CN108504185A - A kind of preparation method of ink-jet nano silver conductive ink - Google Patents
A kind of preparation method of ink-jet nano silver conductive ink Download PDFInfo
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- CN108504185A CN108504185A CN201810444416.0A CN201810444416A CN108504185A CN 108504185 A CN108504185 A CN 108504185A CN 201810444416 A CN201810444416 A CN 201810444416A CN 108504185 A CN108504185 A CN 108504185A
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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
- C09D11/30—Inkjet printing inks
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- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
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Abstract
The present invention discloses a kind of preparation method of ink-jet nano silver conductive ink, includes the following steps：Organic silver salts and dispersant are dissolved in ultra-pure water, after stirring evenly at room temperature, are poured into volumetric flask, constant volume, stands, forms organic silver salt solution；Reducing agent and pH adjusting agent are dissolved in ultra-pure water, after stirring evenly at room temperature, poured into brown volumetric flask, constant volume, is stood, reducing agent solution is formed；Organic silver salts solution is poured into the three-necked flask of water bath with thermostatic control, is stirred with blender；Reducing agent solution is instilled in three-necked flask with peristaltic pump with constant speed dropwise and is reacted with organic silver salts；By the solution after reaction through centrifugal purification, nano-Ag particles are obtained after dry；Nano-Ag particles are added in solvent, and auxiliary agent is added；Nano silver conductive ink is obtained after ultrasonic redisperse.Preparation process of the present invention is simple, and good dispersion is prepared by liquid phase reduction, the nano-Ag particles that stability is good and particle diameter distribution is narrow, is suitable for inkjet printing, widely applicable.
Description
Technical field
The present invention relates to the preparing technical fields of nano silver conductive ink, and in particular to a kind of ink-jet nano silver conductive ink
Preparation method.
Background technology
Nanotechnology just causes a new technological revolution, nanometer skill in material, device, the manufacture of system and application field
Art has broad application prospects, and national governments formulate relevant strategies and plans one after another for the development of nanotechnology, and throw
Enter huge fund support.The famous scientist's Qian Xuesen in China once pointed out that ran and nanometer structure below were next stage science and technology
One emphasis of development, can be a technological revolution, to cause 21 century Industrial Revolution again.In the 1980s,
" nanometer material science " and it is put into national " 863 " plan, greatly develops nanosecond science and technology.China is in 1999 at first
" 973 " are just provided nano material as great basic research program project in the works.At present nano silver coating, medicine,
Successful application case in water cleaning systems, textile and plastic industry is too numerous to enumerate, therefore nano material is emerging as one
Material class, will have very vast potential for future development.
Nano material is due to quantum effect, small-size effect and skin effect, showing many distinctive physics, change
Property is learned, is widely used in fields such as catalyst, photoelectric material, magnetic material and biological medicines.Therefore the system of nano-Ag particles
It is standby, in the industry cycle have received widespread attention.The preparation method of conventional nano silver has Physical and chemical method.Physical prepares nanometer
Silver particles, device therefor costliness manufacturing cost is high, and producing cost is expensive, and condition is not easy to control；Chemical method prepares nanometer silver granuel
Sub-operation is simple, be easy to control, be at low cost, yield is big, can prepare the big of different-grain diameter by controlling a certain process conditions
It is small.But chemical method, frequently with toluene, dimethylbenzene, acetone and other organic solvent has greater environmental impacts.
Invention content
In view of the above-mentioned deficiencies in the prior art, the technical problem to be solved by the present invention is that providing a kind of ink-jet nano
The preparation method of silver conductive ink.
The technical solution adopted by the present invention to solve the technical problems：
A kind of preparation method of ink-jet nano silver conductive ink, which is characterized in that include the following steps：
Organic silver salts and dispersant are dissolved in ultra-pure water, after stirring evenly, are poured into volumetric flask, constant volume, are stood, shape
At organic silver salts solution；
Reducing agent and pH adjusting agent are dissolved in ultra-pure water, after stirring evenly, poured into brown volumetric flask, constant volume is quiet
It sets, forms reducing agent solution；
Organic silver salts solution is poured into three-necked flask, is stirred with blender；
Reducing agent solution is instilled in three-necked flask with peristaltic pump with constant speed dropwise and is reacted with organic silver salts；
By the solution after reaction through centrifugal purification, nano-Ag particles are obtained after dry；
Nano-Ag particles are added in solvent, and auxiliary agent is added；
Nano silver conductive ink is obtained after ultrasonic redisperse.
Further, the organic silver salts solution and reducing agent solution react 60min at 40-50 DEG C of temperature.
Further, the dispersant uses polyvinylpyrrolidone.
Further, the reducing agent is sodium borohydride/glucose.
Further, the solvent is the aqueous solution of diethylene glycol (DEG).
Further, the nano silver conductive ink auxiliary agent is pH adjusting agent, dispersant, moisturizer and viscosity-controlling agent.
Further, the nano-Ag particles diameter integrated distribution is in 40-70nm.
Further, the solid content of the nano silver conductive ink is 20wt%.
Further, after the nano silver conductive ink is sintered film forming at a temperature of 150-200 DEG C, resistivity 5-20
Ω·cm。
Compared with the prior art, the present invention has the following advantages：
Preparation process is simple, prepares good dispersion by liquid phase reduction, stability is good and particle diameter distribution is narrow receives
Rice Argent grain；Also it is used as adhesive while PVP is as dispersant, improves electric conductivity；The reducing agent used is NaBH4, belong to
Environmentally friendly reducing agent, and there is strong reducing property, it can be reacted at high speed with AgNO3, generate nano-Ag particles；Nano-silver conductive
Ink slows down ink dried speed using the aqueous solution of DEG as solvent, improves dispersibility and stability；This nano-silver conductive ink
Water is environmentally friendly water-base nano silver conductive ink, is suitable for inkjet printing, widely applicable.
Description of the drawings
Fig. 1 is the nano silver electron-microscope scanning figure prepared provided by the present invention for ink-jet nano silver conductive ink.
Specific implementation mode
To make the object, technical solutions and advantages of the present invention be more clear, each implementation of the present invention is carried out below
It is more detailed to illustrate.The given examples are served only to explain the present invention, is not intended to limit the scope of the present invention.
Referring to Fig. 1, for the nano silver electron-microscope scanning figure prepared provided by the present invention for ink-jet nano silver conductive ink.
A kind of preparation method of ink-jet nano silver conductive ink, which is characterized in that include the following steps：
Organic silver salts and dispersant are dissolved in ultra-pure water, after stirring evenly at room temperature, are poured into volumetric flask, constant volume,
It stands, forms organic silver salt solution；
Reducing agent and pH adjusting agent are dissolved in ultra-pure water, after stirring evenly at room temperature, poured into brown volumetric flask, it is fixed
Hold, stand, forms reducing agent solution；
Organic silver salts solution is poured into the three-necked flask of water bath with thermostatic control, is stirred with blender；
Reducing agent solution is instilled in three-necked flask with organic silver salts at 40-50 DEG C of temperature dropwise with peristaltic pump with constant speed
React 60min；
By the solution after reaction through centrifugal purification, nano-Ag particles are obtained after dry；
Nano-Ag particles are added in solvent, and auxiliary agent is added；
Nano silver conductive ink is obtained after ultrasonic redisperse.
Organic silver salts use silver nitrate, and dispersant is polyvinylpyrrolidone, and polyvinylpyrrolidone is in preparation process
There are dispersion and stabilization to nano-Ag particles, and plays the role of adhesive when in printing to base material.Reducing agent is boron
Sodium hydride/glucose, sodium borohydride reduction is strong, environmental-friendly, completes reaction after being contacted with organic silver salts immediately, and effect is fast
Speed, anion forms nucleus by quick reduction, and maintains certain quantity, and the silver ion being reduced then is adsorbed on nucleus table
Face gradually grows into nano-Ag particles.The solution of gained is reacted through centrifugal purification, after dry, the nano-Ag particles diameter collection of acquisition
In be distributed in 40-70nm, purity is high.The solvent of nano silver is the aqueous solution of diethylene glycol (DEG), since diethylene glycol (DEG) possesses higher
(245.8 DEG C), room temperature volatilization is slow, slows down ink dried speed, selects the aqueous solution of diethylene glycol (DEG) as the dispersion solvent of nano silver,
It effectively prevents the printer nozzle caused by nano silver particles accumulation to block, while can also weaken " coffee ring " effect of ink droplet
It answers.Nano silver conductive ink auxiliary agent is pH adjusting agent, dispersant, moisturizer and other viscosity-controlling agents.
It is using liquid phase reduction, i.e., silver nitrate is soluble in water in the embodiment of the present invention, it makes it dissolve and mixes
It is even, selection sodium borohydride be reducing agent, polyvinylpyrrolidone is dispersant, and particle is precipitated out, by centrifugation, washing and
The compounding that solvent carries out ink is added after obtaining powder in drying.Solvent system used in ink is by ultra-pure water and diethylene glycol (DEG) group
At, it is common to use in home or office formula printer ink, the influence to environment is also far below toluene, dimethylbenzene, acetone etc.
Organic solvent.By liquid phase reduction, preparation process is simple, and yield is high.Preparation process is to carry out in the liquid phase, including water, pole
Property with nonpolar organic solvent, ionic liquid and microemulsion etc..By changing a series of experiment condition, as reducing agent is used
It includes size, distribution, pattern and stability that amount, dispersant dosage, reaction temperature, pH value and liquid feeding speed etc., which can be prepared a series of,
Different metal nanoparticle.
Organic silver salts are silver nitrate (AgNO3), and nitrate ion can be decomposed at 200 DEG C or less.
Reducing agent is sodium borohydride (NaBH4) and glucose dual reducting agents, and reducing power is stronger, can be used to restore various active
Big metal, instead of containing virose hydrazine hydrate, the formaldehyde or reproducibility that need to could be reacted under alkaline environment are weaker
The reducing agents such as sodium citrate.Carry out synthesizing nano-silver using NaBH4/ glucose as reducing agent, this is swift in response, and is almost restoring
Moment completes reaction when agent contacts silver nitrate, and anion forms nucleus by quick reduction, and maintains certain quantity, and by
The silver ion of reduction is then adsorbed on nucleating surface, gradually grows into nano-Ag particles.
Dispersant is polyvinylpyrrolidone (PVP).PVP has good protectiveness and dispersion effect, list to nano silver
Body functional group containing O, N is chemically adsorbed with silver ion formation, therefore the PVP of long-chain uniformly can envelope nano silver and make nano silver
Particle maintains to stablize for a long time in the solution.Further, since PVP is long chain macromolecule, when using PVP as the nano silver of dispersant
For spray printing when on base material, PVP has the function of adhesive agent.
Since diethylene glycol (DEG) (DEG) possesses higher (245.8 DEG C), room temperature volatilization is slow, slows down ink dried speed；It is another
Aspect selects the aqueous solution of DEG as the dispersion solvent of nano silver, effectively prevents the printing caused by nano silver particles accumulation
Machine nozzle blocks, while can also weaken " coffee ring " effect of ink droplet.The above-mentioned nano silver by after appropriate centrifugal purification is added
In the aqueous solution of DEG, it is placed in ultrasound in ultrasonator, makes particle redisperse, a series of ginsengs such as adjustment viscosity, surface tension
Number, forms stable conductive ink, you can inkjet printing experiment is carried out on EpsonStylus1390 printers.The system of ink
It is standby to can be obtained well dispersed nano silver conductive ink without mechanical lapping mode, thus external contamination is avoided, it can
Obtain the higher conductive ink of purity.
Nano silver conductive ink is environmentally friendly water-base nano silver conductive ink, and solid content 20wt% meets
Piezoelectric ink jet printer can spray printing requirement, and conducting wire is produced by inkjet printing mode.Solid content is less than 20wt%'s
There is tiltedly spray phenomenon when ink printed, after printing sintering, silverskin is relatively thin cannot to form uniform film, and has plane of disruption appearance, lead
It is larger to send a telegraph resistance；Solid content, which is more than the ink viscosity of 20wt%, to be steeply risen, and for inkjet printing, viscosity height not only makes ink
Drop in suffered frictional resistance when squeezing out spout to increase, influence amount out of ink, and it is serious when be likely to result in obstruction.
Print substrate is that the PI films of post-modification are handled through soda acid.Acid-alkali treatment method is mainly the acid imide for making PI film surfaces
Group is hydrolyzed into polyamic acid and polyamic acid metal salt, these polar groups enable PI film surfaces to increase, contact angle becomes
Small, wetability improves, and the roughness on surface, which increases, hydrophilic C=O groups increase contributes to the ink droplet of inkjet printing on PI films
It sprawls, surface roughness can reduce the contact angle of drop and film surface, increase the friction in drop spreads stage and relaxation stage
Loss, makes printing conducting wire tend to uniformity.
For the conducting wire that inkjet printing is formed after 150-200 DEG C of temperature sintering film forming, resistivity is 5-20 Ω cm,
The conducting wire of good connection is obtained at a relatively low sintering temperature.Due to the increase of surface atom and surface energy, small particle
Nano silver have lower fusing point, can melt at low temperature, thus by the nano silver of small particle as conductive material when, can compared with
The conducting wire of good connection is obtained under low sintering temperature.Melting phenomenon has occurred when being 150 DEG C in temperature, with receiving for surrounding
Rice corpuscles stick to each other and lead to grain growth, then form percolation conduction path.The dispersion of nanometer silver surface at about 150 DEG C
Agent PVP decomposes because heated, and nano silver is made to contact with each other, and forms more conductive percolation paths, electronics can more more
Free conduction, to make the resistivity of printing circuit be decreased obviously, electric conductivity also improves therewith.With sintering process after
It is continuous, fine and close conductive layer is ultimately formed at 200 DEG C, to make conductivity be remarkably decreased.
By adjusting parameters such as viscosity, surface tension, pH value, conductivity, it is configured to environmentally friendly water nano silver
Conductive ink makes it meet piezoelectric ink jet spray printing requirement, compared with traditional printing electronic technology, inkjet printing conducting wire warp
The thickness of oversintering processing, silver conductive layer is that conventional etch or mode of printing obtain ten parts of conductive layer thickness, and lead
Electrically it can but compare favourably with it.Thus the appearance of inkjet printing mode is radio frequency identification (RFID), organic light-emitting diodes
The development such as pipe (OLED), flexible PCB (PCB), sensor (Sensor), transistor (TFT), conducting wire provide one kind
The manufacture of great competitiveness.
Printing device is commercial color ink-jet printer (EpsonStylus1390, six colors), the resolution which possesses
Rate is 5600dpi, and printer nozzle diameter is about 30 μm, and the minimum ink ejection amount of nozzle is about 3pL.During the experiment, for
To best print quality, selected print parameters are：Print quality is set in best quality, and paper quality is set in
PremiumGlossyPhotoPaper (PGPP) pattern, printing line width is set as 80-100 μm, and is set in the item printed at a slow speed
Under part, best print resolution and print quality can be obtained, promotes the quality of inkjet printing, reduces ink occurrence and distribution not
Equal situation, with reduction " coffee ring effect ".
Embodiment one
By the silver nitrate (AgNO of 0.1mol (1.69g)3) be dissolved in ultra-pure water, and the polyethylene of dispersing agent of 1.67g is added
Pyrrolidones (PVP) forms oxidation solution/dispersant (AgNO3/ PVP) blended liquid；By 0.25-0.5mol (0.96-1.92g)
Sodium borohydride (NaBH4), the glucose of 0.01-0.5mol is dissolved in ultra-pure water, and 0.004-0.008mol (0.16- are added
Sodium hydroxide (NaOH) 0.32g) forms reducing solution；Then reducing solution is pumped into the speed of 1.0mL/min via peristaltic pump
Equipped with oxidation solution/dispersant (AgNO3/ PVP) blended liquid 250mL three-necked flasks in, electric mixer mixing speed is maintained
300-700rpm/min；Peristaltic pump liquid feeding adds to 20-30mL, and 60min is reacted at 40-50 DEG C；By the solution after reaction in high speed
10-15min is centrifuged with the rotating speed of 7000-10000rpm/min under centrifuge, purifying is centrifuged, the nanometer purified
Argent grain, grain diameter 40-70nm；Dispersion solvent of the aqueous solution of diethylene glycol (DEG) (DEG) as nano silver is selected, by this nanometer
Silver is scattered in the suspension that nano silver can be obtained in the aqueous solution of DEG again, and being placed in ultrasonator makes particle redisperse, and
Viscosity is adjusted, the series of parameters such as surface tension form favorable dispersibility, and particle diameter distribution is narrow, the high conductive ink of stability, i.e.,
Inkjet printing experiment can be carried out on EpsonStylus1390 printers.The ink can be in the PI films for handling post-modification through soda acid
The good pattern of upper printing outgoing-line type.Inkjet printing formed conducting wire through 150-200 DEG C of temperature sintering 10-15min at
The resistivity of the print performance having had after film, conducting wire is 6.8 μ Ω cm, has good electric conductivity.
Embodiment two
By the AgNO of 0.1mol (1.69g)3It is dissolved in ultra-pure water, and the dispersant PVP of 1.67g is added according to experimental design,
Form oxidation solution/dispersant (AgNO3/ PVP) blended liquid.By the NaBH of 0.0125mol (0.48g)4, the grape of 0.002mol
Sugar is dissolved in ultra-pure water, and the NaOH of 0.002mol (0.08g) is added according to experimental design, reducing solution is formed, then by reducing solution
It is pumped into equipped with oxidation solution/dispersant (AgNO via peristaltic pump with the speed of 1.0mL/min3/ PVP) blended liquid tri- mouthfuls of 250mL
In flask, electric mixer mixing speed is maintained 400rpm/min；Peristaltic pump liquid feeding adds to 25mL, and 60min is reacted at 50 DEG C；
Solution after reaction is centrifuged into 15min with the rotating speed of 7000rpm/min under supercentrifuge, purifying is centrifuged, obtains
To the nano-Ag particles of purifying, grain diameter 50-70nm；Dispersion solvent of the aqueous solution of DEG as nano silver is selected, by this
Nano silver is scattered in the suspension that nano silver can be obtained in the aqueous solution of DEG again, and being placed in ultrasonator makes particle divide again
It dissipates, and adjusts viscosity, the series of parameters such as surface tension form favorable dispersibility, and particle diameter distribution is narrow, the high conductive ink of stability
Water.The nano silver conductive ink is printed as to the circuit of about 80 μm of line width by ink jet printing, on PI base materials, through 150 DEG C
After sintering, resistivity is about 18.6 Ω/cm.
Embodiment three
By the AgNO of 0.1mol (1.69g)3It is dissolved in ultra-pure water, and the dispersant PVP of 1.67g is added according to experimental design,
Form oxidation solution/dispersant (AgNO3/ PVP) blended liquid.By the NaBH of 0.5mol (1.92g)4, the glucose of 0.01mol is molten
In ultra-pure water, and according to experimental design be added 0.08mol (0.32g) NaOH, formed reducing solution, then by reducing solution with
The speed of 1.0mL/min is pumped into via peristaltic pump equipped with oxidation solution/dispersant (AgNO3/ PVP) blended liquid tri- mouthfuls of 250mL burning
In bottle, electric mixer mixing speed is maintained 500rpm/min；Peristaltic pump liquid feeding adds to mL, and 60min is reacted at 40 DEG C；It will be anti-
Solution after answering centrifuges 10min under supercentrifuge with the rotating speed of 8500rpm/min, and purifying is centrifuged, obtains pure
The nano-Ag particles of change, grain diameter are about 50-70nm；Dispersion solvent of the aqueous solution of DEG as nano silver is selected, this is received
Meter Yin is scattered in the suspension that nano silver can be obtained in the aqueous solution of DEG again, and being placed in ultrasonator makes particle redisperse,
And viscosity is adjusted, the series of parameters such as surface tension form favorable dispersibility, and particle diameter distribution is narrow, the high conductive ink of stability.
The nano silver conductive ink is printed as to the circuit of about 100 μm of line width by ink jet printing, on PI base materials, is burnt through 200 DEG C
After knot, resistivity is about 6.8 Ω/cm.
It carries out an invention above and is merely illustrative of the technical solution of the present invention rather than is limited, the common skill of this field
Art personnel can continue technical scheme of the present invention peaceful modification or equivalent replacement, without departing from the spirit and scope of the present invention,
Protection scope of the present invention should be subject to described in claims.
Many other changes and remodeling can be made by not departing from the spirit and scope of the present invention.It should be appreciated that the present invention is not
It is limited to specific embodiment, the scope of the present invention is defined by the following claims.
Claims (9)
1. a kind of preparation method of ink-jet nano silver conductive ink, which is characterized in that include the following steps：
Organic silver salts and dispersant are dissolved in ultra-pure water, after stirring evenly, are poured into volumetric flask, constant volume, stands, is formed with
Machine silver salt solution；
Reducing agent and pH adjusting agent are dissolved in ultra-pure water, after stirring evenly, poured into brown volumetric flask, constant volume, is stood, shape
At reducing agent solution；
Organic silver salts solution is poured into three-necked flask, is stirred with blender；
Reducing agent solution is instilled in three-necked flask with peristaltic pump with constant speed dropwise and is reacted with organic silver salts；
By the solution after reaction through centrifugal purification, nano-Ag particles are obtained after dry；
Nano-Ag particles are added in solvent, and auxiliary agent is added；
Nano silver conductive ink is obtained after ultrasonic redisperse.
2. a kind of preparation method of ink-jet nano silver conductive ink according to claim 1, which is characterized in that described organic
Silver salt solution and reducing agent solution react 60min at 40-50 DEG C of temperature.
3. a kind of preparation method of ink-jet nano silver conductive ink according to claim 1, which is characterized in that the dispersion
Agent uses polyvinylpyrrolidone.
4. a kind of preparation method of ink-jet nano silver conductive ink according to claim 1, which is characterized in that the reduction
Agent is sodium borohydride/glucose.
5. a kind of preparation method of ink-jet nano silver conductive ink according to claim 1, which is characterized in that the solvent
For the aqueous solution of diethylene glycol (DEG).
6. a kind of preparation method of ink-jet nano silver conductive ink according to claim 1, which is characterized in that the nanometer
Silver conductive ink auxiliary agent is pH adjusting agent, dispersant, moisturizer and viscosity-controlling agent.
7. a kind of preparation method of ink-jet nano silver conductive ink according to claim 1, which is characterized in that the nanometer
Argent grain diameter integrated distribution is in 40-70nm.
8. a kind of preparation method of ink-jet nano silver conductive ink according to claim 1, which is characterized in that the nanometer
The solid content of silver conductive ink is 20wt%.
9. a kind of preparation method of ink-jet nano silver conductive ink according to claim 1, which is characterized in that the nanometer
After silver conductive ink is sintered film forming at a temperature of 150-200 DEG C, resistivity is 5-20 Ω cm.
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| CN110026569B (en) * | 2019-04-30 | 2022-04-15 | 长沙新材料产业研究院有限公司 | Preparation method of nano-silver |
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| CN111180107B (en) * | 2020-01-06 | 2021-09-21 | 青岛理工大学 | Preparation method for electric field driven injection of micro-nano 3D printing nano silver paste |
| CN112735627A (en) * | 2020-12-31 | 2021-04-30 | 苏州思尔维纳米科技有限公司 | High-viscosity self-protective particle-free ink-jet silver paste and preparation method thereof |
| WO2022262801A1 (en) * | 2021-06-18 | 2022-12-22 | 芯体素(杭州)科技发展有限公司 | Nano-metal 3d printing ink and application thereof |
| CN115322623B (en) * | 2022-07-01 | 2023-08-11 | 湖南兴威新材料有限公司 | Reactive ink-jet printing silver ink and preparation method and application thereof |
| CN115322623A (en) * | 2022-07-01 | 2022-11-11 | 湖南兴威新材料有限公司 | Reactive ink-jet printing silver ink and preparation method and application thereof |
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