CN115482953A - Flexible silver paste and preparation method thereof - Google Patents
Flexible silver paste and preparation method thereof Download PDFInfo
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- CN115482953A CN115482953A CN202211157710.6A CN202211157710A CN115482953A CN 115482953 A CN115482953 A CN 115482953A CN 202211157710 A CN202211157710 A CN 202211157710A CN 115482953 A CN115482953 A CN 115482953A
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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 relates to a flexible silver paste and a preparation method thereof, and belongs to the technical field of silver pastes. The flexible silver paste comprises the following components in parts by mass: 50-70 parts of conductive powder, 10-20 parts of organic silicon-based adhesive, 1.5-3.5 parts of toughening agent, 1-3.5 parts of curing crosslinking agent, 1-2.5 parts of tackifier, 0.05-0.2 part of platinum catalyst, 0.01-0.06 part of inhibitor and 10-30 parts of solvent; the organic silicon-based adhesive is prepared from vinyl MQ silicon resin and vinyl-terminated polydimethylsiloxane according to the mass ratio of 12-17:3-8, mixing; the toughening agent is prepared from a fiber powder toughening agent and a spherical toughening agent according to the mass ratio of 2-5:2-3, mixing; the fineness of the fiber powder toughening agent is 1500-5000 meshes; the spherical toughening agent has a core-shell structure. The flexible silver paste has excellent temperature impact resistance, flexibility, strong stability, good conductivity and high adhesion.
Description
Technical Field
The invention belongs to the technical field of silver paste, and particularly relates to flexible silver paste and a preparation method thereof.
Background
The conductive silver paste is a functional paste using silver powder as a conductive filler, and conductive lines are generally formed by using screen printing, gravure printing, relief printing and other process manners. Through decades of technical development, conductive silver paste can be divided into two categories: high-temperature silver paste taking glass powder as a binding phase and sintered at a temperature of more than 500 ℃ to form a film, and low-temperature silver paste taking polymer resin as a binding phase and solidified at a temperature of less than 200 ℃ to form a film. The conductive silver paste has a huge amount in various fields such as film switches, touch screens, capacitance inductors, electric heating components, flexible circuits and the like, and is one of basic materials of the electronic industry at present.
The conductive silver paste has the advantages of low resistance, high stability, flexible use process and the like, but along with the technical development and the emergence of new product requirements, the performance requirements of the conductive silver paste are gradually improved. Specifically, for example, electrical heating is a technology of directly or indirectly converting electric energy into heat energy to heat an object by using the joule effect of current, and an electrical heating component is widely used in the fields of pipeline freezing prevention, railway track deicing, wind power blade deicing, new energy battery component heat preservation and the like besides common house electrical heating. In alpine regions, the electric heating assembly is required to bear cold and hot impact from-40 ℃ to rated working temperature from start to stable operation, and the conductive silver paste is usually used as an electrode material in the electric heating assembly, so that the temperature impact resistance of the conductive silver paste has a key influence on the operation reliability of the electric heating assembly.
However, the conventional conductive silver paste is not designed for use in a severe temperature environment. Under the impact of extreme temperature alternation, the silver paste film layer generates internal stress due to repeated expansion and contraction, so that an electrode circuit is cracked and the adhesive force with a base material cannot be ensured, and the resistance is increased or even broken; when curved surfaces such as pipelines are installed, the required materials have certain flexibility, but the bending stress aggravates the generation and the expansion of cracks of the silver paste film layer, and the risk of overall failure is brought. Therefore, how to develop a conductive silver paste with temperature shock resistance and flexibility characteristics, which still maintains excellent reliability under severe environment, is a problem to be solved in the technical field of paste.
Disclosure of Invention
Therefore, the invention aims to solve the technical problems of poor temperature impact resistance, poor flexibility and the like of the silver paste in the prior art.
In order to solve the technical problems, the invention provides a flexible silver paste and a preparation method thereof. The flexible silver paste has excellent temperature impact resistance, flexibility, strong stability, good conductivity, high adhesive force and stable preparation process.
The first purpose of the invention is to provide a flexible silver paste, which comprises the following components in parts by mass: 50-70 parts of conductive powder, 10-20 parts of organic silicone-based adhesive, 1.5-3.5 parts of toughening agent, 1-3.5 parts of curing crosslinking agent, 1-2.5 parts of tackifier, 0.05-0.2 part of platinum catalyst, 0.01-0.06 part of inhibitor and 10-30 parts of solvent;
the organic silicon-based adhesive is prepared from vinyl MQ silicon resin and vinyl-terminated polydimethylsiloxane according to the mass ratio of 12-17:3-8, mixing;
the toughening agent is prepared from a fiber powder toughening agent and a spherical toughening agent according to the mass ratio of 2-5:2-3, mixing; the fineness of the fiber powder toughening agent is 1500-5000 meshes; the spherical toughening agent has a core-shell structure.
In one embodiment of the present invention, the fiber powder toughening agent is glass fiber powder and/or carbon fiber powder; the spherical toughening agent is one or more of GENIOPERL P52, KANE ACE M-711, KANE ACE M-732, METABLEN S-2001, METABLEN S-2030, METABLEN S-2501, LG Chem EM500 and LG Chem MB 872.
In one embodiment of the invention, the vinyl MQ silicone resin has a viscosity of 3000 to 10000cP and a vinyl content of 0.8 to 1.8wt%.
Further, the viscosity of the vinyl MQ silicon resin is 4000-8000cP, and the vinyl content is 1.0-1.5wt%.
In one embodiment of the invention, the vinyl terminated polydimethylsiloxane has a viscosity of 300 to 6000cP and a vinyl content of 0.1 to 0.7wt%.
Further, the viscosity of the vinyl-terminated polydimethylsiloxane is 500-3000cP, and the vinyl content is 0.15-0.5wt%.
In one embodiment of the present invention, the vinyl MQ silicone resin and the vinyl terminated polydimethylsiloxane are both colorless transparent liquids. The invention uses the vinyl MQ silicon resin with moderate vinyl content and the vinyl-terminated polydimethylsiloxane as the organic silicon-based adhesive. The vinyl is used as a curing crosslinking site, and if the content is too high, the cured product is hard and brittle; if the content is too low, the crosslinking density of the organic silicon-based adhesive is difficult to ensure, so that the cured organic silicon-based adhesive has low mechanical strength and is easy to tear.
In an embodiment of the present invention, the conductive powder is micron-sized plate-shaped silver powder and/or micron-sized spherical silver powder.
In one embodiment of the invention, the particle size of the conductive powder is 1.0-10.0 μm, and the tap density is 1.5-5.0g/cm 3 。
Furthermore, the particle diameter of the conductive powder is 1.0-2.5 μm, and the tap density is 2.5-4.0g/cm 3 . If silver powder with larger particle size and low tap density is used, the organic silicon-based adhesive is difficult to fully coat the silver powder, and the stability and mechanical strength of the silver paste are poor due to poor binding force among components; and the silver powder with smaller particle size and high tap density is used, so that the filling property of the silver powder in the organic silicon-based adhesive is insufficient, and the conductivity of the silver paste is rapidly reduced.
In one embodiment of the invention, the curing crosslinking agent is hydrogen-containing silicone oil, and the hydrogen content is 0.1-1.2wt%.
Further, the curing crosslinking agent is methyl-terminated side chain hydrogen-containing silicone oil, and the hydrogen content is 0.2-0.8wt%.
In one embodiment of the invention, the tackifier is obtained by mixing a silane coupling agent, a titanate coupling agent and acetylacetone salt; the mass ratio of the silane coupling agent to the titanate coupling agent to the acetylacetone salt is 12-15:3-6:1-3.
In one embodiment of the present invention, the silane coupling agent is one or more of gamma-glycidoxypropyltrimethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, and vinyltris (beta-methoxyethoxy) silane.
In one embodiment of the invention, the titanate coupling agent is one or more of isopropoxytrioleate acyloxy titanate, isopropylbis (methacryloyl) isostearoyl titanate, isopropyltris (dioctylpyrophosphate) titanate and bis (dioctylpyrophosphate) ethylene titanate.
In one embodiment of the invention, the acetylacetonate is one or more of aluminum acetylacetonate, zinc acetylacetonate, magnesium acetylacetonate, calcium acetylacetonate, and nickel acetylacetonate.
In one embodiment of the invention, the platinum content of the platinum catalyst is from 500 to 2000ppm.
In one embodiment of the invention, the inhibitor is one or more of 1-ethynylcyclohexanol, 2-methyl-3-butyn-2-ol, 3, 5-dimethyl-1-hexyn-3-ol, and 3,7, 11-trimethyldodecyn-3-ol.
In one embodiment of the invention, the solvent is one or more of n-octane, n-nonane, n-decane, n-undecane, n-dodecane, mineral spirits No. 200, D40 mineral spirits, and D60 mineral spirits.
The second purpose of the invention is to provide a preparation method of the flexible silver paste, which comprises the following steps,
(1) Uniformly stirring the organic silicon-based adhesive, the curing cross-linking agent, the solvent and the toughening agent to obtain an organic carrier, wherein the stirring temperature is 50-80 ℃; the stirring speed is 300rpm-1000rpm; the stirring time is 4-8 h;
(2) Uniformly dispersing the organic carrier, the tackifier, the platinum catalyst and the inhibitor in the step (1) to obtain a silver paste matrix; the rotating speed of the dispersion is 800rpm-2000rpm, and the dispersion time is 1h-2h;
(3) Adding conductive powder into the silver paste matrix in the step (2) for uniform dispersion to obtain a silver paste pre-dispersion body; the rotating speed of the dispersion is 800rpm-2000rpm, and the dispersion time is 1h-2h;
(4) Grinding the silver paste pre-dispersion body obtained in the step (3) to obtain the flexible silver paste; the fineness of the grinding is less than 10 mu m.
Compared with the prior art, the technical scheme of the invention has the following advantages:
(1) The flexible silver paste takes the organic silicon-based adhesive with good flexibility and weather resistance as a binding phase, and the toughening agent is a combination of a fiber powder toughening agent and a spherical toughening agent with a core-shell structure. The fiber powder toughening agent is dispersed in the silver paste film layer and can keep the size of the silver paste film layer stable under temperature impact as a supporting framework; the spherical toughening agent with the core-shell structure is used as a nail anchor, so that the energy of the tip of a crack can be effectively absorbed, the growth of a micro crack caused by temperature impact and stress action is relieved, and the macroscopic damage of the silver paste film layer is further prevented. The silver paste has the characteristic of flexibility, and meanwhile, a point-line structure with a synergistic effect is built through the combination of the toughening agents, so that the extreme temperature impact resistance is obtained, and the reliability under a severe environment is greatly improved.
(2) The flexible silver paste disclosed by the invention uses the compound tackifier, and the coupling agent component in the flexible silver paste can ensure the wetting of the relative adhesion toughening agent and the conductive powder, so that the interface performance is improved; the acetylacetone salt has the reaction characteristic with active groups in a base material, a binding phase and a filler, and is mutually crosslinked to form stable chemical bonding. The synergistic effect of the components in the compound tackifier improves the cohesiveness and the adhesive force of the silver paste system when the bonding phase ratio is low and the filler proportion is high, further improves the use reliability of the silver paste in an extreme environment, and ensures the uniform and stable dispersion of the components of the silver paste through a multi-step mixing process.
Detailed Description
The present invention is further described below with reference to specific examples so that those skilled in the art can better understand the present invention and can practice the present invention, but the examples are not intended to limit the present invention.
Example 1
A flexible silver paste and a preparation method thereof comprise the following steps:
(1) 80g of liquid vinyl MQ silicon resin (viscosity 7000cP, vinyl content 1.4 wt%), 40g of vinyl-terminated polydimethylsiloxane (viscosity 1000cP, vinyl content 0.3 wt%), 15g of methyl-terminated side chain hydrogen-containing silicone oil (hydrogen content 0.35 wt%), 223g of n-undecane, 10g of glass fiber powder (fineness 2000 mesh) and 10g of GENIOPERL P52 are weighed, stirred and dispersed to be in a uniform state at 60 ℃, and the stirring speed is 600rpm for 5 hours to form the organic carrier.
(2) Weighing 14g of gamma- (methacryloyloxy) propyl trimethoxy silane, 4g of isopropoxy triolein acyloxy titanate and 2g of aluminum acetylacetonate, uniformly mixing in a high-speed dispersion machine, and dispersing at the rotating speed of 600rpm for 50min to obtain the tackifier.
(3) And (3) uniformly mixing the organic carrier prepared in the step (1), the tackifier prepared in the step (2), 1.5g of platinum catalyst (with platinum content of 1000 ppm) and 0.5g of 2-methyl-3-butyn-2-ol in a planetary vacuum dispersion machine, wherein the dispersion speed is 1200rpm, and the dispersion time is 1.5 hours, so as to form a silver paste matrix.
(4) 400g of micron-sized flake silver powder (the particle diameter is 3.0-5.0 mu m, and the tap density is 2.6 g/cm) 3 ) Mixing with 200g micron-sized spherical silver powder (particle diameter of 1.0-1.5 μm, tap density of 3.7 g/cm) 3 ) And (4) adding the silver paste into the silver paste matrix prepared in the step (3), uniformly mixing in a planetary vacuum dispersion machine, and forming a silver paste pre-dispersion body at the dispersion rotating speed of 1600rpm for 1.5 h.
(5) And (4) grinding the silver paste pre-dispersion prepared in the step (4) in a three-roll grinder until the fineness is less than 10 mu m to obtain the temperature impact resistant flexible silver paste.
Example 2
A flexible silver paste and a preparation method thereof specifically comprise the following steps:
(1) 100g of liquid vinyl MQ silicon resin (viscosity 7000cP, vinyl content 1.4 wt%), 50g of vinyl terminated polydimethylsiloxane (viscosity 1000cP, vinyl content 0.3 wt%), 20g of methyl terminated side chain hydrogen-containing silicone oil (hydrogen content 0.35 wt%), 85g of n-decane, 43g of No. 200 solvent oil, 20g of glass fiber powder (fineness is 3000 meshes) and 10g of KANE ACE M-732 are weighed, stirred and dispersed to be in a uniform state at 60 ℃, and the stirring speed is 600rpm for 5 hours to form the organic carrier.
(2) Weighing 14.5g of gamma-glycidoxypropyltrimethoxysilane, 4g of isopropoxy trioleate acyloxy titanate and 1.5g of magnesium acetylacetonate, and uniformly mixing in a high-speed dispersion machine at the dispersion rotation speed of 600rpm for 50min to obtain the tackifier.
(3) And (3) uniformly mixing the organic carrier prepared in the step (1), the tackifier prepared in the step (2), 1.5g of platinum catalyst (with platinum content of 1000 ppm) and 0.5g of 2-methyl-3-butyn-2-ol in a planetary vacuum dispersion machine, wherein the dispersion speed is 1200rpm, and the dispersion time is 1.5 hours, so as to form a silver paste matrix.
(4) 350g of micron-sized flaky silver powder (the particle diameter is 3.0-5.0 mu m, and the tap density is 2.6 g/cm) 3 ) Mixing with 300g micron-sized spherical silver powder (particle diameter of 1.0-1.5 μm, tap density of 3.7 g/cm) 3 ) And (4) adding the silver paste into the silver paste matrix prepared in the step (3), uniformly mixing the silver paste matrix and the silver paste matrix in a planetary vacuum dispersion machine, and forming a silver paste pre-dispersion body at the dispersion rotating speed of 1600rpm for 1.5 h.
(5) And (4) grinding the silver paste pre-dispersion prepared in the step (4) in a three-roll grinder until the fineness is less than 10 mu m to obtain the temperature impact resistant flexible silver paste.
Example 3
A flexible silver paste and a preparation method thereof specifically comprise the following steps:
(1) Weighing 136g of liquid vinyl MQ silicon resin (with the viscosity of 5000cP and the vinyl content of 1.1 wt%), 34g of vinyl-terminated polydimethylsiloxane (with the viscosity of 2000cP and the vinyl content of 0.2 wt%), 15g of methyl-terminated side chain hydrogen-containing silicone oil (with the hydrogen content of 0.5 wt%), 217.5g of D40 solvent oil, 18g of carbon fiber powder (with the fineness of 2500 meshes) and 12g of METABLEN S-2030, stirring and dispersing at 70 ℃ until the carbon fiber powder is in a uniform state, and stirring at the rotation speed of 800rpm for 6 hours to form the organic carrier.
(2) Weighing 10g of vinyl tri (beta-methoxyethoxy) silane, 3g of isopropyl tri (dioctyl pyrophosphoryl oxy) titanate and 2g of zinc acetylacetonate, and uniformly mixing in a high-speed dispersion machine at the dispersion rotation speed of 600rpm for 40min to prepare the tackifier.
(3) And (2) uniformly mixing the organic carrier prepared in the step (1), the tackifier prepared in the step (2), 2g of platinum catalyst (platinum content is 1000 ppm) and 0.5g of 3, 5-dimethyl-1-hexyne-3-alcohol in a planetary vacuum dispersion machine, wherein the dispersion speed is 1200rpm, and the dispersion time is 1.5h to form a silver paste matrix.
(4) 550g of micron-sized flake silver powder (the particle diameter is 8.0-10.0 mu m, and the tap density is 1.7 g/cm) 3 ) And (4) adding the silver paste into the silver paste matrix prepared in the step (3), uniformly mixing in a planetary vacuum dispersion machine, and forming a silver paste pre-dispersion body with the dispersion rotation speed of 1200rpm and the time of 1.5 h.
(5) And (4) grinding the silver paste pre-dispersion prepared in the step (4) in a three-roll grinder until the fineness is less than 10 mu m to obtain the temperature impact resistant flexible silver paste.
Example 4
A flexible silver paste and a preparation method thereof specifically comprise the following steps:
(1) 136g of liquid vinyl MQ silicon resin (with the viscosity of 5000cP and the vinyl content of 1.1 wt%), 34g of vinyl-terminated polydimethylsiloxane (with the viscosity of 2000cP and the vinyl content of 0.2 wt%), 15g of methyl-terminated side chain hydrogen-containing silicone oil (with the hydrogen content of 0.5 wt%), 192.5g of D60 solvent oil, 8g of glass fiber powder (with the fineness of 3000 meshes), 8g of carbon fiber powder (with the fineness of 2500 meshes) and 9g of LG Chem MB872 are weighed, stirred and dispersed to be in a uniform state at 70 ℃, the stirring speed is 800rpm, and the stirring time is 6 hours, so that the organic carrier is formed.
(2) Weighing 11g of vinyl tri (beta-methoxyethoxy) silane, 2.5g of bis (dioctyl pyrophosphato acyloxy) ethylene titanate and 1.5g of nickel acetylacetonate, and uniformly mixing in a high-speed dispersion machine at the dispersion rotation speed of 600rpm for 40min to prepare the tackifier.
(3) And (2) uniformly mixing the organic carrier prepared in the step (1), the tackifier prepared in the step (2), 2g of platinum catalyst (platinum content is 1000 ppm) and 0.5g of 3,7, 11-trimethyldodecyne-3-ol in a planetary vacuum dispersion machine, wherein the dispersion speed is 1200rpm, and the dispersion time is 1.5 hours, so as to form a silver paste matrix.
(4) 460g of micron-sized flake silver powder (the particle diameter is 5.0-8.0 mu m, and the tap density is 2.1 g/cm) 3 ) And 120g of micron-sized spherical silver powder (the particle diameter is 1.5-2.0 mu m, and the tap density is 2.9 g/cm) 3 ) And (4) adding the silver paste into the silver paste matrix prepared in the step (3), uniformly mixing in a planetary vacuum dispersion machine, and forming a silver paste pre-dispersion body with the dispersion rotation speed of 1200rpm for 1.5 h.
(5) And (4) grinding the silver paste pre-dispersion prepared in the step (4) in a three-roll grinder until the fineness is less than 10 mu m to obtain the temperature impact resistant flexible silver paste.
Comparative example 1
The process is substantially the same as example 1 except that the toughening agents of glass fiber powder and GeNIOPERLP52 are not added, and the rest materials and the preparation steps are the same.
Comparative example 2
The process is substantially the same as example 1 except that no aluminum acetylacetonate is added to the tackifier, and the remaining materials and preparation steps are the same.
Comparative example 3
The process is substantially the same as example 2 except that no toughening agent glass fiber powder is added, and the rest materials and the preparation steps are the same.
Comparative example 4
The procedure is essentially the same as in example 2, except that the toughening agent KANE ACE M-732 is not added and the remaining materials and preparation steps are the same.
Test example
The temperature impact resistant flexible silver pastes prepared in examples 1 to 4 and comparative examples 1 to 4 were sampled, printed on a ceramic sheet using a 200 mesh screen having a thickness of 10 μm of a photosensitive resist, and baked and cured at 150 ℃ for 30min. After the silver paste is cured, a film thickness meter is used for testing the thickness of a film layer, a four-probe tester is used for testing the square resistance, and the adhesion is tested according to GB/T9286-2021 'test for drawing squares of colored paint and varnish'. After the temperature impact resistance test (from minus 50 ℃ to 300 ℃, temperature maintenance 30min,75 cycles) is finished, the change of the silver paste film layer is observed, the adhesive force and the resistance change rate are tested, and the test results are shown in table 1:
TABLE 1
The temperature impact resistant flexible silver pastes prepared in examples 1 to 4 and comparative examples 1 to 4 were sampled, respectively, printed on a PET film using a 200-mesh screen having a photoresist thickness of 10 μm, and cured by baking at 150 ℃ for 30min. After the silver paste is cured, a film thickness meter is used for testing the thickness of a film layer, a four-probe tester is used for testing the square resistance, and the adhesion is tested according to GB/T9286-2021 'test for drawing squares of colored paint and varnish'. After the bending resistance test (bending diameter 5mm, positive and negative bending 1 time is recorded as 1 cycle, 100 cycles) is finished, the change of the silver paste film layer is observed, the adhesive force and the resistance change rate are tested, and the test results are shown in table 2:
TABLE 2
As can be seen from tables 1-2, the flexible silver paste disclosed by the invention has good conductivity and adhesive force after being cured, achieves a synergistic toughening effect which a single type of toughening agent does not have through the combination of different types of toughening agents, and keeps good cohesiveness and adhesive force when the adhesive phase ratio of the silver paste is low and the filler ratio is high through the component design of the tackifier. After strict temperature impact and bending treatment, the resistance change rate is low, excellent stability and adhesion effect are kept, the application in the fields of electric heating assemblies, flexible circuits, electronic devices and the like under strict temperature conditions can be adapted, and the adaptability of the conductive silver paste to the service temperature environment is greatly expanded.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. This need not be, nor should it be exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the spirit or scope of the invention.
Claims (10)
1. The flexible silver paste is characterized by comprising the following components in parts by mass: 50-70 parts of conductive powder, 10-20 parts of organic silicon-based adhesive, 1.5-3.5 parts of toughening agent, 1-3.5 parts of curing crosslinking agent, 1-2.5 parts of tackifier, 0.05-0.2 part of platinum catalyst, 0.01-0.06 part of inhibitor and 10-30 parts of solvent;
the organic silicon-based adhesive is prepared from vinyl MQ silicon resin and vinyl-terminated polydimethylsiloxane according to the mass ratio of 12-17:3-8, mixing;
the toughening agent is prepared from a fiber powder toughening agent and a spherical toughening agent according to the mass ratio of 2-5:2-3, mixing; the fineness of the fiber powder toughening agent is 1500-5000 meshes; the spherical toughening agent has a core-shell structure.
2. The flexible silver paste of claim 1, wherein the fiber powder toughening agent is glass fiber powder and/or carbon fiber powder; the spherical toughening agent is one or more of GENIOPERL P52, KANE ACE M-711, KANE ACE M-732, METABLEN S-2001, METABLEN S-2030, METABLEN S-2501, LG Chem EM500 and LG Chem MB 872.
3. The flexible silver paste of claim 1, wherein the vinyl MQ silicone resin has a viscosity of 3000-10000cP and a vinyl content of 0.8-1.8wt%.
4. The flexible silver paste of claim 1, wherein the vinyl terminated polydimethylsiloxane has a viscosity of 300-6000cP and a vinyl content of 0.1-0.7wt%.
5. The flexible silver paste of claim 1, wherein the conductive powder is micron-sized flake silver powder and/or micron-sized spherical silver powder.
6. The flexible silver paste of claim 1, wherein the cured crosslinker is a hydrogen-containing silicone oil having a hydrogen content of 0.1-1.2wt%.
7. The flexible silver paste of claim 1, wherein the tackifier is obtained by mixing a silane coupling agent, a titanate coupling agent and acetylacetone salt; the mass ratio of the silane coupling agent to the titanate coupling agent to the acetylacetone salt is 12-15:3-6:1-3.
8. The flexible silver paste of claim 1, wherein the inhibitor is one or more of 1-ethynylcyclohexanol, 2-methyl-3-butyn-2-ol, 3, 5-dimethyl-1-hexyn-3-ol, and 3,7, 11-trimethyldodecyn-3-ol.
9. The flexible silver paste of claim 1, wherein the solvent is one or more of n-octane, n-nonane, n-decane, n-undecane, n-dodecane, mineral spirits No. 200, D40, and D60.
10. The method for preparing flexible silver paste according to any one of claims 1-9, comprising the steps of,
(1) Uniformly stirring the organic silicon-based adhesive, the curing cross-linking agent, the solvent and the toughening agent to obtain an organic carrier, wherein the stirring temperature is 50-80 ℃; the stirring speed is 300rpm-1000rpm; the stirring time is 4-8 h;
(2) Uniformly dispersing the organic carrier, the tackifier, the platinum catalyst and the inhibitor in the step (1) to obtain a silver paste matrix; the rotating speed of the dispersion is 800rpm-2000rpm, and the dispersion time is 1h-2h;
(3) Adding conductive powder into the silver paste matrix in the step (2) for uniform dispersion to obtain a silver paste pre-dispersion body; the rotating speed of the dispersion is 800rpm-2000rpm, and the dispersion time is 1h-2h;
(4) Grinding the silver paste pre-dispersion body in the step (3) to obtain the flexible silver paste; the fineness of the grinding is less than 10 mu m.
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| CN202211157710.6A CN115482953A (en) | 2022-09-22 | 2022-09-22 | Flexible silver paste and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115985553A (en) * | 2023-01-13 | 2023-04-18 | 上海怡上电子科技有限公司 | Halogen-free silver paste with high bending resistance and preparation method thereof |
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2022
- 2022-09-22 CN CN202211157710.6A patent/CN115482953A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115985553A (en) * | 2023-01-13 | 2023-04-18 | 上海怡上电子科技有限公司 | Halogen-free silver paste with high bending resistance and preparation method thereof |
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