CN115985553B - Halogen-free silver paste with high bending resistance and preparation method thereof - Google Patents
Halogen-free silver paste with high bending resistance and preparation method thereof Download PDFInfo
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- CN115985553B CN115985553B CN202310039621.XA CN202310039621A CN115985553B CN 115985553 B CN115985553 B CN 115985553B CN 202310039621 A CN202310039621 A CN 202310039621A CN 115985553 B CN115985553 B CN 115985553B
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 239000004332 silver Substances 0.000 title claims abstract description 35
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 35
- 238000005452 bending Methods 0.000 title claims description 11
- 238000002360 preparation method Methods 0.000 title claims description 10
- 229920005989 resin Polymers 0.000 claims abstract description 39
- 239000011347 resin Substances 0.000 claims abstract description 39
- 240000002853 Nelumbo nucifera Species 0.000 claims abstract description 34
- 235000006508 Nelumbo nucifera Nutrition 0.000 claims abstract description 34
- 239000000835 fiber Substances 0.000 claims abstract description 28
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims description 23
- 239000011265 semifinished product Substances 0.000 claims description 20
- 238000000227 grinding Methods 0.000 claims description 19
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 8
- 229920001225 polyester resin Polymers 0.000 claims description 6
- 239000004645 polyester resin Substances 0.000 claims description 6
- PAAZPARNPHGIKF-UHFFFAOYSA-N 1,2-dibromoethane Chemical compound BrCCBr PAAZPARNPHGIKF-UHFFFAOYSA-N 0.000 claims description 5
- 239000004925 Acrylic resin Substances 0.000 claims description 5
- 229920000178 Acrylic resin Polymers 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 229920005749 polyurethane resin Polymers 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- LXBIFEVIBLOUGU-UHFFFAOYSA-N Deoxymannojirimycin Natural products OCC1NCC(O)C(O)C1O LXBIFEVIBLOUGU-UHFFFAOYSA-N 0.000 claims description 2
- UYAAVKFHBMJOJZ-UHFFFAOYSA-N diimidazo[1,3-b:1',3'-e]pyrazine-5,10-dione Chemical compound O=C1C2=CN=CN2C(=O)C2=CN=CN12 UYAAVKFHBMJOJZ-UHFFFAOYSA-N 0.000 claims description 2
- JDZNTUQRMDAIRO-UHFFFAOYSA-N dimethylmyleran Chemical compound CS(=O)(=O)OC(C)CCC(C)OS(C)(=O)=O JDZNTUQRMDAIRO-UHFFFAOYSA-N 0.000 claims description 2
- 229940116423 propylene glycol diacetate Drugs 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 1
- 239000006185 dispersion Substances 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 18
- 239000012046 mixed solvent Substances 0.000 description 12
- 238000009826 distribution Methods 0.000 description 9
- 239000000758 substrate Substances 0.000 description 6
- 238000002156 mixing Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000007650 screen-printing Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 230000009916 joint effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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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- Powder Metallurgy (AREA)
Abstract
The invention discloses high-bending-resistance halogen-free silver paste which comprises the following raw materials in percentage by weight: 40-55% of silver powder, 43.5-57% of halogen-free carrier, 1-2% of auxiliary agent and 0.5-1% of lotus root silk fiber, wherein the silver powder consists of one or more than one mixture of flake silver powder, spherical silver powder and spheroidal silver powder. According to the invention, a certain amount of lotus root silk fibers are added into the silver paste, so that the dispersion uniformity between silver powder and the resin carrier can be improved, and meanwhile, the flexibility of the resin carrier can be improved by the lotus root silk fibers, and the flexibility of a channel formed by resin is obviously improved.
Description
Technical field:
The invention belongs to the technical field of information electronic materials, and particularly relates to halogen-free silver paste with high bending resistance and a preparation method thereof.
The background technology is as follows:
along with the continuous evolution of electronic technology products, the dielectric substrate of the electronic products is also developed into a flexible substrate such as a screen printing PET substrate, an ITO film substrate and the like from the traditional hard materials, silver paste is a raw material for manufacturing a circuit by printing on the dielectric substrate, and along with the development of the electronic products in the directions of lighter, thinner, more flexible, more environment-friendly and low cost, the performance of the conductive silver paste is also put forward higher requirements.
The conductive silver paste is uniform paste prepared by stirring and dispersing conductive silver powder serving as a conductive filler, polymer resin, solvent, curing agent, auxiliary agent and the like, the flexibility of the silver paste is influenced by various factors such as the dispersibility of the silver powder in the resin, the flexibility of the resin, the adhesive force between the resin and a substrate and the like, and the conventional silver paste is influenced by the problems that the silver powder and the resin cannot be completely and effectively dispersed and the like, and the bending resistance of the silver paste is also deficient.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art.
The invention comprises the following steps:
The invention aims to provide halogen-free silver paste with high bending resistance and a preparation method thereof, thereby overcoming the defects in the prior art.
In order to achieve the above purpose, the invention provides a high-bending-resistance halogen-free silver paste, which comprises the following raw materials in percentage by weight: 40-55% of silver powder, 43.5-57% of halogen-free carrier, 1-2% of auxiliary agent and 0.5-1% of lotus root silk fiber, wherein the silver powder consists of one or more than one mixture of flake silver powder, spherical silver powder and spheroidal silver powder.
Further, as a preferable mode, the halogen-free carrier is composed of the following raw materials in percentage by weight: 15-25% of organic resin and 75-85% of organic solvent.
Further, preferably, the auxiliary agent is one or a mixture of more than one of 15000 mesh graphite, fumed silica, gamma-glycidyl ether methyltrimethoxysilane, modified polyester resin dibenzoate solution, sodium hexametaphosphate, organic bentonite and rosin.
Further, preferably, the auxiliary agent is a mixture of 15000 mesh graphite and gamma-glycidyl ether methyltrimethoxysilane.
Further, preferably, the organic resin is one or a mixture of more than one of a halogen-free polyurethane resin, a halogen-free polyester resin and a halogen-free acrylic resin.
Further, preferably, the organic solvent is one or a mixture of more than one of DBE, N-methyl pyrrolidone, DMM, isophorone and propylene glycol diacetate.
The invention further provides a preparation method of the halogen-free silver paste with high bending resistance, which comprises the following steps:
(1) The raw materials are prepared according to the following weight percentages: 40-55% of silver powder, 43.5-57% of halogen-free carrier, 1-2% of auxiliary agent and 0.5-1% of lotus root silk fiber;
(2) Taking half of halogen-free carrier and lotus root silk fiber, premixing, grinding and dispersing to fineness less than or equal to 5 mu m by a three-roller machine, and preparing a semi-finished product;
(3) Adding the semi-finished product, the rest halogen-free carrier, silver powder and an auxiliary agent into a planetary dispersing machine together, stirring for 25-35min, and defoaming to obtain semi-finished product slurry;
(4) And (3) grinding the obtained semi-finished product slurry again through a three-roller machine until the fineness of the slurry is less than or equal to 5 mu m, defoaming and filtering to obtain a halogen-free silver slurry finished product.
Further, the raw materials in the step (1) are prepared according to the following weight percentages: 48% of silver powder, 50.5% of halogen-free carrier, 0.8% of auxiliary agent and 0.7% of lotus root silk fiber.
Compared with the prior art, one aspect of the invention has the following beneficial effects:
(1) According to the invention, a certain amount of lotus root silk fibers are added into the silver paste, so that the dispersion uniformity between silver powder and a resin carrier can be improved, and meanwhile, the flexibility of the resin carrier can be improved by the lotus root silk fibers, and the flexibility of a channel formed by resin is obviously improved;
(2) The carrier adopts a halogen-free carrier, and the halogen-free carrier is combined with lotus root fibers, so that the flexibility of the carrier is improved, and the prepared silver paste is better in environmental protection;
(3) The silver powder adopts various silver powder and combines 15000 mesh graphite and gamma-glycidyl ether methyltrimethoxysilane mixture as an auxiliary agent, so that the lap joint effect between the resin carrier and silver powder particles is better, and the film forming performance during screen printing can be improved;
(4) When the preparation method is used, part of halogen-free carrier and lotus root silk fiber are premixed, ground and dispersed, and then mixed, ground, defoamed and other raw materials are carried out, so that the dispersibility between the obtained silver paste carrier and silver powder is better, and various performances such as film forming property, flexibility and the like of the silver paste can be improved.
The specific embodiment is as follows:
the following detailed description of specific embodiments of the invention is, but it should be understood that the invention is not limited to specific embodiments.
The following presents a simplified summary of one or more aspects in order to provide a basic understanding of such aspects. This summary is not an extensive overview of all contemplated aspects, and is intended to neither identify key or critical elements of all aspects nor delineate the scope of any or all aspects. Its sole purpose is to present some concepts of one or more aspects in a simplified form as a prelude to the more detailed description that is presented later.
Example 1:
the halogen-free silver paste with high bending resistance consists of the following raw materials in percentage by weight:
48.0% of silver powder;
35.2% of organic resin;
15% of DBE and N-methylpyrrolidone mixed solvent;
1.0% of lotus root silk fiber;
0.5% of gamma-glycidyl ether methyltrimethoxysilane;
0.3% of 15000 mesh graphite powder.
Wherein the silver powder consists of three flaky silver powders of flaky silver powder A, spherical silver powder B and spherical-like silver powder C, the apparent density of the silver powder A is 0.6g/cm 3～0.9g/cm3, the tap density is 1.5g/cm 3～2.5g/cm3, the particle size distribution Dmax is less than or equal to 10 mu m-20 mu m, the average particle size is 4.5 mu m-6.0 mu m, the specific surface area is 1.0m 2/kg～2.0m2/kg, and the burning loss ratio is less than or equal to 1.2%; the loose packing density of the spherical silver powder B is 1.5g/cm 3～2.0g/cm3, the tap density is 2.5g/cm 3～3.5g/cm3, the particle size distribution Dmax is less than or equal to 5 mu m, the average particle size is 2.0 mu m-3.0 mu m, the burning loss ratio is less than or equal to 0, and 01%; the apparent density of the spherical silver powder C is 1.5g/cm 3～2.0g/cm3, the tap density is 3.0g/cm 3～4.0g/cm3, the particle size distribution Dmax is less than or equal to 1 mu m, the specific surface area is 6.5m 2/kg～8.5m2/kg, and the burning loss ratio is less than 0.5%.
The organic resin is one or more of halogen-free polyurethane resin, halogen-free polyester resin and halogen-free acrylic resin.
The lotus root fiber is also called lotus root fiber, and is produced by Jiangxi Xialotus industry limited company, and the lotus root fiber refers to natural growth and elongation fiber of tubular molecules (guide pipes or tube cells) of secondary wall parts (lotus leaves or stems between lotus seedings) of lotus root stems, and is specifically produced by breaking clean fresh lotus root stems with the length of 6-10 cm, twisting the lotus root stems into threads while spinning the lotus root stems, and drying the lotus root stems.
The preparation method of the halogen-free silver paste comprises the following steps:
(1) The raw materials are prepared according to the following weight percentages: flake silver powder A16%, spherical silver powder B16%, spherical silver powder C16%, organic resin 35.2%, DBE, N-methyl pyrrolidone mixed solvent 15%, lotus root silk fiber 1.0%, gamma-glycidyl ether methyl trimethoxy silane 0.5% and 15000 mesh graphite powder 0.3%;
(2) Adding organic resin into a mixed solvent of DBE and N-methyl pyrrolidone, and stirring in a constant-temperature water bath kettle at 75-80 ℃ until the organic resin is completely dissolved to obtain a resin carrier solution;
(3) Taking half of the resin carrier solution and lotus root silk fibers, uniformly mixing in a planetary disperser, and grinding and dispersing until the fineness is less than or equal to 5 mu m to prepare a semi-finished product;
(4) Adding the prepared semi-finished product, the rest resin carrier solution, silver powder, DBE, N-methylpyrrolidone mixed solvent, 15000 mesh graphite powder and gamma-glycidyl ether methyl trimethoxy silane into a planetary dispersing machine together, stirring for 30min, and defoaming to obtain semi-finished product slurry;
(5) And (3) grinding the semi-finished product slurry again by a three-roller machine, dispersing from coarse to fine, firstly grinding for 4-5 times by a roller with a wider width until the slurry on a grinding roller is smooth and does not hang on the roller, then grinding for 2-3 times by a roller with a narrower width until the slurry fineness is less than or equal to 5 mu m, and then defoaming and filtering to obtain a halogen-free silver slurry finished product.
Example 2:
the halogen-free silver paste with high bending resistance consists of the following raw materials in percentage by weight:
48.0% of flake silver powder;
38.5% of organic resin;
12% of DBE and N-methylpyrrolidone mixed solvent;
0.7% of lotus root silk fiber;
0.5% of gamma-glycidyl ether methyltrimethoxysilane;
0.3% of 15000 mesh graphite powder.
Wherein the flake silver powder consists of three flake silver powder, namely flake silver powder 1, flake silver powder 2 and flake silver powder 3, wherein the apparent density of the flake silver powder 1 is 0.6g/cm 3～0.9g/cm3, the tap density is 1.5g/cm 3～2.5g/cm3, the particle size distribution Dmax is less than or equal to 10 mu m-20 mu m, the average particle size is 4.5 mu m-6.0 mu m, the specific surface area is 1.0m 2/kg～2.0m2/kg, and the burning loss ratio is less than or equal to 1.2%; the apparent density of the flake silver powder 2 is 0.6g/cm 3～1.0g/cm3, the tap density is 1.0g/cm 3～2.0g/cm3, the particle size distribution Dmax is less than or equal to 9.0 mu m to 1.0 mu m, the average particle size is 2.0 mu m to 3.0 mu m, the specific surface area is 2.0m 2/kg～3.0m2/kg, and the burning loss ratio is less than or equal to 0.24%; the apparent density of the flake silver powder 3 is 0.6g/cm 3～0.8g/cm3, the tap density is 1.0g/cm 3～1.3g/cm3, the particle size distribution Dmax is less than or equal to 10 mu m-20 mu m, the average particle size is 0.5 mu m-1.5 mu m, the specific surface area is 0.5m 2/kg～1.0m2/kg, and the burning loss ratio is less than 1.0%.
The organic resin is one or more of halogen-free polyurethane resin, halogen-free polyester resin and halogen-free acrylic resin.
The preparation method of the halogen-free silver paste comprises the following steps:
(1) The raw materials are prepared according to the following weight percentages: 16% of flake silver powder 1, 16% of flake silver powder 2, 16% of flake silver powder 3, 38.5% of organic resin, 12% of DBE, N-methylpyrrolidone mixed solvent, 0.7% of lotus root silk fiber, 0.5% of gamma-glycidyl ether methyltrimethoxysilane and 0.3% of 15000-mesh graphite powder;
(2) Adding organic resin into a mixed solvent of DBE and N-methyl pyrrolidone, and stirring in a constant-temperature water bath kettle at 75-80 ℃ until the organic resin is completely dissolved to obtain a resin carrier solution;
(3) Taking half of the resin carrier solution and lotus root silk fibers, uniformly mixing in a planetary disperser, and grinding and dispersing until the fineness is less than or equal to 5 mu m to prepare a semi-finished product;
(4) Adding the prepared semi-finished product, the rest resin carrier solution, silver powder, DBE, N-methylpyrrolidone mixed solvent, 15000 mesh graphite powder and gamma-glycidyl ether methyl trimethoxy silane into a planetary dispersing machine together, stirring for 35min, and defoaming to obtain semi-finished product slurry;
(5) And (3) grinding the semi-finished product slurry again by a three-roller machine, dispersing from coarse to fine, firstly grinding for 4-5 times by a roller with a wider width until the slurry on a grinding roller is smooth and does not hang on the roller, then grinding for 2-3 times by a roller with a narrower width until the slurry fineness is less than or equal to 5 mu m, and then defoaming and filtering to obtain a halogen-free silver slurry finished product.
Example 3:
the halogen-free silver paste with high bending resistance consists of the following raw materials in percentage by weight:
48.0% of flake silver powder;
35.4% of organic resin;
12% of DBE and N-methylpyrrolidone mixed solvent;
0.8% of lotus root silk fiber;
0.5% of gamma-glycidyl ether methyltrimethoxysilane;
0.3% of 15000 mesh graphite powder.
Wherein the flake silver powder consists of three flake silver powder, namely flake silver powder 1, flake silver powder 2 and flake silver powder 3, the apparent density of the silver powder 1 is 0.6g/cm 3～0.9g/cm3, the tap density is 1.5g/cm 3～2.5g/cm3, the particle size distribution Dmax is less than or equal to 10 mu m-20 mu m, the average particle size is 4.5 mu m-6.0 mu m, the specific surface area is 1.0m 2/kg～2.0m2/kg, and the burning loss ratio is less than or equal to 1.2%; the apparent density of the flake silver powder 2 is 0.6g/cm 3～1.0g/cm3, the tap density is 1.0g/cm 3～2.0g/cm3, the particle size distribution Dmax is less than or equal to 9.0 mu m to 1.0 mu m, the average particle size is 2.0 mu m to 3.0 mu m, the specific surface area is 2.0m 2/kg～3.0m2/kg, and the burning loss ratio is less than or equal to 0.24%; the apparent density of the flake silver powder 3 is 0.6g/cm 3～0.8g/cm3, the tap density is 1.0g/cm 3～1.3g/cm3, the particle size distribution Dmax is less than or equal to 10 mu m-20 mu m, the average particle size is 0.5 mu m-1.5 mu m, the specific surface area is 0.5m 2/kg～1.0m2/kg, and the burning loss ratio is less than 1.0%.
The organic resin is one or more of halogen-free polyurethane resin, halogen-free polyester resin and halogen-free acrylic resin.
The preparation method of the halogen-free silver paste comprises the following steps:
(1) The raw materials are prepared according to the following weight percentages: 15% of flake silver powder 1, 15% of flake silver powder 2, 18% of flake silver powder 3, 35.4% of organic resin, 12% of DBE, N-methylpyrrolidone mixed solvent, 0.8% of lotus root silk fiber, 0.5% of gamma-glycidyl ether methyltrimethoxysilane and 0.3% of 15000-mesh graphite powder;
(2) Adding organic resin into a mixed solvent of DBE and N-methyl pyrrolidone, and stirring in a constant-temperature water bath kettle at 75-80 ℃ until the organic resin is completely dissolved to obtain a resin carrier solution;
(3) Taking half of the resin carrier solution and lotus root silk fibers, uniformly mixing in a planetary disperser, and grinding and dispersing until the fineness is less than or equal to 5 mu m to prepare a semi-finished product;
(4) Adding the prepared semi-finished product, the rest resin carrier solution, silver powder, DBE, N-methylpyrrolidone mixed solvent, 15000 mesh graphite powder and gamma-glycidyl ether methyl trimethoxy silane into a planetary dispersing machine together, stirring for 35min, and defoaming to obtain semi-finished product slurry;
(5) And (3) grinding the semi-finished product slurry again by a three-roller machine, dispersing from coarse to fine, firstly grinding for 4-5 times by a roller with a wider width until the slurry on a grinding roller is smooth and does not hang on the roller, then grinding for 2-3 times by a roller with a narrower width until the slurry fineness is less than or equal to 5 mu m, and then defoaming and filtering to obtain a halogen-free silver slurry finished product.
The silver pastes prepared in examples 1 to 3 were subjected to performance test, and the results of the test are shown in Table 1 below.
From the test results, the halogen-free silver paste prepared by the invention has better bending resistance and superior film forming performance, and can improve the wire line.
The foregoing descriptions of specific exemplary embodiments of the present invention are presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain the specific principles of the invention and its practical application to thereby enable one skilled in the art to make and utilize the invention in various exemplary embodiments and with various modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (4)
1. The halogen-free silver paste with high bending resistance is characterized by comprising the following raw materials in percentage by weight: 40-55% of silver powder, 43.5-57% of halogen-free carrier, 0.8% of auxiliary agent and 0.5-1% of lotus root silk fiber, wherein the silver powder consists of one or more than one mixture of flake silver powder, spherical silver powder and spheroidal silver powder; the halogen-free carrier consists of organic resin and organic solvent; the auxiliary agent is a mixture of 15000 mesh graphite and gamma-glycidyl ether methyltrimethoxysilane; the preparation method of the halogen-free silver paste comprises the following steps:
(1) The raw materials are prepared according to the following weight percentages: 40-55% of silver powder, 43.5-57% of halogen-free carrier, 0.8% of auxiliary agent and 0.5-1% of lotus root silk fiber;
(2) Taking half of halogen-free carrier and lotus root silk fiber, premixing, grinding and dispersing to fineness less than or equal to 5 mu m by a three-roller machine, and preparing a semi-finished product;
(3) Adding the semi-finished product, the rest halogen-free carrier, silver powder and an auxiliary agent into a planetary dispersing machine together, stirring for 25-35min, and defoaming to obtain semi-finished product slurry;
(4) And (3) grinding the obtained semi-finished product slurry again through a three-roller machine until the fineness of the slurry is less than or equal to 5 mu m, defoaming and filtering to obtain a halogen-free silver slurry finished product.
2. The high-bending-resistance halogen-free silver paste according to claim 1, wherein the organic resin is one or a mixture of more than one of halogen-free polyurethane resin, halogen-free polyester resin and halogen-free acrylic resin.
3. The high-bending-resistance halogen-free silver paste according to claim 1, wherein the organic solvent is one or more of DBE, N-methyl pyrrolidone, DMM, isophorone, propylene glycol diacetate.
4. The method for preparing the high-bending-resistance halogen-free silver paste according to claim 1, wherein the raw materials in the step (1) are prepared according to the following weight percentages: 48% of silver powder, 50.5% of halogen-free carrier, 0.8% of auxiliary agent and 0.7% of lotus root silk fiber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310039621.XA CN115985553B (en) | 2023-01-13 | 2023-01-13 | Halogen-free silver paste with high bending resistance and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310039621.XA CN115985553B (en) | 2023-01-13 | 2023-01-13 | Halogen-free silver paste with high bending resistance and preparation method thereof |
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| CN103165221A (en) * | 2011-12-15 | 2013-06-19 | 上海宝银电子材料有限公司 | Halogen-free silver paste for laptop and preparation method thereof |
| CN112002459A (en) * | 2020-08-07 | 2020-11-27 | 中国科学院理化技术研究所 | Flexible conductive material preparation method and flexible conductive material prepared by using same |
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| WO2015040639A1 (en) * | 2013-09-19 | 2015-03-26 | Council Of Scientific And Industrial Research | Gold coated natural fibre as electrode materials and process for preparation thereof |
| CN106085340B (en) * | 2016-06-12 | 2019-01-11 | 江苏明昊新材料科技股份有限公司 | High heat-conductivity conducting elargol with thixotropic behavior and preparation method thereof |
| CN108641123A (en) * | 2018-03-28 | 2018-10-12 | 山东建邦胶体材料有限公司 | The nanocrystalline organic carrier preparation method of containing cellulose and the application in silver paste |
| CN113087972A (en) * | 2021-03-25 | 2021-07-09 | 北京林业大学 | MXene/silver nanowire/nanocellulose composite film and preparation method thereof |
| CN115482953A (en) * | 2022-09-22 | 2022-12-16 | 苏州银古电子科技有限公司 | Flexible silver paste and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103165221A (en) * | 2011-12-15 | 2013-06-19 | 上海宝银电子材料有限公司 | Halogen-free silver paste for laptop and preparation method thereof |
| CN112002459A (en) * | 2020-08-07 | 2020-11-27 | 中国科学院理化技术研究所 | Flexible conductive material preparation method and flexible conductive material prepared by using same |
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