CN105632588A - High-conductivity silver paste and preparation method thereof - Google Patents
High-conductivity silver paste and preparation method thereof Download PDFInfo
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- CN105632588A CN105632588A CN201610096137.0A CN201610096137A CN105632588A CN 105632588 A CN105632588 A CN 105632588A CN 201610096137 A CN201610096137 A CN 201610096137A CN 105632588 A CN105632588 A CN 105632588A
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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
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Abstract
The invention provides a high-conductivity silver paste and a preparation method thereof. The high-conductivity silver paste comprises metal silver powder, wherein the metal silver powder is a mixture of micro-order sheet-shaped silver powder, submicron-order spherical silver powder and nanometer silver powder. The high-conductivity silver paste has the advantages that silver powders with different grain sizes and morphological structures are fully utilized and mutually matched, so that the silver powder can form a more compact status on the structure, and the low-temperature sintered nanometer silver powder is added to be further connected with the conductive silver powder; after mixing the silver paste with macromolecule resin, a solvent, an additive and an assistant agent, the paste can acquire relatively high conductivity under a condition of low-temperature curing (less than or equal to 150 DEG C); and meanwhile, the paste has favorable printing adaptability and favorable attachment performance, and can be applied to the fields of a printed conductive circuit, a radio frequency identification (RFID) label antenna and the like.
Description
Technical field
The present invention relates to conductive silver paste field, particularly relate to a kind of high conductivity silver slurry and preparation method thereof.
Background technology
Along with printed electronics industrial expansion, the demands such as thin film switch, flexible printed circuit board, electromagnetic shielding, radio frequency identification system increase sharply, and conductive silver paste is as the functional material preparing these type of electronic devices and components, its development and application receives the extensive concern of people.
Low-temperature cured conductive silver slurry refers to the solidification temperature silver slurry 80-200 DEG C of scope, can be prepared on plastics or flexible parent metal by the mode printed. As the silver slurry of conductive material, should have the performances such as excellent electric conductivity and adhesive force after hardening. For conductive silver paste, as argentum powder most important of main conductive medium. In general, flake silver powder is conducive to the high conductivity of rete, but flake silver powder exists substantial amounts of hole in stacking process, thus the further raising of silver slurry electric conductivity can be affected; Spherical argentum powder has good stacking density, it is possible to play the pore filling of part; Nanometer silver has characteristic able to sinter at low temp, and along with the reduction of nanometer particle size, the temperature needed for sintering is also more low, when being typically in lower 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 mylar.
In the application of major part low-temperature conductive silver paste, Problems existing is not high mainly due to electric conductivity at present, causes that device sensitivity is poor.
Summary of the invention
The technical problem to be solved is to provide a kind of high conductivity silver slurry and preparation method thereof, solves the problems referred to above that prior art exists, described conductive silver paste has good printing printability and excellent electric conductivity.
In order to solve the problems referred to above, the invention provides a kind of high conductivity silver slurry, including silver powder, described silver powder is the mixture of micro-order platy silver powder, the spherical argentum powder of submicron order and nano-scale silver powder.
Preferably, the mass ratio of described micro-order platy silver powder, the spherical argentum powder of submicron order and nano-scale silver powder is 6��7:2��3:0.5��1. .
Preferably, the particle diameter of described micro-order platy silver powder is 4��15 ��m, and apparent density is 0.9��1.5g/ml.
Preferably, the particle diameter of the spherical argentum powder of described submicron order is 0.3��0.9 ��m, and apparent density is 2.9��3.7g/ml.
Preferably, the particle diameter of described nano-scale silver powder is 5��15nm, and apparent density is 3.4��5.5g/ml.
Preferably, described conductive silver paste includes following component, and the weight/mass percentage composition of each component is as follows:
Preferably, described macromolecule resin is selected from one or more of thermoplastic epoxy resin, vinyl chloride-vinyl acetate resin and acrylic resin.
Preferably, described solvent is selected from one or more of esters or ketone.
Preferably, described additive selected from conductive black, electrically conductive graphite one or more.
Preferably, described auxiliary agent selected from thickening agent, coupling agent, defoamer one or more.
The present invention provides the preparation method that a kind of high conductivity silver is starched, and comprises the steps:
Preparing organic carrier: macromolecule resin and solvent are put in proportion in stirred tank, the stirring some time obtains organic carrier; Preparation high conductivity silver slurry: in proportion additive and auxiliary agent stirred with described organic carrier and mix, add silver powder stirring mixing, obtain mixture, grind and roll described mixture to room temperature dynamic viscosity at 15000-50000 centipoise, namely obtain described high conductivity silver slurry.
Further, in preparing organic carrier step, whipping temp is 60��80 DEG C.
The further raising of silver slurry electric conductivity it is an advantage of the current invention that flake silver powder is conducive to the high conductivity of rete, but flake silver powder exists substantial amounts of hole in stacking process, thus can be affected; Spherical argentum powder has good stacking density, it is possible to play the pore filling of part; Nanometer silver has characteristic able to sinter at low temp, and along with the reduction of nanometer particle size, the temperature needed for sintering is also more low, when being typically in lower 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 mylar.
The present invention makes full use of the argentum powder of different-grain diameter and appearance structure and cooperates, and makes argentum powder structurally form finer and close state, is simultaneously introduced nanometer silver powder able to sinter at low temp, connects conductive silver powder further. By with macromolecule resin, solvent, additive and auxiliary agent blended after, when low-temperature setting (��150 DEG C), slurry can obtain higher electrical conductivity. Slurry has good printing printability and good adhesion property simultaneously, it is possible to be applied to the field such as conductive circuit, RFID label antenna.
Detailed description of the invention
Below the detailed description of the invention of high conductivity silver slurry provided by the invention and preparation method thereof is elaborated.
High conductivity silver of the present invention is starched, and including silver powder, described silver powder is the mixture of micro-order platy silver powder, the spherical argentum powder of submicron order and nano-scale silver powder.
Wherein, the mass ratio of described micro-order platy silver powder, the spherical argentum powder of submicron order and nano-scale silver powder is 6��7:2��3:0.5��1. The particle diameter of described micro-order platy silver powder is 4��15 ��m, and apparent density is 0.9��1.5g/ml. The particle diameter of the spherical argentum powder of described submicron order is 0.3��0.9 ��m, and apparent density is 2.9��3.7g/ml. The particle diameter of described nano-scale silver powder is 5��15nm, and apparent density is 3.4��5.5g/ml.
The present invention makes full use of the argentum powder of different-grain diameter and appearance structure and cooperates, and makes argentum powder structurally form finer and close state, is simultaneously introduced nanometer silver powder able to sinter at low temp, connect conductive silver powder further, forms good electric conductivity.
High conductivity silver of the present invention is starched, and including following component, the weight/mass percentage composition of each component is as follows:
Wherein, described macromolecule resin is selected from one or more of thermoplastic epoxy resin, vinyl chloride-vinyl acetate resin and acrylic resin. Described solvent is selected from one or more of esters or ketone. Described additive selected from conductive black, electrically conductive graphite one or more. Described auxiliary agent selected from thickening agent, coupling agent, defoamer one or more. Described thickening agent selected from cellulose ether, polyvinyl alcohol, Tissuemat E, organobentonite, castor oil hydrogenated, aerosil one or more. Described coupling agent selected from titanate coupling agent, silane coupler one or more. Described defoamer is selected from silicone based.
The silver powder of the mixture containing micro-order platy silver powder, the spherical argentum powder of submicron order and nano-scale silver powder by with macromolecule resin, solvent, additive and auxiliary agent blended after, when low-temperature setting (��150 DEG C), slurry can obtain higher electrical conductivity. Slurry has good printing printability and good adhesion property simultaneously, it is possible to be applied to the field such as conductive circuit, RFID label antenna.
The preparation method of a kind of high conductivity silver slurry of the present invention, comprises the steps:
Preparing organic carrier: macromolecule resin and solvent are put in proportion in stirred tank, the stirring some time obtains organic carrier. Such as, putting in stirred tank by macromolecule resin and solvent example in mass ratio, 60-80 DEG C obtains organic carrier in high-speed stirred 4-6 hour.
Preparation high conductivity silver slurry: in proportion additive and auxiliary agent stirred with described organic carrier and mix, add silver powder stirring mixing, obtain mixture, grind and roll described mixture to room temperature dynamic viscosity at 15000-50000 centipoise, namely obtain described high conductivity silver slurry. Such as, additive and auxiliary agent are mixed homogeneously by example with described organic carrier high-speed stirred 1h in mass ratio, are subsequently added silver powder high-speed stirred 0.5h, and are ground by three-roll grinder and roll 4-8 time, to room temperature dynamic viscosity at 15000-50000 centipoise, namely obtain described high conductivity silver slurry.
The present invention several embodiment is set forth below, so that of the present invention high conductivity silver slurry and preparation method thereof is explained further.
Embodiment 1
A kind of high conductivity silver slurry of low-temperature setting, its component is as follows with mass percent:
The flake silver powder that mean diameter is 15 ��m: 41.6%;
0.8 ��m of spherical argentum powder of mean diameter: 16.9%;
Mean diameter 10nm nanometer silver powder: 6.5%;
Thermoplastics type's bisphenol A type epoxy resin: 9%;
Isophorone: 15%;
DBE mixed ester: 7%
Electrically conductive graphite: 2%
Castor oil hydrogenated: 0.7%;
Titanate coupling agent: 0.8%;
Organic silicon defoamer: 0.5%.
The preparation method of above-mentioned high conductivity silver slurry is as follows:
Step one, adds isophorone 15g, DBE mixed ester 7g in the mixing container, is subsequently added thermoplastics type bisphenol A type epoxy resin 9g, water bath with thermostatic control 60-80 DEG C, and 1000RPM high-speed stirred 4.5h obtains organic carrier.
Step 2, by electrically conductive graphite 2g, castor oil hydrogenated 0.7g, titanate coupling agent 0.8g, organic silicon defoamer 0.5 is put in the carrier that step one obtains, 800rpm high-speed stirred 1h mix homogeneously, it is subsequently added mean diameter 15um flake silver powder A41.6g, the spherical argentum powder B16.9g of mean diameter 0.8um, mean diameter 10nm nanometer silver powder C6.5g, 1000rpm high-speed stirred 0.5h, and ground by three-roll grinder and roll 6 times, room temperature dynamic viscosity, at 32000 �� 5000 centipoises, obtains high conductivity silver slurry.
Embodiment 2
A kind of high conductivity silver slurry of low-temperature setting, its component is as follows with mass percent:
10 ��m of flake silver powders of mean diameter: 44.8%;
0.5 ��m of spherical argentum powder of mean diameter: 18.2%
Mean diameter 15nm nanometer silver powder: 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 slurry is as follows:
Step one: adding isophorone 10g, diethylene glycol ether butyrate 8g in the mixing container, be subsequently added thermoplastics type bisphenol A type epoxy resin 5g, thermoplastics type vinyl chloride-vinyl acetate resin 3g, water bath with thermostatic control 60-80 DEG C, 1000RPM high-speed stirred 5h obtains organic carrier.
Step 2, by electrically conductive graphite 1.5g, ethyl cellulose 1.2g, titanate coupling agent 0.8g, organic silicon defoamer 0.5 is put in the carrier that step one obtains, 800rpm high-speed stirred 1h mix homogeneously, it is subsequently added mean diameter 10um flake silver powder A44.8g, the spherical argentum powder B18.2g of mean diameter 0.5um, mean diameter 15nm nanometer silver powder C7g, 1000rpm high-speed stirred 0.5h, and ground by three-roll grinder and roll 8 times, room temperature dynamic viscosity, at 40000 �� 5000 centipoises, obtains high conductivity silver slurry.
By the high conductivity silver slurry that above-described embodiment prepares, by 300 order polyester net printing 100mm �� 1mm line segments on 50 �� m thick polyester base materials, after heat cure (140 DEG C �� 1h), it is possible to obtain following performance:
Embodiment 1: electrical conductivity 9.5 �� 10-6�� cm, adhesive force 5B is without coming off.
Embodiment 2: electrical conductivity 7.8 �� 10-6�� cm, adhesive force 5B is without coming off.
The above is only the preferred embodiment of the present invention; it should be pointed out that, for those skilled in the art, under the premise without departing from the principles of the invention; can also making some improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (12)
1. a high conductivity silver slurry, including silver powder, it is characterised in that described silver powder is the mixture of micro-order platy silver powder, the spherical argentum powder of submicron order and nano-scale silver powder.
2. high conductivity silver according to claim 1 slurry, it is characterised in that the mass ratio of the spherical argentum powder of described micro-order platy silver powder, submicron order and nano-scale silver powder is 6��7:2��3:0.5��1.
3. high conductivity silver according to claim 1 slurry, it is characterised in that the particle diameter of described micro-order platy silver powder is 4��15 ��m, and apparent density is 0.9��1.5g/ml.
4. high conductivity silver according to claim 1 slurry, it is characterised in that the particle diameter of the spherical argentum powder of described submicron order is 0.3��0.9 ��m, and apparent density is 2.9��3.7g/ml.
5. high conductivity silver according to claim 1 slurry, it is characterised in that the particle diameter of described nano-scale silver powder is 5��15nm, and apparent density is 3.4��5.5g/ml.
6. high conductivity silver according to claim 1 slurry, it is characterised in that described conductive silver paste includes following component, and the weight/mass percentage composition of each component is as follows:
7. high conductivity silver according to claim 6 slurry, it is characterised in that described macromolecule resin is selected from one or more of thermoplastic epoxy resin, vinyl chloride-vinyl acetate resin and acrylic resin.
8. high conductivity silver according to claim 6 slurry, it is characterised in that described solvent is selected from one or more of esters or ketone.
9. high conductivity silver according to claim 6 slurry, it is characterised in that described additive selected from conductive black, electrically conductive graphite one or more.
10. high conductivity silver according to claim 6 slurry, it is characterised in that described auxiliary agent selected from thickening agent, coupling agent, defoamer one or more.
11. the preparation method of a high conductivity silver slurry, it is characterised in that comprise the steps:
Preparing organic carrier: macromolecule resin and solvent are put in proportion in stirred tank, the stirring some time obtains organic carrier;
Preparation high conductivity silver slurry: in proportion additive and auxiliary agent stirred with described organic carrier and mix, add silver powder stirring mixing, obtain mixture, grind and roll described mixture to room temperature dynamic viscosity at 15000-50000 centipoise, namely obtain described high conductivity silver slurry.
12. the preparation method of high conductivity silver according to claim 11 slurry, it is characterised in that in preparing organic carrier step, whipping temp is 60��80 DEG C.
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