CN116313218A - Ultralow-temperature-cured wear-resistant conductive paste and preparation method and application thereof - Google Patents
Ultralow-temperature-cured wear-resistant conductive paste and preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title abstract description 11
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 84
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 43
- 239000000843 powder Substances 0.000 claims abstract description 42
- 239000004925 Acrylic resin Substances 0.000 claims abstract description 27
- 229920000178 Acrylic resin Polymers 0.000 claims abstract description 27
- 229910001338 liquidmetal Inorganic materials 0.000 claims abstract description 24
- 229910052709 silver Inorganic materials 0.000 claims abstract description 24
- 239000004332 silver Substances 0.000 claims abstract description 24
- 239000003822 epoxy resin Substances 0.000 claims abstract description 22
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 22
- 239000000805 composite resin Substances 0.000 claims abstract description 10
- 239000011231 conductive filler Substances 0.000 claims abstract description 10
- 239000002131 composite material Substances 0.000 claims abstract description 8
- 238000001723 curing Methods 0.000 claims description 32
- 238000003756 stirring Methods 0.000 claims description 23
- 238000002156 mixing Methods 0.000 claims description 20
- 239000002904 solvent Substances 0.000 claims description 19
- 229910052751 metal Inorganic materials 0.000 claims description 18
- 239000002184 metal Substances 0.000 claims description 18
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- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
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- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 claims description 4
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- 239000004593 Epoxy Substances 0.000 claims description 3
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 3
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- YOBOXHGSEJBUPB-MTOQALJVSA-N (z)-4-hydroxypent-3-en-2-one;zirconium Chemical compound [Zr].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O YOBOXHGSEJBUPB-MTOQALJVSA-N 0.000 claims description 2
- LZDKZFUFMNSQCJ-UHFFFAOYSA-N 1,2-diethoxyethane Chemical compound CCOCCOCC LZDKZFUFMNSQCJ-UHFFFAOYSA-N 0.000 claims description 2
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims description 2
- CUDYYMUUJHLCGZ-UHFFFAOYSA-N 2-(2-methoxypropoxy)propan-1-ol Chemical compound COC(C)COC(C)CO CUDYYMUUJHLCGZ-UHFFFAOYSA-N 0.000 claims description 2
- XBIUWALDKXACEA-UHFFFAOYSA-N 3-[bis(2,4-dioxopentan-3-yl)alumanyl]pentane-2,4-dione Chemical compound CC(=O)C(C(C)=O)[Al](C(C(C)=O)C(C)=O)C(C(C)=O)C(C)=O XBIUWALDKXACEA-UHFFFAOYSA-N 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-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
- 239000004952 Polyamide Substances 0.000 claims description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 150000004645 aluminates Chemical class 0.000 claims description 2
- 229940043232 butyl acetate Drugs 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-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
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 2
- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropanol acetate Natural products CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 claims description 2
- 229940011051 isopropyl acetate Drugs 0.000 claims description 2
- GWYFCOCPABKNJV-UHFFFAOYSA-N isovaleric acid Chemical compound CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 claims description 2
- 239000012046 mixed solvent Substances 0.000 claims description 2
- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 claims description 2
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- 229940090181 propyl acetate Drugs 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 239000002562 thickening agent Substances 0.000 claims description 2
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 2
- OEOIWYCWCDBOPA-UHFFFAOYSA-N 6-methyl-heptanoic acid Chemical compound CC(C)CCCCC(O)=O OEOIWYCWCDBOPA-UHFFFAOYSA-N 0.000 claims 1
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- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
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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
-
- 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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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Conductive Materials (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the technical field of new materials, in particular to ultralow-temperature curing wear-resistant conductive paste, and a preparation method and application thereof. The conductive paste comprises the following components in parts by weight: 44.5-67 parts of conductive filler, 6-14 parts of composite resin and 1.2-4 parts of composite curing agent; wherein the conductive filler comprises 40-60 weight percent: 4-5:0.5-2 of micrometer silver powder, nanometer silver powder and silver-coated liquid metal powder; the composite resin comprises the following components in percentage by weight: 2-6 of epoxy resin and acrylic resin; the composite curing agent comprises the following components in percentage by weight of 0.2-1:1-3 and an imidazole curing agent. The sheet resistance of the conductive paste is less than 12mΩ/≡m/ml, and the conductive paste is completely cured within 120min at 70 ℃; when the printing thickness is controlled between 15 and 20 mu m, the conductive paste can realize the RCA paper tape load of 1kg, the rotating speed of 60r/min, and the wear-resistant 2000 circles of the paper tape cannot penetrate the bottom.
Description
Technical Field
The invention relates to the technical field of new materials, in particular to ultralow-temperature curing wear-resistant conductive paste, and a preparation method and application thereof.
Background
In the prior art, conductive paste is mainly divided into two types according to actual use processes: 1) Conductive paste for traditional screen printing process (printing by using the basic principle that the mesh of the image-text part of a screen plate can be penetrated by paste and the mesh of the non-image-text part can not be penetrated by paste); 2) Conductive paste for pad printing process (capable of printing characters, figures and images on the surface of irregular shaped objects).
In recent years, conductive pastes for conventional screen printing processes have been relatively mature, and are commonly used in consumer electronics fields, such as: the method is used in the fields of membrane switches, touch screens, capacitive electrodes and the like. The market share of the conductive paste used for the pad printing process is relatively small, research and development investment of researchers on the pad printing paste is much less than that of the screen printing paste, and the technical performance of the pad printing paste is generally not high; however, with the development of printing technology, pad printing process is becoming an important printing means, and at the same time, the technical requirements for pad printing paste are also increasing, for example: in order to meet the requirements of pad printing technology, the slurry needs to have both low-temperature (below 80 ℃) curability, high conductivity (Fang Zuxiao to 12mΩ/≡per liter) and high wear resistance (1 kg 60r/min load wear-resistant 2000 circles of non-penetrating bottom).
At present, most of the existing conductive pastes used for pad printing processes have curing temperatures exceeding 100 ℃, and have insufficient conductivity and wear resistance, so that the application requirements are difficult to meet.
In view of this, the present invention has been made.
Disclosure of Invention
The invention aims to provide a conductive paste which has both low-temperature (below 80 ℃) curability, high conductivity (Fang Zuxiao to 12mΩ/≡per liter) and high wear resistance (1 kg 60r/min for wear resistance 2000 circles without penetrating through); another object of the present invention is to provide a method for preparing the conductive paste and an application thereof.
Specifically, the invention provides the following technical scheme:
the invention provides a conductive paste, which comprises the following components in parts by weight:
44.5-67 parts of conductive filler, 6-14 parts of composite resin and 1.2-4 parts of composite curing agent;
wherein,,
the conductive filler comprises the following components in percentage by weight (40-60): (4-5): (0.5-2) micro silver powder, nano silver powder and silver-coated liquid metal powder;
the composite resin comprises the following components in percentage by weight (4-8): the epoxy resin and the acrylic resin of (2-6);
the composite curing agent comprises the following components in percentage by weight (0.2-1): isocyanate and imidazole curing agents of (1-3).
The invention takes ultralow-temperature curing wear-resistant conductive paste as a research and development aim, tries a large number of compounding modes of monomers and compounds, and unexpectedly discovers that in a paste system, the mixture of epoxy resin and acrylic resin is used as compound resin, the mixture of isocyanate and imidazole curing agent is used as compound curing agent, and the two are synergistic, so that the paste can be rapidly cured at a lower temperature, and simultaneously, the mixture of micron silver powder, nanometer silver powder and silver-coated liquid metal powder is used as conductive filler, so that the wear resistance of the paste can be further improved on the basis of reducing the sheet resistance of the paste.
Further controlling the weight ratio of the conductive filler, the composite resin and the composite curing agent to be (44.5-67): (6-14): (1.2-4), and controlling the weight ratio of the micron silver powder to the nanometer silver powder to the silver-coated liquid metal powder to be (40-60): (4-5): (0.5-2), the weight ratio of the epoxy resin to the acrylic resin is controlled to be (4-8): (2-6), controlling the weight ratio of isocyanate and imidazole curing agent to be (0.2-1): between (1-3), it is more advantageous to improve the low-temperature curability, conductivity, and abrasion resistance of the slurry at the same time.
Preferably, the micron silver powder is in the shape of flake, the average grain diameter is 2-5 mu m, and the tap density is 1.4-3g/cm 3 Between them; the micron silver powder with the characteristics forms line contact or surface contact in the cured conductive paste, and the contact area is larger than that of other micron silver powder with the conventional characteristics, so that the conductivity of the paste can be further effectively improved.
Preferably, the nanometer silver powder is spherical, the grain diameter is 100-500nm, and the tap density is 3-5g/cm 3 Between them.
In the slurry system, the nano silver powder is used as a conductive auxiliary phase to be filled in the gaps of the flaky micro silver powder, and the high activity of the nano silver powder can realize semi-sintering in the baking process, so that the sheet resistance of the whole slurry is further reduced; when the nano silver powder with the characteristics is selected, the effect is better.
Further, the nano silver powder is pre-treated, and the treatment is specifically as follows: and (3) pretreating the nano silver powder by using a silane coupling agent, and drying the nano silver powder at the temperature of less than 60 ℃ under vacuum. By adopting the mode to pretreat the nano silver powder, the occurrence of agglomeration can be effectively avoided, so that the nano silver powder is better dispersed in a slurry system.
The invention adopts silver-coated liquid metal powder as one of the conductive fillers. The silver-coated liquid metal powder is characterized in that silver powder is coated on the surface of liquid metal, and compared with pure liquid metal, the silver powder is easier to disperse in a slurry system and is fused with the system; meanwhile, the silver-coated liquid metal powder can also effectively avoid oxidation of liquid metal.
Preferably, the epoxy resin is linear bisphenol A epoxy resin with ultrahigh molecular weight, the epoxy value is 7000-9000, the molecular weight is more than 5 ten thousand, and the softening point is more than 50 ℃;
preferably, the acrylic resin is hydroxyl-terminated acrylic resin, and the hydroxyl value of the acrylic resin is 36-100;
aiming at the slurry system, the epoxy resin and the acrylic resin are selected to be compounded, so that the curing speed of the slurry can be further improved.
The person skilled in the art can arrange the other functional components of the formulation according to common general knowledge, which all achieve an effect comparable to the above description of the invention. However, there are also more preferable technical solutions concerning other components, and for this purpose, the present invention has been further studied and the following preferable solutions have been obtained.
Preferably, the conductive paste further comprises, in parts by weight: 10-15 parts of wear-resistant metal filler;
the wear-resistant metal filler is one or more selected from electrolytic nickel powder, silver-coated nickel powder, nickel-coated graphite powder and graphene.
Further, the electrolytic nickel powder has a particle size of 1-5 μm.
Preferably, the conductive paste further comprises, in parts by weight: 5-20 parts of solvent, 0.1-1 part of catalyst, 1-1.5 parts of coupling agent, 0.1-1 part of anti-settling agent and 0.1-1 part of additive.
Further, the solvent is a mixed solvent of an ether solvent and an ester solvent; the ether solvent is selected from one or more of dipropylene glycol methyl ether, propylene glycol methyl ether and dipropylene dibutyl ether; the ester solvent is one or more selected from propylene glycol methyl ether acetate, ethyl acetate, n-butyl acetate, ethylene glycol diethyl ether acetate, dimethyl glutarate, propylene glycol methyl ether acetate, dimethyl adipate, butyl acetate, propyl acetate and isopropyl acetate.
Further, the catalyst is selected from one or more of organic tin, cobalt iso-octoate, aluminum acetylacetonate, zirconium acetylacetonate and diethylenetriamine.
Further, the coupling agent is one or more selected from titanate coupling agent, aluminate coupling agent and silane coupling agent.
Further, the anti-settling agent is selected from one or more of silicon dioxide, polyamide wax powder, BYK420 and carbon black.
Further, the additive is one or more selected from leveling agent, defoamer and thickener.
The above technical solutions can be combined by a person skilled in the art according to common general knowledge to obtain a preferred embodiment of the conductive paste according to the present invention.
As a preferred embodiment of the present invention, the conductive paste comprises the following components in parts by weight:
4-8 parts of epoxy resin, 2-6 parts of acrylic resin, 5-20 parts of solvent, 40-60 parts of micron silver powder, 4-5 parts of nano silver powder, 0.5-2 parts of silver-coated liquid metal powder, 10-15 parts of wear-resistant metal filler, 0.2-1 part of isocyanate, 1-3 parts of imidazole curing agent, 0.1-1 part of catalyst, 1-1.5 parts of coupling agent, 0.1-1 part of anti-settling agent and 0.1-1 part of additive.
The invention also provides a preparation method of the conductive paste, which comprises the following steps:
(1) Mixing acrylic resin, a solvent and epoxy resin, and filtering and impurity removing to obtain a high polymer resin carrier;
(2) Mixing micrometer silver powder, nanometer silver powder, silver-coated liquid metal powder, wear-resistant metal filler, the high polymer resin carrier, isocyanate, imidazole curing agent, coupling agent, anti-settling agent and additive to obtain premix;
(3) And mixing the premix and the catalyst, and filtering and impurity removing treatment to obtain the conductive paste.
The invention also discovers that the conductive paste prepared by adopting the mode can further ensure that all the components are uniformly mixed and ensure that the properties of the product are not changed differently.
Preferably, in step (1), the mixing specifically includes: mixing acrylic resin and solvent, stirring at 200-300rpm and 80 deg.c for 1 + -0.5 hr, adding epoxy resin, and stirring at 200-300rpm and 80 deg.c for 6 + -1 hr.
Preferably, in the step (2), the mixing specifically includes: mixing the micrometer silver powder, the nanometer silver powder, the silver-coated liquid metal powder and the wear-resistant metal filler, adding the high polymer resin carrier in batches, uniformly stirring at the temperature of 5-10 ℃, and finally sequentially adding isocyanate, an imidazole curing agent, a coupling agent, an anti-settling agent and an additive.
Preferably, in the step (3), the mixing specifically includes: the premix is firstly subjected to high-speed shearing, grinding and dispersing, then a catalyst is added in a stirring state, and stirring is carried out for 30+/-5 min at the temperature of between 0 and 5 ℃ at the speed of between 100 and 300 rpm.
The person skilled in the art can combine the technical schemes according to common knowledge to obtain a preferred embodiment of the preparation method according to the invention.
As a preferred embodiment, the preparation method comprises the steps of:
(1) Mixing acrylic resin and a solvent, stirring for 1+/-0.5 h at 80 ℃ at 200-300rpm, adding epoxy resin, stirring for 6+/-1 h at 80 ℃ at 200-300rpm, and filtering and removing impurities by a 400-mesh screen to obtain a polymer resin carrier;
(2) Firstly mixing micrometer silver powder, nanometer silver powder, silver-coated liquid metal powder and wear-resistant metal filler, then adding the high polymer resin carrier in batches, uniformly stirring at 5-10 ℃, and finally sequentially adding isocyanate, imidazole curing agent, coupling agent, anti-settling agent and additive, and uniformly stirring to obtain premix;
(3) The premix is firstly subjected to high-speed shearing, grinding and dispersing, then a catalyst is added in a stirring state, stirring is carried out for 30+/-5 min at 100-300rpm and 0-5 ℃, and the conductive paste is obtained after filtering and impurity removing treatment by a 1000-1500 mesh screen.
The invention also provides application of the conductive paste in a circuit board; preferably in flexible circuit boards.
The invention also provides an electronic device, which comprises a substrate and a conductive line positioned on the substrate, wherein the conductive line is formed by printing, heating and curing the conductive paste.
Preferably, the printing mode is pad printing.
Preferably, the material of the substrate includes, but is not limited to, PC, PA, metal, PET, PI.
Based on the scheme, the beneficial effects of the invention are as follows:
according to the invention, micron silver powder, nano silver powder and silver-coated liquid metal powder are used as conductive fillers, and wear-resistant metal fillers are used as auxiliary materials, so that the conductivity and wear resistance of the slurry can be effectively improved; the epoxy resin and the acrylic resin are used as composite resin, and the structure of the composite resin contains a large number of polar structures, so that the composite resin has good coating property on silver powder, the conductivity of the slurry can be further improved, and meanwhile, the adhesive force between the slurry and a base material is improved; isocyanate and imidazole curing agents are used as composite curing agents, and a catalyst is used as auxiliary materials, so that the curing speed of the slurry can be greatly improved, and the low-temperature curing of the slurry is realized.
Fang Zuxiao to 12mΩ/≡m/ml of the conductive paste of the invention, and curing completely at 70 ℃ within 120 min; when the printing thickness is controlled between 15 and 20 mu m, the conductive paste can realize the RCA paper tape load of 1kg, the rotating speed of 60r/min, and the wear-resistant 2000 circles of the paper tape cannot penetrate the bottom.
Drawings
Fig. 1 is a graph showing the abrasion resistance test of the conductive paste of example 1;
fig. 2 is a graph showing the abrasion resistance test of the conductive paste of example 2;
fig. 3 is a graph showing the abrasion resistance test of the conductive paste of example 3;
fig. 4 is a graph showing the abrasion resistance test of the conductive paste of example 4;
fig. 5 is a graph of abrasion resistance test of the conductive paste of comparative example 1;
fig. 6 is a graph of abrasion resistance test of the conductive paste of comparative example 2.
Detailed Description
The following examples are illustrative of the invention and are not intended to limit the scope of the invention.
In order to facilitate the comparison effect, the micrometer silver powder mentioned in the following examples is in the form of flakes having an average particle diameter of 2-5 μm and a tap density of 1.4-3g/cm 3 Between them;
the nano silver powder mentioned in the following examples is spherical and has a particle size of 100-500nm and tap density of 3-5g/cm 3 Between them; the nano silver powder is pre-treated, and the treatment is specifically as follows: pretreating the nano silver powder by using a silane coupling agent, and drying the nano silver powder at the temperature of less than 60 ℃ under vacuum;
the epoxy resins mentioned in the examples below are ultra-high molecular weight linear bisphenol A epoxy resins having an epoxy value of 7000 to 9000, a molecular weight of more than 5 ten thousand and a softening point of more than 50 ℃;
the acrylic resins mentioned in the examples below are hydroxyl-terminated acrylic resins having hydroxyl numbers of from 36 to 100;
the wear-resistant metal filler mentioned in the following examples is selected from one or more of electrolytic nickel powder, silver-coated nickel powder, nickel-coated graphite powder and graphene.
The specific techniques or conditions are not identified in the examples and are described in the literature in this field or are carried out in accordance with the product specifications. The reagents or equipment used were conventional products available for purchase by regular vendors without the manufacturer's attention.
Example 1
The embodiment provides a conductive paste, which comprises the following formula:
5 parts of epoxy resin, 5 parts of acrylic resin, 10 parts of solvent, 50 parts of micrometer silver powder, 4 parts of nanometer silver powder, 1 part of silver-coated liquid metal powder, 10 parts of wear-resistant metal filler, 1 part of isocyanate, 2 parts of imidazole curing agent, 0.5 part of catalyst, 1 part of silane coupling agent, 0.5 part of anti-settling agent and 0.5 part of additive.
The embodiment further provides a preparation method of the conductive paste, which specifically comprises the following steps:
(1) Mixing acrylic resin and solvent, stirring for 1h at 200-300rpm and 80 ℃, then adding epoxy resin, stirring for 6h at 200-300rpm and 80 ℃, filtering by a 400-mesh screen, and removing impurities to obtain a polymer resin carrier;
(2) Mixing micrometer silver powder, nanometer silver powder, silver-coated liquid metal powder and wear-resistant metal filler, adding the polymer resin carrier in batches, stirring for 10-20min to uniformity after adding the polymer resin carrier each time, stirring for 30min to uniformity at 5-10 ℃ after all the polymer resin carriers are added, and finally sequentially adding isocyanate, imidazole curing agent, silane coupling agent, anti-settling agent and additive, and stirring for 60min to uniformity to obtain premix;
(3) The premix is firstly subjected to high-speed shearing, grinding and dispersing on a three-roller machine, then a catalyst is added in a stirring state, stirring is carried out for 30min at 100-300rpm and 0-5 ℃, and the conductive paste is obtained after filtering and impurity removing treatment by a 1000-1500 mesh screen.
Example 2
The embodiment provides a conductive paste, which comprises the following formula:
4 parts of epoxy resin, 6 parts of acrylic resin, 10 parts of solvent, 50 parts of micrometer silver powder, 5 parts of nanometer silver powder, 1 part of silver-coated liquid metal powder, 10 parts of wear-resistant metal filler, 0.5 part of isocyanate, 3 parts of imidazole curing agent, 0.5 part of catalyst, 1 part of silane coupling agent, 0.5 part of anti-settling agent and 0.5 part of additive.
The preparation method of the conductive paste provided in this embodiment is the same as that of embodiment 1.
Example 3
The embodiment provides a conductive paste, which comprises the following formula:
7 parts of epoxy resin, 3 parts of acrylic resin, 10 parts of solvent, 50 parts of micrometer silver powder, 4 parts of nanometer silver powder, 1 part of silver-coated liquid metal powder, 15 parts of wear-resistant metal filler, 0.5 part of isocyanate, 1.5 parts of imidazole curing agent, 0.5 part of catalyst, 1.5 parts of silane coupling agent, 0.5 part of anti-settling agent and 0.5 part of additive.
The preparation method of the conductive paste provided in this embodiment is the same as that of embodiment 1.
Example 4
The embodiment provides a conductive paste, which comprises the following formula:
8 parts of epoxy resin, 2 parts of acrylic resin, 10 parts of solvent, 50 parts of micrometer silver powder, 4 parts of nanometer silver powder, 1 part of silver-coated liquid metal powder, 10 parts of wear-resistant metal filler, 0.2 part of isocyanate, 2.5 parts of imidazole curing agent, 0.5 part of catalyst, 1.5 parts of silane coupling agent, 0.5 part of anti-settling agent and 0.5 part of additive.
The preparation method of the conductive paste provided in this embodiment is the same as that of embodiment 1.
Comparative example 1
This comparative example provides a conductive paste which is different from example 1 in that the amount of silver-coated liquid metal powder used in the formulation is 0 parts by weight.
Comparative example 2
This comparative example provides a conductive paste which is different from example 4 in that the amount of epoxy resin used in the formulation is 10 parts by weight and the amount of acrylic resin used in the formulation is 0 parts by weight.
Test example 1
In the test example, conductive lines are formed on a PC substrate by transfer printing of the conductive pastes of the examples and the comparative examples, the thickness is between 15 and 20 mu m, the conductive lines are cured for 120min at 70 ℃, the curing condition of each conductive line is observed, and the conductive lines formed by the conductive pastes of the examples 1 to 4 are found to be completely cured, and the conductive lines formed by the conductive pastes of the comparative examples 1 to 2 are not completely cured.
Test example 2
In the test example, conductive pastes of the example and the comparative example are respectively formed into conductive lines on a PC substrate in a pad printing mode, the thickness is between 15 and 20 mu m, and performance tests are respectively carried out on the conductive lines with the same shape after heating and curing, and the test method is as follows:
1. abrasion resistance test
(1) The testing method comprises the following steps: the RCA paper tape is loaded with 1kg and the rotating speed is 60r/min;
(2) Test results: the test result of the conductive circuit made of the conductive paste of example 1 is shown in fig. 1, and as can be seen from fig. 1, the wear-resistant 2000 circles are not penetrated; the test result of the conductive circuit made of the conductive paste of example 2 is shown in fig. 2, and as can be seen from fig. 2, the wear-resistant 2000 circles are not penetrated; the test result of the conductive circuit made of the conductive paste of example 3 is shown in fig. 3, and as can be seen from fig. 3, the wear-resistant 2000 circles are not penetrated; the test result of the conductive circuit made of the conductive paste of example 4 is shown in fig. 4, and as can be seen from fig. 4, the wear-resistant 2000 turns are not penetrated; the test result of the conductive circuit made of the conductive paste of comparative example 1 is shown in fig. 5, and as can be seen from fig. 5, the bottom penetration phenomenon occurs in the wear-resistant 2000 circles; the test result of the conductive circuit made of the conductive paste of comparative example 2 is shown in fig. 6, and it can be seen from fig. 6 that the bottom penetration phenomenon occurs in the abrasion-resistant 2000 circles.
2. Sheet resistance test
(1) The testing method comprises the following steps: testing each conductive circuit by using a universal meter;
(2) The test results are shown in Table 1.
3. Viscosity test
(1) The testing method comprises the following steps: testing each conductive line by using a Bowler-Nordheim viscometer at 25 ℃ and rotor 14#, and 100 rpm;
(2) The test results are shown in Table 1.
4. Adhesion test
(1) The testing method comprises the following steps: using a 3M 610 adhesive tape to adhere to the surfaces of all the conductive circuits, standing for 1min, rapidly removing the 3M 610 adhesive tape by means of external force, and observing whether the appearance of each conductive circuit falls off or not; if no falling-off condition exists, the adhesive force is good; if the falling-off condition occurs, the adhesive force is poor;
(2) The test results are shown in Table 1.
TABLE 1
While the invention has been described in detail in the foregoing general description and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.
Claims (10)
1. The conductive paste is characterized by comprising the following components in parts by weight:
44.5-67 parts of conductive filler, 6-14 parts of composite resin and 1.2-4 parts of composite curing agent;
wherein,,
the conductive filler comprises the following components in percentage by weight (40-60): (4-5): (0.5-2) micro silver powder, nano silver powder and silver-coated liquid metal powder;
the composite resin comprises the following components in percentage by weight (4-8): the epoxy resin and the acrylic resin of (2-6);
the composite curing agent comprises the following components in percentage by weight (0.2-1): isocyanate and imidazole curing agents of (1-3).
2. The conductive paste as claimed in claim 1, wherein the micrometer silver powder is in the form of a plate having an average particle diameter of 2 to 5 μm and a tap density of 1.4 to 3g/cm 3 Between them; and/or the number of the groups of groups,
the nanometer silver powder is spherical, the grain diameter is 100-500nm, and the tap density is 3-5g/cm 3 Between them.
3. The conductive paste according to claim 2, wherein the nano silver powder is previously treated, specifically: and (3) pretreating the nano silver powder by using a silane coupling agent, and drying the nano silver powder at the temperature of less than 60 ℃ under vacuum.
4. The conductive paste according to claim 1, wherein the epoxy resin is an ultra-high molecular weight linear bisphenol a epoxy resin having an epoxy value of 7000 to 9000, a molecular weight of more than 5 ten thousand, and a softening point of more than 50 ℃; and/or the number of the groups of groups,
the acrylic resin is hydroxyl-terminated acrylic resin, and the hydroxyl value of the acrylic resin is 36-100.
5. The electroconductive paste according to any one of claims 1-4, further comprising, in parts by weight: 10-15 parts of wear-resistant metal filler;
the wear-resistant metal filler is one or more selected from electrolytic nickel powder, silver-coated nickel powder, nickel-coated graphite powder and graphene.
6. The electroconductive paste according to any one of claims 1-4, further comprising, in parts by weight: 5-20 parts of solvent, 0.1-1 part of catalyst, 1-1.5 parts of coupling agent, 0.1-1 part of anti-settling agent and 0.1-1 part of additive.
7. The electroconductive paste according to claim 6, wherein the solvent is a mixed solvent of an ether solvent and an ester solvent; the ether solvent is selected from one or more of dipropylene glycol methyl ether, propylene glycol methyl ether and dipropylene dibutyl ether; the ester solvent is one or more selected from propylene glycol methyl ether acetate, ethyl acetate, n-butyl acetate, ethylene glycol diethyl ether acetate, dimethyl glutarate, propylene glycol methyl ether acetate, dimethyl adipate, butyl acetate, propyl acetate and isopropyl acetate;
and/or the catalyst is selected from one or more of organic tin, cobalt isooctanoate, aluminum acetylacetonate, zirconium acetylacetonate and diethylenetriamine;
and/or the coupling agent is selected from one or more of titanate coupling agent, aluminate coupling agent and silane coupling agent;
and/or the anti-settling agent is selected from one or more of silicon dioxide, polyamide wax powder, BYK420 and carbon black;
and/or the additive is one or more selected from flatting agents, defoamers and thickeners.
8. The method for preparing a conductive paste according to any one of claims 1 to 7, comprising the steps of:
(1) Mixing acrylic resin, a solvent and epoxy resin, and filtering and impurity removing to obtain a high polymer resin carrier;
(2) Mixing micrometer silver powder, nanometer silver powder, silver-coated liquid metal powder, wear-resistant metal filler, the high polymer resin carrier, isocyanate, imidazole curing agent, coupling agent, anti-settling agent and additive to obtain premix;
(3) And mixing the premix and the catalyst, and filtering and impurity removing treatment to obtain the conductive paste.
9. The method according to claim 8, wherein in step (1), the mixing is specifically: firstly, mixing acrylic resin and a solvent, stirring for 1+/-0.5 h at the temperature of 80 ℃ at 200-300rpm, then adding epoxy resin, and stirring for 6+/-1 h at the temperature of 80 ℃ at 200-300 rpm;
and/or, in the step (2), the mixing specifically comprises: firstly mixing micrometer silver powder, nanometer silver powder, silver-coated liquid metal powder and wear-resistant metal filler, then adding the high polymer resin carrier in batches, uniformly stirring at 5-10 ℃, and finally sequentially adding isocyanate, imidazole curing agent, coupling agent, anti-settling agent and additive;
and/or, in the step (3), the mixing specifically comprises: the premix is firstly subjected to high-speed shearing, grinding and dispersing, then a catalyst is added in a stirring state, and stirring is carried out for 30+/-5 min at the temperature of between 0 and 5 ℃ at the speed of between 100 and 300 rpm.
10. Use of the electroconductive paste according to any one of claims 1-7 in a circuit board; preferably in flexible circuit boards.
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