CN116031012A - Nano conductive silver paste and preparation method thereof - Google Patents
Nano conductive silver paste and preparation method thereof Download PDFInfo
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- CN116031012A CN116031012A CN202310034716.2A CN202310034716A CN116031012A CN 116031012 A CN116031012 A CN 116031012A CN 202310034716 A CN202310034716 A CN 202310034716A CN 116031012 A CN116031012 A CN 116031012A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 90
- 239000011521 glass Substances 0.000 claims abstract description 59
- 239000002245 particle Substances 0.000 claims abstract description 24
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 20
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 20
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 15
- 238000000498 ball milling Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 15
- 239000002002 slurry Substances 0.000 claims description 13
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 10
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 10
- 239000005751 Copper oxide Substances 0.000 claims description 10
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 claims description 10
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 10
- 229910000431 copper oxide Inorganic materials 0.000 claims description 10
- 229910000464 lead oxide Inorganic materials 0.000 claims description 10
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 10
- 229910001947 lithium oxide Inorganic materials 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 claims description 10
- 229920005989 resin Polymers 0.000 claims description 10
- 239000011347 resin Substances 0.000 claims description 10
- 239000000377 silicon dioxide Substances 0.000 claims description 10
- 235000012239 silicon dioxide Nutrition 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 5
- 229920000084 Gum arabic Polymers 0.000 claims description 5
- 241000978776 Senegalia senegal Species 0.000 claims description 5
- 239000000205 acacia gum Substances 0.000 claims description 5
- 235000010489 acacia gum Nutrition 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 5
- 239000008103 glucose Substances 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000010791 quenching Methods 0.000 claims description 5
- 230000000171 quenching effect Effects 0.000 claims description 5
- 238000007670 refining Methods 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 4
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 4
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 229920008347 Cellulose acetate propionate Polymers 0.000 claims description 3
- 239000001856 Ethyl cellulose Substances 0.000 claims description 3
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 3
- 229920006217 cellulose acetate butyrate Polymers 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 3
- 229920001249 ethyl cellulose Polymers 0.000 claims description 3
- LZDKZFUFMNSQCJ-UHFFFAOYSA-N 1,2-diethoxyethane Chemical compound CCOCCOCC LZDKZFUFMNSQCJ-UHFFFAOYSA-N 0.000 claims description 2
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 claims description 2
- PTTPXKJBFFKCEK-UHFFFAOYSA-N 2-Methyl-4-heptanone Chemical compound CC(C)CC(=O)CC(C)C PTTPXKJBFFKCEK-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
- UDSFAEKRVUSQDD-UHFFFAOYSA-N Dimethyl adipate Chemical compound COC(=O)CCCCC(=O)OC UDSFAEKRVUSQDD-UHFFFAOYSA-N 0.000 claims description 2
- 239000002114 nanocomposite Substances 0.000 claims description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 2
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 239000004843 novolac epoxy resin Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 7
- 239000006185 dispersion Substances 0.000 abstract description 4
- 230000005855 radiation Effects 0.000 abstract description 2
- 239000004065 semiconductor Substances 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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- Conductive Materials (AREA)
Abstract
The invention discloses a nanometer conductive silver paste and a preparation method thereof, belonging to the technical field of conductive silver paste, and comprising nanometer silver powder, nanometer glass powder and an organic carrier; the median particle diameter of the nanometer silver powder is 35-50nm, the median particle diameter of the nanometer glass powder is 20-40nm, and the product has the advantages of good dispersion stability, high electrical conductivity, high thermal conductivity, strong adhesion, high reliability, sprayability and good process stability. The product can be applied to a chip heat radiation module, a mobile phone industry, a power supply industry, a network power supply, a 5G base station, a data center and the like, and can also be used for semiconductor electromagnetic shielding, replace a shielding cover, simplify the process and reduce the volume of electronic products.
Description
Technical Field
The invention relates to the technical field of conductive silver paste, in particular to nano conductive silver paste and a preparation method thereof.
Background
In recent years, with rapid development of the electronic industry, demands for electronic products such as membrane switches, flexible printed circuit boards, electromagnetic shields, potentiometers, radio frequency identification systems, solar cells and the like are rapidly increasing, and development and application of conductive silver paste as a key functional material for preparing such electronic components are also receiving attention. It was analyzed that there are billions of dollars of market size per year for the conductive silver paste market alone. In the course of the rapid development of the information industry, slurries are important as a key material. The high-performance low-cost slurry can greatly improve the competitiveness of the product, and is a necessary trend of the development of electronic slurry.
The conductive silver paste in the prior art has the disadvantages of poor dispersion stability, low electrical conductivity, low thermal conductivity, weak adhesion, low reliability, spraying performance and poor process stability.
Disclosure of Invention
The embodiment of the invention provides nano conductive silver paste and a preparation method thereof, which are used for solving the technical problems of poor dispersion stability, low electrical conductivity, low thermal conductivity, weak adhesion, low reliability, sprayability and poor process stability of the conductive silver paste, and comprise the following steps:
one aspect of the invention provides a nano conductive silver paste, which comprises, by weight, 15-30 parts of nano silver powder, 6-10 parts of nano glass powder and 30-50 parts of organic carrier; the median particle diameter of the nanometer silver powder is 35-50nm, and the median particle diameter of the nanometer glass powder is 20-40nm.
Optionally, the preparation method of the nano silver powder comprises the following steps:
preparing a silver nitrate solution, adding silver nitrate into deionized water, and uniformly stirring to obtain the silver nitrate solution;
adding ammonia water into the silver nitrate solution, and stirring for 5-15min at a rotating speed of 200-300rmp to obtain a silver ammonia solution;
adding modified gum arabic powder into the silver ammonia solution, and stirring for 10-20min at a rotating speed of 200-300rmp to obtain a mixed solution;
and fourthly, adding glucose into the mixed solution according to the mass ratio of 10 (2-3), regulating the temperature to 50-55 ℃, preserving heat, stirring and reacting for 4-6 hours, and then carrying out suction filtration, washing and drying to obtain the nano-composite material.
Optionally, the specific surface area of the nano silver powder is 4-12m 2 Per gram, the tap density of the nano silver powder is 2.0-5.0g/cm 3 。
Optionally, the particle size distribution of the nano glass powder is D100 is less than or equal to 800nm, D50 is less than or equal to 400nm, D10 is more than or equal to 100nm, and the softening temperature Tg of the nano glass powder is less than or equal to 200 ℃.
Optionally, the nano glass powder comprises, by weight, 40-50 parts of silicon dioxide, 8-15 parts of lead oxide, 1-5 parts of copper oxide, 10-20 parts of tellurium dioxide, 6-10 parts of bismuth trioxide and 2-4 parts of lithium oxide.
Optionally, the preparation method of the nano glass powder comprises the following steps: pouring silicon dioxide, lead oxide, copper oxide, tellurium dioxide, bismuth trioxide and lithium oxide into a ball milling tank, ball milling, discharging, and drying at 160-200 ℃; heating the dried powder at 1200-1300 ℃ for 150-180min, quenching the solution with water, ball milling, refining, drying and sieving to obtain the nano glass powder with the median particle diameter of 20-40nm.
Optionally, the organic carrier comprises 30-50 parts by weight of resin and 50-70 parts by weight of solvent.
Optionally, the resin is at least one of ethyl cellulose, cellulose acetate propionate, cellulose acetate butyrate, polyvinyl formal, polyvinyl butyral, epoxy resin, phenolic epoxy resin and acrylic resin.
Optionally, the solvent is at least one of ethanol, isopropanol, n-butanol, acetone, cyclohexanone, acetylacetone, diisobutylketone, ethylene glycol diethyl ether, ethyl propionate, diethylene glycol butyl ether acetate, propylene glycol methyl ether acetate and dimethyl adipate.
The invention also provides a preparation method of the nano conductive silver paste, which comprises the steps of weighing the components according to the proportion, and preparing an organic carrier and low-softening-point glass powder to form glass paste;
placing the nano glass powder slurry into a multi-roller machine for multiple multi-roller grinding treatment;
adding the nano silver powder mixture into the ground nano glass powder slurry, and centrifuging to obtain the nano conductive silver slurry.
Compared with the prior art, the nano conductive silver paste and the preparation method thereof can achieve the following
The beneficial effects are that:
the nano conductive silver paste comprises nano silver powder, nano glass powder and an organic carrier; the median particle diameter of the nanometer silver powder is 35-50nm, the median particle diameter of the nanometer glass powder is 20-40nm, and the product has the advantages of good dispersion stability, high electrical conductivity, high thermal conductivity, strong adhesion, high reliability, sprayability and good process stability. The product can be applied to a chip heat radiation module, a mobile phone industry, a power supply industry, a network power supply, a 5G base station, a data center and the like, and can also be used for semiconductor electromagnetic shielding, replace a shielding cover, simplify the process and reduce the volume of electronic products.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below in connection with specific embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A nano conductive silver paste comprises 22.5kg of nano silver powder, 8kg of nano glass powder and 40kg of organic carrier; the median particle diameter of the nanometer silver powder is 42.5nm, and the median particle diameter of the nanometer glass powder is 30nm.
Further, the preparation method of the nano silver powder comprises the following steps:
preparing a silver nitrate solution, adding silver nitrate into deionized water, and uniformly stirring to obtain the silver nitrate solution;
adding ammonia water into the silver nitrate solution, and stirring for 10min at the rotating speed of 250rmp to obtain a silver ammonia solution;
adding modified gum arabic powder into the silver ammonia solution, and stirring for 15min at the rotating speed of 250rmp to obtain a mixed solution;
and fourthly, adding glucose into the mixed solution according to the mass ratio of 4:1, adjusting the temperature to 52.5 ℃, carrying out heat preservation and stirring reaction for 5 hours, and then carrying out suction filtration, washing and drying to obtain the compound.
Further, the specific surface area of the nano silver powder is 8m 2 Per gram, the tap density of the nano silver powder is 3.5g/cm 3 。
Further, the particle size distribution of the nano glass powder is D100 is less than or equal to 800nm, D50 is less than or equal to 400nm, D10 is more than or equal to 100nm, and the softening temperature Tg of the nano glass powder is less than or equal to 200 ℃.
Further, the nano glass powder comprises 45kg of silicon dioxide, 11.5kg of lead oxide, 3kg of copper oxide, 15kg of tellurium dioxide, 8kg of bismuth trioxide and 3kg of lithium oxide.
Further, the preparation method of the nano glass powder comprises the following steps: pouring silicon dioxide, lead oxide, copper oxide, tellurium dioxide, bismuth trioxide and lithium oxide into a ball milling tank, ball milling, discharging, and drying at 180 ℃; and heating the dried powder for 165min at 1250 ℃, carrying out water quenching, ball milling and refining on the solution after heating, drying and sieving to obtain the nano glass powder with the median particle size of 30nm.
Further, the organic vehicle includes 40kg of resin and 60kg of solvent.
Further, the resin is ethyl cellulose.
Further, the solvent is ethanol.
According to the formula, the preparation method of the nano conductive silver paste comprises the steps of weighing the components according to the proportion, and preparing an organic carrier and low-softening-point glass powder to form glass paste;
placing the nano glass powder slurry into a multi-roller machine for multiple multi-roller grinding treatment;
adding the nano silver powder mixture into the ground nano glass powder slurry, and centrifuging to obtain the nano conductive silver slurry.
Example 2
A nano conductive silver paste comprises 15kg of nano silver powder, 6kg of nano glass powder and 30kg of organic carrier; the median particle diameter of the nanometer silver powder is 35nm, and the median particle diameter of the nanometer glass powder is 20nm.
Further, the preparation method of the nano silver powder comprises the following steps:
preparing a silver nitrate solution, adding silver nitrate into deionized water, and uniformly stirring to obtain the silver nitrate solution;
adding ammonia water into the silver nitrate solution, and stirring for 15min at the rotating speed of 200rmp to obtain a silver ammonia solution;
adding modified gum arabic powder into the silver ammonia solution, and stirring for 20min at a rotating speed of 200rmp to obtain a mixed solution;
and fourthly, adding glucose into the mixed solution according to the mass ratio of 5:1, adjusting the temperature to 50 ℃, preserving heat, stirring and reacting for 6 hours, and then carrying out suction filtration, washing and drying to obtain the compound.
Further, the specific surface area of the nano silver powder is 4m 2 Per gram, the tap density of the nano silver powder is 2.0g/cm 3 。
Further, the particle size distribution of the nano glass powder is D100 is less than or equal to 800nm, D50 is less than or equal to 400nm, D10 is more than or equal to 100nm, and the softening temperature Tg of the nano glass powder is less than or equal to 200 ℃.
Further, the nano glass powder comprises 40kg of silicon dioxide, 8kg of lead oxide, 1kg of copper oxide, 10kg of tellurium dioxide, 6kg of bismuth trioxide and 2kg of lithium oxide.
Further, the preparation method of the nano glass powder comprises the following steps: pouring silicon dioxide, lead oxide, copper oxide, tellurium dioxide, bismuth trioxide and lithium oxide into a ball milling tank, ball milling, discharging, and drying at 160-200 ℃; and heating the dried powder at 1200 ℃ for 180min, quenching the solution with water, ball milling, refining, drying and sieving to obtain the nano glass powder with the median particle diameter of 20nm.
Further, the organic vehicle includes 30kg of resin and 70kg of solvent.
Further, the resin is cellulose acetate propionate.
Further, the solvent is isopropyl alcohol.
According to the formula, the preparation method of the nano conductive silver paste comprises the steps of weighing the components according to the proportion, and preparing an organic carrier and low-softening-point glass powder to form glass paste;
placing the nano glass powder slurry into a multi-roller machine for multiple multi-roller grinding treatment;
adding the nano silver powder mixture into the ground nano glass powder slurry, and centrifuging to obtain the nano conductive silver slurry.
Example 3
A nano conductive silver paste comprises 30kg of nano silver powder, 10kg of nano glass powder and 50kg of organic carrier; the median particle diameter of the nanometer silver powder is 50nm, and the median particle diameter of the nanometer glass powder is 40nm.
Further, the preparation method of the nano silver powder comprises the following steps:
preparing a silver nitrate solution, adding silver nitrate into deionized water, and uniformly stirring to obtain the silver nitrate solution;
adding ammonia water into the silver nitrate solution, and stirring for 5min at the rotating speed of 300rmp to obtain a silver ammonia solution;
adding modified gum arabic powder into the silver ammonia solution, and stirring for 10min at the rotating speed of 300rmp to obtain a mixed solution;
and fourthly, adding glucose into the mixed solution according to the mass ratio of 10:2, adjusting the temperature to 55 ℃, preserving heat, stirring and reacting for 4 hours, and then carrying out suction filtration, washing and drying to obtain the compound.
Further, the specific surface area of the nano silver powder is 4-12m 2 Per gram, the tap density of the nano silver powder is 5.0g/cm 3 。
Further, the particle size distribution of the nano glass powder is D100 is less than or equal to 800nm, D50 is less than or equal to 400nm, D10 is more than or equal to 100nm, and the softening temperature Tg of the nano glass powder is less than or equal to 200 ℃.
Further, the nano glass powder comprises 50kg of silicon dioxide, 15kg of lead oxide, 5kg of copper oxide, 20kg of tellurium dioxide, 10kg of bismuth trioxide and 4kg of lithium oxide.
Further, the preparation method of the nano glass powder comprises the following steps: pouring silicon dioxide, lead oxide, copper oxide, tellurium dioxide, bismuth trioxide and lithium oxide into a ball milling tank, ball milling, discharging, and drying at 200 ℃; and heating the dried powder at 1300 ℃ for 150min, quenching the solution with water, ball milling, refining, drying and sieving to obtain the nano glass powder with the median particle diameter of 40nm.
Further, the organic vehicle includes 50kg of resin and 50kg of solvent.
Further, the resin is cellulose acetate butyrate.
Further, the solvent is n-butanol.
According to the formula, the preparation method of the nano conductive silver paste comprises the steps of weighing the components according to the proportion, and preparing an organic carrier and low-softening-point glass powder to form glass paste;
placing the nano glass powder slurry into a multi-roller machine for multiple multi-roller grinding treatment;
adding the nano silver powder mixture into the ground nano glass powder slurry, and centrifuging to obtain the nano conductive silver slurry.
Test examples
The nano conductive silver paste prepared in the examples 1-3 is subjected to parameter test, and the specific test method and test result are shown in Table 1:
table 1 product parameter tables of the examples
| Performance of | Example 1 | Example 2 | Example 3 |
| Volume resistivity (Ω cm) | 6.5×10 -6 | 5.5×10 -6 | 6.3×10 -6 |
| Viscosity (mPa. S) | 550 | 540 | 530 |
| Thixotropic index | 2.7 | 2.6 | 2.5 |
| Curing conditions | 60min@150℃ | 60min@150℃ | 60min@150℃ |
| Shielding effectiveness (dB) | 90 | 89 | 88 |
| Adhesive force (Baige method) | 5B | 5B | 5B |
The nano conductive silver paste filler can be sprayed in a co-mode, and has the advantages of low viscosity, high conductivity, high heat conductivity coefficient, high adhesive force and good electromagnetic shielding effect.
The foregoing is merely exemplary of the present invention and is not intended to limit the present invention. Various modifications and variations of the present invention will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the invention are to be included in the scope of the claims of the present invention.
Claims (10)
1. The nano conductive silver paste is characterized by comprising, by weight, 15-30 parts of nano silver powder, 6-10 parts of nano glass powder and 30-50 parts of organic carrier; the median particle diameter of the nanometer silver powder is 35-50nm, and the median particle diameter of the nanometer glass powder is 20-40nm.
2. The nano conductive silver paste according to claim 1, wherein the preparation method of the nano silver powder comprises the following steps:
preparing a silver nitrate solution, adding silver nitrate into deionized water, and uniformly stirring to obtain the silver nitrate solution;
adding ammonia water into the silver nitrate solution, and stirring for 5-15min at a rotating speed of 200-300rmp to obtain a silver ammonia solution;
adding modified gum arabic powder into the silver ammonia solution, and stirring for 10-20min at a rotating speed of 200-300rmp to obtain a mixed solution;
and fourthly, adding glucose into the mixed solution according to the mass ratio of 10 (2-3), regulating the temperature to 50-55 ℃, preserving heat, stirring and reacting for 4-6 hours, and then carrying out suction filtration, washing and drying to obtain the nano-composite material.
3. The nano conductive silver paste according to any one of claims 1 or 2, wherein the specific surface area of the nano silver powder is 4-12m 2 Per gram, the tap density of the nano silver powder is 2.0-5.0g/cm 3 。
4. The nano conductive silver paste according to claim 1, wherein the nano glass powder has a particle size distribution of D 100 ≤800nm，D 50 ≤400nm，D 10 The softening temperature Tg of the nano glass powder is more than or equal to 100nm and less than or equal to 200 ℃.
5. The nano conductive silver paste according to any one of claims 1 or 4, wherein the nano glass powder comprises, in parts by weight, 40 to 50 parts by weight of silicon dioxide, 8 to 15 parts by weight of lead oxide, 1 to 5 parts by weight of copper oxide, 10 to 20 parts by weight of tellurium dioxide, 6 to 10 parts by weight of bismuth trioxide and 2 to 4 parts by weight of lithium oxide.
6. The nano conductive silver paste according to claim 5, wherein the preparation method of the nano glass powder comprises the following steps: pouring silicon dioxide, lead oxide, copper oxide, tellurium dioxide, bismuth trioxide and lithium oxide into a ball milling tank, ball milling, discharging, and drying at 160-200 ℃; heating the dried powder at 1200-1300 ℃ for 150-180min, quenching the solution with water, ball milling, refining, drying and sieving to obtain the nano glass powder with the median particle diameter of 20-40nm.
7. The nano-conductive silver paste according to claim 1, wherein the organic carrier comprises 30-50 parts by weight of resin and 50-70 parts by weight of solvent.
8. The nano-conductive silver paste according to claim 7, wherein the resin is at least one of ethyl cellulose, cellulose acetate propionate, cellulose acetate butyrate, polyvinyl formal, polyvinyl butyral, epoxy, novolac epoxy, and acrylic resin.
9. The nano-conductive silver paste according to claim 7, wherein the solvent is at least one of ethanol, isopropanol, n-butanol, acetone, cyclohexanone, acetylacetone, diisobutylketone, ethylene glycol diethyl ether, ethyl propionate, diethylene glycol butyl ether acetate, propylene glycol methyl ether acetate, and dimethyl adipate.
10. The preparation method of the nano conductive silver paste is characterized by comprising the steps of weighing the components according to the proportion, and preparing an organic carrier and nano glass powder to form nano glass paste;
placing the nano glass powder slurry into a multi-roller machine for multiple multi-roller grinding treatment;
adding the nano silver powder mixture into the ground nano glass powder slurry, and centrifuging to obtain the nano conductive silver slurry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310034716.2A CN116031012B (en) | 2023-01-10 | 2023-01-10 | Nano conductive silver paste and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310034716.2A CN116031012B (en) | 2023-01-10 | 2023-01-10 | Nano conductive silver paste and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116031012A true CN116031012A (en) | 2023-04-28 |
| CN116031012B CN116031012B (en) | 2023-09-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310034716.2A Active CN116031012B (en) | 2023-01-10 | 2023-01-10 | Nano conductive silver paste and preparation method thereof |
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101582328A (en) * | 2009-06-26 | 2009-11-18 | 彩虹集团公司 | Nanometer silver paste for terminal electrode of multi-layer ceramic capacitor and method for preparing same |
| CN102290117A (en) * | 2011-04-25 | 2011-12-21 | 深圳市唯特偶新材料股份有限公司 | Low temperature-sintered nano silver paste and preparation method thereof |
| CN105469857A (en) * | 2015-12-28 | 2016-04-06 | 苏州华一新能源科技有限公司 | Silver paste used for silicon nitride substrate and preparation method thereof |
| CN105869706A (en) * | 2016-05-11 | 2016-08-17 | 东莞珂洛赫慕电子材料科技有限公司 | Low-temperature sintering thick film paste applied to PI films and preparation method of low-temperature sintering thick film paste |
| CN108735339A (en) * | 2018-05-25 | 2018-11-02 | 重庆邦锐特新材料有限公司 | A kind of high performance sintered conductive silver paste and preparation method thereof and sintering method |
| CN109935380A (en) * | 2019-04-01 | 2019-06-25 | 南京航空航天大学 | A kind of AIN thick film circuit conductive silver paste and preparation method thereof |
| CN114210996A (en) * | 2021-12-29 | 2022-03-22 | 上海腾烁电子材料有限公司 | High-sintering-activity nano silver powder and preparation method thereof |
| CN114464338A (en) * | 2021-11-29 | 2022-05-10 | 无锡帝科电子材料股份有限公司 | Solar cell front conductive silver paste and preparation method thereof |
| CN115394471A (en) * | 2022-08-31 | 2022-11-25 | 成都中金黎阳新材料科技有限公司 | Conductive paste and application thereof in N-type silicon wafer solar cell |
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2023
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Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101582328A (en) * | 2009-06-26 | 2009-11-18 | 彩虹集团公司 | Nanometer silver paste for terminal electrode of multi-layer ceramic capacitor and method for preparing same |
| CN102290117A (en) * | 2011-04-25 | 2011-12-21 | 深圳市唯特偶新材料股份有限公司 | Low temperature-sintered nano silver paste and preparation method thereof |
| CN105469857A (en) * | 2015-12-28 | 2016-04-06 | 苏州华一新能源科技有限公司 | Silver paste used for silicon nitride substrate and preparation method thereof |
| CN105869706A (en) * | 2016-05-11 | 2016-08-17 | 东莞珂洛赫慕电子材料科技有限公司 | Low-temperature sintering thick film paste applied to PI films and preparation method of low-temperature sintering thick film paste |
| CN108735339A (en) * | 2018-05-25 | 2018-11-02 | 重庆邦锐特新材料有限公司 | A kind of high performance sintered conductive silver paste and preparation method thereof and sintering method |
| CN109935380A (en) * | 2019-04-01 | 2019-06-25 | 南京航空航天大学 | A kind of AIN thick film circuit conductive silver paste and preparation method thereof |
| CN114464338A (en) * | 2021-11-29 | 2022-05-10 | 无锡帝科电子材料股份有限公司 | Solar cell front conductive silver paste and preparation method thereof |
| CN114210996A (en) * | 2021-12-29 | 2022-03-22 | 上海腾烁电子材料有限公司 | High-sintering-activity nano silver powder and preparation method thereof |
| CN115394471A (en) * | 2022-08-31 | 2022-11-25 | 成都中金黎阳新材料科技有限公司 | Conductive paste and application thereof in N-type silicon wafer solar cell |
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| CN116031012B (en) | 2023-09-22 |
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