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
- Publication number
- 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
- Authority
- CN
- China
- Prior art keywords
- component
- silver powder
- silver paste
- low
- solvent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 238000013035 low temperature curing Methods 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 31
- 229910052709 silver Inorganic materials 0.000 claims abstract description 18
- 239000004332 silver Substances 0.000 claims abstract description 18
- 238000001723 curing Methods 0.000 claims abstract description 16
- 229920005989 resin Polymers 0.000 claims abstract description 16
- 239000011347 resin Substances 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 229920001187 thermosetting polymer Polymers 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 9
- 239000011521 glass Substances 0.000 claims abstract description 6
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 4
- 239000010703 silicon Substances 0.000 claims abstract description 4
- 235000012431 wafers Nutrition 0.000 claims abstract description 4
- 230000001804 emulsifying effect Effects 0.000 claims abstract description 3
- 239000003995 emulsifying agent Substances 0.000 claims description 18
- 239000006185 dispersion Substances 0.000 claims description 12
- 239000003822 epoxy resin Substances 0.000 claims description 12
- 229920000647 polyepoxide Polymers 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 4
- -1 polyoxypropylene Polymers 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- FPZWZCWUIYYYBU-UHFFFAOYSA-N 2-(2-ethoxyethoxy)ethyl acetate Chemical compound CCOCCOCCOC(C)=O FPZWZCWUIYYYBU-UHFFFAOYSA-N 0.000 claims description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 2
- 239000004925 Acrylic resin Substances 0.000 claims description 2
- 229920000178 Acrylic resin Polymers 0.000 claims description 2
- MQJKPEGWNLWLTK-UHFFFAOYSA-N Dapsone Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=C1 MQJKPEGWNLWLTK-UHFFFAOYSA-N 0.000 claims description 2
- UDSFAEKRVUSQDD-UHFFFAOYSA-N Dimethyl adipate Chemical compound COC(=O)CCCCC(=O)OC UDSFAEKRVUSQDD-UHFFFAOYSA-N 0.000 claims description 2
- MUXOBHXGJLMRAB-UHFFFAOYSA-N Dimethyl succinate Chemical compound COC(=O)CCC(=O)OC MUXOBHXGJLMRAB-UHFFFAOYSA-N 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 229920000877 Melamine resin Polymers 0.000 claims description 2
- 239000004952 Polyamide Substances 0.000 claims description 2
- 239000004642 Polyimide Substances 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- 229920001807 Urea-formaldehyde Polymers 0.000 claims description 2
- 150000008065 acid anhydrides Chemical class 0.000 claims description 2
- 150000004982 aromatic amines Chemical class 0.000 claims description 2
- 150000007942 carboxylates Chemical class 0.000 claims description 2
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 2
- XTDYIOOONNVFMA-UHFFFAOYSA-N dimethyl pentanedioate Chemical compound COC(=O)CCCC(=O)OC XTDYIOOONNVFMA-UHFFFAOYSA-N 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 229920001568 phenolic resin Polymers 0.000 claims description 2
- 239000005011 phenolic resin Substances 0.000 claims description 2
- 229920002647 polyamide Polymers 0.000 claims description 2
- 229920001721 polyimide Polymers 0.000 claims description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 2
- 229920001451 polypropylene glycol Polymers 0.000 claims description 2
- 229920000053 polysorbate 80 Polymers 0.000 claims description 2
- 239000004814 polyurethane Substances 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 claims description 2
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 claims 1
- 239000000853 adhesive Substances 0.000 abstract description 4
- 230000001070 adhesive effect Effects 0.000 abstract description 4
- 238000004381 surface treatment Methods 0.000 abstract description 3
- 229920000728 polyester Polymers 0.000 abstract description 2
- 238000007650 screen-printing Methods 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 229910000679 solder Inorganic materials 0.000 description 6
- 238000003466 welding Methods 0.000 description 6
- 238000005245 sintering Methods 0.000 description 4
- 238000005476 soldering Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052745 lead Inorganic materials 0.000 description 3
- 229910052718 tin Inorganic materials 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000007772 electroless plating Methods 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
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
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Conductive Materials (AREA)
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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010234774.6A CN111341484A (en) | 2020-03-30 | 2020-03-30 | Low-temperature curing type conductive silver paste and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010234774.6A CN111341484A (en) | 2020-03-30 | 2020-03-30 | Low-temperature curing type conductive silver paste and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111341484A true CN111341484A (en) | 2020-06-26 |
Family
ID=71184708
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010234774.6A Pending CN111341484A (en) | 2020-03-30 | 2020-03-30 | Low-temperature curing type conductive silver paste and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111341484A (en) |
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 | A kind of high reliability low temperature curing silver paste for ferrite and preparation method thereof |
| CN115312230A (en) * | 2022-09-05 | 2022-11-08 | 无锡帝科电子材料股份有限公司 | A kind of conductive silver paste, its preparation method and application |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101710497A (en) * | 2009-12-08 | 2010-05-19 | 华中科技大学 | Nano-silver conductive slurry |
| JP2013114836A (en) * | 2011-11-28 | 2013-06-10 | Kyoto Elex Kk | Heat curable conductive paste composition |
| TW201419312A (en) * | 2012-09-07 | 2014-05-16 | Namics Corp | Silver paste composition and method for manufacturing the same |
| CN105513668A (en) * | 2016-01-25 | 2016-04-20 | 深圳市思迈科新材料有限公司 | Conductive silver paste for nano-silver film low-temperature setting and preparation method thereof |
| CN106098145A (en) * | 2016-07-06 | 2016-11-09 | 东莞珂洛赫慕电子材料科技有限公司 | A kind of low-temperature cured conductive paste based on flexible parent metal and preparation method thereof |
| CN109887639A (en) * | 2019-01-18 | 2019-06-14 | 昆明贵金属研究所 | A kind of solderable low temperature curing functional silver paste and preparation method thereof |
-
2020
- 2020-03-30 CN CN202010234774.6A patent/CN111341484A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101710497A (en) * | 2009-12-08 | 2010-05-19 | 华中科技大学 | Nano-silver conductive slurry |
| JP2013114836A (en) * | 2011-11-28 | 2013-06-10 | Kyoto Elex Kk | Heat curable conductive paste composition |
| TW201419312A (en) * | 2012-09-07 | 2014-05-16 | Namics Corp | Silver paste composition and method for manufacturing the same |
| CN105513668A (en) * | 2016-01-25 | 2016-04-20 | 深圳市思迈科新材料有限公司 | Conductive silver paste for nano-silver film low-temperature setting and preparation method thereof |
| CN106098145A (en) * | 2016-07-06 | 2016-11-09 | 东莞珂洛赫慕电子材料科技有限公司 | A kind of low-temperature cured conductive paste based on flexible parent metal and preparation method thereof |
| CN109887639A (en) * | 2019-01-18 | 2019-06-14 | 昆明贵金属研究所 | A kind of solderable low temperature curing functional silver paste and preparation method thereof |
Cited By (7)
| 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 |
| 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 |
| CN115188520A (en) * | 2022-07-05 | 2022-10-14 | 大连海外华昇电子科技有限公司 | A kind of high reliability low temperature curing silver paste for ferrite and preparation method thereof |
| CN115188520B (en) * | 2022-07-05 | 2024-10-22 | 大连海外华昇电子科技有限公司 | A high reliability low temperature curing silver paste for ferrite and preparation method thereof |
| CN115312230A (en) * | 2022-09-05 | 2022-11-08 | 无锡帝科电子材料股份有限公司 | A kind of conductive silver paste, its preparation method and application |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111341484A (en) | Low-temperature curing type conductive silver paste and preparation method thereof | |
| US6149857A (en) | Method of making films and coatings having anisotropic conductive pathways therein | |
| JP3900248B2 (en) | Multilayer wiring board and method for forming the same | |
| US6180226B1 (en) | Method of forming a monolayer of particles, and products formed thereby | |
| JP4677900B2 (en) | Mixed conductive powder and its use | |
| US6977025B2 (en) | Method of forming a monolayer of particles having at least two different sizes, and products formed thereby | |
| CN106590173A (en) | Nano-metal ink capable of being cured at low temperatures, preparation method therefor and application of nano-metal ink | |
| CN101760147A (en) | Solvent type aeolotropic nano conductive adhesive and manufacturing method thereof | |
| JP2004265901A (en) | Conductive paste, circuit forming substrate using the same, and its manufacturing method | |
| WO2021023162A1 (en) | Conductive material and preparation method therefor, and electronic device | |
| CN114864134A (en) | Nano-alloy composite low-temperature slurry, preparation method and application thereof | |
| CN101514281B (en) | Conductive silver ink for encapsulating LED and preparation method thereof | |
| KR100538503B1 (en) | Adhesives and Adhesive Films | |
| Daniel Lu et al. | Recent advances in nano-conductive adhesives | |
| CN113831876B (en) | Conductive adhesive, solid conductive adhesive film, and preparation methods and applications thereof | |
| JP2022169512A (en) | Nano copper paste and film for sintered die attach and similar applications | |
| JP2004223559A (en) | Metallic powder composition for electrode connection and method for connecting electrode | |
| CN112961633A (en) | Low-temperature cured conductive adhesive and preparation method thereof | |
| JP2004265607A (en) | Conductive paste, circuit board using the same, and manufacturing method of the circuit board | |
| Jin et al. | Anisotropically conductive polymer films with a uniform dispersion of particles | |
| CN105419674A (en) | Floating all-dimensional conductive adhesive film | |
| CN110428926A (en) | Copper-based composite conducting slurry, preparation method and applications | |
| CN110493952B (en) | Micropore filling slurry for circuit board, preparation method and application thereof | |
| CN213803596U (en) | Anisotropic conductive adhesive film | |
| JP2001297631A (en) | Anisotropic conductive film |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200626 |