CN106098145B - 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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- CN106098145B CN106098145B CN201610528661.0A CN201610528661A CN106098145B CN 106098145 B CN106098145 B CN 106098145B CN 201610528661 A CN201610528661 A CN 201610528661A CN 106098145 B CN106098145 B CN 106098145B
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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 discloses a kind of low-temperature cured conductive paste based on flexible parent metal, the electrocondution slurry includes complex function phase, organic carrier, complex function is mutually for the mixed powder of the spherical silver powder of nanometer and nano-sheet nickel powder, the mixture that organic carrier is made of organic solvent, self-curing type macromolecule resin, dispersant, defoamer, thixotropic agent；The invention also discloses the preparation method of the low-temperature cured conductive paste.Electrocondution slurry prepared by the present invention has the advantages that cost is low, conducts electricity very well, strong adhesive force, printing characteristic, sintering characteristic, environmental-protecting performance is excellent and matches with flexible parent metal.
Description
Technical field：
The present invention relates to technical field of electronic materials, is specifically related to a kind of low-temperature cured conductive slurry based on flexible parent metal
Material.
Background technology：
Electrocondution slurry is the critical material of electronic component encapsulation, electrode and interconnection, mainly includes burning infiltration type electrocondution slurry
With two major class of curing type conducting resinl.Electrocondution slurry is different according to filler therein, can be divided into carbon slurry (graphite conductor), metal pulp
Expect (bronze, silver powder, copper powder, yellow gold), and modified ceramic slurry.Classified 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 protection, presently used
Also some harmful substances are often contained in conducting resinl, and cost is higher.A kind of environmentally friendly electrocondution slurry is worked out, not only preparation process
Simply, size performance is improved, prepares the unleaded electrocondution slurry of low-temperature setting and low-cost solidification conducting resinl, to meet market need
Ask.
In present applicable electrocondution slurry product, the content of silver powder in the slurry is 50%-70%, and silver is that your gold belonged to
One kind in category, its cost are 3-4 times of conventional base metal, and market purchases that foreign brand name is expensive, this just leads mostly
The high expensive of whole electronic market is caused.And low-end product price drops, under keen competition causes products quotation further
Fall, electronic market is developed to inexpensive direction at present, and domestic low-temperature solidified silver paste year usage amount is more than 120 tons.Produce
Low cost, high performance electrocondution slurry are our technical problems in the urgent need to address.Also have using base metal in the prior art
To replace part noble metal to be used as the function phase of electrocondution slurry, but it is obtained electrocondution slurry electric conductivity, impressionability, attached
It is not ideal the performance such as to put forth effort.
The content of the invention：
The object of the present invention is to provide a kind of low-temperature cured conductive paste based on flexible parent metal, it conducts electricity very well, is attached
It is excellent to put forth effort strong, printing characteristic, sintering characteristic, environmental-protecting performance, and match with flexible parent metal, with resistance slurry wettability, phase
Capacitive is excellent, and cost is low.
The object of the present invention is to provide the preparation method of the low-temperature cured conductive paste.
To achieve the above object, the present invention uses following technical scheme：
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%；
The complex function phase, by weight percentage, including following components：
The spherical silver powder 40-65% of nanometer,
Nano-sheet nickel powder 35-60%；
The organic carrier, by weight percentage, including following components：
As the preferred of above-mentioned technical proposal, the particle size values of the spherical silver powder of nanometer are 20-50nm, tap density is
3.0~4.0g/cm3, the particle size values of nano-sheet nickel powder are 10-60nm, tap density is 2.0~3.0g/cm3。
As the preferred of above-mentioned technical proposal, the flexible parent metal includes polyethylene terephthalate (PET), is poly- to benzene
One in dioctyl phthalate fourth diester (PBT), polyethylene naphthalate (PEN), polyimides (PI), polyamide (PA) film
Kind.
As the preferred of above-mentioned technical proposal, the 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 a kind of or at least two mixtures formed.
As the preferred of above-mentioned technical proposal, the organic solvent for turpentine oil, terpinol, hexadecanol, butyl carbitol,
Diethylene glycol monomethyl ether, dibutyl ethylene glycol ether, butyl carbitol acetate, ethylene glycol ether acetate, tributyl citrate,
Tributyl phosphate, 1,4-butyrolactone, mixed dibasic acid ester, 1-methyl-2-pyrrolidinone, n,N-Dimethylformamide, N, N- dimethyl
A kind of or at least two mixtures formed in acetamide, dimethyl sulfoxide.
As the preferred of above-mentioned technical proposal, the dispersant is triammonium citrate, polymethyl acid amide, Isosorbide-5-Nitrae-dihydroxy
A kind of or at least two mixtures formed in base sulfanilic acid.
As the preferred of above-mentioned technical proposal, the defoamer is organosiloxane, polyethers, polyethylene glycol, ethylene-propylene
One kind or at least two groups in acid copolymer, polyglyceryl fatty acid ester, dimethyl silicone polymer, organic silicon modified by polyether
Into mixture.
As the preferred of above-mentioned technical proposal, the thixotropic agent for hexadecanol, span85, polyamide wax, rilanit special,
A kind of or at least two mixtures formed in thixotropy alkyd resin, organobentonite or aerosil.
A kind of preparation method of the low-temperature cured conductive paste based on flexible parent metal, comprises the following steps：
(1) complex function phase is prepared：The spherical silver powder of nanometer, nano-sheet nickel powder are uniformly mixed to prepare mixed function
Phase；
(2) organic carrier is prepared：By organic solvent, self-curing type macromolecule resin, dispersant, defoamer, thixotropic agent in
Dissolved in 80 DEG C of water-baths 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 200mPas-300mPas；
(3) electrocondution slurry is prepared：Complex function phase, organic carrier are dispersed with stirring in container, then carry out three rollers again
Rolling, to obtain electrocondution slurry of the range of viscosities as 100Pas ± 20Pas.
Compared with prior art, the present invention has the following advantages：
(1) present invention is used as function phase using the spherical silver powder of nanometer and the compound of nano-sheet nickel powder, is used to prepare low temperature
Curing conductive slurry, both ensure that effective covering surface of electrode, and had reduced the sky between electrode and flexible parent metal to greatest extent
Gap, reduces electrode and the contact resistance of flexible substrates, while base metal nickel part substitutes noble silver (Ag) and reaches suitable
Performance, greatly reduces the manufacture cost of low-temperature cured conductive paste, while can meet that the electrical properties such as capacity, loss will again
Ask；
(2) present invention is using 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 the organic carrier has excellent adhesive force, while the electrode layer flawless prepared and pin stomata etc. lack
Fall into；
(3) printing characteristic of the low-temperature cured conductive paste based on flexible parent metal of the invention and characteristic good is burnt till, side
The advantages that hindering reheating change rate and be less than 5%, and matching with flexible parent metal, is cheap.
Embodiment：
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
The present invention is released, any restriction will not be formed to the present invention.
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%；
The complex function phase, by weight percentage, including following components：
The spherical silver powder 40% of nanometer,
Nano-sheet nickel powder 60%；
The 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：The spherical silver powder of nanometer, nano-sheet nickel powder are uniformly mixed to prepare mixed function
Phase；
(2) organic carrier is prepared：By N,N-dimethylformamide, self-curing type epoxy resin, polymethyl acid amide, poly-
Ether modified organic silicon, polyamide wax are dissolved in 80 DEG C of water-baths to obtain organic carrier, and containing by adjusting macromolecule resin
Amount, so that the viscosity of organic carrier is controlled in the range of 200mPas-300mPas；
(3) electrocondution slurry is prepared：Complex function phase, organic carrier are dispersed with stirring in container, then carry out three rollers again
Rolling, to obtain electrocondution slurry of the range of viscosities as 100Pas ± 20Pas.
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%；
The complex function phase, by weight percentage, including following components：
The spherical silver powder 50% of nanometer,
Nano-sheet nickel powder 50%；
The 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：The spherical silver powder of nanometer, nano-sheet nickel powder are uniformly mixed to prepare mixed function
Phase；
(2) organic carrier is prepared：By n,N-dimethylacetamide, self-curing type polyurethane resin, polymethyl acid amide,
Dimethyl silicone polymer, polyamide wax are dissolved to obtain organic carrier in 80 DEG C of water-baths, and by adjusting macromolecule resin
Content, so that the viscosity of organic carrier is controlled in the range of 200mPas-300mPas；
(3) electrocondution slurry is prepared：Complex function phase, organic carrier are dispersed with stirring in container, then carry out three rollers again
Rolling, to obtain electrocondution slurry of the range of viscosities as 100Pas ± 20Pas.
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%；
The complex function phase, by weight percentage, including following components：
The spherical silver powder 55% of nanometer,
Nano-sheet nickel powder 45%；
The organic carrier, by weight percentage, including following components：
Flexible parent metal is PI films；
Its preparation method comprises the following steps：
(1) complex function phase is prepared：The spherical silver powder of nanometer, nano-sheet nickel powder are uniformly mixed to prepare mixed function
Phase；
(2) organic carrier is prepared：By 1-methyl-2-pyrrolidinone, self-curing type phenolic resin, 1,4- dihydroxy sulfanilic acid, poly-
Ether modified organic silicon, polyamide wax are dissolved in 80 DEG C of water-baths to obtain organic carrier, and containing by adjusting macromolecule resin
Amount, so that the viscosity of organic carrier is controlled in the range of 200mPas-300mPas；
(3) electrocondution slurry is prepared：Complex function phase, organic carrier are dispersed with stirring in container, then carry out three rollers again
Rolling, to obtain electrocondution slurry of the range of viscosities as 100Pas ± 20Pas.
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%；
The complex function phase, by weight percentage, including following components：
The spherical silver powder 45% of nanometer,
Nano-sheet nickel powder 55%；
The 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：The spherical silver powder of nanometer, nano-sheet nickel powder are uniformly mixed to prepare mixed function
Phase；
(2) organic carrier is prepared：By 1-methyl-2-pyrrolidinone, self-curing polyimide type resin, polymethyl acid amide,
Dimethyl silicone polymer, rilanit special are dissolved to obtain organic carrier in 80 DEG C of water-baths, and by adjusting macromolecule resin
Content so that organic carrier viscosity control in the range of 200mPas-300mPas；
(3) electrocondution slurry is prepared：Complex function phase, organic carrier are dispersed with stirring in container, then carry out three rollers again
Rolling, to obtain electrocondution slurry of the range of viscosities as 100Pas ± 20Pas.
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%；
The complex function phase, by weight percentage, including following components：
The spherical silver powder 45% of nanometer,
Nano-sheet nickel powder 55%；
The 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：The spherical silver powder of nanometer, nano-sheet nickel powder are uniformly mixed to prepare mixed function
Phase；
(2) organic carrier is prepared：By 1-methyl-2-pyrrolidinone, self-curing type polyester resin, 1,4- dihydroxy sulfanilic acid, poly-
Ether modified organic silicon, polyamide wax are dissolved in 80 DEG C of water-baths to obtain organic carrier, and containing by adjusting macromolecule resin
Amount, so that the viscosity of organic carrier is controlled in the range of 200mPas-300mPas；
(3) electrocondution slurry is prepared：Complex function phase, organic carrier are dispersed with stirring in container, then carry out three rollers again
Rolling, to obtain electrocondution slurry of the range of viscosities as 100Pas ± 20Pas.
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%；
The complex function phase, by weight percentage, including following components：
The spherical silver powder 45% of nanometer,
Nano-sheet nickel powder 55%；
The 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：The spherical silver powder of nanometer, nano-sheet nickel powder are uniformly mixed to prepare mixed function
Phase；
(2) organic carrier is prepared：By 1-methyl-2-pyrrolidinone, self-curing type acrylic resin, polymethyl acid amide, poly-
Dimethyl siloxane, rilanit special are dissolved to obtain organic carrier in 80 DEG C of water-baths, and by adjusting macromolecule resin
Content, so that the viscosity of organic carrier is controlled in the range of 200mPas-300mPas；
(3) electrocondution slurry is prepared：Complex function phase, organic carrier are dispersed with stirring in container, then carry out three rollers again
Rolling, to obtain electrocondution slurry of the range of viscosities as 100Pas ± 20Pas.
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%；
The complex function phase, by weight percentage, including following components：
The spherical silver powder 60% of nanometer,
Nano-sheet nickel powder 40%；
The 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：The spherical silver powder of nanometer, nano-sheet nickel powder are uniformly mixed to prepare mixed function
Phase；
(2) organic carrier is prepared：By 1-methyl-2-pyrrolidinone, self-curing type novolac epoxy resin, polymethyl acid amide,
Organic silicon modified by polyether, polyamide wax are dissolved to obtain organic carrier in 80 DEG C of water-baths, and by adjusting macromolecule resin
Content, so that the viscosity of organic carrier is controlled in the range of 200mPas-300mPas；
(3) electrocondution slurry is prepared：Complex function phase, organic carrier are dispersed with stirring in container, then carry out three rollers again
Rolling, to obtain electrocondution slurry of the range of viscosities as 100Pas ± 20Pas.
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%；
The complex function phase, by weight percentage, including following components：
The spherical silver powder 50% of nanometer,
Nano-sheet nickel powder 50%；
The 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：The spherical silver powder of nanometer, nano-sheet nickel powder are uniformly mixed 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 are dissolved in 80 DEG C of water-baths to obtain organic carrier, and containing by adjusting macromolecule resin
Amount, so that the viscosity of organic carrier is controlled in the range of 200mPas-300mPas；
(3) electrocondution slurry is prepared：Complex function phase, organic carrier are dispersed with stirring in container, then carry out three rollers again
Rolling, to obtain electrocondution slurry of the range of viscosities as 100Pas ± 20Pas.
The performance parameter of low-temperature cured conductive paste produced by the present invention is as shown in table 1.
Table 1
Slurry produced by the present invention can print on flexible substrates, and drying 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, there will be changes, this specification content should not be construed as to the present invention in specific embodiments and applications
Limitation.
Claims (7)
1. a kind of low-temperature cured conductive paste based on flexible parent metal, it is characterised in that by weight percentage, including with the following group
Point：
Complex function phase 60-80%,
Organic carrier 20-40%；
The complex function phase, by weight percentage, including following components：
The spherical silver powder 40-65% of nanometer,
Nano-sheet nickel powder 35-60%；
The organic carrier, by weight percentage, including following components：
The dispersant is triammonium citrate, polymethyl acid amide, one kind in 1,4- dihydroxy sulfanilic acids or at least two
The formed mixture of kind；
Its preparation method comprises the following steps：
(1) complex function phase is prepared：The spherical silver powder of nanometer, nano-sheet nickel powder are uniformly mixed to prepare complex function phase；
(2) organic carrier is prepared：By organic solvent, self-curing type macromolecule resin, dispersant, defoamer, thixotropic agent are in 80 DEG C
Dissolved in water-bath to obtain organic carrier, and by adjusting the content of macromolecule resin, so that the viscosity control of organic carrier exists
In the range of 200mPas-300mPas；
(3) electrocondution slurry is prepared：Complex function phase, organic carrier are dispersed with stirring in container, then carry out three-roll rolling again,
To obtain electrocondution slurry of the range of viscosities as 100Pas ± 20Pas.
A kind of 2. low-temperature cured conductive paste based on flexible parent metal as claimed in claim 1, it is characterised in that the nanometer
The particle size values of spherical silver powder are 20-50nm, tap density is 3.0~4.0g/cm3, the particle size values of nano-sheet nickel powder are 10-
60nm, tap density are 2.0~3.0g/cm3。
A kind of 3. low-temperature cured conductive paste based on flexible parent metal as claimed in claim 1, it is characterised in that the flexibility
Base material includes polyethylene terephthalate (PET), polybutylene terephthalate (PBT), polyethylene naphthalate
(PEN), one kind in polyimides (PI), polyamide (PA) film.
4. a kind of low-temperature cured conductive paste based on flexible parent metal as claimed in claim 1, 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, third
A kind of or at least two mixtures formed in olefin(e) acid resin.
5. a kind of low-temperature cured conductive paste based on flexible parent metal as claimed in claim 1, it is characterised in that described organic
Solvent is turpentine oil, terpinol, hexadecanol, butyl carbitol, diethylene glycol monomethyl ether, dibutyl ethylene glycol ether, butyl card must
Alcohol acetate, ethylene glycol ether acetate, tributyl citrate, tributyl phosphate, 1,4-butyrolactone, mixed dibasic acid ester, N-
One kind or at least two institutes in methyl pyrrolidone, n,N-Dimethylformamide, n,N-dimethylacetamide, dimethyl sulfoxide
The mixture of composition.
A kind of 6. low-temperature cured conductive paste based on flexible parent metal as claimed in claim 1, it is characterised in that the defoaming
Agent for organosiloxane, polyethers, polyethylene glycol, ethylene-acrylic acid copolymer, polyglyceryl fatty acid ester, dimethyl silicone polymer,
A kind of or at least two mixtures formed in organic silicon modified by polyether.
A kind of 7. low-temperature cured conductive paste based on flexible parent metal as claimed in claim 1, it is characterised in that the thixotroping
Agent is hexadecanol, span85, polyamide wax, rilanit special, thixotropy alkyd resin, organobentonite or aerosil
In a kind of or at least two mixtures formed.
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| CN106623968B (en) * | 2016-11-09 | 2018-08-17 | 南昌大学 | A kind of preparation method of the super fine silver powder with the narrow characteristic of particle diameter distribution |
| CN106782885B (en) * | 2016-12-19 | 2018-07-03 | 西安工程大学 | A kind of preparation method of nano silver wire-copper staple fiber-copper composite electron slurry |
| CN106683747B (en) * | 2017-01-23 | 2017-12-22 | 湖南省国银新材料有限公司 | A kind of touch-screen silver paste and preparation method thereof |
| CN109300614B (en) * | 2018-09-26 | 2020-07-31 | 常州市利多合金材料有限公司 | Flexible elastic stress sensing conductive film and preparation method thereof |
| CN110007391A (en) * | 2019-04-12 | 2019-07-12 | 徐圣最 | A kind of low temperature preparation method of polyimide coating optical fiber |
| CN110267451A (en) * | 2019-05-29 | 2019-09-20 | 西安工程大学 | A kind of preparation method of flexible substrates conducting wire |
| CN111341484A (en) * | 2020-03-30 | 2020-06-26 | 善仁（浙江）新材料科技有限公司 | Low-temperature curing type conductive silver paste and preparation method thereof |
| CN112442257A (en) * | 2020-11-19 | 2021-03-05 | 贵州振华电子信息产业技术研究有限公司 | Modified epoxy resin and application thereof |
| CN112735628B (en) * | 2020-12-01 | 2022-03-29 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Low-temperature polymer conductive silver paste and preparation method thereof |
| CN112735629B (en) * | 2020-12-01 | 2022-04-12 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Low-temperature polymer conductive silver paste with low silver content and preparation method thereof |
| CN113555145B (en) * | 2021-09-23 | 2022-03-25 | 西安宏星电子浆料科技股份有限公司 | Flexible high-temperature-resistant conductive paste |
| CN116417178A (en) * | 2021-12-30 | 2023-07-11 | 北京梦之墨科技有限公司 | Low-temperature curing conductive paste and electronic device |
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