CN111341484A - Low-temperature curing type conductive silver paste and preparation method thereof - Google Patents
Low-temperature curing type conductive silver paste and preparation method thereof Download PDFInfo
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- CN111341484A CN111341484A CN202010234774.6A CN202010234774A CN111341484A CN 111341484 A CN111341484 A CN 111341484A CN 202010234774 A CN202010234774 A CN 202010234774A CN 111341484 A CN111341484 A CN 111341484A
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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
Abstract
The invention discloses a low-temperature curing type conductive silver paste and a preparation method thereof, and the low-temperature curing type conductive silver paste comprises a binary structure silver paste formed by emulsifying a component A and a component B, wherein the component A specifically comprises silver powder A, thermosetting resin A, a curing agent A and a solvent A, the component B specifically comprises silver powder B and a solvent B, the solvent A and the solvent B are two immiscible solvents, and the component A and the component B are emulsified to form the binary structure silver paste A-B; the conductive silver paste provided by the invention can be attached to the surfaces of different materials such as glass, aluminum plates, silicon wafers and polyester through screen printing, has the characteristics of good conductivity and strong adhesive force after being cured at the temperature of 80-250 ℃, and can be directly welded without surface treatment.
Description
Technical Field
The invention relates to the technical field of conductive paste, in particular to low-temperature curing type conductive silver paste and a preparation method thereof.
Background
The conductive silver paste is a paste functional material integrating multiple technologies such as metallurgy, chemical engineering, electronics and the like, is widely applied to electronic industries such as film switch circuits, printed circuit boards and the like and solar photovoltaic industries at present, has higher and higher requirements on the conductive silver paste serving as a key material along with the increasing development of electronic information technology, and has more and more requirements on the weldability of the conductive paste while meeting the conductivity, mechanical properties and printing properties.
In order to achieve electrical connection with other components, the conductive paste is usually subjected to surface treatment after curing/sintering, and is soldered to a solder wire or other substrate by electroless plating (nickel plating, etc.). However, the waste liquid generated in the electroless plating process causes great environmental pollution, and thus the solderability of the conductive paste itself is particularly important. At present, the research on the weldability of the paste mainly focuses on the selection of silver powder and resin, and because the welding temperature is generally 200-300 ℃, the resin is melted in the welding process, the adhesion of the solder wire to silver particles is reduced, and the welding effect is poor. Patent CN109887639A proposes a weldable low-temperature curable functional paste and a preparation method thereof, which improves the heat resistance of the resin by modifying polymethyl methacrylate resin, thereby being able to withstand the temperature impact generated during the welding process. However, the modification treatment of organic resin involves monomer copolymerization, the process is complicated and not easy to control, and a simpler and more effective method needs to be found to meet the weldability requirement of the slurry.
Disclosure of Invention
The invention aims to provide a low-temperature curing type conductive silver paste and a preparation method thereof, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a low-temperature curing type conductive silver paste comprises a binary structure silver paste formed by emulsifying a component A and a component B, wherein the component A comprises silver powder A, thermosetting resin A, a curing agent A and a solvent A, the component B comprises silver powder B and a solvent B, the solvent A and the solvent B are two immiscible solvents, and the component A and the component B are emulsified to form the A-B binary structure silver paste;
the silver paste comprises the following components in percentage by mass: 59.9-94.9 wt% of component A, 5-40 wt% of component B and 0.01-15 wt% of emulsifier.
Further, the component A comprises silver powder A, thermosetting resin A, a curing agent A and a solvent A, wherein the silver powder A accounts for 50-95 wt% (mass percent A/A is 100%), the thermosetting resin A accounts for 2-30 wt%, the curing agent A accounts for 0.1-25 wt%, and the solvent A accounts for 0-48 wt%;
the component B comprises silver powder B and a solvent B, wherein the silver powder B accounts for 50-98 wt% (mass percent B/B is 100%) and the solvent B accounts for 2-50 wt%.
Further, the emulsifier comprises one or more of polyoxyethylene ether, polyoxypropylene ether, carboxylate, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and sodium stearate.
Because the invention designs the silver paste with the A-B binary structure, the component A and the solvent B in the component B are two incompatible solvents, and the solvent B is water or a water/alcohol mixed solvent, and the solvent A is one or more of ethyl acetate, dimethyl succinate, dimethyl glutarate, dimethyl adipate, diethylene glycol butyl ether acetate and diethylene glycol ethyl ether acetate, which is preferable from the viewpoint of environmental protection.
In order to improve the conductivity, the silver powder A and the silver powder B are both one or more of flaky, spherical and sphere-like silver powders, and the silver powders with different shapes and sizes are combined to form a more compact stacking structure, so that the conductivity is improved.
Further, the silver powder A and the silver powder B have the size of nanometer or micron, and according to the summary of experiments of the technical personnel of the invention, the flake silver powder preferably has the maximum flake diameter less than or equal to 15 microns and the tap density of 2.5-6.0g/cm3The tap density of the spherical silver powder is 3-5.8g/cm3(ii) a It should be noted that, because the surface of the silver powder is coated with a layer of organic substance, the affinity of different silver powders to the solvent is different, and because the different solvents in the component a and the component B are different, the choice of the silver powder a and the silver powder B is also different, and will not be described here.
Further, the thermosetting resin A is one of epoxy resin, phenolic resin, acrylic resin, urea resin, melamine-formaldehyde resin, polyurethane and polyimide; preferably, in consideration of the advantages of easy curing of epoxy resin, good heat resistance, strong adhesion to aluminum, stainless steel, glass, silicon wafers and various flexible materials, etc., epoxy resin with strong heat resistance is preferably taken as the thermosetting base resin; correspondingly, the curing agent A is one or more of aliphatic amine, aromatic amine, polyamide, acid anhydride or other curing agents containing active hydrogen.
A preparation method of low-temperature curing type conductive silver paste comprises the following steps:
1) adding the components in the component A into a high-speed dispersion machine according to the proportion, mixing for 20min, and controlling the temperature to be less than or equal to 60 ℃ in the stirring process;
2) adding two components of the component B into a high-speed dispersion machine according to the proportion, and mixing for 20 min;
3) mixing the component A, the component B and the emulsifier, and fully stirring in a high-speed dispersion machine for 20-60 min;
4) and finally grinding for 2-20 times by a three-roll grinder to obtain uniform and stable slurry.
Compared with the prior art, the invention has the beneficial effects that:
the component A has the characteristic of good adhesive force after curing/sintering due to the fact that the component A contains the thermosetting resin in a certain proportion, and the solvent in the component B continuously volatilizes in the temperature rising process, so that only the silver powder is finally left. The silver has good wettability to the solder material and excellent welding performance. Therefore, the A-B binary structure silver paste provided by the invention has the characteristic of good wettability to a solder material after being cured, and simultaneously retains the advantages of good conductivity and strong adhesive force, and is not easy to fall off from the surface of a matrix.
The conductive silver paste provided by the invention can be attached to the surfaces of different materials such as glass, aluminum plates, silicon wafers and polyester through screen printing, has the characteristics of good conductivity and strong adhesive force after being cured at the temperature of 80-250 ℃, and can be directly welded without surface treatment.
Drawings
Fig. 1 is a schematic view of a low-temperature curing type conductive silver paste.
Detailed Description
The technical solution of the present patent will be described in further detail with reference to the following embodiments.
The embodiment I is a low-temperature curing type conductive silver paste, which comprises the following components in percentage by mass:
the component A comprises: flake silver powder A, D50 ═ 4 μm, tap density ═ 5g/cm3Mass percent (tablet)Silver powder a/a component 100%) was 70 wt%; 10 wt% of epoxy resin E51; 593 curing agent 2 wt%; diethylene glycol butyl ether acetate 18 wt%;
and B component: spherical silver powder B, D50 ═ 3 μm, mass percent (spherical silver powder B/B component × 100%) was 95 wt%; 5 wt% of water;
emulsifier: sodium dodecylbenzenesulfonate.
A preparation method of low-temperature curing type conductive silver paste comprises the steps of stirring a component A and a component B uniformly (20min) in a high-speed dispersion machine in advance, then taking 76 wt% of the component A, 20 wt% of the component B and 4 wt% of an emulsifier, dispersing for 20-60min in the high-speed dispersion machine, and grinding for 5 times by a three-roll grinding machine;
the obtained silver paste is printed on the surface of glass to prepare a 2 x 5cm strip sample, and the sintering condition is 80 ℃ for 4 hours. The manual soldering test was carried out with an electric iron, and it was found that 60% Pb 40% Sn solder wire adheres relatively firmly to the surface of the sample with a shear force of 2N.
Embodiment 2, a low-temperature curing conductive silver paste, which comprises the following components in percentage by mass:
the component A comprises: flake silver powder A, D50 ═ 4 μm, tap density ═ 5g/cm3The mass percentage (flake silver powder A/A component x 100%) is 70 wt%; 8 wt% of epoxy resin; 1 wt% of Diethylenetriamine (DETA); 21 wt% of diethylene glycol butyl ether acetate;
and B component: flake silver powder B, D50 ═ 4 μm, and the mass percentage (flake silver powder B/B component × 100%) was 93 wt%; 7 wt% of water;
emulsifier: tween-80.
A preparation method of low-temperature curing type conductive silver paste comprises the steps of stirring a component A and a component B uniformly (20min) in a high-speed dispersion machine in advance, then taking 85 wt% of the component A, 10 wt% of the component B and 5 wt% of an emulsifier, dispersing for 60min in the high-speed dispersion machine, and grinding for 10 times by a three-roll grinder;
the obtained silver paste is printed on the surface of an aluminum plate to prepare a 2 x 5cm strip sample, the sample is cured in an oven (120 ℃ for 15min), a manual soldering test is carried out by using an electric iron, and through the test, a 60% Pb 40% Sn soldering wire can be firmly attached to the surface of the sample, and the shearing force is 3N.
Embodiment 3, a low-temperature curing conductive silver paste, which comprises the following components in percentage by mass:
the component A comprises: flake silver powder A, D50 ═ 4 μm, tap density ═ 5g/cm3The mass percentage (flake silver powder A/A component 100%) is 75 wt%; 8 wt% of epoxy resin; 1.2 wt% of diaminodiphenyl sulfone; diethylene glycol monobutyl ether acetate 15.8 wt%.
And B component: the nano silver powder B has the maximum particle size of below 100nm and the mass percentage (nano silver powder B/B component x 100%) of 96 wt%; 4 wt% of water;
emulsifier: sodium dodecylbenzenesulfonate.
A preparation method of low-temperature curing type conductive silver paste comprises the steps of stirring an A component and a B component uniformly (20min) in a high-speed dispersion machine in advance, then taking 79 wt% of the A component, 20 wt% of the B component and 1 wt% of an emulsifier, dispersing for 40min in the high-speed dispersion machine, and grinding for 10 times by a three-roll grinder;
printing the obtained silver paste on the surface of glass to prepare a 2 x 5cm strip sample, and sintering at 200 ℃ for 30 min; the manual soldering test was carried out with an electric iron, and it was found that 60% Pb 40% Sn solder wire adheres relatively firmly to the surface of the sample with a shear force of 2.5N.
The method is novel in concept, the wettability of the welding material and the conducting layer is greatly improved due to the existence of the component B in the formed binary-structure conducting layer, the method is simple, the practicability is high, and the requirement on the weldability can be met while the mechanical property and the electrical property of the conductive silver paste are ensured.
Although the preferred embodiments of the present patent have been described in detail, the present patent is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present patent within the knowledge of those skilled in the art.
Claims (10)
1. The low-temperature curing type conductive silver paste is characterized by comprising a binary structure silver paste formed by emulsifying a component A and a component B, wherein the component A comprises silver powder A, thermosetting resin A, a curing agent A and a solvent A, the component B comprises silver powder B and a solvent B, and the solvent A and the solvent B are two immiscible solvents; the silver paste comprises the following components in percentage by mass: 59.9-94.9 wt% of component A, 5-40 wt% of component B and 0.01-15 wt% of emulsifier.
2. The low-temperature curing type conductive silver paste according to claim 1, wherein the component A comprises 50-95 wt% of silver powder A, 2-30 wt% of thermosetting resin A, 0.1-25 wt% of curing agent A and 0-48 wt% of solvent A;
the component B comprises silver powder B and a solvent B, wherein the silver powder B accounts for 50-98 wt%, and the solvent B accounts for 2-50 wt%.
3. The low-temperature curing type conductive silver paste according to claim 1, wherein the emulsifier comprises one or more of polyoxyethylene ether, polyoxypropylene ether, carboxylate, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and sodium stearate.
4. The low-temperature curing type conductive silver paste according to claim 1, wherein the solvent B is water or a water/alcohol mixed solvent, and the solvent A is one or more of ethyl acetate, dimethyl succinate, dimethyl glutarate, dimethyl adipate, diethylene glycol butyl ether acetate and diethylene glycol ethyl ether acetate.
5. The low-temperature curing conductive silver paste according to claim 1, wherein the silver powder A and the silver powder B are both composed of one or more of flake-like, spherical and sphere-like silver powders; the silver powder A and the silver powder B are nano-sized or micro-sized, preferably, the maximum plate diameter of the flaky silver powder is less than or equal to 15 micrometers, and the tap density is 2.5-6.0g/cm3The tap density of the spherical silver powder is 3-5.8g/cm3。
6. The low-temperature curing type conductive silver paste according to claim 1, wherein the thermosetting resin A is one of epoxy resin, phenolic resin, acrylic resin, urea resin, melamine-formaldehyde resin, polyurethane and polyimide; preferably, in consideration of the advantages of easy curing of epoxy resin, good heat resistance, strong adhesion to aluminum, stainless steel, glass, silicon wafers and various flexible materials, etc., epoxy resin with strong heat resistance is preferably taken as the thermosetting base resin; correspondingly, the curing agent A is one or more of aliphatic amine, aromatic amine, polyamide, acid anhydride or other curing agents containing active hydrogen.
7. The low-temperature curing type conductive silver paste according to claims 1-6, wherein the low-temperature curing type conductive silver paste consists of the following components: 76 wt% of component A, 20 wt% of component B and 4 wt% of emulsifier;
specifically, the component A: flake silver powder A, D50 is 4 μm, tap density is 5g/cm3, and mass percent (flake silver powder A/A component 100%) is 70 wt%; 10 wt% of epoxy resin E51; 593 curing agent 2 wt%; diethylene glycol butyl ether acetate 18 wt%;
and B component: spherical silver powder B, D50 ═ 3 μm, mass percent (spherical silver powder B/B component × 100%) was 95 wt%; 5 wt% of water;
emulsifier: sodium dodecylbenzenesulfonate.
8. The low-temperature curing type conductive silver paste according to claims 1-6, wherein the low-temperature curing type conductive silver paste consists of the following components: 85 wt% of component A, 10 wt% of component B and 5 wt% of emulsifier;
specifically, the component A: flake silver powder A, D50 is 4 μm, tap density is 5g/cm3, and mass percent (flake silver powder A/A component 100%) is 70 wt%; 8 wt% of epoxy resin; 1 wt% of Diethylenetriamine (DETA); 21 wt% of diethylene glycol butyl ether acetate;
and B component: flake silver powder B, D50 ═ 4 μm, and the mass percentage (flake silver powder B/B component × 100%) was 93 wt%; 7 wt% of water;
emulsifier: tween-80.
9. The low-temperature curing type conductive silver paste according to claims 1-6, wherein the low-temperature curing type conductive silver paste consists of the following components: 79 wt% of component A, 20 wt% of component B and 1 wt% of emulsifier;
specifically, the component A: the flake silver powder A, D50 is 4 μm, the tap density is 5g/cm3, and the mass percentage (flake silver powder A/A component 100%) is 75 wt%; 8 wt% of epoxy resin; 1.2 wt% of diaminodiphenyl sulfone; diethylene glycol butyl ether acetate 15.8 wt%;
and B component: the nano silver powder B has the maximum particle size of below 100nm and the mass percentage (nano silver powder B/B component x 100%) of 96 wt%; 4 wt% of water;
emulsifier: sodium dodecylbenzenesulfonate.
10. The preparation method of the low-temperature curing type conductive silver paste is characterized by comprising the following steps of:
1) adding the components in the component A into a high-speed dispersion machine according to the proportion, mixing for 20min, and controlling the temperature to be less than or equal to 60 ℃ in the stirring process;
2) adding two components of the component B into a high-speed dispersion machine according to the proportion, and mixing for 20 min;
3) mixing the component A, the component B and the emulsifier, and fully stirring in a high-speed dispersion machine for 20-60 min;
4) and finally grinding for 2-20 times by a three-roll grinder to obtain uniform and stable slurry.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112750552A (en) * | 2020-12-25 | 2021-05-04 | 邯郸学院 | Sintered silver paste and preparation method thereof |
| CN113555145A (en) * | 2021-09-23 | 2021-10-26 | 西安宏星电子浆料科技股份有限公司 | Flexible high-temperature-resistant conductive paste |
| CN114023490A (en) * | 2021-11-03 | 2022-02-08 | 苏州晶银新材料科技有限公司 | Low-temperature conductive silver paste and heterojunction battery |
| CN115188520A (en) * | 2022-07-05 | 2022-10-14 | 大连海外华昇电子科技有限公司 | High-reliability low-temperature curing silver paste for ferrite and preparation method thereof |
| CN114023490B (en) * | 2021-11-03 | 2024-05-03 | 苏州晶银新材料科技有限公司 | Low-temperature conductive silver paste and heterojunction battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112750552A (en) * | 2020-12-25 | 2021-05-04 | 邯郸学院 | Sintered silver paste and preparation method thereof |
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Application publication date: 20200626 |