CN106098145A - A kind of low-temperature cured conductive paste based on flexible parent metal and preparation method thereof - Google Patents
A kind of low-temperature cured conductive paste based on flexible parent metal and preparation method thereof Download PDFInfo
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- CN106098145A CN106098145A CN201610528661.0A CN201610528661A CN106098145A CN 106098145 A CN106098145 A CN 106098145A CN 201610528661 A CN201610528661 A CN 201610528661A CN 106098145 A CN106098145 A CN 106098145A
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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
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Abstract
The invention discloses a kind of low-temperature cured conductive paste based on flexible parent metal, this electrocondution slurry includes complex function phase, organic carrier, complex function is the mixed powder of the spherical argentum powder of nanometer and nano-sheet nikel powder mutually, the mixture that organic carrier is organic solvent, self-curing type macromolecule resin, dispersant, defoamer, thixotropic agent are formed；The invention also discloses the preparation method of this low-temperature cured conductive paste.Electrocondution slurry prepared by the present invention have low cost, conduct electricity very well, adhesive force is strong, printing characteristic, sintering characteristic, environmental-protecting performance are excellent and with the advantage such as flexible parent metal matches.
Description
Technical field:
The present invention relates to technical field of electronic materials, be specifically related to a kind of low-temperature cured conductive based on flexible parent metal slurry
Material.
Background technology:
Electrocondution slurry is electronic devices and components encapsulation, electrode and the critical material of interconnection, mainly includes burning infiltration type electrocondution slurry
Class big with curing type conducting resinl two.Electrocondution slurry is different according to filler therein, carbon can be divided into starch (graphite conductor), metal pulp
Material (bronze, argentum powder, copper powder, yellow gold), and the ceramic size of modification.Classify according to condition of cure, thermosetting can be divided into
Change, ultra-violet curing etc..Traditional burning infiltration type electrocondution slurry contains substantial amounts of lead, is highly detrimental to environmental conservation, presently used
The most often containing some harmful substances in conducting resinl and relatively costly.Work out the electrocondution slurry of a kind of environmental protection, not only preparation technology
Simply, improve size performance, prepare the unleaded electrocondution slurry of low-temperature setting and low-cost solidification conducting resinl, meet market need
Ask.
In present applicable electrocondution slurry product, argentum powder content in the slurry is 50%-70%, and your gold silver is belonging to
One in genus, its cost is 3-4 times of conventional base metal, and mostly to purchase foreign brand name expensive in market, and this just leads
Cause the high expensive of whole electronic market.And low-end product price drops, under keen competition makes products quotation further
Falling, current electronic market is all to develop to low cost direction, and domestic low-temperature solidified silver paste year, usage amount was more than 120 tons.Produce
Low cost, high performance electrocondution slurry is the technical problem that we are in the urgent need to address.Prior art also has employing base metal
Part noble metal is replaced to be used as the function phase of electrocondution slurry, but the electrocondution slurry electric conductivity prepared, impressionability, attached
The performance such as put forth effort not ideal.
Summary of the invention:
It is an object of the invention to provide a kind of low-temperature cured conductive paste based on flexible parent metal, it conducts electricity very well, attached
Put forth effort strong, printing characteristic, sintering characteristic, environmental-protecting performance are excellent, and match with flexible parent metal and resistance slurry wettability, phase
Capacitive is excellent, low cost.
It is an object of the invention to provide the preparation method of this low-temperature cured conductive paste.
For achieving the above object, the present invention is by the following technical solutions:
A kind of low-temperature cured conductive paste based on flexible parent metal, by weight percentage, including following components:
Complex function phase 60-80%,
Organic carrier 20-40%；
Described complex function phase, by weight percentage, including following components:
Nanometer spherical argentum powder 40-65%,
Nano-sheet nikel powder 35-60%；
Described organic carrier, by weight percentage, including following components:
Preferred as technique scheme, the particle size values of the spherical argentum powder of described nanometer is 20-50nm, tap density is
3.0～4.0g/cm3, the particle size values of nano-sheet nikel powder is 10-60nm, tap density is 2.0～3.0g/cm3。
Preferred as technique scheme, described flexible parent metal includes polyethylene terephthalate (PET), poly-to benzene
In dioctyl phthalate fourth diester (PBT), PEN (PEN), polyimides (PI), polyamide (PA) thin film one
Kind.
Preferred as technique scheme, described self-curing type macromolecule resin is self-curing type epoxy resin, poly-ammonia
Ester resin, polyester resin, polyimide resin, phenolic resin, novolac epoxy resin, acrylic resin, methacrylic resin
In the mixture that formed of a kind of or at least two.
Preferred as technique scheme, described organic solvent be Oleum Terebinthinae, terpineol, hexadecanol, butyl carbitol,
Diethylene glycol monomethyl ether, dibutyl ethylene glycol ether, butyl carbitol acetate, ethylene glycol ether acetate, tributyl citrate,
Tributyl phosphate, GBL, mixed dibasic acid ester, N-Methyl pyrrolidone, DMF, N, N-dimethyl
The mixture that a kind of or at least two in acetamide, dimethyl sulfoxide is formed.
Preferred as technique scheme, described dispersant is triammonium citrate, polymethyl acid amide, Isosorbide-5-Nitrae-dihydroxy
The mixture that a kind of or at least two in base sulfanilic acid is formed.
Preferred as technique scheme, described defoamer is organosiloxane, polyethers, Polyethylene Glycol, ethylene-propylene
One in acid copolymer, polyglyceryl fatty acid ester, polydimethylsiloxane, organic silicon modified by polyether or at least two institute group
The mixture become.
Preferred as technique scheme, described thixotropic agent be hexadecanol, span85, polyamide wax, castor oil hydrogenated,
The mixture that a kind of or at least two in thixotropy alkyd resin, organobentonite or aerosil is formed.
The preparation method of a kind of low-temperature cured conductive paste based on flexible parent metal, comprises the following steps:
(1) complex function phase is prepared: by spherical for nanometer argentum powder, nano-sheet nikel powder mix homogeneously to prepare mixed function
Phase；
(2) prepare organic carrier: by organic solvent, self-curing type macromolecule resin, dispersant, defoamer, thixotropic agent in
80 DEG C of water-baths are dissolved to obtain organic carrier, and by adjusting the content of macromolecule resin, so that the viscosity control of organic carrier
System is in the range of 200mPa s-300mPa s；
(3) prepare electrocondution slurry: by complex function phase, organic carrier dispersed with stirring in container, carry out three rollers the most again
Rolling, to obtain the range of viscosities electrocondution slurry for 100Pa s ± 20Pa s.
Compared with prior art, the invention have the advantages that
(1) present invention uses the compound as function phase of the spherical argentum powder of nanometer and nano-sheet nikel powder, is used for preparing low temperature
Curing conductive slurry, both ensure that effective coverage rate of electrode, had reduced the sky between electrode and flexible parent metal to greatest extent
Gap, reduces electrode and the contact resistance of flexible substrates, and base metal nickel part substitutes noble silver (Ag) and reaches suitable simultaneously
Performance, greatly reduces the manufacturing cost of low-temperature cured conductive paste, can meet again the electrical property such as capacity, loss simultaneously and want
Ask；
(2) present invention uses self curable epoxy resin, polyurethane resin, polyester resin, polyimide resin, phenolic aldehyde tree
Fat, novolac epoxy resin, acrylic resin, methacrylic resin prepare low-temperature cured conductive paste organic carrier, use
Electrocondution slurry prepared by this organic carrier has excellent adhesive force, and the electrode layer flawless simultaneously prepared and pin pore etc. lack
Fall into；
(3) printing characteristic of the low-temperature cured conductive paste based on flexible parent metal of the present invention and burn till characteristic good, side
Resistance reheating rate of change is less than 5%, and match with flexible parent metal, the advantage such as cheap.
Detailed description of the invention:
In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solving
Release the present invention, the present invention will not be constituted any restriction.
Embodiment 1
A kind of low-temperature cured conductive paste based on flexible parent metal, by weight percentage, including following components:
Complex function phase 60%,
Organic carrier 40%；
Described complex function phase, by weight percentage, including following components:
The spherical argentum powder of nanometer 40%,
Nano-sheet nikel powder 60%；
Described organic carrier, by weight percentage, including following components:
Flexible parent metal is PET film；
Its preparation method comprises the following steps:
(1) complex function phase is prepared: by spherical for nanometer argentum powder, nano-sheet nikel powder mix homogeneously to prepare mixed function
Phase；
(2) organic carrier is prepared: by N,N-dimethylformamide, self-curing type epoxy resin, polymethyl acid amide, gather
Ether modified organic silicon, polyamide wax dissolve to obtain organic carrier in 80 DEG C of water-baths, and by adjusting containing of macromolecule resin
Amount, so that the viscosity of organic carrier controls in the range of 200mPa s-300mPa s；
(3) prepare electrocondution slurry: by complex function phase, organic carrier dispersed with stirring in container, carry out three rollers the most again
Rolling, to obtain the range of viscosities electrocondution slurry for 100Pa s ± 20Pa s.
Embodiment 2
A kind of low-temperature cured conductive paste based on flexible parent metal, by weight percentage, including following components:
Complex function phase 70%,
Organic carrier 30%；
Described complex function phase, by weight percentage, including following components:
The spherical argentum powder of nanometer 50%,
Nano-sheet nikel powder 50%；
Described organic carrier, by weight percentage, including following components:
Flexible parent metal is PBT；
Its preparation method comprises the following steps:
(1) complex function phase is prepared: by spherical for nanometer argentum powder, nano-sheet nikel powder mix homogeneously to prepare mixed function
Phase；
(2) prepare organic carrier: by N,N-dimethylacetamide, self-curing type polyurethane resin, polymethyl acid amide,
Polydimethylsiloxane, polyamide wax dissolve to obtain organic carrier in 80 DEG C of water-baths, and by adjusting macromolecule resin
Content, so that the viscosity of organic carrier controls in the range of 200mPa s-300mPa s；
(3) prepare electrocondution slurry: by complex function phase, organic carrier dispersed with stirring in container, carry out three rollers the most again
Rolling, to obtain the range of viscosities electrocondution slurry for 100Pa s ± 20Pa s.
Embodiment 3
A kind of low-temperature cured conductive paste based on flexible parent metal, by weight percentage, including following components:
Complex function phase 65%,
Organic carrier 35%；
Described complex function phase, by weight percentage, including following components:
The spherical argentum powder of nanometer 55%,
Nano-sheet nikel powder 45%；
Described organic carrier, by weight percentage, including following components:
Flexible parent metal is PI thin film；
Its preparation method comprises the following steps:
(1) complex function phase is prepared: by spherical for nanometer argentum powder, nano-sheet nikel powder mix homogeneously to prepare mixed function
Phase；
(2) organic carrier is prepared: by N-Methyl pyrrolidone, self-curing type phenolic resin, 1,4-dihydroxy sulfanilic acid, gather
Ether modified organic silicon, polyamide wax dissolve to obtain organic carrier in 80 DEG C of water-baths, and by adjusting containing of macromolecule resin
Amount, so that the viscosity of organic carrier controls in the range of 200mPa s-300mPa s；
(3) prepare electrocondution slurry: by complex function phase, organic carrier dispersed with stirring in container, carry out three rollers the most again
Rolling, to obtain the range of viscosities electrocondution slurry for 100Pa s ± 20Pa s.
Embodiment 4
A kind of low-temperature cured conductive paste based on flexible parent metal, by weight percentage, including following components:
Complex function phase 80%,
Organic carrier 20%；
Described complex function phase, by weight percentage, including following components:
The spherical argentum powder of nanometer 45%,
Nano-sheet nikel powder 55%；
Described organic carrier, by weight percentage, including following components:
Flexible parent metal is PI；
Its preparation method comprises the following steps:
(1) complex function phase is prepared: by spherical for nanometer argentum powder, nano-sheet nikel powder mix homogeneously to prepare mixed function
Phase；
(2) prepare organic carrier: by N-Methyl pyrrolidone, self-curing polyimide type resin, polymethyl acid amide,
Polydimethylsiloxane, castor oil hydrogenated dissolve to obtain organic carrier in 80 DEG C of water-baths, and by adjusting macromolecule resin
Content so that the viscosity of organic carrier controls in the range of 200mPa s-300mPa s；
(3) prepare electrocondution slurry: by complex function phase, organic carrier dispersed with stirring in container, carry out three rollers the most again
Rolling, to obtain the range of viscosities electrocondution slurry for 100Pa s ± 20Pa s.
Embodiment 5
A kind of low-temperature cured conductive paste based on flexible parent metal, by weight percentage, including following components:
Complex function phase 75%,
Organic carrier 25%；
Described complex function phase, by weight percentage, including following components:
The spherical argentum powder of nanometer 45%,
Nano-sheet nikel powder 55%；
Described organic carrier, by weight percentage, including following components:
Flexible parent metal is PI；
Its preparation method comprises the following steps:
(1) complex function phase is prepared: by spherical for nanometer argentum powder, nano-sheet nikel powder mix homogeneously to prepare mixed function
Phase；
(2) organic carrier is prepared: by N-Methyl pyrrolidone, self-curing type polyester resin, 1,4-dihydroxy sulfanilic acid, gather
Ether modified organic silicon, polyamide wax dissolve to obtain organic carrier in 80 DEG C of water-baths, and by adjusting containing of macromolecule resin
Amount, so that the viscosity of organic carrier controls in the range of 200mPa s-300mPa s；
(3) prepare electrocondution slurry: by complex function phase, organic carrier dispersed with stirring in container, carry out three rollers the most again
Rolling, to obtain the range of viscosities electrocondution slurry for 100Pa s ± 20Pa s.
Embodiment 6
A kind of low-temperature cured conductive paste based on flexible parent metal, by weight percentage, including following components:
Complex function phase 80%,
Organic carrier 20%；
Described complex function phase, by weight percentage, including following components:
The spherical argentum powder of nanometer 45%,
Nano-sheet nikel powder 55%；
Described organic carrier, by weight percentage, including following components:
Flexible parent metal is PEN；
Its preparation method comprises the following steps:
(1) complex function phase is prepared: by spherical for nanometer argentum powder, nano-sheet nikel powder mix homogeneously to prepare mixed function
Phase；
(2) organic carrier is prepared: by N-Methyl pyrrolidone, self-curing type acrylic resin, polymethyl acid amide, gather
Dimethyl siloxane, castor oil hydrogenated dissolve to obtain organic carrier in 80 DEG C of water-baths, and by adjusting macromolecule resin
Content, so that the viscosity of organic carrier controls in the range of 200mPa s-300mPa s；
(3) prepare electrocondution slurry: by complex function phase, organic carrier dispersed with stirring in container, carry out three rollers the most again
Rolling, to obtain the range of viscosities electrocondution slurry for 100Pa s ± 20Pa s.
Embodiment 7
A kind of low-temperature cured conductive paste based on flexible parent metal, by weight percentage, including following components:
Complex function phase 75%,
Organic carrier 25%；
Described complex function phase, by weight percentage, including following components:
The spherical argentum powder of nanometer 60%,
Nano-sheet nikel powder 40%；
Described organic carrier, by weight percentage, including following components:
Flexible parent metal is PI；
Its preparation method comprises the following steps:
(1) complex function phase is prepared: by spherical for nanometer argentum powder, nano-sheet nikel powder mix homogeneously to prepare mixed function
Phase；
(2) prepare organic carrier: by N-Methyl pyrrolidone, self-curing type novolac epoxy resin, polymethyl acid amide,
Organic silicon modified by polyether, polyamide wax dissolve to obtain organic carrier in 80 DEG C of water-baths, and by adjusting macromolecule resin
Content, so that the viscosity of organic carrier controls in the range of 200mPa s-300mPa s；
(3) prepare electrocondution slurry: by complex function phase, organic carrier dispersed with stirring in container, carry out three rollers the most again
Rolling, to obtain the range of viscosities electrocondution slurry for 100Pa s ± 20Pa s.
Embodiment 8
A kind of low-temperature cured conductive paste based on flexible parent metal, by weight percentage, including following components:
Complex function phase 65%,
Organic carrier 35%；
Described complex function phase, by weight percentage, including following components:
The spherical argentum powder of nanometer 50%,
Nano-sheet nikel powder 50%；
Described organic carrier, by weight percentage, including following components:
Flexible parent metal is PA；
Its preparation method comprises the following steps:
(1) complex function phase is prepared: by spherical for nanometer argentum powder, nano-sheet nikel powder mix homogeneously to prepare mixed function
Phase；
(2) organic carrier is prepared: by dimethyl sulfoxide, self-curing type methacrylic resin, triammonium citrate, polyether-modified
Organosilicon, thixotropy alkyd resin dissolve to obtain organic carrier in 80 DEG C of water-baths, and by adjusting containing of macromolecule resin
Amount, so that the viscosity of organic carrier controls in the range of 200mPa s-300mPa s；
(3) prepare electrocondution slurry: by complex function phase, organic carrier dispersed with stirring in container, carry out three rollers the most again
Rolling, to obtain the range of viscosities electrocondution slurry for 100Pa s ± 20Pa s.
The performance parameter of the low-temperature cured conductive paste that the present invention prepares is as shown in table 1.
Table 1
The slurry that the present invention prepares can print on flexible substrates, and baking temperature is 150 DEG C, and drying time is 30 minutes.
Above content is only presently preferred embodiments of the present invention, for those of ordinary skill in the art, according to the present invention's
Thought, the most all will change, and this specification content should not be construed as the present invention
Restriction.
Claims (9)
1. a low-temperature cured conductive paste based on flexible parent metal, it is characterised in that by weight percentage, including following group
Point:
Complex function phase 60-80%,
Organic carrier 20-40%；
Described complex function phase, by weight percentage, including following components:
Nanometer spherical argentum powder 40-65%,
Nano-sheet nikel powder 35-60%；
Described organic carrier, by weight percentage, including following components:
A kind of low-temperature cured conductive paste based on flexible parent metal, it is characterised in that described nanometer
The particle size values of spherical argentum powder is 20-50nm, tap density is 3.0～4.0g/cm3, the particle size values of nano-sheet nikel powder is 10-
60nm, tap density are 2.0～3.0g/cm3。
A kind of low-temperature cured conductive paste based on flexible parent metal, it is characterised in that described flexibility
Base material includes polyethylene terephthalate (PET), polybutylene terephthalate (PBT), PEN
(PEN), the one in polyimides (PI), polyamide (PA) thin film.
A kind of low-temperature cured conductive paste based on flexible parent metal, it is characterised in that described from solid
Change type macromolecule resin is self-curing type epoxy resin, polyurethane resin, polyester resin, polyimide resin, phenolic resin, phenol
The mixture that a kind of or at least two in formaldehyde epoxy resin, acrylic resin, methacrylic resin is formed.
A kind of low-temperature cured conductive paste based on flexible parent metal, it is characterised in that described organic
Solvent is Oleum Terebinthinae, terpineol, hexadecanol, butyl carbitol, diethylene glycol monomethyl ether, dibutyl ethylene glycol ether, butyl card must
Alcohol acetate, ethylene glycol ether acetate, tributyl citrate, tributyl phosphate, GBL, mixed dibasic acid ester, N-
One in methyl pyrrolidone, DMF, N,N-dimethylacetamide, dimethyl sulfoxide or at least two institute
The mixture of composition.
A kind of low-temperature cured conductive paste based on flexible parent metal, it is characterised in that described dispersion
It is mixed that agent is triammonium citrate, a kind of or at least two in polymethyl acid amide, 1,4-dihydroxy sulfanilic acid is formed
Compound.
A kind of low-temperature cured conductive paste based on flexible parent metal, it is characterised in that described froth breaking
Agent be organosiloxane, polyethers, Polyethylene Glycol, ethylene-acrylic acid copolymer, polyglyceryl fatty acid ester, polydimethylsiloxane,
The mixture that a kind of or at least two in organic silicon modified by polyether is formed.
A kind of low-temperature cured conductive paste based on flexible parent metal, it is characterised in that described thixotroping
Agent is hexadecanol, span85, polyamide wax, castor oil hydrogenated, thixotropy alkyd resin, organobentonite or aerosil
In the mixture that formed of a kind of or at least two.
9. the preparation method of a kind of based on flexible parent metal the low-temperature cured conductive paste as described in claim 1 to 8 is arbitrary, its
It is characterised by, comprises the following steps:
(1) complex function phase is prepared: by spherical for nanometer argentum powder, nano-sheet nikel powder mix homogeneously to prepare mixed function phase；
(2) organic carrier is prepared: by organic solvent, self-curing type macromolecule resin, dispersant, defoamer, thixotropic agent are in 80 DEG C
Water-bath dissolves to obtain organic carrier, and by adjusting the content of macromolecule resin, so that the viscosity of organic carrier controls
In the range of 200mPa s-300mPa s；
(3) prepare electrocondution slurry: by complex function phase, organic carrier dispersed with stirring in container, carry out three-roll rolling the most again,
To obtain the electrocondution slurry that range of viscosities is 100Pa s ± 20Pa s.
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| CN106623968A (en) * | 2016-11-09 | 2017-05-10 | 南昌大学 | Preparing method for superfine silver powder with characteristic of narrow particle size distribution |
| CN106683747A (en) * | 2017-01-23 | 2017-05-17 | 湖南省国银新材料有限公司 | Touch screen silver paste and preparation method thereof |
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