CN105632588B - A kind of high conductivity silver paste and preparation method thereof - Google Patents
A kind of high conductivity silver paste and preparation method thereof Download PDFInfo
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- CN105632588B CN105632588B CN201610096137.0A CN201610096137A CN105632588B CN 105632588 B CN105632588 B CN 105632588B CN 201610096137 A CN201610096137 A CN 201610096137A CN 105632588 B CN105632588 B CN 105632588B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Abstract
The present invention provides a kind of high conductivity silver paste and preparation method thereof, and the high conductivity silver paste includes silver powder, and the silver powder is the mixture of micro-order platy silver powder, the spherical silver powder of submicron order and nano-scale silver powder.It is an advantage of the current invention that making full use of different-grain diameter and the silver powder of appearance structure to cooperate, silver powder is formed finer and close state in structure, while add nano-silver powder able to sinter at low temp, further connect conductive silver powder.After the blending with macromolecule resin, solvent, additive and auxiliary agent, under conditions of low-temperature setting (≤150 DEG C), slurry can obtain higher electrical conductivity.Slurry has good printing printability and good adhesion property simultaneously, can apply to the fields such as conductive circuit, RFID label antenna.
Description
Technical field
The present invention relates to conductive silver paste field, more particularly to a kind of high conductivity silver paste and preparation method thereof.
Background technology
With printed electronics industrial expansion, thin film switch, flexible printed circuit board, electromagnetic shielding, radio frequency identification
The demands such as system increase sharply, and conductive silver paste is as the functional material for preparing such electronic component, its development and application
Receive the extensive concern of people.
Low-temperature cured conductive silver paste refers to silver paste of the solidification temperature in 80-200 DEG C of scope, can be prepared by way of printing
On plastics or flexible parent metal.As the silver paste of conductive material, should have excellent electric conductivity and adhesive force after hardening
Etc. performance.For conductive silver paste, as main conductive medium silver powder it is most important.In general, flake silver powder is advantageous to
The high conductivity of film layer, but substantial amounts of hole in stacking process be present in flake silver powder, so as to which silver paste electric conductivity can be influenceed
Further improve；Spherical silver powder, which has, preferably stacks density, can play the pore filling of part；Nano Silver has low temperature can
The characteristic of sintering, with the reduction of nanometer particle size, it is also lower to sinter required temperature, typically when less than 20nm, can meet low
Temperature sintering (<150 DEG C), and at such a temperature, the flex-print material such as applicable general class such as polyester film.
Problem present in most of low-temperature conductive silver paste application is not high mainly due to electric conductivity at present, causes device clever
Sensitivity is poor.
The content of the invention
The technical problem to be solved by the invention is to provide a kind of high conductivity silver paste and preparation method thereof, solves existing
Above mentioned problem existing for technology, the conductive silver paste has good printing printability and excellent electric conductivity.
In order to solve the above problems, the invention provides a kind of high conductivity silver paste, including silver powder, the argent
Powder is the mixture of micro-order platy silver powder, the spherical silver powder of submicron order and nano-scale silver powder.
Preferably, the mass ratio of the spherical silver powder of the micro-order platy silver powder, submicron order and nano-scale silver powder is 6~7：
2~3：0.5~1..
Preferably, the particle diameter of the micro-order platy silver powder is 4~15 μm, and apparent density is 0.9~1.5g/ml.
Preferably, the particle diameter of the spherical silver powder of the submicron order is 0.3~0.9 μm, and apparent density is 2.9~3.7g/ml.
Preferably, the particle diameter of the nano-scale silver powder is 5~15nm, and apparent density is 3.4~5.5g/ml.
Preferably, the conductive silver paste includes following component, and the weight/mass percentage composition of each component is as follows：
Preferably, the macromolecule resin is selected from the one of thermoplastic epoxy resin, vinyl chloride-vinyl acetate resin and acrylic resin
Kind is several.
Preferably, the solvent is selected from esters or the one or more of ketone.
Preferably, the additive is selected from conductive black, the one or more of electrically conductive graphite.
Preferably, the auxiliary agent is selected from thickener, coupling agent, the one or more of defoamer.
The present invention provides a kind of preparation method of high conductivity silver paste, comprises the following steps：
Prepare organic carrier：Macromolecule resin and solvent are put into stirred tank in proportion, the stirring some time is had
Airborne body；Prepare high conductivity silver paste：Additive and auxiliary agent are stirred and mixed with the organic carrier in proportion, adds gold
Category silver powder is stirred, and is obtained mixture, is ground and roll the mixture to room temperature dynamic viscosity at 15000-50000 lis
Pool, that is, obtain the high conductivity silver paste.
Further, in organic carrier step is prepared, whipping temp is 60~80 DEG C.
It is an advantage of the current invention that flake silver powder is advantageous to the high conductivity of film layer, but flake silver powder is in stacking process
In the presence of substantial amounts of hole, so as to which the further raising of silver paste electric conductivity can be influenceed；Spherical silver powder, which has, preferably stacks density,
The pore filling of part can be played；Nano Silver has characteristic able to sinter at low temp, with the reduction of nanometer particle size, needed for sintering
Temperature it is also lower, typically when less than 20nm, can meet low-temperature sintering (<150 DEG C), and at such a temperature, it is applicable general
The flex-print materials such as class such as polyester film.
The present invention makes full use of different-grain diameter and the silver powder of appearance structure to cooperate, and silver powder is formed more in structure
Fine and close state, while nano-silver powder able to sinter at low temp is added, further connect conductive silver powder.By with macromolecule resin,
After the blending of solvent, additive and auxiliary agent, under conditions of low-temperature setting (≤150 DEG C), slurry can obtain higher conductance
Rate.Slurry has good printing printability and good adhesion property simultaneously, can apply to conductive circuit, RFID
The fields such as label antenna.
Embodiment
The embodiment of high conductivity silver paste provided by the invention and preparation method thereof is elaborated below.
High conductivity silver paste of the present invention, including silver powder, the silver powder are micro-order platy silver powder, submicron order
The mixture of spherical silver powder and nano-scale silver powder.
Wherein, the mass ratio of the spherical silver powder of the micro-order platy silver powder, submicron order and nano-scale silver powder is 6~7：2
~3：0.5~1.The particle diameter of the micro-order platy silver powder is 4~15 μm, and apparent density is 0.9~1.5g/ml.The sub-micro
The particle diameter of the spherical silver powder of meter level is 0.3~0.9 μm, and apparent density is 2.9~3.7g/ml.The particle diameter of the nano-scale silver powder is 5
~15nm, apparent density are 3.4~5.5g/ml.
The present invention makes full use of different-grain diameter and the silver powder of appearance structure to cooperate, and silver powder is formed more in structure
Fine and close state, while nano-silver powder able to sinter at low temp is added, conductive silver powder is further connected, forms good electric conductivity.
High conductivity silver paste of the present invention, including following component, the weight/mass percentage composition of each component are as follows：
Wherein, the macromolecule resin is selected from one kind of thermoplastic epoxy resin, vinyl chloride-vinyl acetate resin and acrylic resin
It is or several.The solvent is selected from esters or the one or more of ketone.The additive is selected from conductive black, the one of electrically conductive graphite
Kind is several.The auxiliary agent is selected from thickener, coupling agent, the one or more of defoamer.The thickener be selected from cellulose ether,
Polyvinyl alcohol, Tissuemat E, organobentonite, rilanit special, the one or more of aerosil.The coupling agent choosing
From the one or more of titanate coupling agent, silane coupler.The defoamer is selected from organic silicon.
The silver powder of mixture containing micro-order platy silver powder, the spherical silver powder of submicron order and nano-scale silver powder passes through
After blending with macromolecule resin, solvent, additive and auxiliary agent, under conditions of low-temperature setting (≤150 DEG C), slurry can obtain
Obtain higher electrical conductivity.Slurry has good printing printability and good adhesion property simultaneously, can apply to print
The fields such as conducting wire, RFID label antenna.
A kind of preparation method of high conductivity silver paste of the present invention, comprises the following steps：
Prepare organic carrier：Macromolecule resin and solvent are put into stirred tank in proportion, the stirring some time is had
Airborne body.For example, macromolecule resin and solvent example in mass ratio are put into stirred tank, 60-80 DEG C of high-speed stirred 4-6 hour is obtained
Obtain organic carrier.
Prepare high conductivity silver paste：Additive and auxiliary agent are stirred and mixed with the organic carrier in proportion, is added
Silver powder is stirred, and obtains mixture, grinds and roll the mixture to room temperature dynamic viscosity at 15000-50000 lis
Pool, that is, obtain the high conductivity silver paste.For example, example in mass ratio is by additive and auxiliary agent and the organic carrier high-speed stirred
1h is well mixed, and then adds silver powder high-speed stirred 0.5h, and is ground and rolled 4-8 times by three-roll grinder, to room
Warm dynamic viscosity obtains the high conductivity silver paste in 15000-50000 centipoises.
The several embodiments of the present invention are set forth below, so that high conductivity silver paste of the present invention and preparation method thereof is explained further.
Embodiment 1
A kind of high conductivity silver paste of low-temperature setting, its component and mass percent are as follows：
The flake silver powder that 15 μm of average grain diameter：41.6%；
0.8 μm of spherical silver powder of average grain diameter：16.9%；
Average grain diameter 10nm nano-silver powders：6.5%；
Thermoplastics type's bisphenol A type epoxy resin：9%；
Isophorone：15%；
DBE mixed esters：7%
Electrically conductive graphite：2%
Rilanit special：0.7%；
Titanate coupling agent：0.8%；
Organic silicon defoamer：0.5%.
The preparation method of above-mentioned high conductivity silver paste is as follows：
Step 1, isophorone 15g, DBE mixed ester 7g is added in the mixing container, then adds thermoplastics type's bisphenol A-type
Epoxy resin 9g, 60-80 DEG C of water bath with thermostatic control, 1000RPM high-speed stirreds 4.5h obtain organic carrier.
Step 2, electrically conductive graphite 2g, rilanit special 0.7g, titanate coupling agent 0.8g, organic silicon defoamer 0.5 are put
In the carrier for entering step 1 acquisition, 800rpm high-speed stirreds 1h is well mixed, and then adds average grain diameter 15um flake silver powders
The spherical silver powder B16.9g of A41.6g, average grain diameter 0.8um, average grain diameter 10nm nano-silver powders C6.5g, 1000rpm high-speed stirred
0.5h, and grind and roll 6 times by three-roll grinder, room temperature dynamic viscosity obtains high conductivity in 32000 ± 5000 centipoises
Silver paste.
Embodiment 2
A kind of high conductivity silver paste of low-temperature setting, its component and mass percent are as follows：
10 μm of flake silver powders of average grain diameter：44.8%；
0.5 μm of spherical silver powder of average grain diameter：18.2%
Average grain diameter 15nm nano-silver powders：7%；
Thermoplastics type's bisphenol A type epoxy resin：5%；
Thermoplastics type's vinyl chloride-vinyl acetate resin：3%；
Isophorone：10%；
Diethylene glycol ether butyrate：8%；
Electrically conductive graphite：1.5%；
Ethyl cellulose：1.2%；
Titanate coupling agent：0.8%；
Organic silicon defoamer：0.5%.
The preparation method of above-mentioned silver paste is as follows：
Step 1：Isophorone 10g is added in the mixing container, diethylene glycol ether butyrate 8g, then adds thermoplastic
Type bisphenol A type epoxy resin 5g, thermoplastics type vinyl chloride-vinyl acetate resin 3g, 60-80 DEG C of water bath with thermostatic control, 1000RPM high-speed stirreds 5h are had
Airborne body.
Step 2, by electrically conductive graphite 1.5g, ethyl cellulose 1.2g, titanate coupling agent 0.8g, organic silicon defoamer 0.5
It is put into the carrier of step 1 acquisition, 800rpm high-speed stirreds 1h is well mixed, and then adds average grain diameter 10um flake silver powders A
The spherical silver powder B 18.2g of 44.8g, average grain diameter 0.5um, average grain diameter 15nm nano-silver powder C 7g, 1000rpm high-speed stirreds
0.5h, and grind and roll 8 times by three-roll grinder, room temperature dynamic viscosity obtains high conductivity in 40000 ± 5000 centipoises
Silver paste.
The high conductivity silver paste being prepared by above-described embodiment, gathered on 50 μ m thick polyester base materials by 300 mesh
Ester silk-screen printing 100mm × 1mm line segments, after heat cure (140 DEG C × 1h), following performance can be obtained：
Embodiment 1：Electrical conductivity 9.5 × 10-6Ω cm, adhesive force 5B are without coming off.
Embodiment 2：Electrical conductivity 7.8 × 10-6Ω cm, adhesive force 5B are without coming off.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
Member, under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be regarded as
Protection scope of the present invention.
Claims (10)
1. a kind of high conductivity silver paste of low-temperature setting, including silver powder, it is characterised in that the silver powder is micron order
The mixture of the spherical silver powder of flake silver powder, submicron order and nano-scale silver powder, the particle diameter of the nano-scale silver powder is 5~15nm,
Apparent density is 3.4~5.5g/ml；
The high conductivity silver paste includes following component, and the weight/mass percentage composition of each component is as follows：
2. the high conductivity silver paste of low-temperature setting according to claim 1, it is characterised in that the micron-stage sheet-like silver
The mass ratio of the spherical silver powder of powder, submicron order and nano-scale silver powder is (6~7)：(2~3)：
(0.5~1).
3. the high conductivity silver paste of low-temperature setting according to claim 1, it is characterised in that the micro-order platy silver powder
Particle diameter be 4~15 μm, apparent density is 0.9~1.5g/ml.
4. the high conductivity silver paste of low-temperature setting according to claim 1, it is characterised in that the submicron order spherical silver
The particle diameter of powder is 0.3~0.9 μm, and apparent density is 2.9~3.7g/ml.
5. the high conductivity silver paste of low-temperature setting according to claim 1, it is characterised in that the macromolecule resin is selected from
The one or more of thermoplastic epoxy resin, vinyl chloride-vinyl acetate resin and acrylic resin.
6. the high conductivity silver paste of low-temperature setting according to claim 1, it is characterised in that the solvent be selected from esters or
The one or more of ketone.
7. the high conductivity silver paste of low-temperature setting according to claim 1, it is characterised in that the additive is selected from conduction
The one or more of carbon black, electrically conductive graphite.
8. the high conductivity silver paste of low-temperature setting according to claim 1, it is characterised in that the auxiliary agent is selected from thickening
Agent, coupling agent, the one or more of defoamer.
9. the preparation method of the high conductivity silver paste of a kind of low-temperature setting, it is characterised in that comprise the following steps：
Prepare organic carrier：Macromolecule resin and solvent are put into stirred tank in proportion, the acquisition of stirring some time has airborne
Body；
Prepare high conductivity silver paste：Additive and auxiliary agent are stirred and mixed with the organic carrier in proportion,
Add silver powder to be stirred, obtain mixture, grind and roll the mixture to room temperature dynamic viscosity and exist
15000-50000 centipoises, that is, obtain the high conductivity silver paste；
Wherein, the high conductivity silver paste includes following component, and the weight/mass percentage composition of each component is as follows：
The silver powder is the mixture of micro-order platy silver powder, the spherical silver powder of submicron order and nano-scale silver powder, described to receive
The particle diameter of meter level silver powder is 5~15nm, and apparent density is 3.4~5.5g/ml.
10. the preparation method of the high conductivity silver paste of low-temperature setting according to claim 9, it is characterised in that preparing
In organic carrier step, whipping temp is 60~80 DEG C.
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