CN107793842A - A kind of preparation method of Nano silver conductive ink - Google Patents
A kind of preparation method of Nano silver conductive ink Download PDFInfo
- Publication number
- CN107793842A CN107793842A CN201710986060.9A CN201710986060A CN107793842A CN 107793842 A CN107793842 A CN 107793842A CN 201710986060 A CN201710986060 A CN 201710986060A CN 107793842 A CN107793842 A CN 107793842A
- Authority
- CN
- China
- Prior art keywords
- nano silver
- solution
- silver
- conductive ink
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- 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
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0545—Dispersions or suspensions of nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- 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
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- 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
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09D11/107—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from unsaturated acids or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- 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
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
-
- C—CHEMISTRY; METALLURGY
- 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
Abstract
A kind of preparation method of Nano silver conductive ink disclosed by the invention, is first reducing agent using silver ammino solution as silver-colored forerunner, glucose and polyvinylpyrrolidone is that Nano Silver alcohol dispersion liquid is prepared in scattered protective agent；Nano silver conductive ink is prepared in aqueous polyurethane/polyacrylate and Nano Silver alcohol dispersion liquid again.The raw material of selection is to human body and environment nonhazardous, and preparation technology is simple, and production cost is low, and energy resource consumption is few, meets the requirement of modernization " energy-conserving and environment-protective, green production "；Obtained electrically conductive ink content of nanometer silver is higher, without adding other auxiliary agents, has good stability；There is excellent electric conductivity after cold curing, and ink viscosity is adjustable, suitable for mode of printings such as ink-jet and silk screens.
Description
Technical field
The invention belongs to print to use technical field of electronic materials, it is related to a kind of preparation method of Nano silver conductive ink.
Background technology
With the innovation and development of nanometer technology and printing technology, the mixing together with modern electronic technology is strong to promote
Research and application of the nano metal in electrically conductive ink.Electrically conductive ink has been widely applied to electronics industry production at present,
Many fields such as medicine, life products, such as RFID antenna, sensor, Organic Light Emitting Diode (OLED), flexible display, modeling
Expect thin-film solar cells, patch etc. of making up.The development of printed electronic industry and new expansion are using the performance to electrically conductive ink
More, higher requirement is proposed, this causes electrically conductive ink more to pursue the application of nanometer technology, has become and leads both at home and abroad
The development trend of electric ink.
Electrically conductive ink is a kind of functional ink with electric current transmission function of current, by conductive filler, binder, solvent
Formed with auxiliary agent etc., it is conductive after cured.Conductive filler directly decides the electric conductivity of electrically conductive ink.Common conduction
Filler has metal class conductive filler, such as gold, silver, copper, nickel；Also there is non-metal kind conductive filler, such as carbon ink, graphite, carbon fiber
Deng.The electrically conductive ink of radio frequency inserts, than relatively low, can not meet the needs of electronic printing at present on electric conductivity.Receive
Rice silver chemical stability is high, good conductivity, is to prepare low-resistivity, the most potential material of high conductivity electrically conductive ink.Receive
Meter Yin has special nano-meter characteristic, size is small, and specific surface area is big as nano-particle so that Nano silver conductive ink is conductive
Performance is higher than conventional conductive ink.Conventional conductive ink uses a large amount of toxic solvents, and solvent volatilization causes greatly to pollute to environment,
And conductive filler granule is big, it is necessary to can just make electric conductivity reach requirement, while these big using more conductive filler
Grain can also increase the ink film thickness and post-processing temperature of ink.
The content of the invention
It is an object of the invention to provide a kind of preparation method of Nano silver conductive ink, after solving existing electrically conductive ink
The problem for the treatment of temperature is high.
The technical solution adopted in the present invention is a kind of preparation method of Nano silver conductive ink, first using silver ammino solution as
Silver-colored forerunner, glucose are reducing agent and polyvinylpyrrolidone is that Nano Silver alcohol dispersion liquid is prepared in scattered protective agent；
Nano silver conductive ink is prepared in aqueous polyurethane/polyacrylate and Nano Silver alcohol dispersion liquid again.
The features of the present invention also resides in,
A kind of preparation method of Nano silver conductive ink, specifically includes following steps：
Step 1, polyvinylpyrrolidone is added in silver ammino solution being well mixed, temperature rises to 55 DEG C~65 DEG C, and
Solution A is obtained after stirring 25min~35min；
Step 2, into solution A be added dropwise glucose ethanol solution, and continue react 0.8h~1.2h, it is molten to obtain Nano Silver
Liquid；25min~35min is stirred after first Nano silver solution is cooled down, then is centrifuged after Nano silver solution is diluted, then with nothing
Water-ethanol repeated washing 5~7 times, finally take out lower floor's colloid and add absolute ethyl alcohol and re-start ultrasonic disperse, obtain nanometer
Silver-colored alcohol dispersion liquid；
Step 3, the mass fraction of the Nano Silver in the Nano Silver alcohol dispersion liquid obtained through step 2 is first adjusted to 30%
~70%, then add solvent into Nano Silver alcohol dispersion liquid and obtain solution B, aqueous polyurethane/poly- is then added into solution B
Acrylic acid ester emulsion, solution C is obtained, continue to stir by being transferred on magnetic stirring apparatus after solution C ultrasonic disperse, obtain Nano Silver
Electrically conductive ink.
In step 1：The mol ratio of polyvinylpyrrolidone and the nitric acid silver ion in silver ammino solution is 1.5:1.
In step 2：The concentration of the ethanol solution of glucose is 1mol/L；The solvent for diluting Nano silver solution is anhydrous second
Alcohol, and the volume of absolute ethyl alcohol is 3~5 times of Nano silver solution.
In centrifugal process：The rotating speed of centrifuge is 10000rpm, time 10min.
In step 3, solvent is the mixture of deionized water, ethanol and glycerine, and the volume ratio of three is 1：2：3, it is molten
The mass fraction of agent is 10%~50%.
In the Nano silver conductive ink of step 3：The mass fraction of aqueous polyurethane/polyacrylate dispersion be 15%~
30%.
The beneficial effects of the present invention are：
(1) preparation method of the invention, the raw material of selection is to human body and environment nonhazardous, and preparation technology is simple, production
Cost is low, and energy resource consumption is few, meets the requirement of modernization " energy-conserving and environment-protective, green production "；
(2) preparation method of the invention, obtained nano-Ag particles are uniform, good dispersion, can preserve for a long time；
(3) preparation method of the invention, obtained electrically conductive ink content of nanometer silver is higher, without adding other auxiliary agents, tool
There is good stability；There is excellent electric conductivity after cold curing, and ink viscosity is adjustable, suitable for ink-jet and silk screen etc.
Mode of printing.
Brief description of the drawings
The sintering temperature of electrically conductive ink and the graph of a relation of electrical conductivity that the preparation method of Fig. 1 present invention obtains.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
A kind of preparation method of Nano silver conductive ink, first by silver-colored forerunner, glucose of silver ammino solution be reducing agent and
Polyvinylpyrrolidone is that nano-Ag particles are prepared in scattered protective agent；Again by aqueous polyurethane/polyacrylate and nanometer
Nano silver conductive ink is prepared in Argent grain.
A kind of preparation method of Nano silver conductive ink, it is characterised in that specifically implement according to following steps：
Step 1, under the conditions of lucifuge, silver nitrate is dissolved in be configured in absolute ethyl alcohol 0.1mol/L silver nitrate ethanol it is molten
Liquid, the ammoniacal liquor that volume fraction is 25% is then slowly added into, obtains silver ammino solution, and it is 9~11 to adjust it to adjust pH value；Will be poly-
Vinylpyrrolidone is added in silver ammino solution and is well mixed, and temperature rises to 55 DEG C~65 DEG C, and after stirring 25min~35min
Obtain solution A；
Step 2, into solution A be added dropwise 1mol/L glucose ethanol solution, continue after being added dropwise to complete react 0.8h~
1.2h, obtain Nano silver solution；Nano silver solution first is cooled into room temperature to continue to stir 25min~35min, then Nano Silver is molten
Liquid is centrifuged after being diluted with absolute ethyl alcohol, and the volume of absolute ethyl alcohol is 3~5 times of Nano silver solution；Then with anhydrous second
Alcohol repeated washing 5~7 times, finally remove a layer colloid addition absolute ethyl alcohol and re-start ultrasonic disperse, obtain Nano Silver ethanol point
Dispersion liquid；
The mol ratio of polyvinylpyrrolidone and the nitric acid silver ion in silver ammino solution is 1.5:1；
In centrifugal process：The rotating speed of centrifuge is 10000rpm, time 10min.
Step 3, the mass fraction of the Nano Silver in the Nano Silver alcohol dispersion liquid obtained through step 2 is first adjusted to 30%
~70%, solvent is then added into Nano Silver alcohol dispersion liquid and obtains solution B, then adds into solution B aqueous polyurethane/poly-
Acrylic acid ester emulsion, solution C is obtained, will be transferred to after solution C ultrasonic disperse 30min on magnetic stirring apparatus and continue to stir 30min,
Obtain Nano silver conductive ink；
Solvent is the mixture of deionized water, ethanol and glycerine, and the volume ratio of three is 1：2：3, the quality of solvent
Fraction is 10%~50%；
The mass fraction of aqueous polyurethane/polyacrylate dispersion is 15%~30%.
By with upper type, preparation method of the invention, using silver ammino solution as silver-colored forerunner, can effectively control silver ion
Rate of release, be easy to control galactic nucleus growth rate；It by the use of ethanol as solvent, can unfold polyvinylpyrrolidone macromolecular,
Be advantageous to quickly generate the spherical nano-Ag particles that particle diameter is small and the uniformity is excellent；Polyvinylpyrrolidone and silver ion, which are formed, matches somebody with somebody
Compound, make silver ion be easier to be reduced, effectively prevent growing up and reuniting for Argent grain；Using glucose as reducing agent, to environment
Friendly nonhazardous；The process of Nano silver solution is prepared without drying, the secondary agglomeration of Nano Silver can be reduced, it is ensured that the stabilization of ink
Property；Aqueous polyurethane/polyacrylate is binder, its have high intensity, tear-proof, it is wear-resisting the advantages of, and with excellent
Dissolubility.
Embodiment 1
Step 1, under the conditions of lucifuge, silver nitrate is dissolved in be configured in absolute ethyl alcohol 0.1mol/L silver nitrate ethanol it is molten
Liquid, the ammoniacal liquor that volume fraction is 25% is then slowly added into, obtains silver ammino solution, and it is 9 to adjust it to adjust pH value；By polyethylene
Pyrrolidones is added in silver ammino solution and is well mixed, and temperature rises to 60 DEG C and obtains solution A after stirring 30min；
The mol ratio of polyvinylpyrrolidone and the nitric acid silver ion in silver ammino solution is 1.5:1.
Step 2, the ethanol solution that 1mol/L glucose is added dropwise using constant pressure funnel into solution A, time for adding 5min,
Continue to react 1h after being added dropwise to complete, obtain Nano silver solution；Nano silver solution first is cooled into room temperature to continue to stir 30min, then
Centrifuged after Nano silver solution is diluted with absolute ethyl alcohol, the rotating speed of centrifuge is 10000rpm, time 10min, and nothing
The volume of water-ethanol is 5 times of Nano silver solution volume；Then use absolute ethyl alcohol repeated washing 7 times, finally remove a layer colloid and add
Enter absolute ethyl alcohol and re-start ultrasonic disperse, obtain Nano Silver alcohol dispersion liquid.
Step 3, first the Nano Silver alcohol dispersion liquid obtained through step 2 is placed in vacuum drying chamber, by the matter of Nano Silver
Amount fraction is adjusted to 30%, and solvent is then added into Nano Silver alcohol dispersion liquid obtains solution B, then matter is added into solution B
Aqueous polyurethane/polyacrylate dispersion that fraction is 15% is measured, obtains solution C；It will be shifted after solution C ultrasonic disperse 30min
Continue to stir 30min on to magnetic stirring apparatus, obtain Nano silver conductive ink and obtain Nano silver conductive ink；
Solvent is the mixture of deionized water, ethanol and glycerine, and the volume ratio of three is 1：2：3, mass fraction is
50%.
Embodiment 2
Step 1, under the conditions of lucifuge, silver nitrate is dissolved in be configured in absolute ethyl alcohol 0.1mol/L silver nitrate ethanol it is molten
Liquid, the ammoniacal liquor that volume fraction is 25% is then slowly added into, obtains silver ammino solution, and it is 10 to adjust it to adjust pH value；By poly- second
Alkene pyrrolidone is added in silver ammino solution and is well mixed, and temperature rises to 55 DEG C and obtains solution A after stirring 25min；
The mol ratio of polyvinylpyrrolidone and the nitric acid silver ion in silver ammino solution is 1.5:1.
Step 2, the ethanol solution that 1mol/L glucose is added dropwise using constant pressure funnel into solution A, time for adding 5min,
Continue to react 0.8h after being added dropwise to complete, obtain Nano silver solution；Nano silver solution first is cooled into room temperature to continue to stir 25min,
Being centrifuged after Nano silver solution is diluted with absolute ethyl alcohol again, the rotating speed of centrifuge is 10000rpm, time 10min, and
The volume of absolute ethyl alcohol is 4 times of Nano silver solution volume；Then use absolute ethyl alcohol repeated washing 6 times, finally remove a layer colloid
Add absolute ethyl alcohol and re-start ultrasonic disperse, obtain Nano Silver alcohol dispersion liquid.
Step 3, first the Nano Silver alcohol dispersion liquid obtained through step 2 is placed in vacuum drying chamber, by the matter of Nano Silver
Amount fraction is adjusted to 40%, and solvent is then added into Nano Silver alcohol dispersion liquid obtains solution B, then matter is added into solution B
Aqueous polyurethane/polyacrylate dispersion that fraction is 20% is measured, obtains solution C；It will be shifted after solution C ultrasonic disperse 25min
Continue to stir 30min on to magnetic stirring apparatus, obtain Nano silver conductive ink and obtain Nano silver conductive ink；
Solvent is the mixture of deionized water, ethanol and glycerine, and the volume ratio of three is 1：2：3, mass fraction is
40%.
Embodiment 3
Step 1, under the conditions of lucifuge, silver nitrate is dissolved in be configured in absolute ethyl alcohol 0.1mol/L silver nitrate ethanol it is molten
Liquid, the ammoniacal liquor that volume fraction is 25% is then slowly added into, obtains silver ammino solution, and adjust its pH value as 10；By polyethylene pyrrole
Pyrrolidone is added in silver ammino solution and is well mixed, and temperature rises to 65 DEG C and obtains solution A after stirring 35min；
The mol ratio of polyvinylpyrrolidone and the nitric acid silver ion in silver ammino solution is 1.5:1.
Step 2, the ethanol solution that 1mol/L glucose is added dropwise using constant pressure funnel into solution A, time for adding 5min,
Continue to react 1.2h after being added dropwise to complete, obtain Nano silver solution；Nano silver solution first is cooled into room temperature to continue to stir 35min,
Being centrifuged after Nano silver solution is diluted with absolute ethyl alcohol again, the rotating speed of centrifuge is 10000rpm, time 10min, and
The volume of absolute ethyl alcohol is 3 times of Nano silver solution volume；Then use absolute ethyl alcohol repeated washing 5 times, finally remove a layer colloid
Add absolute ethyl alcohol and re-start ultrasonic disperse, obtain Nano Silver alcohol dispersion liquid.
Step 3, first the Nano Silver alcohol dispersion liquid obtained through step 2 is placed in vacuum drying chamber, by the matter of Nano Silver
Amount fraction is adjusted to 50%, and solvent is then added into Nano Silver alcohol dispersion liquid obtains solution B, then matter is added into solution B
Aqueous polyurethane/polyacrylate dispersion that fraction is 20% is measured, obtains solution C；It will be shifted after solution C ultrasonic disperse 35min
Continue to stir 35min on to magnetic stirring apparatus, obtain Nano silver conductive ink and obtain Nano silver conductive ink；
Solvent is the mixture of deionized water, ethanol and glycerine, and the volume ratio of three is 1：2：3, mass fraction is
30%.
Embodiment 4
Step 1, under the conditions of lucifuge, silver nitrate is dissolved in be configured in absolute ethyl alcohol 0.1mol/L silver nitrate ethanol it is molten
Liquid, the ammoniacal liquor that volume fraction is 25% is then slowly added into, obtains silver ammino solution, and adjust its pH value as 10；By polyethylene pyrrole
Pyrrolidone is added in silver ammino solution and is well mixed, and temperature rises to 60 DEG C and obtains solution A after stirring 30min；
The mol ratio of polyvinylpyrrolidone and the nitric acid silver ion in silver ammino solution is 1.5:1.
Step 2, the ethanol solution that 1mol/L glucose is added dropwise using constant pressure funnel into solution A, time for adding 5min,
Continue to react 1.0h after being added dropwise to complete, obtain Nano silver solution；Nano silver solution first is cooled into room temperature to continue to stir 30min,
Being centrifuged after Nano silver solution is diluted with absolute ethyl alcohol again, the rotating speed of centrifuge is 10000rpm, time 10min, and
The volume of absolute ethyl alcohol is 5 times of Nano silver solution volume；Then use absolute ethyl alcohol repeated washing 5-7 times, finally remove a layer glue
Body adds absolute ethyl alcohol and re-starts ultrasonic disperse, obtains Nano Silver alcohol dispersion liquid.
Step 3, first the Nano Silver alcohol dispersion liquid obtained through step 2 is placed in vacuum drying chamber, by the matter of Nano Silver
Amount fraction is adjusted to 60%, and solvent is then added into Nano Silver alcohol dispersion liquid obtains solution B, then matter is added into solution B
Aqueous polyurethane/polyacrylate dispersion that fraction is 20% is measured, obtains solution C；It will be shifted after solution C ultrasonic disperse 30min
Continue to stir 30min on to magnetic stirring apparatus, obtain Nano silver conductive ink and obtain Nano silver conductive ink；
Solvent is the mixture of deionized water, ethanol and glycerine, and the volume ratio of three is 1：2：3, mass fraction is
20%.
Embodiment 5
Step 1, under the conditions of lucifuge, silver nitrate is dissolved in be configured in absolute ethyl alcohol 0.1mol/L silver nitrate ethanol it is molten
Liquid, the ammoniacal liquor that volume fraction is 25% is then slowly added into, obtains silver ammino solution, and adjust its pH value as 10；By polyethylene pyrrole
Pyrrolidone is added in silver ammino solution and is well mixed, and temperature rises to 60 DEG C and obtains solution A after stirring 30min；
The mol ratio of polyvinylpyrrolidone and the nitric acid silver ion in silver ammino solution is 1.5:1.
Step 2, the ethanol solution that 1mol/L glucose is added dropwise using constant pressure funnel into solution A, time for adding 5min,
Continue to react 1.0h after being added dropwise to complete, obtain Nano silver solution；Nano silver solution first is cooled into room temperature to continue to stir 35min,
Being centrifuged after Nano silver solution is diluted with absolute ethyl alcohol again, the rotating speed of centrifuge is 10000rpm, time 10min, and
The volume of absolute ethyl alcohol is 3 times of Nano silver solution volume；Then use absolute ethyl alcohol repeated washing 5 times, finally remove a layer colloid
Add absolute ethyl alcohol and re-start ultrasonic disperse, obtain Nano Silver alcohol dispersion liquid.
Step 3, first the Nano Silver alcohol dispersion liquid obtained through step 2 is placed in vacuum drying chamber, by the matter of Nano Silver
Amount fraction is adjusted to 70%, and solvent is then added into Nano Silver alcohol dispersion liquid obtains solution B, then matter is added into solution B
Aqueous polyurethane/polyacrylate dispersion that fraction is 20% is measured, obtains solution C；It will be shifted after solution C ultrasonic disperse 30min
Continue to stir 30min on to magnetic stirring apparatus, obtain Nano silver conductive ink and obtain Nano silver conductive ink；
Solvent is the mixture of deionized water, ethanol and glycerine, and the volume ratio of three is 1：2：3, mass fraction is
10%.
The electrically conductive ink that the preparation method of the present invention obtains is coated on art paper with four sides preparing device, is 25 in temperature
DEG C, 70 DEG C, 100 DEG C, sinter 1h under conditions of 130 DEG C and 160 DEG C, you can obtain printing product.
Detection indicate that ink film Glabrous pierces after the electrically conductive ink printing that preparation method of the invention obtains, film layer is thick
Spend for 20 μm, electric conductivity is good, and ink resistivity as shown in Figure 1 is minimum to can reach 1.67 × 10-7Ω m, energy printability is in soft
Property base material.
Claims (7)
- A kind of 1. preparation method of Nano silver conductive ink, it is characterised in that first using silver ammino solution be silver-colored forerunner, glucose be and also Former agent and polyvinylpyrrolidone are that Nano Silver alcohol dispersion liquid is prepared in scattered protective agent；Again by aqueous polyurethane/poly- Nano silver conductive ink is prepared with Nano Silver alcohol dispersion liquid in acrylate.
- 2. a kind of preparation method of Nano silver conductive ink as claimed in claim 1, it is characterised in that specifically include following step Suddenly：Step 1, by polyvinylpyrrolidone be added in silver ammino solution be well mixed, temperature rises to 55 DEG C~65 DEG C, and stirs Solution A is obtained after 25min~35min；Step 2, into solution A be added dropwise glucose ethanol solution, and continue react 0.8h~1.2h, obtain Nano silver solution； 25min~35min is stirred after first Nano silver solution is cooled down, then is centrifuged after Nano silver solution is diluted, then with anhydrous Ethanol repeated washing 5~7 times, finally take out lower floor's colloid and add absolute ethyl alcohol and re-start ultrasonic disperse, obtain Nano Silver Alcohol dispersion liquid；Step 3, the mass fraction of the Nano Silver in the Nano Silver alcohol dispersion liquid obtained through step 2 is first adjusted to 30%~ 70%, then add solvent into Nano Silver alcohol dispersion liquid and obtain solution B, aqueous polyurethane/poly- third is then added into solution B Olefin(e) acid ester emulsion, obtains solution C, continues to stir by being transferred on magnetic stirring apparatus after solution C ultrasonic disperse, obtains Nano Silver and lead Electric ink.
- 3. a kind of preparation method of Nano silver conductive ink as claimed in claim 2, it is characterised in that in the step 1：It is poly- The mol ratio of vinylpyrrolidone and the nitric acid silver ion in silver ammino solution is 1.5:1.
- 4. a kind of preparation method of Nano silver conductive ink as claimed in claim 2, it is characterised in that in the step 2：Portugal The concentration of the ethanol solution of grape sugar is 1mol/L；The solvent of dilution Nano silver solution is absolute ethyl alcohol, and the volume of absolute ethyl alcohol For 3~5 times of Nano silver solution.
- A kind of 5. preparation method of Nano silver conductive ink as claimed in claim 2, it is characterised in that the centrifugal process In：The rotating speed of centrifuge is 10000rpm, time 10min.
- 6. a kind of preparation method of Nano silver conductive ink as claimed in claim 2, it is characterised in that molten in the step 3 Agent is the mixture of deionized water, ethanol and glycerine, and the volume ratio of three is 1：2：3, the mass fraction of solvent is 10% ~50%.
- 7. a kind of preparation method of Nano silver conductive ink as claimed in claim 2, it is characterised in that the step 3 is received In the silver-colored electrically conductive ink of rice：The mass fraction of aqueous polyurethane/polyacrylate dispersion is 15%~30%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710986060.9A CN107793842A (en) | 2017-10-20 | 2017-10-20 | A kind of preparation method of Nano silver conductive ink |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710986060.9A CN107793842A (en) | 2017-10-20 | 2017-10-20 | A kind of preparation method of Nano silver conductive ink |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107793842A true CN107793842A (en) | 2018-03-13 |
Family
ID=61533807
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710986060.9A Pending CN107793842A (en) | 2017-10-20 | 2017-10-20 | A kind of preparation method of Nano silver conductive ink |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107793842A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108659624A (en) * | 2018-04-17 | 2018-10-16 | 句容市合力印刷有限公司 | A kind of preparation method of nano silver composite conducting ink |
| CN108907228A (en) * | 2018-07-24 | 2018-11-30 | 郑州阿弗雷德化工科技有限公司 | Nano silver solution and its inexpensive synthetic method |
| CN109535847A (en) * | 2018-11-26 | 2019-03-29 | 国宏中晶集团有限公司 | The electrically conductive ink and preparation method and flexible-paper-base conducting wire of a kind of containing graphene |
| CN110181071A (en) * | 2019-05-14 | 2019-08-30 | 深圳先进技术研究院 | Nano-Ag particles and its preparation method and application |
| CN110922812A (en) * | 2018-08-31 | 2020-03-27 | 王笑非 | Low-temperature high-conductivity nano-silver conductive ink and preparation method and application thereof |
| CN111097922A (en) * | 2020-02-21 | 2020-05-05 | 深圳先进技术研究院 | Nano silver particle and preparation method and application thereof |
| CN111992736A (en) * | 2020-08-28 | 2020-11-27 | 西北有色金属研究院 | Preparation method of silver nanoparticles |
| CN111992737A (en) * | 2020-09-02 | 2020-11-27 | 深圳市普瑞威科技有限公司 | Preparation method of conductive silver paste |
| CN114226747A (en) * | 2021-12-20 | 2022-03-25 | 贵阳学院 | Preparation method of nano-silver particles with good ethanol dispersibility |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102220045A (en) * | 2010-04-16 | 2011-10-19 | 上海亿金纳米科技有限公司 | Low-temperature-sintered solvent-based nano-silver electroconductive ink and preparation process thereof |
| CN102286226A (en) * | 2011-06-20 | 2011-12-21 | 中国科学院宁波材料技术与工程研究所 | Colorless transparent conductive ink as well as preparation method and application thereof |
-
2017
- 2017-10-20 CN CN201710986060.9A patent/CN107793842A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102220045A (en) * | 2010-04-16 | 2011-10-19 | 上海亿金纳米科技有限公司 | Low-temperature-sintered solvent-based nano-silver electroconductive ink and preparation process thereof |
| CN102286226A (en) * | 2011-06-20 | 2011-12-21 | 中国科学院宁波材料技术与工程研究所 | Colorless transparent conductive ink as well as preparation method and application thereof |
Non-Patent Citations (5)
| Title |
|---|
| 唐宝玲: "UV型纳米银导电油墨的制备及性能研究", 《中国博士学位论文全文数据库工程技术I辑》 * |
| 支力: "金属导电油墨（铜、银及铜银核壳颗粒）的制备及其导电性能研究", 《中国优秀硕士学位论文全文数据库 工程技术Ⅱ辑》 * |
| 李路海: "《印刷包装功能材料》", 31 January 2013, 中国轻工业出版社 * |
| 陈艳艳等: "不同溶剂体系生成纳米银形貌研究", 《包装工程》 * |
| 霍李江: "《丝网印刷实用技术》", 31 July 2008, 印刷工业出版社 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108659624A (en) * | 2018-04-17 | 2018-10-16 | 句容市合力印刷有限公司 | A kind of preparation method of nano silver composite conducting ink |
| CN108907228A (en) * | 2018-07-24 | 2018-11-30 | 郑州阿弗雷德化工科技有限公司 | Nano silver solution and its inexpensive synthetic method |
| CN110922812A (en) * | 2018-08-31 | 2020-03-27 | 王笑非 | Low-temperature high-conductivity nano-silver conductive ink and preparation method and application thereof |
| CN109535847A (en) * | 2018-11-26 | 2019-03-29 | 国宏中晶集团有限公司 | The electrically conductive ink and preparation method and flexible-paper-base conducting wire of a kind of containing graphene |
| CN109535847B (en) * | 2018-11-26 | 2021-12-28 | 国宏中晶集团有限公司 | Graphene-containing conductive ink, preparation method thereof and flexible paper-based conductive circuit |
| CN110181071A (en) * | 2019-05-14 | 2019-08-30 | 深圳先进技术研究院 | Nano-Ag particles and its preparation method and application |
| CN111097922A (en) * | 2020-02-21 | 2020-05-05 | 深圳先进技术研究院 | Nano silver particle and preparation method and application thereof |
| CN111992736A (en) * | 2020-08-28 | 2020-11-27 | 西北有色金属研究院 | Preparation method of silver nanoparticles |
| CN111992737A (en) * | 2020-09-02 | 2020-11-27 | 深圳市普瑞威科技有限公司 | Preparation method of conductive silver paste |
| CN111992737B (en) * | 2020-09-02 | 2023-03-10 | 深圳市普瑞威科技有限公司 | Preparation method of conductive silver paste |
| CN114226747A (en) * | 2021-12-20 | 2022-03-25 | 贵阳学院 | Preparation method of nano-silver particles with good ethanol dispersibility |
| CN114226747B (en) * | 2021-12-20 | 2024-02-20 | 贵阳学院 | Preparation method of nano silver particles with good ethanol dispersibility |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107793842A (en) | A kind of preparation method of Nano silver conductive ink | |
| CN104923801B (en) | A kind of method that mass prepares nano-silver powder | |
| CN104263082B (en) | Graphene organic silver conductive printing ink and preparation method thereof | |
| CN101805538B (en) | Lower-temperature sintered conductive ink | |
| CN104277592B (en) | A kind of graphene-based water-base ink and the application of the transparent pattern conductive electrode of inkjet printing thereof | |
| CN102093774B (en) | Conductive ink and preparation method thereof | |
| CN106928773A (en) | It is a kind of to can be used for graphene composite conductive ink of inkjet printing and preparation method thereof | |
| CN101719392B (en) | Preparation method of screen printing water-based conductive paste based on carbon-copper composite packing | |
| CN109773211A (en) | A kind of preparation method in flake silver powder surface cladding nano-Ag particles | |
| CN106590173A (en) | Nano-metal ink capable of being cured at low temperatures, preparation method therefor and application of nano-metal ink | |
| CN108659624A (en) | A kind of preparation method of nano silver composite conducting ink | |
| CN106205776A (en) | Low temperature curing type Graphene/conductive silver slurry and its preparation method and application | |
| CN106903324A (en) | A kind of preparation method of Graphene-nano silver dispersion | |
| CN109226993A (en) | A kind of micron of copper-silver paste Heat Conduction Material and preparation method thereof | |
| CN104479456B (en) | The application of a kind of gold contracted payment-graphene-based water-base ink and the transparent pattern conductive electrode of spray ink Printing thereof | |
| CN105086630A (en) | Preparation methods of silver nanowires for conductive ink and silver nanowire electrode | |
| CN104569093B (en) | A kind of electrochemical detection test strip is starched and preparation method thereof and a kind of electrochemical detection test strip and preparation method thereof with carbon | |
| CN109401442A (en) | A kind of silver-plated electrically conductive ink of UV curing nano and preparation method thereof | |
| CN109754904A (en) | A kind of laser ablation electrocondution slurry and preparation method thereof | |
| CN105788756B (en) | A kind of transparent metal conducting film and preparation method thereof | |
| TW201307208A (en) | Micro-scaled flake silver particles and method for producing the same | |
| CN105885540A (en) | Preparation method of nano-silver ink for conductive layer of touch screen | |
| CN108641487A (en) | A kind of nano conductive printing ink and preparation method thereof and its RFID antenna and application | |
| CN108735338A (en) | A kind of preparation method of epoxy resin silver powder composite conducting silver paste | |
| CN112820440A (en) | High-conductivity conductive silver paste and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180313 |
|
| RJ01 | Rejection of invention patent application after publication |