CN109401442A - A kind of silver-plated electrically conductive ink of UV curing nano and preparation method thereof - Google Patents
A kind of silver-plated electrically conductive ink of UV curing nano and preparation method thereof Download PDFInfo
- Publication number
- CN109401442A CN109401442A CN201811331838.3A CN201811331838A CN109401442A CN 109401442 A CN109401442 A CN 109401442A CN 201811331838 A CN201811331838 A CN 201811331838A CN 109401442 A CN109401442 A CN 109401442A
- Authority
- CN
- China
- Prior art keywords
- silver
- electrically conductive
- conductive ink
- preparation
- added
- 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
- C09D11/52—Electrically conductive inks
-
- 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
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
-
- 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
- C09D11/101—Inks specially adapted for printing processes involving curing by wave energy or particle radiation, e.g. with UV-curing following the printing
-
- 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
Abstract
The invention discloses a kind of silver-plated electrically conductive inks of UV curing nano and preparation method thereof, and preparation method includes the following steps: cladding substrate being added in reproducibility mixed liquor, ultrasonic wave dispersion instills silver-colored source solution and silver plating reaction occurs；Centrifugation, cleaning, drying, obtain nanometer silver plating particle powder；Nanometer silver plating particle powder 0.5g is weighed, ethyl acetate is added and is stirred evenly, conductive rubber dispersion liquid is obtained；The mass fraction that electrically conductive ink 25% is accounted for according to conductive rubber dispersion liquid calculates the amount that the bridging agent resin for needing to be added and auxiliary agent need；Ultrasonic disperse is carried out to mixed liquor made of bridging agent resin and auxiliary agent, conductive rubber dispersion liquid is added and is stirred evenly, the silver-plated electrically conductive ink of UV curing nano is obtained.The present invention not only can guarantee the excellent electromagnetic performance of silver by the way of silver-plated, but also can be reduced usage amount silver-colored in electrically conductive ink, and the silver layer smoother coated is fine and close, and effect is good, considerably reduces the cost using silver.
Description
Technical field
The present invention relates to light industry chemical technology fields, and in particular to a kind of silver-plated electrically conductive ink of UV curing nano and its preparation
Method.
Background technique
Currently, electrically conductive ink is the key factor of printed electronic in printed electronics.Traditional electrically conductive ink makes
It is volatilized with there are a large amount of organic solvents in the process, and the manufacturing process of electronic circuit is cumbersome, it is at high cost, pole is caused to environment
Big pollution, the problem of also seriously compromising health.UV light-curable ink is one of environmentally protective ink, it, which has, is free of
Have the advantages that the volatile quantity of heavy metal, V DEG C of discharge amount and hazardous solvent is relatively low, therefore prepares UV light curable conductive ink ten
Divide significant.
Particle of the nano silver as Nano grade has special nano-meter characteristic, so that the electric conductivity of nanometer silver ink
Conventional Conductive Inks are also significantly less than far better than Conventional Conductive Inks, sintering temperature.It is organic after nano conductive printing ink is dry
Metallic compound links together nano particle, obtains the electrical efficiency of three times or more.But the cost of nano silver is very high, this
A little it is greatly limited in the application of every field.Therefore under the premise of guaranteeing every characteristic of silver, the use of silver is reduced
It is contemporary problem urgently to be resolved.
Composite granule is the new material that the formation core-shell structure of another substance is coated with a kind of substance.With compound
The appearance of material concept, more and more scientific research scholars start to look for a kind of more preferably combination, more than the two or both
The properties of material are overlapped, to expand the application field of composite material.Core-shell structure is exactly a kind of good composite square
Formula.By cladding so that the substrate being wrapped by not only has the performance of itself, but also the various excellent of coating can also be had both
Function, this has exactly catered to the multi-faceted requirement in production application for composite material.
Summary of the invention
For overcome the deficiencies in the prior art, the purpose of the present invention is to provide a kind of silver-plated electrically conductive inks of UV curing nano
Preparation method.
For achieving the above object, the present invention adopts the following technical scheme:
A kind of preparation method of the silver-plated electrically conductive ink of UV curing nano, comprising the following steps:
(1) preparation of nanometer silver plating particle: cladding substrate is added in reproducibility mixed liquor, ultrasonic wave dispersion；Pass through
Constant pressure funnel, which instills silver-colored source solution in mixed solution, occurs silver plating reaction；After reaction, it is centrifuged, cleans, repeat 3~5 times,
It is dry, obtain nanometer silver plating particle powder；
(2) preparation of ink: weighing nanometer silver plating particle powder 0.5g, and acetic acid second will be added in nanometer silver plating particle powder
Ester simultaneously stirs evenly, and obtains conductive rubber dispersion liquid；Then the quality point of electrically conductive ink 25% is accounted for according to conductive rubber dispersion liquid
Number calculates the amount that the bridging agent resin for needing to be added and auxiliary agent need；It will be mixed made of bridging agent resin and auxiliary agent later
Liquid, which is put into ultrasonic cleaner, carries out ultrasonic disperse；It is dispersed in conductive rubber homogeneous dispersion in mixed liquor, stirs evenly,
Obtain the silver-plated electrically conductive ink of UV curing nano.
As a preferred embodiment of the present invention, the cladding substrate is the micro-sphere material of modified processing, the microballoon
Material is one of silicon dioxide microsphere, charcoal powder, polymer microballoon；Modification, which refers to, reduces cladding substrate surface energy
Processing means, such as electric shock, heat treatment, modifier treatment, preferably modifier treatment.The modifying agent is silane coupling agent, excellent
Select mercaptopropyl trimethoxysilane (MPTMS)；The dosage of the modifying agent is mercaptopropyl trimethoxysilane: micro-sphere material=
0.05~1 (g/g).
As a preferred embodiment of the present invention, the reproducibility mixed liquor refers to that the mixing of reducing agent and dispersing agent is molten
The mass ratio of liquid, the reducing agent and dispersing agent is 0.5~2；The dispersing agent be soluble starch or polyethylene pyrrole network alkanone,
It is preferred that soluble starch；The reducing agent refers to the substance with reproducibility functional group, and reproducibility functional group is aldehyde radical, goes back
Originality hydroxyl etc., preferably corn stover extract.The preparation process of the corn stover extract is as follows: corn stover is washed
Only, dry, wear into maize straw powder；Add boiling to boil maize straw powder again, is crushed through supersonic cell, filtering, freezing
After drying, corn stover extract paste is obtained.
As a preferred embodiment of the present invention, the silver-colored source solution refers to the substance containing silver ion, such as nitric acid
Silver-colored solution or silver ammino solution, preferably silver ammino solution；Silver ammino solution is that laboratory is ready-to-use, the preparation method comprises the following steps: with dilute hydroxide
Sodium (NaOH, 2%) pre-processes 50mL beaker；Take AgNO3It is placed in a beaker, deionized water is added to obtain 10ml AgNO3Solution；By ammonia
Water (2%) is added dropwise in beaker, until the brown oxidation silver dissolution of appearance, obtains silver ammino solution.The concentration of the silver-colored source solution
For 0.06~0.16mol/L.
As a preferred embodiment of the present invention, the reaction temperature of the silver plating reaction be 50 DEG C~90 DEG C, reaction time
For 1~6h.
As a preferred embodiment of the present invention, the quality of the nanometer silver plating particle powder in the conductive rubber dispersion liquid
Score is 50~100%.
As a preferred embodiment of the present invention, the bridging agent resin is super branched polyurethane acrylic resin, described
Auxiliary agent is glycerine or diethylene glycol (DEG).
The present invention also provides a kind of according to the silver-plated electrically conductive ink of UV curing nano made from above-mentioned preparation method.
To solve the above problems, the technical solution adopted in the present invention is as follows:
(1) present invention uses corn stover extract as reducing agent, in safety, environmental protection, sustainability, reproducibility
Etc. have the advantages that it is very big；
(2) present invention is using silica as cladding substrate, acquisition pattern is simple, raw material sources range is wide, it is low at
Originally, stable in physicochemical property；
(3) present invention not only can guarantee the excellent electromagnetic performance of silver by the way of silver-plated, but also can be reduced silver-colored in electrically conductive ink
Usage amount.The smooth densification of cladding silver layer obtained using this preparation method, effect are good.Preferably, as MPTMS and titanium dioxide
Silicon mass ratio 1:5, silver nitrate concentration 0.08mol/L, when silver-plated powder quality score is 90% in dispersion liquid, silver-plated electrically conductive ink
Resistance be 1.09 Ω, conductivity be 9.17 × 104S/m, silver-colored utilization rate reduce 25.4%, considerably reduce answering for silver
Use cost.
Detailed description of the invention
The present invention will be further described with reference to the accompanying drawings, but the embodiment in attached drawing is not constituted to any limit of the invention
System, for those of ordinary skill in the art, without creative efforts, can also obtain according to the following drawings
Other attached drawings.
Fig. 1 is nanometer silver plating particle characterization result obtained in the embodiment of the present invention 3；
Fig. 2 is the energy spectrum diagram of nanometer silver plating particle obtained in the embodiment of the present invention 3.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Based on the contents of the disclosure of the present invention and the scope of each parameter, this can be achieved in the those of ordinary skill of the technical field
Goal of the invention.Each starting material is commercially available in preparation method of the present invention.
Embodiment 1:
A kind of preparation method of the silver-plated electrically conductive ink of UV curing nano, comprising the following steps:
(1) silica is dispersed in dehydrated alcohol, then according to MPTMS:SiO2The ratio of=1:20 (g/g) is added
Mercaptopropyl trimethoxysilane is modified processing, reacts 6h at 70 DEG C；Again by modified suspension 10000rpm's
Under the conditions of be centrifuged, after outwelling supernatant liquor, be added dehydrated alcohol cleaned, repetitive operation 3~5 times, obtain pure
Improved silica；It is finally dried in air dry oven, obtains improved silica.
(2) 50mL beaker is pre-processed with dilute sodium hydroxide (NaOH, 2%)；Take AgNO3It is placed in a beaker, deionization is added
Water obtains 10ml 0.06mol/L AgNO3Solution；Ammonium hydroxide (2%) is added dropwise in beaker, until the brown oxidation silver of appearance
Dissolution, obtains silver ammino solution.At this point, Ag+With [Ag (NH in transparent mixture3)2] form of OH complex compound exists, and use
Deionized water is by [Ag (NH3)2] OH complex solution is diluted to 20mL.Then, by the dosage of corn stover extract and silver nitrate
Than 1g:0.20g, corn stover extract powder and soluble starch are put into 150mL flask, and 70 DEG C at a temperature of with
Deionized water (18ml) mixing dispersion 30 minutes, obtain reproducibility mixed liquor；Improved silica is added, ultrasonic wave disperses 30 points
Clock；Later, by constant pressure funnel with the speed of 20 drop per minute by [Ag (NH3)2] OH complex solution instill reproducibility mixing it is molten
In liquid, 3h is reacted at 70 DEG C；After reaction, reactant solution is centrifuged under conditions of 10000rpm, outwells upper layer
After clear liquid, dehydrated alcohol is added and is cleaned, repetitive operation 3~5 times, obtains nanometer silver plating particle；Finally in air dry oven
In dried, obtain nanometer silver plating particle powder.
(3) the nanometer silver plating particle powder 0.5g for weighing above-mentioned preparation, is added into ethyl acetate and stirs evenly, according to
The mass fraction of nanometer silver plating particle powder is that 50%, conductive rubber dispersion liquid accounts for electrically conductive ink 25% in conductive rubber dispersion liquid
Mass fraction, calculate the amount for needing the bridging agent resin that is added and auxiliary agent to need.Later by bridging agent resin and auxiliary agent system
At mixed liquor be put into ultrasonic cleaner and carry out ultrasonic disperse；It is dispersed in conductive rubber homogeneous dispersion in mixed liquor,
It stirs evenly, obtains the silver-plated electrically conductive ink of UV curing nano.
Embodiment 2:
A kind of preparation method of the silver-plated electrically conductive ink of UV curing nano, comprising the following steps:
(1) silica is dispersed in dehydrated alcohol, then according to MPTMS:SiO2The ratio of=1:10 (g/g) is added
Mercaptopropyl trimethoxysilane is modified processing, reacts 6h at 70 DEG C；Again by modified suspension 10000rpm's
Under the conditions of be centrifuged, after outwelling supernatant liquor, be added dehydrated alcohol cleaned, repetitive operation 3~5 times, obtain pure
Improved silica；It is finally dried in air dry oven, obtains improved silica.
(2) 50mL beaker is pre-processed with dilute sodium hydroxide (NaOH, 2%)；Take AgNO3It is placed in a beaker, deionization is added
Water obtains 10ml 0.01mol/L AgNO3Solution；Ammonium hydroxide (2%) is added dropwise in beaker, until the brown oxidation silver of appearance
Dissolution, obtains silver ammino solution.At this point, Ag+With [Ag (NH in transparent mixture3)2] form of OH complex compound exists, and use
Deionized water is by [Ag (NH3)2] OH complex solution is diluted to 20mL.Then, by the dosage of corn stover extract and silver nitrate
Than 1g:0.20g, corn stover extract powder and soluble starch are put into 150mL flask, and 70 DEG C at a temperature of with
Deionized water (18ml) mixing dispersion 30 minutes, obtain reproducibility mixed liquor；Improved silica is added, ultrasonic wave disperses 30 points
Clock；Later, by constant pressure funnel with the speed of 20 drop per minute by [Ag (NH3)2] OH complex solution instill reproducibility mixing it is molten
In liquid, 2h is reacted at 60 DEG C；After reaction, reactant solution is centrifuged under conditions of 10000rpm, outwells upper layer
After clear liquid, dehydrated alcohol is added and is cleaned, repetitive operation 3~5 times, obtains nanometer silver plating particle；Finally in air dry oven
In dried, obtain nanometer silver plating particle powder.
(3) the nanometer silver plating particle powder 0.5g for weighing above-mentioned preparation, is added into ethyl acetate and stirs evenly, according to
The mass fraction of nanometer silver plating particle powder is that 60%, conductive rubber dispersion liquid accounts for electrically conductive ink 25% in conductive rubber dispersion liquid
Mass fraction, calculate the amount for needing the bridging agent resin that is added and auxiliary agent to need.Later by bridging agent resin and auxiliary agent system
At mixed liquor be put into ultrasonic cleaner and carry out ultrasonic disperse；It is dispersed in conductive rubber homogeneous dispersion in mixed liquor,
It stirs evenly, obtains the silver-plated electrically conductive ink of UV curing nano.
Embodiment 3:
A kind of preparation method of the silver-plated electrically conductive ink of UV curing nano, comprising the following steps:
(1) silica is dispersed in dehydrated alcohol, then according to MPTMS:SiO2The ratio of=1:5 (g/g) is added
Mercaptopropyl trimethoxysilane is modified processing, reacts 6h at 70 DEG C；Again by modified suspension 10000rpm's
Under the conditions of be centrifuged, after outwelling supernatant liquor, be added dehydrated alcohol cleaned, repetitive operation 3~5 times, obtain pure
Improved silica；It is finally dried in air dry oven, obtains improved silica.
(2) 50mL beaker is pre-processed with dilute sodium hydroxide (NaOH, 2%)；Take AgNO3It is placed in a beaker, deionization is added
Water obtains 10ml 0.08mol/L AgNO3Solution；Ammonium hydroxide (2%) is added dropwise in beaker, until the brown oxidation silver of appearance
Dissolution, obtains silver ammino solution.At this point, Ag+With [Ag (NH in transparent mixture3)2] form of OH complex compound exists, and use
Deionized water is by [Ag (NH3)2] OH complex solution is diluted to 20mL.Then, by the dosage of corn stover extract and silver nitrate
Than 1g:0.20g, corn stover extract powder and soluble starch are put into 150mL flask, and 70 DEG C at a temperature of with
Deionized water (18ml) mixing dispersion 30 minutes, obtain reproducibility mixed liquor；Improved silica is added, ultrasonic wave disperses 30 points
Clock；Later, by constant pressure funnel with the speed of 20 drop per minute by [Ag (NH3)2] OH complex solution instill reproducibility mixing it is molten
In liquid, 1h is reacted at 70 DEG C；After reaction, reactant solution is centrifuged under conditions of 10000rpm, outwells upper layer
After clear liquid, dehydrated alcohol is added and is cleaned, repetitive operation 3~5 times, obtains nanometer silver plating particle；Finally in air dry oven
In dried, obtain nanometer silver plating particle powder.As shown in Figure 1, being plated on the silicon-dioxide powdery surface that partial size is 80nm
A layer thickness is about the silver of 4nm, and the silver layer smoother coated is fine and close, illustrates that covered effect is fine.Fig. 2 is silver-colored packet
The energy spectrum diagram for covering silicon dioxide granule can intuitively be found out very much from Fig. 2, and there are SiO in the ingredient of particle2And Ag, counterevidence
The coating of particle is exactly silver on transmission electron microscope.
(3) the nanometer silver plating particle powder 0.5g for weighing above-mentioned preparation, is added into ethyl acetate and stirs evenly, according to
The mass fraction of nanometer silver plating particle powder is that 70%, conductive rubber dispersion liquid accounts for electrically conductive ink 25% in conductive rubber dispersion liquid
Mass fraction, calculate the amount for needing the bridging agent resin that is added and auxiliary agent to need.Later by bridging agent resin and auxiliary agent system
At mixed liquor be put into ultrasonic cleaner and carry out ultrasonic disperse；It is dispersed in conductive rubber homogeneous dispersion in mixed liquor,
It stirs evenly, obtains the silver-plated electrically conductive ink of UV curing nano.
Embodiment 4:
A kind of preparation method of the silver-plated electrically conductive ink of UV curing nano, comprising the following steps:
(1) silica is dispersed in dehydrated alcohol, then according to MPTMS:SiO2The ratio of=2:5 (g/g) is added
Mercaptopropyl trimethoxysilane is modified processing, reacts 6h at 70 DEG C；Again by modified suspension 10000rpm's
Under the conditions of be centrifuged, after outwelling supernatant liquor, be added dehydrated alcohol cleaned, repetitive operation 3~5 times, obtain pure
Improved silica；It is finally dried in air dry oven, obtains improved silica.
(2) 50mL beaker is pre-processed with dilute sodium hydroxide (NaOH, 2%)；Take AgNO3It is placed in a beaker, deionization is added
Water obtains 10ml 0.08mol/L AgNO3Solution；Ammonium hydroxide (2%) is added dropwise in beaker, until the brown oxidation silver of appearance
Dissolution, obtains silver ammino solution.At this point, Ag+With [Ag (NH in transparent mixture3)2] form of OH complex compound exists, and use
Deionized water is by [Ag (NH3)2] OH complex solution is diluted to 20mL.Then, by the dosage of corn stover extract and silver nitrate
Than 1g:0.20g, corn stover extract powder and soluble starch are put into 150mL flask, and 70 DEG C at a temperature of with
Deionized water (18ml) mixing dispersion 30 minutes, obtain reproducibility mixed liquor；Improved silica is added, ultrasonic wave disperses 30 points
Clock；Later, by constant pressure funnel with the speed of 20 drop per minute by [Ag (NH3)2] OH complex solution instill reproducibility mixing it is molten
In liquid, 1h is reacted at 80 DEG C；After reaction, reactant solution is centrifuged under conditions of 10000rpm, outwells upper layer
After clear liquid, dehydrated alcohol is added and is cleaned, repetitive operation 3~5 times, obtains nanometer silver plating particle；Finally in air dry oven
In dried, obtain nanometer silver plating particle powder.
(3) the nanometer silver plating particle powder 0.5g for weighing above-mentioned preparation, is added into ethyl acetate and stirs evenly, according to
The mass fraction of nanometer silver plating particle powder is that 90%, conductive rubber dispersion liquid accounts for electrically conductive ink 25% in conductive rubber dispersion liquid
Mass fraction, calculate the amount for needing the bridging agent resin that is added and auxiliary agent to need.Later by bridging agent resin and auxiliary agent system
At mixed liquor be put into ultrasonic cleaner and carry out ultrasonic disperse；It is dispersed in conductive rubber homogeneous dispersion in mixed liquor,
It stirs evenly, obtains the silver-plated electrically conductive ink of UV curing nano.
Embodiment 5:
A kind of preparation method of the silver-plated electrically conductive ink of UV curing nano, comprising the following steps:
(1) silica is dispersed in dehydrated alcohol, then according to MPTMS:SiO2The ratio of=3:5 (g/g) is added
Mercaptopropyl trimethoxysilane is modified processing, reacts 6h at 70 DEG C；Again by modified suspension 10000rpm's
Under the conditions of be centrifuged, after outwelling supernatant liquor, be added dehydrated alcohol cleaned, repetitive operation 3~5 times, obtain pure
Improved silica；It is finally dried in air dry oven, obtains improved silica.
(2) 50mL beaker is pre-processed with dilute sodium hydroxide (NaOH, 2%)；Take AgNO3It is placed in a beaker, deionization is added
Water obtains 10ml 0.12mol/L AgNO3Solution；Ammonium hydroxide (2%) is added dropwise in beaker, until the brown oxidation silver of appearance
Dissolution, obtains silver ammino solution.At this point, Ag+With [Ag (NH in transparent mixture3)2] form of OH complex compound exists, and use
Deionized water is by [Ag (NH3)2] OH complex solution is diluted to 20mL.Then, by the dosage of corn stover extract and silver nitrate
Than 1g:0.20g, corn stover extract powder and soluble starch are put into 150mL flask, and 70 DEG C at a temperature of with
Deionized water (18ml) mixing dispersion 30 minutes, obtain reproducibility mixed liquor；Improved silica is added, ultrasonic wave disperses 30 points
Clock；Later, by constant pressure funnel with the speed of 20 drop per minute by [Ag (NH3)2] OH complex solution instill reproducibility mixing it is molten
In liquid, 4h is reacted at 80 DEG C；After reaction, reactant solution is centrifuged under conditions of 10000rpm, outwells upper layer
After clear liquid, dehydrated alcohol is added and is cleaned, repetitive operation 3~5 times, obtains nanometer silver plating particle；Finally in air dry oven
In dried, obtain nanometer silver plating particle powder.
(3) the nanometer silver plating particle powder 0.5g for weighing above-mentioned preparation, is added into ethyl acetate and stirs evenly, according to
The mass fraction of nanometer silver plating particle powder is that 100%, conductive rubber dispersion liquid accounts for electrically conductive ink in conductive rubber dispersion liquid
25% mass fraction calculates the amount that the bridging agent resin for needing to be added and auxiliary agent need.It by bridging agent resin and helps later
Mixed liquor made of agent, which is put into ultrasonic cleaner, carries out ultrasonic disperse；Conductive rubber homogeneous dispersion is set to be dispersed in mixed liquor
In, it stirs evenly, obtains the silver-plated electrically conductive ink of UV curing nano.
Embodiment 6:
A kind of preparation method of the silver-plated electrically conductive ink of UV curing nano, comprising the following steps:
(1) silica is dispersed in dehydrated alcohol, then according to MPTMS:SiO2The ratio of=4:5 (g/g) is added
Mercaptopropyl trimethoxysilane is modified processing, reacts 6h at 70 DEG C；Again by modified suspension 10000rpm's
Under the conditions of be centrifuged, after outwelling supernatant liquor, be added dehydrated alcohol cleaned, repetitive operation 3~5 times, obtain pure
Improved silica；It is finally dried in air dry oven, obtains improved silica.
(2) 50mL beaker is pre-processed with dilute sodium hydroxide (NaOH, 2%)；Take AgNO3It is placed in a beaker, deionization is added
Water obtains 10ml 0.14mol/L AgNO3Solution；Ammonium hydroxide (2%) is added dropwise in beaker, until the brown oxidation silver of appearance
Dissolution, obtains silver ammino solution.At this point, Ag+With [Ag (NH in transparent mixture3)2] form of OH complex compound exists, and use
Deionized water is by [Ag (NH3)2] OH complex solution is diluted to 20mL.Then, by the dosage of corn stover extract and silver nitrate
Than 1g:0.20g, corn stover extract powder and soluble starch are put into 150mL flask, and 70 DEG C at a temperature of with
Deionized water (18ml) mixing dispersion 30 minutes, obtain reproducibility mixed liquor；Improved silica is added, ultrasonic wave disperses 30 points
Clock；Later, by constant pressure funnel with the speed of 20 drop per minute by [Ag (NH3)2] OH complex solution instill reproducibility mixing it is molten
In liquid, 5h is reacted at 90 DEG C；After reaction, reactant solution is centrifuged under conditions of 10000rpm, outwells upper layer
After clear liquid, dehydrated alcohol is added and is cleaned, repetitive operation 3~5 times, obtains nanometer silver plating particle；Finally in air dry oven
In dried, obtain nanometer silver plating particle powder.
(3) the nanometer silver plating particle powder 0.5g for weighing above-mentioned preparation, is added into ethyl acetate and stirs evenly, according to
The mass fraction of nanometer silver plating particle powder is that 70%, conductive rubber dispersion liquid accounts for electrically conductive ink 25% in conductive rubber dispersion liquid
Mass fraction, calculate the amount for needing the bridging agent resin that is added and auxiliary agent to need；Later by bridging agent resin and auxiliary agent system
At mixed liquor be put into ultrasonic cleaner and carry out ultrasonic disperse；It is dispersed in conductive rubber homogeneous dispersion in mixed liquor,
It stirs evenly, obtains the silver-plated electrically conductive ink of UV curing nano.
Embodiment 7:
A kind of preparation method of the silver-plated electrically conductive ink of UV curing nano, comprising the following steps:
(1) silica is dispersed in dehydrated alcohol, then according to MPTMS:SiO2The ratio of=1:1 (g/g) is added
Mercaptopropyl trimethoxysilane is modified processing, reacts 6h at 70 DEG C；Again by modified suspension 10000rpm's
Under the conditions of be centrifuged, after outwelling supernatant liquor, be added dehydrated alcohol cleaned, repetitive operation 3~5 times, obtain pure
Improved silica；It is finally dried in air dry oven, obtains improved silica.
(2) 50mL beaker is pre-processed with dilute sodium hydroxide (NaOH, 2%)；Take AgNO3It is placed in a beaker, deionization is added
Water obtains 10ml 0.16mol/L AgNO3Solution；Ammonium hydroxide (2%) is added dropwise in beaker, until the brown oxidation silver of appearance
Dissolution, obtains silver ammino solution.At this point, Ag+With [Ag (NH in transparent mixture3)2] form of OH complex compound exists, and use
Deionized water is by [Ag (NH3)2] OH complex solution is diluted to 20mL.Then, by the dosage of corn stover extract and silver nitrate
Than 1g:0.20g, corn stover extract powder and soluble starch are put into 150mL flask, and 70 DEG C at a temperature of with
Deionized water (18ml) mixing dispersion 30 minutes, obtain reproducibility mixed liquor；Improved silica is added, ultrasonic wave disperses 30 points
Clock；Later, by constant pressure funnel with the speed of 20 drop per minute by [Ag (NH3)2] OH complex solution instill reproducibility mixing it is molten
In liquid, 6h is reacted at 70 DEG C；After reaction, reactant solution is centrifuged under conditions of 10000rpm, outwells upper layer
After clear liquid, dehydrated alcohol is added and is cleaned, repetitive operation 3~5 times, obtains nanometer silver plating particle；Finally in air dry oven
In dried, obtain nanometer silver plating particle powder.
(3) the nanometer silver plating particle powder 0.5g for weighing above-mentioned preparation, is added into ethyl acetate and stirs evenly, according to
The mass fraction of nanometer silver plating particle powder is that 80%, conductive rubber dispersion liquid accounts for electrically conductive ink 25% in conductive rubber dispersion liquid
Mass fraction, calculate the amount for needing the bridging agent resin that is added and auxiliary agent to need.Later by bridging agent resin and auxiliary agent system
At mixed liquor be put into ultrasonic cleaner and carry out ultrasonic disperse；It is dispersed in conductive rubber homogeneous dispersion in mixed liquor,
It stirs evenly, obtains the silver-plated electrically conductive ink of UV curing nano.
Compliance test result:
The electrically conductive ink that nanometer fine silver particle content is 30%~80% in conductive rubber dispersion liquid is prepared with fine silver, as
Comparative example；On the basis of embodiment 3, change nanometer silver plating particle content in conductive rubber dispersion liquid, prepares nanometer plating respectively
The silver-plated electrically conductive ink of UV curing nano that silver particles content is 70%~100%, as experimental example；It is tested and is distinguished using four probes
Electric conductivity is measured, the results are shown in Table 1:
The silver-plated electrically conductive ink of table 1 is compared with fine silver electrically conductive ink electric conductivity
As known from Table 1, when fine silver particle content is 80%, the conductivity best (2.3 × 10 of fine silver electrically conductive ink5S/
M), it is contemplated that the cost of nano silver, select fine silver particle content for 70% fine silver electrically conductive ink as optimum formula, the formula
Conductivity preferably simultaneously cost is relatively low.It is corresponding to it, when nanometer silver plating particle content of the invention is 90%, conductivity is
9.17×104S/m, at this point, the conductivity of silver-plated electrically conductive ink is not only much higher than the conductivity of fine silver electrically conductive ink optimum formula,
And the utilization rate of nano silver reduces 25.4%, to considerably reduce ink cost.
It can be seen that silver-plated electrically conductive ink obtained by the present invention, not only can guarantee the excellent electromagnetic performance of silver, but also can be significantly
Usage amount silver-colored in electrically conductive ink is reduced, reduces ink cost well.
Finally it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than the present invention is protected
The limitation of range is protected, although explaining in detail referring to preferred embodiment to the present invention, those skilled in the art are answered
Work as understanding, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the reality of technical solution of the present invention
Matter and range.
Claims (10)
1. a kind of preparation method of the silver-plated electrically conductive ink of UV curing nano, it is characterised in that: the following steps are included:
(1) preparation of nanometer silver plating particle: cladding substrate is added in reproducibility mixed liquor, ultrasonic wave dispersion；Pass through constant pressure
Funnel, which instills silver-colored source solution in mixed solution, occurs silver plating reaction；After reaction, it is centrifuged, cleans, repeat 3~5 times, do
It is dry, obtain nanometer silver plating particle powder；
(2) preparation of ink: weighing nanometer silver plating particle powder 0.5g, ethyl acetate will be added simultaneously in nanometer silver plating particle powder
It stirs evenly, obtains conductive rubber dispersion liquid；Then the mass fraction of electrically conductive ink 25% is accounted for according to conductive rubber dispersion liquid, is counted
Calculate the amount that the bridging agent resin for needing to be added and auxiliary agent need；Mixed liquor made of bridging agent resin and auxiliary agent is put into later
Ultrasonic disperse is carried out in ultrasonic cleaner；It is dispersed in conductive rubber homogeneous dispersion in mixed liquor, stirs evenly, obtain UV
The silver-plated electrically conductive ink of curing nano.
2. the preparation method of the silver-plated electrically conductive ink of UV curing nano according to claim 1, it is characterised in that: the cladding
Substrate is the micro-sphere material of modified dose of modification, and the micro-sphere material is silicon dioxide microsphere, charcoal powder, polymer microballoon
One of.
3. the preparation method of the silver-plated electrically conductive ink of UV curing nano according to claim 2, it is characterised in that: the modification
Agent is mercaptopropyl trimethoxysilane；The dosage of the modifying agent is mercaptopropyl trimethoxysilane: micro-sphere material=0.05~
1。
4. the preparation method of the silver-plated electrically conductive ink of UV curing nano according to claim 1, it is characterised in that: the reduction
Property mixed liquor refer to the mixed solution of reducing agent and dispersing agent, the mass ratio of the reducing agent and dispersing agent is 0.5~2；It is described
Dispersing agent is soluble starch or polyethylene pyrrole network alkanone；The reducing agent is corn stover extract paste.
5. the preparation method of the silver-plated electrically conductive ink of UV curing nano according to claim 4, it is characterised in that: the corn
The preparation process of straw extractive paste is as follows: by corn stover cleaning, drying, wearing into maize straw powder；Again by corn
Stalk powder adds boiling to boil, and crushes, filters through supersonic cell, after freeze-drying, obtaining corn stover extract paste.
6. the preparation method of the silver-plated electrically conductive ink of UV curing nano according to claim 1, it is characterised in that: the silver source
Solution is silver nitrate solution or silver ammino solution；The concentration of the silver-colored source solution is 0.06~0.16mol/L.
7. the preparation method of the silver-plated electrically conductive ink of UV curing nano according to claim 1, it is characterised in that: described silver-plated
The reaction temperature of reaction is 50 DEG C~90 DEG C, the reaction time is 1~6h.
8. the preparation method of the silver-plated electrically conductive ink of UV curing nano according to claim 1, it is characterised in that: the conduction
The mass fraction of nanometer silver plating particle powder in colloidal dispersion is 50~100%.
9. the preparation method of the silver-plated electrically conductive ink of UV curing nano according to claim 1, it is characterised in that: the connection
Agent resin is super branched polyurethane acrylic resin, and the auxiliary agent is glycerine or diethylene glycol (DEG).
10. a kind of according to the silver-plated electrically conductive ink of UV curing nano made from preparation method described in any one of 1~9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811331838.3A CN109401442A (en) | 2018-11-09 | 2018-11-09 | A kind of silver-plated electrically conductive ink of UV curing nano and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811331838.3A CN109401442A (en) | 2018-11-09 | 2018-11-09 | A kind of silver-plated electrically conductive ink of UV curing nano and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109401442A true CN109401442A (en) | 2019-03-01 |
Family
ID=65472544
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811331838.3A Pending CN109401442A (en) | 2018-11-09 | 2018-11-09 | A kind of silver-plated electrically conductive ink of UV curing nano and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109401442A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109971257A (en) * | 2019-04-03 | 2019-07-05 | 长沙集智创新工业设计有限公司 | A kind of nano-graphene electrically conductive ink and preparation method thereof |
| CN111500121A (en) * | 2020-05-09 | 2020-08-07 | 哈尔滨工业大学(深圳)(哈尔滨工业大学深圳科技创新研究院) | Conductive ink for flexible printed electronics and phonochemical synthesis method |
| CN111560217A (en) * | 2020-06-17 | 2020-08-21 | 江苏睿浦树脂科技有限公司 | Environment-friendly UV (ultraviolet) photocuring water-based silver paint as well as preparation method and use method thereof |
| CN112955983A (en) * | 2019-07-29 | 2021-06-11 | 韩国铸造,安全印刷与Id卡操作公司 | Magnetic particles for forgery-preventing ink and forgery-preventing ink containing same |
| CN114192770A (en) * | 2021-11-19 | 2022-03-18 | 苏州大学 | Silver colloid and preparation method thereof |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5093038A (en) * | 1989-06-14 | 1992-03-03 | Key-Tech, Inc. | Ultraviolet curable ink composition |
| CN101215401A (en) * | 2008-01-18 | 2008-07-09 | 厦门大学 | Method for preparing composite material of organic-inorganic nano spherical shell structure |
| CN103945652A (en) * | 2014-04-30 | 2014-07-23 | 张瑜 | Manufacturing method for flexible printed circuit board |
| CN104152882A (en) * | 2014-07-17 | 2014-11-19 | 广东致卓精密金属科技有限公司 | Preparation method of chemically-silvered active carbon as composite conductive filler |
| CN105521745A (en) * | 2014-10-21 | 2016-04-27 | 中国科学院深圳先进技术研究院 | Method for preparing organic polymer-based heat-conduction microsphere |
| CN105542574A (en) * | 2016-01-29 | 2016-05-04 | 华南理工大学 | Preparation method of UV (ultraviolet) nano-silver conductive ink |
| CN106867314A (en) * | 2015-12-14 | 2017-06-20 | 华南理工大学 | A kind of high accuracy RFID antenna electrically conductive ink and its preparation, printing process |
| CN107520461A (en) * | 2017-07-31 | 2017-12-29 | 华南理工大学 | It is a kind of that Nano Silver prepared and preparation method thereof and the application in anti-bacteria paper are reduced using maize straw extract |
| US10577678B2 (en) * | 2014-05-07 | 2020-03-03 | The Regents Of The University Of California | Fully alloyed AG—AU nanostructures |
-
2018
- 2018-11-09 CN CN201811331838.3A patent/CN109401442A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5093038A (en) * | 1989-06-14 | 1992-03-03 | Key-Tech, Inc. | Ultraviolet curable ink composition |
| CN101215401A (en) * | 2008-01-18 | 2008-07-09 | 厦门大学 | Method for preparing composite material of organic-inorganic nano spherical shell structure |
| CN103945652A (en) * | 2014-04-30 | 2014-07-23 | 张瑜 | Manufacturing method for flexible printed circuit board |
| US10577678B2 (en) * | 2014-05-07 | 2020-03-03 | The Regents Of The University Of California | Fully alloyed AG—AU nanostructures |
| CN104152882A (en) * | 2014-07-17 | 2014-11-19 | 广东致卓精密金属科技有限公司 | Preparation method of chemically-silvered active carbon as composite conductive filler |
| CN105521745A (en) * | 2014-10-21 | 2016-04-27 | 中国科学院深圳先进技术研究院 | Method for preparing organic polymer-based heat-conduction microsphere |
| CN106867314A (en) * | 2015-12-14 | 2017-06-20 | 华南理工大学 | A kind of high accuracy RFID antenna electrically conductive ink and its preparation, printing process |
| CN105542574A (en) * | 2016-01-29 | 2016-05-04 | 华南理工大学 | Preparation method of UV (ultraviolet) nano-silver conductive ink |
| CN107520461A (en) * | 2017-07-31 | 2017-12-29 | 华南理工大学 | It is a kind of that Nano Silver prepared and preparation method thereof and the application in anti-bacteria paper are reduced using maize straw extract |
Non-Patent Citations (3)
| Title |
|---|
| 朱国庆: "《空心玻璃微珠偶联化学镀银的研究》", 《电镀与精饰》 * |
| 王国建: "《功能高分子材料》", 31 August 2006, 华东理工大学出版社 * |
| 钱军浩: "《新型油墨印刷技术》", 31 January 2002, 中国轻工业出版社 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109971257A (en) * | 2019-04-03 | 2019-07-05 | 长沙集智创新工业设计有限公司 | A kind of nano-graphene electrically conductive ink and preparation method thereof |
| CN112955983A (en) * | 2019-07-29 | 2021-06-11 | 韩国铸造,安全印刷与Id卡操作公司 | Magnetic particles for forgery-preventing ink and forgery-preventing ink containing same |
| CN111500121A (en) * | 2020-05-09 | 2020-08-07 | 哈尔滨工业大学(深圳)(哈尔滨工业大学深圳科技创新研究院) | Conductive ink for flexible printed electronics and phonochemical synthesis method |
| CN111500121B (en) * | 2020-05-09 | 2022-07-22 | 哈尔滨工业大学(深圳)(哈尔滨工业大学深圳科技创新研究院) | Conductive ink for flexible printed electronics and sonochemical synthesis method |
| CN111560217A (en) * | 2020-06-17 | 2020-08-21 | 江苏睿浦树脂科技有限公司 | Environment-friendly UV (ultraviolet) photocuring water-based silver paint as well as preparation method and use method thereof |
| CN111560217B (en) * | 2020-06-17 | 2022-03-08 | 江苏睿浦树脂科技有限公司 | Environment-friendly UV (ultraviolet) photocuring water-based silver paint as well as preparation method and use method thereof |
| CN114192770A (en) * | 2021-11-19 | 2022-03-18 | 苏州大学 | Silver colloid and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109401442A (en) | A kind of silver-plated electrically conductive ink of UV curing nano and preparation method thereof | |
| CN108735339B (en) | A kind of high performance sintered conductive silver paste and preparation method thereof and sintering method | |
| CN106694904A (en) | Preparation method of highly dispersed micron order flake silver powder with large radius-thickness ratio | |
| CN103192074A (en) | Highly dispersed sliver powder and conductive silver paste for film batteries | |
| CN104801709B (en) | Nickel-coated copper clad metal powder and preparation method and application thereof | |
| CN109215829B (en) | Front electrode silver paste and silver powder for solar cell and preparation method thereof | |
| CN109423637A (en) | A kind of preparation method of high conductive material | |
| CN110340348B (en) | Nano silver powder, preparation method, silver paste and application | |
| CN103219090A (en) | Preparation method of nano-silver wrapping polymer microsphere composite conductive silver paste | |
| CN105788703B (en) | A kind of anti-oxidant silver-bearing copper slurry for being used to be electromagnetically shielded and preparation method thereof | |
| CN109773211A (en) | A kind of preparation method in flake silver powder surface cladding nano-Ag particles | |
| CN109692971A (en) | A kind of nano-silver powder and its preparation and the application in low-temperature cured conductive silver paste | |
| CN104668572A (en) | Silver powder and silver paste for back electrode of solar cell and solar cell | |
| CN105762334A (en) | Lithium iron phosphate nanocomposite cathode material suitable for aqueous binder system and preparation method thereof | |
| CN110706842B (en) | Front silver paste and preparation method thereof | |
| CN109749105A (en) | A kind of highly conductive electromagnetic shielding composite material and preparation method thereof | |
| CN108962425A (en) | A kind of preparation method of graphene conductive slurry | |
| CN106847371A (en) | A kind of anti-aging back silver paste | |
| CN109848438B (en) | Double-mode particle size nano silver particle and preparation method thereof | |
| CN104282356A (en) | Low-silver-content composite conductive silver paste and preparation method thereof | |
| CN102103895B (en) | Silver paste used for positive electrodes of solar batteries and grid lines, preparation method thereof and solar battery containing same | |
| CN104387828B (en) | A kind of carbon series conductive coating and preparation method thereof | |
| CN108795155A (en) | A kind of silver nano-grain/Nano silver piece composite conducting ink and preparation method thereof | |
| CN107331438A (en) | A kind of environment protection solar cell front electrode conductor paste and preparation method thereof | |
| CN104599740B (en) | Conductive silver paste with nanocarbon |
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: 20190301 |
|
| RJ01 | Rejection of invention patent application after publication |