can be benzene,toluene,xylene, sherwood oil, the carbon atom number is wherein one or several such as the alkane of 3-15 or isoparaffin, and its specific inductivity is 2～14.
10. according to claim item 1 described a kind of low sintering solvent-borne type nano-silver conductive printing ink and preparation method thereof, it is characterized in that: the particle diameter of described nanometer silver is 3-15nm, and the content in electrically conductive ink is 5-70wt%.
11. according to claim item 1 described a kind of low sintering solvent-borne type nano-silver conductive printing ink and preparation method thereof, it is characterized in that: step 2) described in additive can be hexadecyldimethyl benzyl ammonium ammonium chloride (1631), octadecyl trimethyl ammonium chloride (1831), cation guar gum (C-14S), the positively charged ion panthenol, positively charged ion silicone oil, dimethyl dodecyl amine oxide cats products such as (OB-2), also can be anion surfactants such as polyoxyethylenated alcohol sodium sulfate and sodium lauryl sulphate, it also can be Varion CDG-K, amphotericses such as carboxylic acid type tetrahydroglyoxaline, can also be alkylol amide (FFA), fatty alcohol-polyoxyethylene ether (AE), alkylphenol polyoxyethylene nonionogenic tensides such as (APE or OP), its addition is the 0.1-2wt% of total weight.
12. according to claim item 1 described a kind of low sintering solvent-borne type nano-silver conductive printing ink and preparation method thereof, it is characterized in that: described nanometer silver is 50-150 ℃ in the sintering temperature of electrically conductive ink, and specific conductivity is greater than 1mS/cm.
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| CN102816462A (en) * | 2012-08-13 | 2012-12-12 | 中国科学院宁波材料技术与工程研究所 | Preparation method for nano-silver particles coated with organic protection agent on surfaces |
| CN103613986A (en) * | 2013-11-28 | 2014-03-05 | 张家港市威迪森油墨有限公司 | Preparation method of nano graphite conductive ink |
| CN103952034A (en) * | 2014-05-19 | 2014-07-30 | 北京印刷学院 | Resin-free nano-silver electrically conductive printing ink as well as preparation method and applications thereof |
| CN105562712A (en) * | 2016-01-30 | 2016-05-11 | 北京印刷学院青岛研究院有限公司 | Method for concentrating nano-silver particles in water |
| GB2535251A (en) * | 2015-02-13 | 2016-08-17 | Dst Innovations Ltd | Conductive ink |
| CN106623971A (en) * | 2016-12-08 | 2017-05-10 | 中国科学院深圳先进技术研究院 | Nano-silver particles for conductive ink and preparation method of nano-silver particles |
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| CN103613986A (en) * | 2013-11-28 | 2014-03-05 | 张家港市威迪森油墨有限公司 | Preparation method of nano graphite conductive ink |
| CN103952034A (en) * | 2014-05-19 | 2014-07-30 | 北京印刷学院 | Resin-free nano-silver electrically conductive printing ink as well as preparation method and applications thereof |
| CN103952034B (en) * | 2014-05-19 | 2016-07-06 | 北京印刷学院 | One exempts from resin nano silver electrically conductive ink and its preparation method and application |
| GB2535251B (en) * | 2015-02-13 | 2019-08-07 | Dst Innovations Ltd | Conductive ink |
| GB2535251A (en) * | 2015-02-13 | 2016-08-17 | Dst Innovations Ltd | Conductive ink |
| GB2535214A (en) * | 2015-02-13 | 2016-08-17 | Dst Innovation Ltd | Printable conductive ink and method of forming transparent printed electrodes |
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| CN105562712A (en) * | 2016-01-30 | 2016-05-11 | 北京印刷学院青岛研究院有限公司 | Method for concentrating nano-silver particles in water |
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| CN106623971A (en) * | 2016-12-08 | 2017-05-10 | 中国科学院深圳先进技术研究院 | Nano-silver particles for conductive ink and preparation method of nano-silver particles |
| CN110998748A (en) * | 2017-08-08 | 2020-04-10 | 田中贵金属工业株式会社 | Metal printing ink |
| CN107541739A (en) * | 2017-08-28 | 2018-01-05 | 重庆立道表面技术有限公司 | A kind of alkaline non-cyanide decoating liquid for Electropolating hangers and preparation method thereof |
| CN107793842A (en) * | 2017-10-20 | 2018-03-13 | 西安理工大学 | A kind of preparation method of Nano silver conductive ink |
| CN108735343A (en) * | 2018-08-30 | 2018-11-02 | 浙江纳沛新材料有限公司 | A kind of conductive silver paste and preparation method thereof for low-temperature co-fired ceramic substrate |
| CN110548507A (en) * | 2019-08-01 | 2019-12-10 | 厦门大学 | Preparation method of carbon-supported nano-silver catalyst |
| CN110548507B (en) * | 2019-08-01 | 2020-11-13 | 厦门大学 | Preparation method of carbon-supported nano-silver catalyst |
| CN111334129A (en) * | 2020-03-30 | 2020-06-26 | 善仁（浙江）新材料科技有限公司 | Preparation method of low-temperature sintered nano-silver conductive ink |
| CN113223748A (en) * | 2021-05-12 | 2021-08-06 | 东南大学 | Low-temperature sintered conductive silver paste, and preparation method and application thereof |
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