CN112908513A - Conductive silver paste for flexible circuit and preparation method thereof - Google Patents
Conductive silver paste for flexible circuit and preparation method thereof Download PDFInfo
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- CN112908513A CN112908513A CN202110075577.9A CN202110075577A CN112908513A CN 112908513 A CN112908513 A CN 112908513A CN 202110075577 A CN202110075577 A CN 202110075577A CN 112908513 A CN112908513 A CN 112908513A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 108
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000004593 Epoxy Substances 0.000 claims abstract description 31
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 29
- 229920005989 resin Polymers 0.000 claims abstract description 29
- 239000011347 resin Substances 0.000 claims abstract description 29
- 239000002245 particle Substances 0.000 claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 22
- 239000003960 organic solvent Substances 0.000 claims abstract description 21
- 239000002562 thickening agent Substances 0.000 claims abstract description 18
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 11
- 239000004332 silver Substances 0.000 claims abstract description 8
- 229910052709 silver Inorganic materials 0.000 claims abstract description 8
- 229920006395 saturated elastomer Polymers 0.000 claims description 37
- 239000003822 epoxy resin Substances 0.000 claims description 30
- 229920000647 polyepoxide Polymers 0.000 claims description 30
- 229920001225 polyester resin Polymers 0.000 claims description 27
- 239000004645 polyester resin Substances 0.000 claims description 27
- 239000003054 catalyst Substances 0.000 claims description 20
- 239000002904 solvent Substances 0.000 claims description 17
- 239000002105 nanoparticle Substances 0.000 claims description 11
- BVFSYZFXJYAPQJ-UHFFFAOYSA-N butyl(oxo)tin Chemical group CCCC[Sn]=O BVFSYZFXJYAPQJ-UHFFFAOYSA-N 0.000 claims description 10
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 239000012948 isocyanate Substances 0.000 claims description 7
- 150000002513 isocyanates Chemical class 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 229920005862 polyol Polymers 0.000 claims description 7
- 150000003077 polyols Chemical class 0.000 claims description 7
- 150000007519 polyprotic acids Polymers 0.000 claims description 7
- 239000003223 protective agent Substances 0.000 claims description 7
- 239000002002 slurry Substances 0.000 claims description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 239000003849 aromatic solvent Substances 0.000 claims description 6
- 239000000084 colloidal system Substances 0.000 claims description 6
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 5
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 5
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 5
- 239000008096 xylene Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910021485 fumed silica Inorganic materials 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 4
- 239000011265 semifinished product Substances 0.000 claims description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical group [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- 230000009477 glass transition Effects 0.000 claims description 3
- 150000002576 ketones Chemical class 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229920005749 polyurethane resin Polymers 0.000 claims description 3
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical group CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims 1
- 239000000853 adhesive Substances 0.000 abstract description 8
- 230000001070 adhesive effect Effects 0.000 abstract description 8
- 238000007639 printing Methods 0.000 abstract description 7
- 239000000758 substrate Substances 0.000 abstract description 7
- 125000003700 epoxy group Chemical group 0.000 abstract description 5
- 238000005452 bending Methods 0.000 abstract description 4
- 238000001723 curing Methods 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 10
- 230000006872 improvement Effects 0.000 description 10
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 description 7
- 239000006185 dispersion Substances 0.000 description 6
- FPZWZCWUIYYYBU-UHFFFAOYSA-N 2-(2-ethoxyethoxy)ethyl acetate Chemical compound CCOCCOCCOC(C)=O FPZWZCWUIYYYBU-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229920000728 polyester Polymers 0.000 description 3
- NQBXSWAWVZHKBZ-UHFFFAOYSA-N 2-butoxyethyl acetate Chemical compound CCCCOCCOC(C)=O NQBXSWAWVZHKBZ-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 150000002148 esters Chemical group 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- -1 depends on import Chemical compound 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007646 gravure printing Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000007644 letterpress printing Methods 0.000 description 1
- 238000013035 low temperature curing Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000007645 offset printing Methods 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Conductive Materials (AREA)
Abstract
The invention provides a conductive silver paste for a flexible circuit and a preparation method thereof, wherein the conductive silver paste for the flexible circuit comprises the following components in percentage by weight: 5-12 wt% of epoxy modified flexible resin, 30-50 wt% of organic solvent, 40-55 wt% of conductive silver powder, 3-15 wt% of nano silver powder, 0.5-2 wt% of flatting agent, 0.5-2 wt% of thickening agent, 0.5-2 wt% of defoaming agent and 0.5-5 wt% of curing agent; wherein the particle size of the conductive silver powder is micron-sized. By adopting the technical scheme of the invention, the epoxy group is introduced through the epoxy modified flexible resin, so that the adhesive force between the silver paste and the substrate is improved, and meanwhile, good flexibility is ensured; the flexible printed circuit board has excellent conductive performance, good printing performance, bending resistance and certain hardness, and can better meet the requirements of the flexible printed circuit board.
Description
Technical Field
The invention belongs to the technical field of conductive materials, and particularly relates to conductive silver paste for a flexible circuit and a preparation method of the conductive silver paste.
Background
With the rapid development of the electronic industry in recent years, the demand of electronic products such as membrane switches, flexible printed circuit boards, electromagnetic shields, potentiometers, radio frequency identification systems, solar cells and the like is rapidly increased, and the development and application of conductive silver paste as a key functional material for preparing such electronic components are also widely concerned by people. The analysis shows that the market for conductive silver paste alone has a billion dollars of market size each year. In the rapid development process of the information industry, the slurry plays an important role as a key material. Along with the development of the intelligent Internet of things, the demand of brushing flexible circuits is more and more extensive, and new requirements are also put forward for the bank award.
The low-temperature curing conductive silver paste refers to a type of silver paste with lower curing temperature (between 100 ℃ and 200 ℃), and can be printed on non-conductive printing stocks such as plastics, glass, ceramics or paper cloth materials. The printing method is wide, such as silk screen printing, letterpress printing, flexographic printing, gravure printing, offset printing and the like can be adopted. The silver paste for the flexible circuit board also belongs to low-temperature conductive silver paste, is environment-friendly conductive silver paste, mainly depends on import, has no major breakthrough in domestic preparation technology, and has certain gap with products of foreign manufacturers. At present, the silver paste for most of domestic flexible circuit boards has the following main problems: poor printing adhesion of polyester base materials, poor bending resistance of flexible base materials and the like.
Disclosure of Invention
Aiming at the technical problems, the invention discloses conductive silver paste for a flexible circuit and a preparation method thereof, which overcome the defects in the prior art, realize low-temperature rapid curing and can adapt to flexible circuit boards with various substrates.
In contrast, the technical scheme adopted by the invention is as follows:
the conductive silver paste comprises the following components in percentage by weight: 5-12 wt% of epoxy modified flexible resin, 30-50 wt% of organic solvent, 40-55 wt% of conductive silver powder, 3-15 wt% of nano silver powder, 0.5-2 wt% of flatting agent, 0.5-2 wt% of thickening agent, 0.5-2 wt% of defoaming agent and 0.5-5 wt% of curing agent; wherein the particle size of the conductive silver powder is micron-sized.
By adopting the technical scheme, the epoxy modified flexible resin is adopted, the epoxy group is introduced, the adhesiveness of the conductive silver paste and the substrate is improved while the conductive silver paste has good conductivity, the good flexibility is also ensured, the bending resistance of the flexible substrate after the conductive silver paste is adhered to the flexible substrate is improved, and the flexible substrate has good printing performance and hardness.
As a further improvement of the invention, the epoxy modified flexible resin is epoxy modified polyester resin or epoxy modified polyurethane resin.
As a further improvement of the invention, the elongation at break of the epoxy modified flexible resin after curing is more than 200%.
As a further improvement of the invention, the epoxy modified flexible resin is epoxy resin modified saturated polyester resin, the weight average molecular weight of the epoxy resin modified saturated polyester resin is 20000-45000, and the glass transition temperature is 0-50 ℃.
As a further improvement of the invention, the epoxy resin modified saturated polyester resin is prepared by adopting the following components and mass parts to react:
6-12 parts of epoxy resin, 25-30 parts of saturated polyol, 25-30 parts of saturated polybasic acid, 0.0001-0.005 part of catalyst, 2-3 parts of solvent and 30-40 parts of high-boiling-point aromatic solvent; wherein the catalyst is a tin-based catalyst.
By means of graft modification of polyester, epoxy groups are introduced, so that good flexibility is guaranteed while adhesion is improved. In the using process, the requirements of customers on reducing energy consumption and improving efficiency are considered, the baking time of the slurry and the baking temperature can be shortened and reduced by optimizing a solvent system, and the curing condition can be optimized to 140 ℃ (20-30 min) from the original 150 ℃ time (30-40 min).
As a further improvement of the invention, the solvent is xylene or toluene.
As a further development of the invention, the catalyst is monobutyltin oxide or a derivative of monobutyltin oxide.
As a further improvement of the invention, the particle size of the conductive silver powder is 2-15 μm; the particle size of the nano silver powder is 20-50 nm. Further, the particle size of the conductive silver powder is 2-12 μm,
as a further improvement of the invention, the conductive silver powder is spherical, spheroidal, flaky or dendritic; the nano silver powder is nano particles treated by an active protective agent.
As a further improvement of the invention, the thickening agent is one or a mixture of more than two of hydroxyethyl cellulose, polyvinyl butyral and fumed silica.
As a further improvement of the invention, the curing agent is a blocked isocyanate with an unblocking temperature of less than 120 ℃.
As a further improvement of the invention, the organic solvent is an ester and/or ketone solvent. More preferably, the solvent is one or a mixture of more than two of ethylene glycol butyl ether acetate, diethylene glycol butyl ether acetate and diethylene glycol ethyl ether acetate, wherein the mixture of diethylene glycol butyl ether acetate, diethylene glycol ethyl ether acetate or the mixture of more than two is preferred.
The invention also discloses a preparation method of the conductive silver paste for the flexible circuit, which comprises the following steps:
step S1, preparing epoxy modified flexible resin;
step S2, mixing, stirring and dispersing the epoxy modified flexible resin, the organic solvent, the leveling agent, the defoaming agent, the curing agent and the thickening agent in sequence to obtain premixed solvent colloid;
step S3, adding nano silver powder into the premixed solvent colloid for stirring, and then adding conductive silver powder for stirring to obtain a semi-finished conductive slurry;
and step S4, grinding the semi-finished product of the conductive paste to the fineness of 5-10 microns to obtain the conductive silver paste. Preferably, the semi-finished product of the conductive slurry is ground by a three-roll grinder.
Compared with the prior art, the invention has the beneficial effects that:
by adopting the technical scheme of the invention, the epoxy group is introduced through the epoxy modified flexible resin, so that the adhesive force between the silver paste and the substrate is improved, and meanwhile, good flexibility is ensured; the flexible printed circuit board has excellent conductive performance, good printing performance, bending resistance and certain hardness, and can better meet the requirements of the flexible printed circuit board.
Detailed Description
Preferred embodiments of the present invention are described in further detail below.
The conductive silver paste for the flexible circuit comprises the following components in percentage by weight: 5-12 wt% of epoxy modified flexible resin, 30-50 wt% of organic solvent, 40-55 wt% of conductive silver powder, 3-15 wt% of nano silver powder, 0.5-2 wt% of flatting agent, 0.5-2 wt% of thickening agent, 0.5-2 wt% of defoaming agent and 0.5-5 wt% of curing agent; wherein the particle size of the conductive silver powder is micron-sized.
The epoxy modified flexible resin is epoxy modified polyester resin or epoxy modified polyurethane resin. The elongation at break of the cured epoxy modified flexible resin is more than 200%. The boiling point of the organic solvent is 120-240 ℃; the particle size of the nano silver powder is 20-50 nm; the thickening agent is selected from one or more of hydroxyethyl cellulose, polyvinyl butyral ester or fumed silica; the curing agent is blocked isocyanate with deblocking temperature lower than 120 ℃. The organic solvent is an ester solvent and/or a ketone solvent. The organic solvent is one or more of ethylene glycol butyl ether acetate, diethylene glycol butyl ether acetate and diethylene glycol ethyl ether acetate, wherein the preferred organic solvent is diethylene glycol butyl ether acetate, diethylene glycol ethyl ether acetate or a mixture thereof. The particle size of the conductive silver powder is 2-12 microns; the shape of the conductive silver powder is spherical, spheroidal, flaky or dendritic. The nano silver powder is high-dispersion nano particles treated by an active protective agent.
Further, the epoxy modified flexible resin is epoxy resin modified saturated polyester resin, the weight average molecular weight of the epoxy resin modified saturated polyester resin is 20000-45000, and the glass transition temperature is 0-50 ℃. The epoxy resin modified saturated polyester resin is prepared by the following components in parts by mass:
6-12 parts of epoxy resin, 25-30 parts of saturated polyol, 25-30 parts of saturated polybasic acid, 0.0001-0.005 part of catalyst, 2-3 parts of dimethylbenzene and 30-40 parts of high-boiling-point aromatic solvent; wherein the catalyst is a tin-based catalyst. The catalyst is monobutyl tin oxide or a derivative of monobutyl tin oxide.
By means of graft modification of polyester, epoxy groups are introduced, so that good flexibility is guaranteed while adhesion is improved. In the using process, the requirements of customers on reducing energy consumption and improving efficiency are considered, the baking time of the slurry and the baking temperature can be shortened and reduced by optimizing a solvent system, and the curing condition can be optimized to 140 ℃ (20-30 min) from the original 150 ℃ time (30-40 min).
The preparation method of the conductive silver paste for the flexible circuit comprises the following steps:
step S1, preparing epoxy modified flexible resin;
step S2, mixing, stirring and dispersing the epoxy modified flexible resin, the organic solvent, the leveling agent, the defoaming agent, the curing agent and the thickening agent in sequence to obtain premixed solvent colloid;
step S3, adding nano silver powder into the premixed solvent colloid for stirring, and then adding conductive silver powder for stirring to obtain a semi-finished conductive slurry;
and step S4, grinding the semi-finished product of the conductive paste by a three-roll grinder to the grinding fineness of 5-10 microns to obtain the conductive silver paste.
Above-mentioned technical scheme improves the adhesive force when keeping good pliability through designing the resin adhesive, and the resin adhesive adds appropriate amount nanometer silver powder and the abundant dispersion in preparation process, and nanometer silver powder can form the electrically conductive route in the resin adhesive, improves the electric conductive property of resin adhesive, borrows this whole electric conductive property that improves electrically conductive silver thick liquid.
The following description will be made with reference to the conductive silver paste using epoxy resin modified saturated polyester resin in combination with examples.
Example 1
The conductive silver paste comprises the following components in percentage by weight: 8 wt% of epoxy resin modified saturated polyester resin, 33 wt% of organic solvent, 35 wt% of conductive silver powder, 20 wt% of nano silver powder, 0.5 wt% of flatting agent, 1 wt% of thickening agent, 0.5 wt% of defoaming agent and 2 wt% of curing agent; wherein the particle size of the conductive silver powder is micron-sized.
Wherein the organic solvent is diethylene glycol butyl ether acetate, the thickening agent is hydroxyethyl cellulose, and the curing agent is blocked isocyanate with the deblocking temperature lower than 120 ℃. The particle size of the nano particles is 20-50 nm; the particle size of the conductive silver powder is 2-12 microns; the morphology of the conductive silver powder comprises spherical shape and dendritic shape. The nano silver powder is high-dispersion nano particles treated by an active protective agent.
The epoxy modified flexible resin is epoxy resin modified saturated polyester resin, and the epoxy resin modified saturated polyester resin is prepared by the following components in parts by mass through reaction:
6 parts of epoxy resin, 30 parts of saturated polyol, 30 parts of saturated polybasic acid, 0.005 part of catalyst, 3 parts of dimethylbenzene and 40 parts of high-boiling-point aromatic hydrocarbon solvent; wherein the catalyst is monobutyl tin oxide.
The conductive silver paste was prepared according to the preparation method described above.
Example 2
The conductive silver paste comprises the following components in percentage by weight: 10 wt% of epoxy resin modified saturated polyester resin, 31 wt% of organic solvent, 35 wt% of conductive silver powder, 20 wt% of nano silver powder, 0.5 wt% of flatting agent, 0.5 wt% of thickening agent, 0.5 wt% of defoaming agent and 2.5 wt% of curing agent; wherein the particle size of the conductive silver powder is micron-sized.
Wherein the organic solvent is diethylene glycol ethyl ether acetate, the thickening agent is polyvinyl butyral, and the curing agent is blocked isocyanate with deblocking temperature lower than 120 ℃. The particle size of the nano particles is 20-50 nm; the particle size of the conductive silver powder is 2-12 microns; the morphology of the conductive silver powder comprises spherical shape and flake shape. The nano silver powder is high-dispersion nano particles treated by an active protective agent.
The epoxy modified flexible resin is epoxy resin modified saturated polyester resin, and the epoxy resin modified saturated polyester resin is prepared by the following components in parts by mass through reaction:
12 parts of epoxy resin, 28 parts of saturated polyol, 28 parts of saturated polybasic acid, 0.0003 part of catalyst, 3 parts of xylene and 30 parts of high-boiling-point aromatic solvent; wherein the catalyst is monobutyl tin oxide.
The conductive silver paste was prepared according to the preparation method described above.
Example 3
The conductive silver paste comprises the following components in percentage by weight: 10 wt% of epoxy resin modified saturated polyester resin, 31 wt% of organic solvent, 40 wt% of conductive silver powder, 15 wt% of nano silver powder, 0.5 wt% of flatting agent, 0.5 wt% of thickening agent, 0.5 wt% of defoaming agent and 2.5 wt% of curing agent; wherein the particle size of the conductive silver powder is micron-sized.
The organic solvent is diethylene glycol butyl ether acetate, the thickening agent is fumed silica, and the curing agent is blocked isocyanate with deblocking temperature lower than 120 ℃. The particle size of the nano particles is 20-50 nm; the particle size of the conductive silver powder is 2-12 microns; the morphology of the conductive silver powder comprises spheroidal and dendritic shapes. The nano silver powder is high-dispersion nano particles treated by an active protective agent.
The epoxy modified flexible resin is epoxy resin modified saturated polyester resin, and the epoxy resin modified saturated polyester resin is prepared by the following components in parts by mass through reaction:
10 parts of epoxy resin, 25 parts of saturated polyol, 25 parts of saturated polybasic acid, 0.0002 part of catalyst, 2 parts of xylene and 25 parts of high-boiling-point aromatic solvent; wherein the catalyst is monobutyl tin oxide.
The conductive silver paste was prepared according to the preparation method described above.
Comparative example 1
The conductive silver paste comprises the following components in percentage by weight: 10 wt% of epoxy resin modified saturated polyester resin, 31 wt% of organic solvent, 55 wt% of conductive silver powder, 0% of nano silver powder, 0.5 wt% of flatting agent, 0.5 wt% of thickening agent, 0.5 wt% of defoaming agent and 2.5 wt% of curing agent; wherein the particle size of the conductive silver powder is micron-sized.
Wherein the organic solvent is diethylene glycol butyl ether acetate, the thickening agent is hydroxyethyl cellulose, and the curing agent is blocked isocyanate with the deblocking temperature lower than 120 ℃. The particle size of the nano particles is 20-50 nm; the particle size of the conductive silver powder is 2-12 microns; the morphology of the conductive silver powder comprises spherical shape and dendritic shape. The nano silver powder is high-dispersion nano particles treated by an active protective agent.
The epoxy modified flexible resin is epoxy resin modified saturated polyester resin, and the epoxy resin modified saturated polyester resin is prepared by the following components in parts by mass through reaction:
8 parts of epoxy resin, 26 parts of saturated polyol, 26 parts of saturated polybasic acid, 0.0001 part of catalyst, 2 parts of xylene and 37 parts of high-boiling-point aromatic solvent; wherein the catalyst is monobutyl tin oxide.
The conductive silver paste was prepared according to the preparation method described above.
Comparative example 2
On the basis of example 1, the comparative example adopts the conventional polyester resin, and other proportions and process methods are the same as those of example 1.
The formulations of examples 1 to 3, comparative example 1 and comparative example 2 are shown in table 1, and the conductive silver pastes obtained in examples 1 to 3, comparative example 1 and comparative example 2 were tested, and the results are shown in table 2. Therefore, the conductive silver paste adopting the technical scheme of the invention has better adhesive force, keeps good flexibility, and has better hardness and conductivity. Comparative example 1, in which only 55 wt% of the conductive silver powder was used and no nano silver powder was used, was inferior to examples 1 to 3 in conductivity as seen from the comparison of properties.
TABLE 1 formulation List of examples and comparative examples
TABLE 2 comparison of the properties of the examples and comparative examples
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (10)
1. The utility model provides a flexible line is with electrically conductive silver thick liquid which characterized in that: the composite material comprises the following components in percentage by weight: 5-12 wt% of epoxy modified flexible resin, 30-50 wt% of organic solvent, 40-55 wt% of conductive silver powder, 3-15 wt% of nano silver powder, 0.5-2 wt% of flatting agent, 0.5-2 wt% of thickening agent, 0.5-2 wt% of defoaming agent and 0.5-5 wt% of curing agent; wherein the particle size of the conductive silver powder is micron-sized.
2. The conductive silver paste for flexible circuits according to claim 1, characterized in that: the epoxy modified flexible resin is epoxy modified polyester resin or epoxy modified polyurethane resin.
3. The conductive silver paste for flexible circuits according to claim 2, characterized in that: the epoxy modified flexible resin is epoxy resin modified saturated polyester resin, the weight average molecular weight of the epoxy resin modified saturated polyester resin is 20000-45000, and the glass transition temperature of the epoxy resin modified saturated polyester resin is 0-50 ℃.
4. The conductive silver paste for the flexible circuit according to claim 3, wherein the epoxy resin modified saturated polyester resin is prepared by reacting the following components in parts by mass:
6-12 parts of epoxy resin, 25-30 parts of saturated polyol, 25-30 parts of saturated polybasic acid, 0.0001-0.005 part of catalyst, 2-3 parts of solvent and 30-40 parts of high-boiling-point aromatic solvent; wherein the catalyst is a tin-based catalyst.
5. The conductive silver paste for flexible circuits according to claim 4, wherein: the solvent is xylene or toluene.
6. The conductive silver paste for flexible circuits according to claim 4, wherein: the catalyst is monobutyl tin oxide or a derivative of monobutyl tin oxide.
7. The conductive silver paste for the flexible circuit according to any one of claims 1 to 6, wherein: the particle size of the conductive silver powder is 2-15 μm; the particle size of the nano silver powder is 20-50 nm.
8. The conductive silver paste for flexible circuits according to claim 7, wherein: the conductive silver powder is spherical, spheroidal, flaky or dendritic; the nano silver powder is nano particles treated by an active protective agent.
9. The conductive silver paste for flexible circuits according to claim 7, wherein: the thickening agent is one or a mixture of more than two of hydroxyethyl cellulose, polyvinyl butyral and fumed silica; the curing agent is blocked isocyanate with deblocking temperature lower than 120 ℃; the organic solvent is an ester solvent and/or a ketone solvent.
10. The method for preparing the conductive silver paste for the flexible circuit according to any one of claims 1 to 9, characterized by comprising the following steps:
step S1, preparing epoxy modified flexible resin;
step S2, mixing, stirring and dispersing the epoxy modified flexible resin, the organic solvent, the leveling agent, the defoaming agent, the curing agent and the thickening agent in sequence to obtain premixed solvent colloid;
step S3, adding nano silver powder into the premixed solvent colloid for stirring, and then adding conductive silver powder for stirring to obtain a semi-finished conductive slurry;
and step S4, grinding the semi-finished product of the conductive paste to the fineness of 5-10 microns to obtain the conductive silver paste.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114628082A (en) * | 2022-03-23 | 2022-06-14 | 广东南海启明光大科技有限公司 | Environment-aging-resistant conductive silver paste and preparation method thereof |
CN114974651A (en) * | 2022-05-12 | 2022-08-30 | 北京梦之墨科技有限公司 | Epoxy resin-based conductive slurry and preparation method and application thereof |
CN116386929A (en) * | 2023-04-20 | 2023-07-04 | 深圳市信维通信股份有限公司 | Graphene composite conductive silver paste, preparation method and application thereof |
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CN105632588A (en) * | 2016-02-22 | 2016-06-01 | 昆山海斯电子有限公司 | High-conductivity silver paste and preparation method thereof |
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CN108770194A (en) * | 2018-05-29 | 2018-11-06 | 东莞市通美电子科技有限公司 | The preparation method of conductive silver paste used for printed circuit |
KR20200099101A (en) * | 2019-02-12 | 2020-08-21 | 주식회사 잉크테크 | Paste composition for outer electrode of inductor |
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CN114628082A (en) * | 2022-03-23 | 2022-06-14 | 广东南海启明光大科技有限公司 | Environment-aging-resistant conductive silver paste and preparation method thereof |
CN114628082B (en) * | 2022-03-23 | 2023-09-05 | 广东南海启明光大科技有限公司 | Environment-aging-resistant conductive silver paste and preparation method thereof |
CN114974651A (en) * | 2022-05-12 | 2022-08-30 | 北京梦之墨科技有限公司 | Epoxy resin-based conductive slurry and preparation method and application thereof |
CN116386929A (en) * | 2023-04-20 | 2023-07-04 | 深圳市信维通信股份有限公司 | Graphene composite conductive silver paste, preparation method and application thereof |
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