CN109535849B - Ink-jet nano silver conductive ink and preparation method thereof - Google Patents
Ink-jet nano silver conductive ink and preparation method thereof Download PDFInfo
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- 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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- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
Abstract
The invention provides an ink-jet nano silver conductive ink and a preparation method thereof, wherein the ink-jet nano silver conductive ink comprises the following components: 12-30 parts of nano silver, 55-80 parts of deionized water, 0.02-2 parts of cosolvent, 0.1-1.0 part of wetting dispersant, 0.4-3.0 parts of binder, 0.2-0.6 part of defoamer, 3.0-10.0 parts of humectant, 0.01-0.5 part of flatting agent, 0.3-1.5 parts of anti-settling agent and 0.5-0.6 part of viscosity regulator. The preparation method of the conductive ink comprises two steps: preparing nano silver powder and preparing nano silver conductive ink. The conductive ink disclosed by the invention has the advantages that a certain auxiliary dispersing agent is added to protect silver from being oxidized in the storage process, and meanwhile, the stability of nano silver particles in water is improved by adjusting the pH value of a system; by adding the cosolvent, the blockage of the nozzle caused by too fast volatilization of the ink solvent can be inhibited, and the conductive ink has good conductivity, adhesiveness and printing adaptability.
Description
Technical Field
The invention belongs to the technical field of printing electronic paste, and particularly relates to water-based inkjet conductive ink and a preparation method thereof.
Background
With the development of information technology, researchers have developed a new field of electronic inkjet printing (electronic ink printing) by preparing functional ink by replacing a pigment in conventional ink with a functional material and successfully applying the technology to the preparation of electronic products. Therefore, the inkjet printing technology for directly manufacturing a circuit on a substrate is receiving attention, and the traditional printed circuit industry uses the photolithography technology, which involves the processes of etching, metal deposition, electroplating and the like, and is accompanied by the generation of a large amount of toxic chemical wastes. The nano metal ink-jet printing technology only needs two steps of printing and coating post-treatment when electronic products are produced, so that the preparation process is greatly simplified, the production efficiency is improved, and waste and pollution are avoided. Compared with the traditional electronic product manufacturing technology such as photoetching (photolitography), the electronic ink-jet printing has the characteristics of non-contact, addition type, low cost and the like, so that the large area production of electronic products and the flexibility of substrates become possible; compared with traditional printing processes such as silk screen printing and the like, the ink-jet printing does not need a screen printing plate, so that the research and development cost of new products is reduced, and in addition, the ink-jet printing has obvious advantages in the aspects of resolution and multi-layer printing.
The water-based ink-jet nano silver conductive ink mainly faces three key problems at present: one is stability, including chemical stability which is not prone to decomposition and physical stability which is not prone to agglomeration and precipitation; secondly, the rheological property, the viscosity and the surface tension of which are in proper ranges, is adopted to realize smooth ink jet; and thirdly, the adhesive force is good, and the solvent has good adhesive force with the substrate after being volatilized. The nano silver particles have large specific surface area and high surface energy, and are easy to agglomerate in a solution, so that the nano silver conductive ink with high stability is difficult to obtain. Particularly, nano silver conductive ink for inkjet printing requires a suitably low viscosity in order to meet the requirements of inkjet printing, and requires a relatively high nano silver content in order to satisfy the requirements of conductivity, and thus it is more difficult to obtain high stability of nano silver conductive ink.
Stability is generally enhanced by the introduction of suitable dispersants to prevent particle agglomeration. However, the conductivity of the lead after heat treatment is affected by adsorbing more dispersant on the surface of the nano silver particles. The flexible base material suitable for the ink-jet nano silver conductive ink mainly comprises base materials such as polyethylene terephthalate (PET), polyethylene naphthalate (PEN), Polyimide (PI), Polyetherimide (PEI), PP synthetic paper and the like. PET, PEN, PI and PEI substrates are generally hydrophobic, and the adhesive force of the aqueous inkjet nano silver conductive ink on the surfaces of the substrates is generally poor, so that the application of the aqueous inkjet nano silver conductive ink is influenced. Therefore, the development of the aqueous nano silver conductive ink which has good conductivity, stability and adhesion and is suitable for ink-jet printing becomes a difficult problem to be solved in the technical field.
Therefore, there is a need to provide an improved solution to the above-mentioned deficiencies of the prior art.
Disclosure of Invention
The invention aims to provide the water-based ink-jet nano silver conductive ink with good stability and the preparation method thereof, and the ink is suitable for PET, PEN, PI and PEI plastic base materials and has good stability, adhesive force and conductivity after heat treatment at a certain temperature.
In order to achieve the above purpose, the invention provides the following technical scheme:
the inkjet nano silver conductive ink comprises the following components in parts by weight: 12-30 parts of nano silver, 55-80 parts of deionized water, 0.02-2 parts of cosolvent, 0.1-1.0 part of wetting dispersant, 0.4-3.0 parts of binder, 0.2-0.6 part of defoamer, 3.0-10.0 parts of humectant, 0.01-0.5 part of flatting agent, 0.3-1.5 parts of anti-settling agent and 0.5-0.6 part of viscosity regulator.
In the inkjet nano silver conductive ink, the cosolvent is preferably ethylene glycol.
In the inkjet nano silver conductive ink, preferably, the wetting dispersant is one of BYK-108, BYK-110, BYK-180, BYK-190, BYK-345, BYK-348, BYK-349, EASYTECH ST-83 and OT-75;
preferably, the binder is one of a water-based acrylic resin AC-3137, a hydroxy acrylic resin HAR868 and a low-hydroxy acrylic resin Har 869;
preferably, the defoaming agent is a silicone oil defoaming agent, and the silicone oil defoaming agent is one of BYK-022, BYK-023, BYK-024 and BYK-028;
preferably, the humectant is one of diethylene glycol, a mixture of ethylene glycol and glycerin, propylene glycol, glycerin, sorbitol, glycerol, polyethylene glycol, hexylene glycol and polyglycerol;
preferably, the leveling agent is one or more of BYK-307, BYK-333, BYK-345, BYK-325 and BYK-331;
preferably, the anti-settling agent is BYK-420;
preferably, the viscosity modifier is BYK-425.
In the inkjet nano silver conductive ink as described above, preferably, the humectant is a mixture of diethylene glycol, ethylene glycol and glycerin;
preferably, the mass ratio of the mixture of diethylene glycol, ethylene glycol and glycerin in the humectant is diethylene glycol: ethylene glycol: 1: 3: 3.
a preparation method of ink-jet nano silver conductive ink comprises the following steps:
s1 preparation of nano silver powder
Preparing dry nano silver, wherein the nano silver is nano silver powder;
s2 preparation of nano-silver conductive ink
s21, adding deionized water into the container, adding cosolvent, sequentially adding wetting dispersant and one half of defoamer under stirring, stirring for 15-20 minutes, dispersing uniformly, adding humectant, and continuously stirring for 5-10 minutes; then adding a binder, a flatting agent and an anti-settling agent, and continuously stirring for 5-10 minutes to obtain a mixed solution;
s22, adding the nano silver powder prepared in the step S1 into the mixed liquid obtained in the step S21, stirring and adding the viscosity regulator and the residual defoaming agent in the step S21, and continuing stirring for 30-50min to obtain the ink-jet nano silver conductive ink.
In the method for preparing the inkjet nano silver conductive ink as described above, preferably, the method for preparing the nano silver powder in step S1 includes the steps of:
s11, preparing a silver nitrate solution, adding deionized water into a three-neck flask with an ice water bath and mechanical stirring, then adding a surfactant, a dispersing agent, an auxiliary dispersing agent and a silver nitrate solution, stirring for 15-20 minutes at room temperature, and gradually changing the solution from colorless to white to obtain a silver nitrate-dispersing agent mixed solution;
s12, heating the silver nitrate-dispersant mixed solution, preparing a reducing agent solution, slowly dripping the reducing agent solution into the silver nitrate-dispersant mixed solution under high-speed stirring, continuing to stir uniformly after dripping is finished, reacting for 40-80 minutes, stopping stirring, and ending the reaction to obtain a nano silver particle suspension;
s13, adding acetone and deionized water into the nano silver particle suspension for centrifugal cleaning to obtain purified nano silver slurry; and drying the nano silver slurry at low temperature to obtain nano silver powder.
In the preparation method of the inkjet nano silver conductive ink, preferably, the dispersion aid in step s11 is diethanolamine; preferably, the addition amount of the auxiliary dispersant diethanolamine is 0.5-6 parts.
In the method for preparing the inkjet nano silver conductive ink as described above, preferably, the surfactant in step s11 is one or more of polyvinylpyrrolidone, cetyltrimethylammonium bromide, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and trisodium citrate;
preferably, in step s11, the dispersant is water-soluble hydroxy cellulose, specifically one or a combination of more of sodium polyacrylate, hydroxymethyl cellulose, hydroxyethyl cellulose and hydroxypropyl cellulose;
preferably, the reducing agent solution in step s12 is Na2S、NaBH4One of ascorbic acid and hydrazine hydrate.
In the method for preparing the inkjet nano silver conductive ink, preferably, the concentration of the silver nitrate solution in the step s11 is 0.3-0.4 mol.L-1。
In the method for preparing the inkjet nano silver conductive ink, preferably, the concentration of the reducing agent solution in the step s12 is 0.5-3.0 mol.L-1。
Compared with the closest prior art, the technical scheme provided by the invention has the following excellent effects:
according to the ink-jet printing nano-silver conductive ink, the solvent is water, so that the ink-jet printing nano-silver conductive ink is clean and environment-friendly; a certain auxiliary dispersant is added to protect silver from being oxidized in the storage process, and meanwhile, the stability of nano silver particles in water is improved by adjusting the pH value of a system; through adding the cosolvent, the blockage of a spray head caused by too fast volatilization of an ink solvent can be inhibited, the freezing of the ink at a low temperature can be prevented, the surface tension of the nano-silver conductive ink at the room temperature is greatly reduced through the distribution ratio of the components, the nano-silver conductive ink can be smoothly spread on a photographic paper substrate, the viscosity and pH value parameters of the conductive ink are reasonably set, and the ink requirements of subsequent ink-jet printing are met.
In addition, the nano-silver conductive ink prepared by the invention has good conductivity, adhesiveness and printing adaptability.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments that can be derived by one of ordinary skill in the art from the embodiments given herein are intended to be within the scope of the present invention.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
According to the ink-jet printing nano-silver conductive ink and the preparation method thereof, the nano-silver conductive ink can be printed on substrates such as PET, PEN, PI, PEI and the like through ink-jet printing, and after the nano-silver conductive ink is sintered at a temperature lower than 200 ℃, the conductivity is superior to 2 mS/cm.
Pure nano silver particles in the nano silver conductive ink are in a colloid form when dispersed in ink of a water system, are not really soluble in water, and have poor storage stability. The auxiliary dispersing agent diethanolamine is added in the process of preparing the nano-silver powder, is easy to dissolve in water, has certain reducibility and can protect silver in the storage process from being oxidized by air, so that certain diethanolamine is added as the auxiliary dispersing agent, and the stability of nano-silver particles in water is improved by adjusting the pH value of a system.
In addition, glycol is also selected as a cosolvent in the preparation process of the nano-silver conductive ink, so that the blockage of a spray head caused by the too fast volatilization of an ink solvent can be inhibited, and the freezing of the ink at a low temperature can be prevented.
The preparation method of the ink-jet printing nano silver conductive ink mainly comprises two steps: firstly, preparing nano silver powder, adding an auxiliary agent into an inorganic silver salt solution, stirring, then adding a reducing agent to obtain nano silver particles, then washing to obtain nano silver slurry, and drying at low temperature to obtain nano silver powder; and secondly, preparing a mixed solution of various additives and a cosolvent, then adding the nano-silver powder, and uniformly stirring to obtain the ink-jet nano-silver conductive ink. The nano-silver conductive ink is simple in preparation process, good in dispersity and excellent in stability, has proper rheological property, can realize smooth ink jet, and has good conductivity and adhesion.
The invention provides ink-jet printing nano silver conductive ink and a preparation method thereof, wherein the ink-jet printing nano silver conductive ink comprises the following steps:
the inkjet nano silver conductive ink comprises the following components in parts by mass: 12 to 30 parts (such as 12 parts, 14 parts, 16 parts, 18 parts, 20 parts, 22 parts, 24 parts, 26 parts, 28 parts and 30 parts) of nano-silver, 55 to 80 parts (such as 56 parts, 58 parts, 60 parts, 62 parts, 64 parts, 66 parts, 68 parts, 70 parts, 72 parts, 74 parts, 76 parts and 78 parts) of deionized water, 0.02 to 2 parts (such as 0.02 part, 0.04 part, 0.06 part, 0.08 part, 0.1 part, 0.12 part, 0.14 part, 0.16 part and 0.18 part) of cosolvent, 0.1 to 1.0 part (such as 0.2 part, 0.3 part, 0.4 part, 0.5 part, 0.6 part, 0.7 part, 0.8 part, 0.9 part and 1.0 part) of wetting dispersant, 0.4 to 3.0 part (such as 0.6 part, 0.8 part, 1 part, 1.2 part, 1.6 part, 1.7 part, 0.8 part, 0.9 part, 1.0 part) of binder, 0 part (such as 0.6 part, 0.8 part, 1.8 part, 2 parts, 1.2 parts, 2.6 parts, 2.8 parts, 2.6 parts, 2.8 parts, 2.6 parts of defoamer, 2, 2.6 parts, 2.8 parts, 2 parts, 2.6 parts, 2.8 parts, 2.6 parts of defoamer, 2.6 parts, 2.8 parts, 2.6 parts, 2 parts, 2.8 parts, 2 parts, 2.6 parts, 2 parts, 2.8 parts, 2.6 parts, 2 parts, 2.6 parts, 2 parts, 2.6 parts, 2.8 parts, 2.6 parts, 2 parts, 2.6 parts, 2, 0.5 part, 0.55 part), 3.0-10.0 parts (such as 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts) of a humectant, 0.01-0.5 part (such as 0.05 part, 0.1 part, 0.15 part, 0.2 part, 0.25 part, 0.3 part, 0.35 part, 0.4 part, 0.45 part) of a leveling agent, 0.3-1.5 parts (such as 0.4 part, 0.5 part, 0.6 part, 0.7 part, 0.8 part, 0.9 part, 1.0 part, 1.1 part, 1.2 parts, 1.3 part, 1.4 part, 1.5 parts) of an anti-settling agent, 0.5-0.6 part (such as 0.51 part, 0.52 part, 0.53 part, 0.54 part, 0.55 part, 0.56 part, 0.57 part, 0.58 part, 0.59 part) of a viscosity regulator.
In a specific embodiment of the invention, the co-solvent is ethylene glycol.
In the specific embodiment of the invention, the wetting dispersant is one of BYK-108, BYK-110, BYK-180, BYK-190, BYK-345, BYK-348, BYK-349, EASYTECH ST-83 and OT-75;
preferably, the binder is one of water-based acrylic resin AC-3137, hydroxy acrylic resin HAR868 and low-hydroxy acrylic resin Har 869;
preferably, the defoaming agent is one of silicone oil defoaming agents such as BYK-022, BYK-023, BYK-024 and BYK-028;
preferably, the humectant is diethylene glycol, a mixture of ethylene glycol and glycerin, or one of propylene glycol, glycerin, sorbitol, glycerol, polyethylene glycol, hexylene glycol, and polyglycerol;
in a particular embodiment of the invention, the humectant is a mixture of diethylene glycol, ethylene glycol and glycerin;
preferably, the mass ratio of the mixture of diethylene glycol, ethylene glycol and glycerin in the humectant is diethylene glycol: ethylene glycol: glycerol 1: 3: 3.
preferably, the leveling agent is one or more of BYK-307, BYK-333, BYK-345, BYK-325 and BYK-331;
preferably, the anti-settling agent is BYK-420;
preferably, the viscosity modifier is BYK-425.
The wetting dispersants BYK-108, BYK-110, BYK-180, BYK-190, BYK-345, BYK-348, BYK-349, EASYTECH ST-83 and OT-75 in the invention are all commercially available products;
the adhesive water-based acrylic resin AC-3137, the hydroxyl acrylic resin HAR868 and the low hydroxyl acrylic resin Har869 are all commercial products;
silicone oil type antifoaming agents BYK-022, BYK-023, BYK-024 and BYK-028 are all commercially available products;
the flatting agents BYK-307, BYK-333, BYK-345, BYK-325 and BYK-331 are all commercially available products;
the anti-settling agent is BYK-420 which is a commercially available product;
the viscosity regulator BYK-425 is a commercial product.
In addition, the specific embodiment of the invention also provides a preparation method of the nano-silver conductive ink, which comprises the following steps:
s1 preparation of nano silver powder
s11, preparing a silver nitrate deionized water solution, adding deionized water into a three-neck flask with an ice water bath and mechanical stirring, then adding a surfactant, a dispersing agent, an auxiliary dispersing agent and a silver nitrate solution, stirring for 15-20min (such as 16min, 17min, 18min, 19min and 20min) at room temperature, and gradually changing the solution from colorless to white to obtain a silver nitrate-dispersing agent mixed solution;
s12, heating the silver nitrate-dispersant mixed solution, preparing a reducing agent solution, slowly dripping the reducing agent solution into the silver nitrate-dispersant mixed solution under high-speed stirring, continuously stirring uniformly after dripping is finished, carrying out reaction for 40-80min (such as 45min, 50min, 55min, 60min, 65min, 70min, 75min and 80min), stopping stirring, and finishing the reaction to obtain a nano silver particle suspension;
s13, adding acetone and deionized water into the nano silver particle suspension for centrifugal cleaning to obtain purified nano silver slurry; and drying the nano silver slurry at low temperature to prepare nano silver, wherein the nano silver is nano silver powder.
In a specific embodiment of the present invention, the dispersion aid additive is diethanolamine.
Preferably, diethanolamine is added in an amount of 0.5 to 6 parts (e.g., 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, 1.0 parts, 1.5 parts, 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts, 5.5 parts).
In a specific embodiment of the present invention, the surfactant in step s11 is one or more of polyvinylpyrrolidone, cetyltrimethylammonium bromide, sodium lauryl sulfate, sodium dodecylbenzenesulfonate, and trisodium citrate.
In a specific embodiment of the present invention, in step s11, the dispersant is water-soluble hydroxy cellulose, specifically, one or more of sodium polyacrylate (MW 15000, 35% aqueous solution), hydroxymethyl cellulose, hydroxyethyl cellulose and hydroxypropyl cellulose.
In an embodiment of the present invention, the reducing agent solution in step s12 is Na2S、NaBH4One of ascorbic acid and hydrazine hydrate.
In a specific embodiment of the invention, the concentration of the silver nitrate solution in step s11 is 0.3-0.4 mol.L-1(e.g., 0.3 mol. L)-1、0.31mol·L-1、0.32mol·L-1、0.33mol·L-1、0.34mol·L-1、 0.35mol·L-1、0.36mol·L-1、0.37mol·L-1、0.38mol·L-1、0.39mol·L-1) The concentration of the reducing agent solution in the step s12 is 0.5-3 mol.L-1(e.g., 0.6 mol. L)-1、0.7mol·L-1、 0.8mol·L-1、0.9mol·L-1、1mol·L-1、1.2·L-1、1.4l·L-1、1.6mol·L-1、1.8mol·L-1、 2mol·L-1、2.2mol·L-1、2.4mol·L-1、2.6mol·L-1、2.8mol·L-1、3mol·L-1)
S2 preparation of nano-silver conductive ink
s21, adding 55-80 parts of deionized water into a container, adding 0.02-2 parts of cosolvent, sequentially adding 0.1-1.0 part of wetting dispersant and one half of 0.2-0.6 part of defoamer under the condition of stirring, stirring for 15-20 minutes, uniformly dispersing, adding 3.0-10.0 parts of humectant, and continuously stirring for 5-10 minutes; then adding 0.4-3.0 parts of binder, 0.01-0.5 part of flatting agent and 0.3-1.5 parts of anti-settling agent, and continuously stirring for 5-10 minutes to obtain a mixed solution;
s22, adding 12 to 30 parts, such as 12 parts, 14 parts, 16 parts, 18 parts, 20 parts, 22 parts, 24 parts, 26 parts, 28 parts and 30 parts of the nano silver powder prepared in the step s13 into the mixed solution obtained in the step s21, stirring and adding 0.5 to 0.6 part of viscosity regulator and the rest of the defoaming agent in the step s21, and continuing stirring for 30 to 50min (such as 32min, 34min, 36min, 38min, 40min, 42min, 44min, 46min, 48min and 50min), and finally obtaining the ink-jet nano silver conductive ink.
Example 1
The invention provides an inkjet nano-silver conductive ink which is prepared from the following components in parts by weight: 17 parts of nano-silver, 69.6 parts of deionized water, 0.1 part of cosolvent, 0.6 part of wetting dispersant, 2.0 parts of binder, 0.5 part of defoaming agent, 3.0 parts of humectant, 0.3 part of flatting agent, 0.4 part of anti-settling agent and 0.5 part of viscosity regulator.
S1, the preparation method of the nano-silver powder is as follows: 0.4mol of the mixture is prepared at room temperature·L-1200mL of silver nitrate deionized water solution, and stirring for 5 minutes; then, polyvinylpyrrolidone, 0.6mL of 0.2mol/l sodium polyacrylate dispersant and 1 part of 1.5mL of auxiliary dispersant diethanolamine are added, the mixture is stirred for 15 minutes to obtain silver nitrate-dispersant mixed solution, and the solution is heated to 50 ℃; preparation of 2 mol. L-130mL of sodium borohydride deionized water solution; at 1500rpm min-1The sodium borohydride solution was added to the silver nitrate-dispersant mixed solution at a rate of 3 mL/min by a syringe with stirring, and the reaction was continued for 70 minutes.
Respectively using acetone and deionized water to prepare nano silver particles at 8000 rpm-min-1Centrifugally washing for 20 minutes at the rotating speed, and washing for 3 times respectively to obtain purified nano silver slurry; drying at low temperature to obtain nano silver powder.
The mass percentage of the nano silver in the slurry is analyzed to be 36.4 parts by a gravimetric method.
S2, the preparation method of the nano silver conductive ink is as follows: 75.6 parts of deionized water are added to a beaker, and 0.1 part of a glycol cosolvent is added at 1600 rpm-min-1Adding 0.6 part of wetting dispersant and 1/2 parts of 0.5 part of defoaming agent in turn under stirring, stirring for 15 minutes, uniformly dispersing, and then adding a mixture of the components in a volume ratio of 1: 3: 3.0 parts of a diethylene glycol-ethylene glycol-glycerin mixed solution, and the mixture was stirred for 10 minutes. Then 2.0 parts of binder, 0.3 part of flatting agent and 0.4 part of anti-settling agent are added, and the mixture is continuously stirred for 10 minutes.
Adding 17 parts of nano-silver powder, stirring for 10 minutes, adding 0.5 part of viscosity regulator, adding the rest 1/2 defoaming agent, and stirring at 1200 rpm-min-1Stirring for 50min to finally obtain the ink-jet nano silver conductive ink.
In the embodiment, the wetting dispersant is BYK-108, the defoaming agent is BYK-022, the binder is AC-3137, the leveling agent is BYK-307, the anti-settling agent is BYK-420, and the viscosity regulator is BYK-425.
The pH value, the viscosity, the conductivity and the surface tension of the ink are respectively measured by a pH meter, a rotational viscometer, a conductivity meter and the surface tension, and the values are respectively 7.5, 2.9 mPa.s and 1.8 mS.cm-1And 34.4 mN · m-1。
Printing the nano-silver conductive ink into lines with the line width of about 10 mu m on a PET substrate by ink-jet printing, sintering the lines at 120 ℃ for 1h in a drying oven, and enabling the conductivity to be 2.1 mS-cm-1The silver content was 0.1 g.
Example 2
The water-based ink-jet nano silver conductive ink is prepared from the following components in parts by weight: 20 parts of nano-silver, 70 parts of deionized water, 0.12 part of cosolvent, 0.7 part of wetting dispersant, 2.2 parts of binder, 0.55 part of defoamer, 5.0 parts of humectant, 0.4 part of flatting agent, 0.6 part of anti-settling agent and 0.45 part of viscosity regulator.
S1, the preparation method of the nano-silver powder is as follows: 0.4 mol.L is prepared at room temperature-1Stirring the silver nitrate deionized water solution for 5 minutes in a volume of 400 mL; then adding cetyl trimethyl ammonium bromide active agent, 0.6mL of 0.2mol/l hydroxymethyl cellulose and 2 parts of auxiliary dispersant diethanolamine and 3mL, stirring for 15 minutes to obtain silver nitrate-dispersant mixed solution, and heating the solution to 50 ℃; preparation of 2 mol. L-130mL of sodium borohydride deionized water solution; at 1500rpm min-1The sodium borohydride solution was added to the silver nitrate-dispersant mixed solution at a rate of 3 mL/min by a syringe with stirring, and the reaction was continued for 70 minutes.
Respectively using acetone and deionized water to prepare nano silver particles at 8000 rpm-min-1Centrifugally washing for 20 minutes at the rotating speed, and washing for 3 times respectively to obtain purified nano silver slurry; drying at low temperature to obtain nano silver powder.
The mass percentage of the nano silver in the slurry is analyzed to be 36.4 parts by a gravimetric method.
S2, the preparation method of the nano-silver conductive ink is as follows: 70 parts of deionized water are added to a beaker, and a trace of 0.1 part of ethylene glycol cosolvent is added at 1600rpm min-1Adding 0.54 part of wetting dispersant and 1/2 parts of 0.2 part of defoaming agent in turn under stirring, stirring for 15 minutes, uniformly dispersing, and then adding a mixture of materials with the volume ratio of 1: 3: 4.0 parts of a diethylene glycol-ethylene glycol-glycerin mixed solution 3, and the mixture was stirred for 10 minutes. Then 2.2 parts of binder, 0.4 part of flatting agent and 0.6 part of anti-settling agent are added, and the mixture is continuously stirred for 10 minutes. Adding 20 parts of nano-silver powder, and stirringFor 10 minutes, add 0.5 part of viscosity modifier and the remainder 1/2 defoamer at 1200rpm min-1Stirring for 50min to finally obtain the ink-jet nano silver conductive ink.
In the embodiment, the wetting dispersant is BYK-180, the defoaming agent is BYK-023, the binder is AC-3137, the leveling agent is BYK-333, the anti-settling agent is BYK-420, and the viscosity regulator is BYK-425.
The pH value, the viscosity, the conductivity and the surface tension of the ink are respectively measured by a pH meter, a rotational viscometer, a conductivity meter and the surface tension, and the values are respectively 7.8, 2.8 mPa.s and 2.3 mS.cm-1And 33.2mN · m-1。
The nano silver conductive ink is printed into lines with the line width of about 15 mu m on a PET substrate through ink jet printing, and is sintered for 0.5h at 150 ℃ in a drying oven, so that the conductivity is 2.82mS/cm, and the silver content is 0.12 g.
Example 3
The water-based ink-jet nano silver conductive ink is prepared from the following components in parts by weight: 26 parts of nano-silver, 62.3 parts of deionized water, 0.15 part of cosolvent, 0.8 part of wetting dispersant, 2.3 parts of binder, 0.4 part of defoaming agent, 6.0 parts of humectant, 0.5 part of flatting agent, 1 part of anti-settling agent and 0.6 part of viscosity regulator.
S1, the preparation method of the nano-silver powder is as follows: 0.4 mol.L is prepared at room temperature-1Stirring the silver nitrate deionized water solution for 5 minutes in a volume of 400 mL; then adding sodium dodecyl benzene sulfonate, trisodium citrate, 0.6mL of 0.2mol/l hydroxyethyl cellulose dispersant, 2.5 parts of auxiliary dispersant diethanolamine and 4mL, stirring for 15 minutes to obtain silver nitrate-dispersant mixed solution, and heating the solution to 50 ℃; preparation of 2 mol. L-130mL of sodium borohydride deionized water solution; at 1500rpm min-1The sodium borohydride solution was added to the silver nitrate-dispersant mixed solution at a rate of 3 mL/min by a syringe with stirring, and the reaction was continued for 70 minutes.
Respectively using acetone and deionized water to prepare nano silver particles at 8000 rpm-min-1Centrifugally washing for 20 minutes at the rotating speed, and washing for 3 times respectively to obtain purified nano silver slurry; drying at low temperature to obtain nano silver powder.
The mass percentage of the nano silver in the slurry is analyzed to be 36.4 parts by a gravimetric method.
S2, the preparation method of the nano-silver conductive ink is as follows: 62.2 parts deionized water and 0.1 part ethylene glycol co-solvent were added to a beaker at 1600rpm min-1Adding 0.8 part of wetting dispersant and 1/2 parts of 0.4 part of defoaming agent in turn under stirring, stirring for 15 minutes, uniformly dispersing, and then adding a mixture of the components in a volume ratio of 1: 3: 6.0 parts of a diethylene glycol-ethylene glycol-glycerin mixed solution 3, and the mixture was stirred for 10 minutes. Then 2.3 parts of binder, 0.5 part of flatting agent and 1 part of anti-settling agent are added, and the mixture is continuously stirred for 10 minutes. Adding 26 parts of nano-silver slurry, stirring for 10 minutes, adding 0.6 part of viscosity regulator and the rest 1/2 defoaming agent, and stirring at 1200 rpm-min-1Stirring for 50min to finally obtain the ink-jet nano silver conductive ink.
In the embodiment, the wetting dispersant is BYK-190, the defoaming agent is BYK-024, the binder is HAR868, the leveling agent is BYK-325, the anti-settling agent is BYK-420, and the viscosity regulator is BYK-425.
The pH value, the viscosity, the conductivity and the surface tension of the ink are respectively measured by a pH meter, a rotational viscometer, a conductivity meter and the surface tension, and the values are respectively 8.35, 2.8 mPa.s and 2.78 mS.cm-1And 32.8 mN. m-1。
The nano silver conductive ink is printed into lines with the line width of about 15 mu m on a PEN substrate by ink jet printing, and is sintered for 0.5h at 150 ℃ in a drying oven, so that the conductivity is 3.56mS/cm, and the silver content is 0.15 g.
Example 4
The water-based ink-jet nano silver conductive ink is prepared from the following components in parts by weight: 28 parts of nano-silver, 59.2 parts of deionized water, 0.2 part of cosolvent, 0.9 part of wetting dispersant, 2.8 parts of binder, 0.6 part of defoaming agent, 6.0 parts of humectant, 0.5 part of flatting agent, 1.3 parts of anti-settling agent and 0.6 part of viscosity regulator.
S1, the preparation method of the nano-silver powder is as follows: 0.4 mol.L is prepared at room temperature-1Stirring the silver nitrate deionized water solution for 5 minutes in a volume of 400 mL; then adding trisodium citrate and 0.6mL of 0.2mol/l hydroxypropyl cellulose dispersing agent,3 parts of auxiliary dispersant diethanolamine, 4.5ml, stirring for 15 minutes to obtain silver nitrate-dispersant mixed solution, and heating the solution to 50 ℃; preparation of 2 mol. L-130mL of sodium borohydride deionized water solution; at 1500rpm min-1The sodium borohydride solution was added to the silver nitrate-dispersant mixed solution at a rate of 3 mL/min by a syringe with stirring, and the reaction was continued for 70 minutes.
Respectively using acetone and deionized water to prepare nano silver particles at 8000 rpm-min-1Centrifugally washing for 20 minutes at the rotating speed, and washing for 3 times respectively to obtain purified nano silver slurry; drying at low temperature to obtain nano silver powder.
And analyzing the mass percentage content of the nano silver in the slurry to be 36.4 parts by adopting a gravimetric method.
S2, the preparation method of the nano silver conductive ink is as follows: 59.2 parts of deionized water and 0.2 part of ethylene glycol cosolvent are added to a beaker at 1600rpm min-1Sequentially adding 0.9 part of wetting dispersant, 0.6 part of 1/2 of defoaming agent, 0.5 part of flatting agent and 1.3 parts of anti-settling agent under the condition of stirring, stirring for 15 minutes, uniformly dispersing, and then adding a mixture of 1: 3: 6.0 parts of a diethylene glycol-ethylene glycol-glycerin mixed solution of 3, and the mixture was further stirred for 10 minutes. Then, 2.8 parts of a binder was added thereto, and stirring was continued for 10 minutes. Adding 28 parts of nano-silver powder, stirring for 10 minutes, adding 0.6 part of viscosity regulator and the rest 1/2 defoaming agent, and stirring at 1200 rpm-min-1Stirring for 50min to finally obtain the ink-jet nano silver conductive ink.
In the embodiment, the adopted wetting dispersant is BYK-348, the defoaming agent is BYK-028, the binder is HAR869, the leveling agent is BYK-345, the anti-settling agent is BYK-420, and the viscosity regulator is BYK-425.
The pH value, the viscosity, the conductivity and the surface tension of the ink are respectively measured by a pH meter, a rotational viscometer, a conductivity meter and the surface tension, and the values are respectively 8.4, 3.1 mPa.s and 3.22 mS.cm-1And 32.9mN · m-1。
The nano silver conductive ink was printed by inkjet printing as lines with a line width of about 20 μm on a PI substrate, dried in a drying oven at 160 ℃ for 0.5h, and measured to have a conductivity of 3.9mS/cm and a silver content of 0.17 g.
Comparative example 1
The difference between comparative example 1 and example 1 is that diethanolamine, a co-dispersant, was not added in the step S1 of preparing the nano silver powder in comparative example 1, and the other steps are the same as example 1 and will not be described again.
Respectively measuring the pH value, the viscosity, the conductivity and the surface tension of the ink by adopting a pH meter, a rotational viscometer, a conductivity meter and the surface tension, wherein the values are respectively 7.4, 3.3 mPa.s and 1.69 mS.cm-1And 39.5mN · m-1。
The nano-silver conductive ink prepared in the comparative example is prepared into lines with the line width of about 10 microns on a PET substrate through ink jet printing, and is sintered for 1h in a drying oven at 120 ℃, and the conductivity parameters of the obtained nano-silver film are as follows: 1.86mS · cm-1. The silver content was 0.1 g.
Comparative example 2
The difference between comparative example 2 and example 2 is that in comparative example 2, no cosolvent ethylene glycol is added in the step S2 for preparing the nano silver ink, and other steps are the same as example 2 and are not repeated herein.
Respectively measuring the pH value, viscosity, conductivity and surface tension of the ink by using a pH meter, a rotational viscometer, a conductivity meter and surface tension, wherein the values are respectively 7.6, 3.4 mPa.s and 1.97 mS.cm-1And 41.8mN · m-1。
The nano silver conductive ink prepared in the comparative example is prepared into lines with the line width of about 15 microns on a PET substrate through ink jet printing, and is sintered for 0.5h in a drying oven at 150 ℃, and the conductivity parameters of the obtained nano silver film are as follows: 2.26 mS. cm-1. The silver content was 0.12 g.
The performance data of the conductive inks prepared in examples 1 to 4 and comparative examples 1 to 2, and the performance data of the nano-silver thin film formed after the ink was inkjet dried are shown in table 1.
TABLE 1 Properties of conductive ink and nano-silver film after ink-jet prepared in various examples and comparative examples
From the data, it can be seen that, compared with example 1, in the comparative example 1, diethanolamine, which is an auxiliary dispersant, is not added in the preparation process of the nano silver powder, so that the surface tension of the prepared nano silver conductive ink is greatly increased, the viscosity is also increased, and the pH value is reduced, which indicates that after the auxiliary dispersant is added, the stability of the nano silver particles in the aqueous solvent is improved, which is helpful for improving the fluidity of the conductive ink, protecting silver from being oxidized in the storage process, and realizing smooth ink jet. After the auxiliary dispersing agent is added, the surface tension of the conductive ink is reduced, the adhesion on the flexible base material is enhanced, the conductivity after heat treatment is higher, and the conductivity is better.
The conductive ink in the comparative example 2 is not added with the cosolvent ethylene glycol in the preparation process, and the surface tension and the viscosity of the conductive ink in the comparative example 2 are greatly improved compared with those in the example 2, which shows that the ethylene glycol cosolvent added in the invention can reduce the viscosity and the surface tension of the conductive ink, prevent the blockage of a spray head caused by the too fast volatilization of the solvent, and realize the smooth ink jet. After the cosolvent is added, the surface tension of the conductive ink is reduced, the adhesion on the flexible base material is enhanced, the conductivity after heat treatment is higher, and the conductivity is better.
In conclusion: according to the ink-jet nano silver conductive ink and the preparation method thereof, the reasonable component proportion is adopted, the surface tension of the nano silver conductive ink at room temperature is reduced to 32.9mN/m from 71.97mN/m of pure water, the nano silver conductive ink can be smoothly spread on a photographic paper substrate, the viscosity and pH value parameters of the conductive ink are reasonable, and the ink requirements of subsequent ink-jet printing are met.
By adding the auxiliary agent, the auxiliary dispersant and the cosolvent with proper proportion and components, the pH value of the system is adjusted, the stability of the nano silver particles in water is improved, the blockage of a spray head caused by the too fast volatilization of the solvent of the conductive ink is inhibited, and the freezing of the ink at low temperature can be prevented.
The nano-silver conductive ink can be printed on substrates such as PET, PEN, PI, PEI and the like through ink-jet printing, and after the nano-silver conductive ink is sintered at the temperature of less than 200 ℃, the conductivity is superior to 2 mS/cm.
In addition, the solvent of the nano-silver conductive ink is all water, so that the nano-silver conductive ink is clean and environment-friendly, and has good conductivity, adhesiveness and printing adaptability.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. The ink-jet nano silver conductive ink is characterized by comprising the following components in parts by weight: 28 parts of nano-silver, 59.2 parts of deionized water, 0.2 part of cosolvent, 0.9 part of wetting dispersant, 2.8 parts of binder, 0.6 part of defoaming agent, 6.0 parts of humectant, 0.5 part of flatting agent, 1.3 parts of anti-settling agent and 0.6 part of viscosity regulator;
the cosolvent is ethylene glycol, the wetting dispersant is BYK-348, the binder is HAR869, the defoaming agent is BYK-028, and the humectant is prepared by mixing the following components in a volume ratio of 1: 3: 3, a diethylene glycol-ethylene glycol-glycerin mixed solution, wherein the flatting agent is BYK-345, the anti-settling agent is BYK-420, and the viscosity regulator is BYK-425;
the preparation method of the conductive ink comprises the following steps:
s1 preparation of nano silver powder
Preparing dried nano silver, wherein the nano silver is nano silver powder;
the preparation method of the nano silver powder in the step S1 includes the steps of:
s11, preparing a silver nitrate solution, adding deionized water into a three-neck flask with an ice water bath and mechanical stirring, then adding a surfactant, a dispersing agent, an auxiliary dispersing agent and a silver nitrate solution with the concentration of 0.4mol/L, stirring for 15-20 minutes at room temperature, and gradually changing the solution from colorless to white to obtain a silver nitrate-dispersing agent mixed solution;
s12, heating the silver nitrate-dispersant mixed solution, preparing a reducing agent solution, slowly dropwise adding the reducing agent solution into the silver nitrate-dispersant mixed solution at a stirring speed of 1500rpm, continuously stirring uniformly after dropwise adding is finished, reacting for 40-80 minutes, stopping stirring, and finishing the reaction to obtain a nano silver particle suspension;
s13, adding acetone and deionized water into the nano silver particle suspension, and carrying out centrifugal cleaning at the rotating speed of 8000rpm to obtain purified nano silver slurry; drying the nano silver slurry at low temperature to obtain nano silver powder;
s2 preparation of nano-silver conductive ink
s21, adding deionized water into a container, adding a cosolvent, sequentially adding one half of wetting dispersant and defoamer under stirring, stirring for 15 minutes, uniformly dispersing, adding a humectant, and continuously stirring for 10 minutes; then adding a binder, a flatting agent and an anti-settling agent, and continuously stirring for 10 minutes to obtain a mixed solution;
s22, adding the nano silver powder prepared in the step S1 into the mixed liquid obtained in the step S21, stirring and adding the viscosity regulator and the residual defoaming agent in the step S21, and continuing stirring for 50min to finally obtain the ink-jet nano silver conductive ink.
2. The inkjet nanosilver conductive ink of claim 1,
the dispersion aid additive in step s11 is diethanolamine.
3. The inkjet nano silver conductive ink according to claim 2, wherein the co-dispersant diethanolamine is added in an amount of 0.5 to 6 parts.
4. The inkjet nanosilver conductive ink of claim 1,
the surfactant in step s11 is one or more of polyvinylpyrrolidone, cetyl trimethyl ammonium bromide, sodium lauryl sulfate, sodium dodecylbenzene sulfonate and trisodium citrate.
5. The inkjet nanosilver conductive ink of claim 4,
in the step s11, the dispersant is water-soluble hydroxy cellulose, specifically one or a combination of more of hydroxymethyl cellulose, hydroxyethyl cellulose and hydroxypropyl cellulose.
6. The inkjet nanosilver conductive ink of claim 4,
in step s12, the reducing agent solution is Na2S、NaBH4One of ascorbic acid and hydrazine hydrate.
7. The inkjet nanosilver conductive ink of claim 4,
the concentration of the silver nitrate solution in the step s11 is 0.3-0.4 mol.L-1。
8. The inkjet nanosilver conductive ink of claim 4, wherein the concentration of the reducing agent solution in step s12 is 0.5-3.0 mol-L-1。
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