CN105733366A - Preparation method of nano-silver conductive ink for ink jet printing - Google Patents
Preparation method of nano-silver conductive ink for ink jet printing Download PDFInfo
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- CN105733366A CN105733366A CN201410751794.5A CN201410751794A CN105733366A CN 105733366 A CN105733366 A CN 105733366A CN 201410751794 A CN201410751794 A CN 201410751794A CN 105733366 A CN105733366 A CN 105733366A
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Abstract
The invention discloses a preparation method of nano-silver conductive ink for ink jet printing. The preparation method comprises the following steps: using hydroxy cellulose which is very good in both dispersibility and adhesion as a stabilizer in the preparation process of silver nano-particles; using a reducer, a precursor and the like in the preparation process, wherein the reducer, the precursor and the like are all substances which can be decomposed in a temperature lower than 200 DEG C; performing reduced-pressure distillation on the prepared silver nano-particle dispersion liquid; and adding other water-soluble accessory ingredients, so that the nano-silver conductive ink which can be sintered in low temperature is prepared. The hydroxy cellulose in the nano-silver conductive ink is utilized both as a stabilizing and dispersing agent during the preparation process of the nano-silver and an adhesive in the final nano-silver conductive ink; thus, resin application amount in the nano-silver conductive ink is reduced and silver solid content is improved, so that the electrical conductivity is obviously improved. When being printed by inkjet printing on bases such as papers, glasses, ceramics, plastics and the like, the nano-silver conductive ink has a relatively good electrical conductivity after sintering in a temperature range that is lower than 200 DEG C, so that the nano-silver conductive ink can be applied in conducting wires of flexible circuits, such as touch screens, radio frequency identification tags and the like.
Description
Technical field:
The preparation method that the present invention relates to a kind of ink jet printing nano silver conductive ink.
Background technology:
At present, the fast development of printed electronic material has promoted the formation of associated industry, development and progress.Microelectric technique constantly develops printed electronic material is proposed requirements at the higher level, develops to directions such as highly dense, multilamellar, high reliability, low cost, short cycle and automatic continuous production further.But, traditional printed circuit industrial application photoetching technique, relate to the technical processs such as etching, metal deposit and plating, along with the generation of substantial amounts of noxious chemical wastes.Therefore, the ink-jet printing technology directly making circuit on substrate gets the attention, and nano metal inkjet technology has only to print and coating post processing two step when carrying out electronic product and producing, and enormously simplify preparation technology, improve production efficiency, it is to avoid wastes and pollution.
Chinese patent CN102120265B discloses a kind of colloid of monodispersed Nano silver grain, the preparation method of nanometer silver powder and electrically conductive ink thereof received: it selects different reducing agent, presoma, stabilizer and solvent to prepare monodispersed silver nanoparticle colloid, monodispersed silver nanoparticle colloid is centrifuged precipitation, clean and drying obtains nanometer silver powder, again nanometer silver powder and various auxiliary agent are mixed with electrically conductive ink, generally the Nano silver grain of preparation is through eccentric cleaning, easily reunite, redispersion difficulty；And this invented technology is complicated.Chinese patent CN101812181A discloses a kind of nano silver dispersion and sprays silver inks water with it, containing stabilizers such as polyvinyl alcohol, diethylene glycol or glycerol in its nano silver dispersion, in order to improve the adhesive force of itself and substrate, add a large amount of sulfonate water dispersible polyesters further.The addition of this large amount of stabilizer and auxiliary agent, will produce impact to electric conductivity.
Summary of the invention:
The preparation method that it is an object of the invention to provide a kind of ink jet printing nano silver conductive ink, by using dispersibility and adhesion all well hydroxylated cellulose in preparing nano grain of silver subprocess, the reducing agent that simultaneously uses, precursor etc. are all at the material that can decompose lower than 200 DEG C of temperature below, so by the silver nanoparticle dispersion liquid of preparation by after distillation of reducing pressure, adding other auxiliary agent, namely obtaining can low sintering nano silver conductive ink.
In order to achieve the above object, the preparation method that the present invention provides a kind of nano silver conductive ink, described in specifically comprise the following steps that
Organic silver salts and stabilizer are dissolved in water, stir under room temperature；Adding ammonia, adjustment pH value is 10-12；Then reducing agent is added dropwise over, stirring reaction 1 hour under room temperature；By reacted solution decompression distillation and concentration；Solution after concentration is sequentially added into various auxiliary agent；Ultrasonic disperse again, obtains good dispersion, the nano silver conductive ink of uniform particle sizes.
Described organic silver salts is silver formate, silver acetate etc., and the anion of its organic silver salts such as acetate can lower than 200 DEG C of volatilizations or decomposition, and organic silver salts concentration is 0.01mol/L to 1.0mol/L.
Described stabilizer is one or more in the water soluble hydroxy celluloses such as hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxylated cellulose plays dispersion in preparing nano grain of silver subprocess and stablizes the effect of Nano silver grain, this hydroxylated cellulose exists in nano silver conductive ink always simultaneously, finally plays the effect of adhesive agent.
Described reducing agent is that hydrazine hydrate, phenylhydrazine, formaldehyde etc. are without metal cation and at the material lower than 200 DEG C of volatilizations or decomposition.
In solution after described decompression distillation, the concentration of Nano silver grain is 10-60%, and Nano silver grain particle diameter is 10-50nm.
Described auxiliary agent is anti-settling agent such as BYK-420, and levelling agent is BYK-333 such as, one or several in defoamer such as BYK-022 and viscosity modifier such as BYK-425, and various auxiliary agents are all water miscible.
Described nano silver conductive ink can pass through ink jet printing in paper, glass, pottery, plastics and other base, and after the temperature range sintering lower than 200 DEG C, resistivity is lower than 1 × 10-5Ω·cm。
A kind of nano silver conductive ink of the present invention, has the advantage that
Prepare the nanometer silver used by nano silver conductive ink not through eccentric cleaning, technical process is greatly reduced；Polyvinyl alcohol derivative is both as the stable dispersant in nanometer silver preparation process, and again as the adhesive agent in final nano silver conductive ink, what reduce resin in silver ink makes consumption, and electric conductivity is had clear improvement；This nano silver conductive ink solvent is all water, clean environmental protection；This nano silver conductive ink has good electric conductivity, adhesiveness and printing adaptability.
Accompanying drawing illustrates:
Fig. 1 represents the scanning electron microscope (SEM) photograph of a kind of nano silver conductive ink prepared in accordance with the present invention.
Detailed description of the invention:
For making the object, technical solutions and advantages of the present invention clearly, below the embodiments of the present invention are explained in detail.Example is served only for explaining the present invention, is not intended to limit the scope of the present invention.
Embodiment 1
The hydroxymethyl cellulose of the silver acetate aqueous solution of 0.5mol/l and 0.1mol/l is dissolved in 100ml water, stirs under room temperature；Adding ammonia, adjustment pH value is 10-12；Then the hydrazine hydrate 100ml of 0.5mol/l is added dropwise over, stirring reaction 1 hour under room temperature；Being distilled by reacted solution decompression, after distillation, in concentrated solution, silver content is 25%；Solution after concentration adds the BYK-333 of BYK-420 and 0.2% of 0.2%；Ultrasonic disperse, obtains good dispersion, the nano silver conductive ink of uniform particle sizes.Described nano silver conductive ink being printed as the lines of live width about 10 μm in glass matrix by ink jet printing, roasting 0.5h at 200 DEG C in ordinary sinter stove, resistivity is less than 0.5 × 10-5Ω·cm。
Embodiment 2
The hydroxymethyl cellulose of the silver acetate aqueous solution of 1.0mol/l and 0.2mol/l is dissolved in 100ml water, stirs under room temperature；Adding ammonia, adjustment pH value is 10-12；Then the hydrazine hydrate 100ml of 1.0mol/l is added dropwise over, stirring reaction 1 hour under room temperature；Being distilled by reacted solution decompression, after distillation, in concentrated solution, silver content is 50%；Solution after concentration adds the BYK-333 of BYK-420 and 0.2% of 0.2%；Ultrasonic disperse, obtains good dispersion, the nano silver conductive ink of uniform particle sizes.Described nano silver conductive ink being printed as the lines of live width about 10 μm in glass matrix by ink jet printing, roasting 0.5h at 200 DEG C in ordinary sinter stove, resistivity is less than 0.5 × 10-5Ω·cm。
The step of various methods divides above, is intended merely to description clear, it is achieved time can be merged into a step or some step is split, and is decomposed into multiple step, as long as comprising identical logical relation, all in the protection domain of this patent；To adding inessential amendment in algorithm or in flow process or introducing inessential design, but do not change the core design of its algorithm and flow process all in the protection domain of this patent.
It will be understood by those skilled in the art that the respective embodiments described above are to realize specific embodiments of the invention, and in actual applications, it is possible in the form and details it is done various change, without departing from the spirit and scope of the present invention.
Claims (7)
1. the preparation method of an ink jet printing nano silver conductive ink, it is characterised in that specifically comprise the following steps that and be dissolved in water by organic silver salts and stabilizer, stirs under room temperature；Adding ammonia, adjustment pH value is 10-12；Then reducing agent is added dropwise over, stirring reaction 1 hour under room temperature；By reacted solution decompression distillation and concentration；Solution after concentration is sequentially added into various auxiliary agent；Ultrasonic disperse again, obtains good dispersion, the nano silver conductive ink of uniform particle sizes.
2. the preparation method of a kind of ink jet printing nano silver conductive ink according to claim 1, it is characterized in that described organic silver salts is silver formate, silver acetate etc., the anion of its organic silver salts such as acetate can lower than 200 DEG C of volatilizations or decomposition, and organic silver salts concentration is 0.01mol/L to 1.0mol/L.
3. the preparation method of a kind of ink jet printing nano silver conductive ink according to claim 1, it is characterized in that described stabilizer is one or more in the water soluble hydroxy celluloses such as hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxylated cellulose plays dispersion in preparing nano grain of silver subprocess and stablizes the effect of Nano silver grain, this hydroxylated cellulose exists in nano silver conductive ink always simultaneously, finally plays the effect of adhesive agent.
4. the preparation method of a kind of ink jet printing nano silver conductive ink according to claim 1, it is characterised in that described reducing agent is that hydrazine hydrate, phenylhydrazine, formaldehyde etc. are without metal cation and at the material lower than 200 DEG C of volatilizations or decomposition.
5. the preparation method of a kind of ink jet printing nano silver conductive ink according to claim 1, it is characterised in that in the solution after described decompression distillation, the concentration of Nano silver grain is 10-60%, and Nano silver grain particle diameter is 10-50nm.
6. the preparation method of a kind of ink jet printing nano silver conductive ink according to claim 1, it is characterised in that described auxiliary agent is one or several in anti-settling agent, levelling agent, defoamer and viscosity modifier, and various auxiliary agents are all water miscible.
7. the preparation method of a kind of ink jet printing nano silver conductive ink according to claim 1, it is characterized in that described nano silver conductive ink can pass through ink jet printing in paper, glass, pottery, plastics and other base, after temperature range sintering lower than 200 DEG C, resistivity is lower than 1 × 10-5Ω·cm。
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| CN201410751794.5A CN105733366B (en) | 2014-12-09 | 2014-12-09 | A kind of preparation method of ink jet printing nano silver conductive ink |
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| CN201410751794.5A CN105733366B (en) | 2014-12-09 | 2014-12-09 | A kind of preparation method of ink jet printing nano silver conductive ink |
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| CN105733366A true CN105733366A (en) | 2016-07-06 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106280716A (en) * | 2016-10-31 | 2017-01-04 | 南京东纳生物科技有限公司 | The preparation method and applications of the conductive silver ink that a kind of surface enhanced raman spectroscopy is sensitive |
| CN106385769A (en) * | 2016-09-08 | 2017-02-08 | 信阳师范学院 | Manufacturing method of sliver fiber flexible circuit based on taking cotton as template |
| CN106634220A (en) * | 2016-09-13 | 2017-05-10 | 江南大学 | Environmental friendly nano silver conductive ink and preparation method and printing application thereof |
| CN107033673A (en) * | 2017-05-25 | 2017-08-11 | 佛山市三水区康立泰无机合成材料有限公司 | A kind of preparation method of inkjet printing cobalt blue ceramic ink |
| CN107419523A (en) * | 2017-04-07 | 2017-12-01 | 中国科学院化学研究所 | One kind prepares flexible electronic fabric sensor based on the method for printing and dyeing |
| CN110117440A (en) * | 2019-05-10 | 2019-08-13 | 齐鲁工业大学 | A kind of conductive ink and preparation method thereof |
| CN110289125A (en) * | 2019-06-18 | 2019-09-27 | 电子科技大学中山学院 | Preparation method of silver nanowire conductive film and additive thereof |
| 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 |
| CN111393893A (en) * | 2020-03-09 | 2020-07-10 | 广东四维新材料有限公司 | Nano silver solution for spraying 5G dielectric ceramic filter, preparation method and spraying method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101870832A (en) * | 2010-05-06 | 2010-10-27 | 复旦大学 | Method for preparing nano silver conductive ink |
| CN103194117A (en) * | 2013-04-08 | 2013-07-10 | 电子科技大学 | Preparation method and application of sintering-free ultrafine silver nanometer printing ink |
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2014
- 2014-12-09 CN CN201410751794.5A patent/CN105733366B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101870832A (en) * | 2010-05-06 | 2010-10-27 | 复旦大学 | Method for preparing nano silver conductive ink |
| CN103194117A (en) * | 2013-04-08 | 2013-07-10 | 电子科技大学 | Preparation method and application of sintering-free ultrafine silver nanometer printing ink |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106385769A (en) * | 2016-09-08 | 2017-02-08 | 信阳师范学院 | Manufacturing method of sliver fiber flexible circuit based on taking cotton as template |
| CN106385769B (en) * | 2016-09-08 | 2018-09-04 | 信阳师范学院 | Production method based on the silver fiber flexible circuit that cotton is template |
| CN106634220A (en) * | 2016-09-13 | 2017-05-10 | 江南大学 | Environmental friendly nano silver conductive ink and preparation method and printing application thereof |
| CN106280716A (en) * | 2016-10-31 | 2017-01-04 | 南京东纳生物科技有限公司 | The preparation method and applications of the conductive silver ink that a kind of surface enhanced raman spectroscopy is sensitive |
| CN107419523A (en) * | 2017-04-07 | 2017-12-01 | 中国科学院化学研究所 | One kind prepares flexible electronic fabric sensor based on the method for printing and dyeing |
| CN107033673A (en) * | 2017-05-25 | 2017-08-11 | 佛山市三水区康立泰无机合成材料有限公司 | A kind of preparation method of inkjet printing cobalt blue ceramic ink |
| CN110117440A (en) * | 2019-05-10 | 2019-08-13 | 齐鲁工业大学 | A kind of conductive ink and preparation method thereof |
| CN110289125A (en) * | 2019-06-18 | 2019-09-27 | 电子科技大学中山学院 | Preparation method of silver nanowire conductive film and additive thereof |
| CN110289125B (en) * | 2019-06-18 | 2022-08-12 | 电子科技大学中山学院 | Preparation method of silver nanowire conductive film and additive thereof |
| CN111393893A (en) * | 2020-03-09 | 2020-07-10 | 广东四维新材料有限公司 | Nano silver solution for spraying 5G dielectric ceramic filter, preparation method and spraying method thereof |
| 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 |
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Address after: No. 8 and Simpson science and Technology Park in Hunan province Zhuzhou City Jinlong Road 412000 Tianyuan District 2 Leadbeater Applicant after: HUNAN LEED ELECTRONIC INK CO.,LTD. Address before: Malaysia Industrial Park No. 88 Jinlong Road 412000 in Hunan province Zhuzhou city Tianyuan District Applicant before: HUNAN LEED ELECTRONIC INK CO.,LTD. |
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Granted publication date: 20190531 Termination date: 20211209 |